Development of real-time PCR assays for the detection of Moraxella macacae associated with bloody nose syndrome in rhesus (Macaca mulatta) and cynomolgus (Macaca fascicularis) macaques

PubMed Central

Whitehouse, Chris A.; Chase, Kitty; Embers, Monica E.; Kulesh, David A.; Ladner, Jason T.; Palacios, Gustavo F.; Minogue, Timothy D.

2016-01-01

Background Moraxella macacae is a recently described bacterial pathogen that causes epistaxis or so-called bloody nose syndrome in captive macaques. The aim of this study was to develop specific molecular diagnostic assays for M. macacae and to determine their performance characteristics. Methods We developed six real-time PCR assays on the Roche LightCycler. The accuracy, precision, selectivity, and limit of detection (LOD) were determined for each assay, in addition to further validation by testing nasal swabs from macaques presenting with epistaxis at the Tulane National Primate Research Center. Results All assays exhibited 100% specificity and were highly sensitive with an LOD of 10 fg for chromosomal assays and 1 fg for the plasmid assay. Testing of nasal swabs from 10 symptomatic macaques confirmed the presence of M. macacae in these animals. Conclusions We developed several accurate, sensitive, and species-specific real-time PCR assays for the detection of M. macacae in captive macaques. PMID:26365904

Medium- and Long-term Prediction of LOD Change with the Leap-step Autoregressive Model

NASA Astrophysics Data System (ADS)

Liu, Q. B.; Wang, Q. J.; Lei, M. F.

2015-09-01

It is known that the accuracies of medium- and long-term prediction of changes of length of day (LOD) based on the combined least-square and autoregressive (LS+AR) decrease gradually. The leap-step autoregressive (LSAR) model is more accurate and stable in medium- and long-term prediction, therefore it is used to forecast the LOD changes in this work. Then the LOD series from EOP 08 C04 provided by IERS (International Earth Rotation and Reference Systems Service) is used to compare the effectiveness of the LSAR and traditional AR methods. The predicted series resulted from the two models show that the prediction accuracy with the LSAR model is better than that from AR model in medium- and long-term prediction.

Simplifying sample pretreatment: application of dried blood spot (DBS) method to blood samples, including postmortem, for UHPLC-MS/MS analysis of drugs of abuse.

PubMed

Odoardi, Sara; Anzillotti, Luca; Strano-Rossi, Sabina

2014-10-01

The complexity of biological matrices, such as blood, requires the development of suitably selective and reliable sample pretreatment procedures prior to their instrumental analysis. A method has been developed for the analysis of drugs of abuse and their metabolites from different chemical classes (opiates, methadone, fentanyl and analogues, cocaine, amphetamines and amphetamine-like substances, ketamine, LSD) in human blood using dried blood spot (DBS) and subsequent UHPLC-MS/MS analysis. DBS extraction required only 100μL of sample, added with the internal standards and then three droplets (30μL each) of this solution were spotted on the card, let dry for 1h, punched and extracted with methanol with 0.1% of formic acid. The supernatant was evaporated and the residue was then reconstituted in 100μL of water with 0.1% of formic acid and injected in the UHPLC-MS/MS system. The method was validated considering the following parameters: LOD and LOQ, linearity, precision, accuracy, matrix effect and dilution integrity. LODs were 0.05-1ng/mL and LOQs were 0.2-2ng/mL. The method showed satisfactory linearity for all substances, with determination coefficients always higher than 0.99. Intra and inter day precision, accuracy, matrix effect and dilution integrity were acceptable for all the studied substances. The addition of internal standards before DBS extraction and the deposition of a fixed volume of blood on the filter cards ensured the accurate quantification of the analytes. The validated method was then applied to authentic postmortem blood samples. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Replication of linkage to quantitative trait loci: variation in location and magnitude of the lod score.

PubMed

Hsueh, W C; Göring, H H; Blangero, J; Mitchell, B D

2001-01-01

Replication of linkage signals from independent samples is considered an important step toward verifying the significance of linkage signals in studies of complex traits. The purpose of this empirical investigation was to examine the variability in the precision of localizing a quantitative trait locus (QTL) by analyzing multiple replicates of a simulated data set with the use of variance components-based methods. Specifically, we evaluated across replicates the variation in both the magnitude and the location of the peak lod scores. We analyzed QTLs whose effects accounted for 10-37% of the phenotypic variance in the quantitative traits. Our analyses revealed that the precision of QTL localization was directly related to the magnitude of the QTL effect. For a QTL with effect accounting for > 20% of total phenotypic variation, > 90% of the linkage peaks fall within 10 cM from the true gene location. We found no evidence that, for a given magnitude of the lod score, the presence of interaction influenced the precision of QTL localization.

Simultaneous Determination of Clidinium Bromide and Chlordiazepoxide in Combined Dosage Forms by High-Performance Liquid Chromatography.

PubMed

Ashour, Safwan; Kattan, Nuha

2013-01-01

A sensitive and precise RP-HPLC method has been developed for the simultaneous estimation of clidinium bromide (CDB) and chlordiazepoxide (CDZ) in pure and pharmaceutical formulations. The separation was achieved on a Nucleodur C8 (250 × 4.6 mm i.d., 5 μm particle size) column at 25°C. CH3CN-MeOH-NH4OAc 0.1M (30 : 40 : 30, v/v/v) was used as the mobile phase at a flow rate of 1.0 mL min(-1) and detector wavelength at 218 nm. Almotriptan (ALT) was used as internal standard. The validation of the proposed method was carried out for linearity, accuracy, precision, LOD, LOQ, and robustness. The method showed good linearity in the ranges of 2.5-300.0 and 3.0-500.0 μg mL(-1) for CDB and CDZ, respectively. The percentage recovery obtained for CDB and CDZ was 100.40-103.38 and 99.98-105.59%, respectively. LOD and LOQ were 0.088 and 0.294 μg mL(-1) for CDB and 0.121 and 0.403 μg mL(-1) for CDZ, respectively. The proposed method was successfully applied to the determination of CDB and CDZ in combined dosage forms and the results tallied well with the label claim.

Development and validation of a reversed-phase high-performance thin-layer chromatography-densitometric method for determination of atorvastatin calcium in bulk drug and tablets.

PubMed

Shirkhedkar, Atul A; Surana, Sanjay J

2010-01-01

Atorvastatin calcium is a synthetic HMG-CoA reductase inhibitor that is used as a cholesterol-lowering agent. A simple, sensitive, selective, and precise RP-HPTLC-densitometric determination of atorvastatin calcium both as bulk drug and from pharmaceutical formulation was developed and validated according to International Conference on Harmonization guidelines. The method used aluminum sheets precoated with silica gel 60 RP18F254S as the stationary phase, and the mobile phase consisted of methanol-water (3.5 + 1.5, v/v). The system gave a compact band for atorvastatin calcium with an Rf value of 0.62 +/- 0.02. Densitometric quantification was carried out at 246 nm. The linear regression analysis data for the calibration plots showed a good linear relationship with r = 0.9992 in the working concentration range of 100-800 ng/band. The method was validated for precision, accuracy, ruggedness, robustness, specificity, recovery, LOD, and LOQ. The LOD and LOQ were 6 and 18 ng, respectively. The drug underwent hydrolysis when subjected to acidic conditions and was found to be stable under alkali, oxidation, dry heat, and photodegradation conditions. Statistical analysis proved that the developed RP-HPTLC-densitometry method is reproducible and selective and that it can be applied for identification and quantitative determination of atorvastatin calcium in bulk drug and tablet formulation.

A validated fast difference spectrophotometric method for 5-hydroxymethyl-2-furfural (HMF) determination in corn syrups.

PubMed

de Andrade, Jucimara Kulek; de Andrade, Camila Kulek; Komatsu, Emy; Perreault, Hélène; Torres, Yohandra Reyes; da Rosa, Marcos Roberto; Felsner, Maria Lurdes

2017-08-01

Corn syrups, important ingredients used in food and beverage industries, often contain high levels of 5-hydroxymethyl-2-furfural (HMF), a toxic contaminant. In this work, an in house validation of a difference spectrophotometric method for HMF analysis in corn syrups was developed using sophisticated statistical tools by the first time. The methodology showed excellent analytical performance with good selectivity, linearity (R 2 =99.9%, r>0.99), accuracy and low limits (LOD=0.10mgL -1 and LOQ=0.34mgL -1 ). An excellent precision was confirmed by repeatability (RSD (%)=0.30) and intermediate precision (RSD (%)=0.36) estimates and by Horrat value (0.07). A detailed study of method precision using a nested design demonstrated that variation sources such as instruments, operators and time did not interfere in the variability of results within laboratory and consequently in its intermediate precision. The developed method is environmentally friendly, fast, cheap and easy to implement resulting in an attractive alternative for corn syrups quality control in industries and official laboratories. Copyright © 2017 Elsevier Ltd. All rights reserved.

Analysis of adulterants in a traditional herbal medicinal product using liquid chromatography-mass spectrometry-mass spectrometry.

PubMed

Lau, Aik-Jiang; Holmes, Michael J; Woo, Soo-On; Koh, Hwee-Ling

2003-02-26

Adulterations with synthetic drugs are common problems with herbal medicine and this can potentially cause serious adverse effects. It is therefore important to determine the presence of synthetic drugs in herbal medicine to ensure patients' safety. The objective of this study was to develop sensitive and specific methods to analyse phenylbutazone, caffeine and oxyphenbutazone present in a traditional Indonesian herbal product. Liquid chromatography-mass spectrometry-mass spectrometry (LC-MS-MS) methods in the selected reaction-monitoring (SRM) mode were developed. It was found that the sample contained 0.53% w/w (n=3, RSD=7.56%) phenylbutazone and 0.04% w/w (n=3, RSD=8.39%) caffeine. This corresponded to 43.17 mg phenylbutazone and 3.23 mg caffeine in each sachet of powder. The methods were validated for linearity, precision, accuracy, LOD and LOQ. LOD and LOQ were found to be 3.69 and 12.29 ng/ml, respectively for phenylbutazone. For caffeine, the LOD and LOQ were 0.84 and 2.80 ng/ml, respectively. Oxyphenbutazone in the sample was found to be present at a level below the quantification level of 10.2 ng/ml. With better methods developed for analysis of adulterants in herbal medicine, the quality and safety of these medicines can be better controlled and regulated to ensure patients' safety.

METHODS OF DEALING WITH VALUES BELOW THE LIMIT OF DETECTION USING SAS

EPA Science Inventory

Due to limitations of chemical analysis procedures, small values cannot be precisely measured. These values are said to be below the limit of detection (LOD). In statistical analyses, these values are often censored and substituted with a constant value, such as half the LOD,...

Accuracy in Rietveld quantitative phase analysis: a comparative study of strictly monochromatic Mo and Cu radiations.

PubMed

León-Reina, L; García-Maté, M; Álvarez-Pinazo, G; Santacruz, I; Vallcorba, O; De la Torre, A G; Aranda, M A G

2016-06-01

This study reports 78 Rietveld quantitative phase analyses using Cu  K α 1 , Mo  K α 1 and synchrotron radiations. Synchrotron powder diffraction has been used to validate the most challenging analyses. From the results for three series with increasing contents of an analyte (an inorganic crystalline phase, an organic crystalline phase and a glass), it is inferred that Rietveld analyses from high-energy Mo  K α 1 radiation have slightly better accuracies than those obtained from Cu  K α 1 radiation. This behaviour has been established from the results of the calibration graphics obtained through the spiking method and also from Kullback-Leibler distance statistic studies. This outcome is explained, in spite of the lower diffraction power for Mo radiation when compared to Cu radiation, as arising because of the larger volume tested with Mo and also because higher energy allows one to record patterns with fewer systematic errors. The limit of detection (LoD) and limit of quantification (LoQ) have also been established for the studied series. For similar recording times, the LoDs in Cu patterns, ∼0.2 wt%, are slightly lower than those derived from Mo patterns, ∼0.3 wt%. The LoQ for a well crystallized inorganic phase using laboratory powder diffraction was established to be close to 0.10 wt% in stable fits with good precision. However, the accuracy of these analyses was poor with relative errors near to 100%. Only contents higher than 1.0 wt% yielded analyses with relative errors lower than 20%.

[Determination of canthaxanthin and astaxanthin in egg yolks by reversed phase high performance liquid chromatography with diode array detection].

PubMed

He, Kang-Hao; Zou, Xiao-Li; Liu, Xiang; Zeng, Hong-Yan

2012-01-01

A method using reversed phase high performance liquid chromatography (RP-HPLC) coupled with diode array detector (DAD) was developed for the simultaneous determination of canthaxanthin and astaxanthin in egg yolks. Samples were extracted with acetonitrile in ultrasonic bath for 20 minutes and then purified by freezing-lipid filtration and solid phase extraction (SPE). After being vaporized to dryness by nitrogen blowing and made up to volume with methanol, the extract solution was chromatographically separated in C18 column with a unitary mobile phase consisting of acetonitrile. The proposed method was validated in terms of linearity, precision, accuracy, and limit of detection (LOD). Regression analysis revealed a good linearity between peak area of each analyte and its concentration (r > or = 0.998). The intra- and inter-day relative standard deviations (RSDs) were less than 3.6% and 5.2%, respectively. LODs of canthaxanthin and astaxanthin were 0.035 and 0.027 microg/mL (S/N = 3). The average recoveries of canthaxanthin and astaxanthin were 91.5% and 88.7%. The proposed method is simple, fast and easy to apply.

Simultaneous Determination of Piperine, Capsaicin, and Dihydrocapsaicin in Korean Instant-Noodle (Ramyun) Soup Base Using High-Performance Liquid Chromatography with Ultraviolet Detection.

PubMed

Shim, You-Shin; Kim, Jong-Chan; Jeong, Seung-Weon

2016-01-01

A simultaneous analytical method for piperine, capsaicin, and dihydrocapsaicin in Korean instant-noodle soup base using HPLC was validated in terms of precision, accuracy, sensitivity, and linearity. The HPLC separation was performed on a reversed-phase C18 column (5 μm particle size, 4.6 mm id, 250 mm length) using a UV detector fixed at 280 nm. The LOD and LOQ of the HPLC analyses ranged from 0.25 to 1.03 mg/kg. The intraday and interday precisions of the individual piperine, capsaicin, and dihydrocapsaicin were <10.55%, and the recovery values ranged from 85.43 to 94.68%. The calibration curves exhibited good linearity (r(2) = 0.999) within the tested ranges. These results suggest that the analytical method in this study can be used to classify Korean instant noodles based on their levels of spiciness.

Development of a candidate reference measurement procedure for the analysis of cortisol in human serum samples by isotope dilution-gas chromatography-mass spectrometry.

PubMed

Kawaguchi, Migaku; Takatsu, Akiko

2009-08-01

A candidate reference measurement procedure involving isotope dilution coupled with gas chromatography-mass spectrometry (GC-MS) has been developed and critically evaluated. An isotopically labeled internal standard, cortisol-d(2), was added to a serum sample. After equilibration, solid-phase extractions (SPE) for sample preparation and derivatization with heptafluorobutyric anhydride (HFBA) were performed for GC-MS analysis. The limit of detection (LOD) and the limit of quantification (LOQ) were 5 and 20 ng g(-1), respectively. The recovery of the added cortisol ranged from 99.8 to 101.0%. Excellent precision was obtained with a within-day variation (RSD) of 0.7% for GC-MS analysis. The accuracy of the measurement was evaluated by comparing of results of this reference measurement procedure on lyophilized human serum reference materials for cortisol (European Reference Materials (ERM)-DA 192) as Certified Reference Materials (CRMs). The results of this method for total cortisol agreed with the certified values within some uncertainty. This method, which demonstrates simply, easy, good accuracy, high precision, and is free from interferences from structural analogues, qualifies as a reference measurement procedure.

Metabolism of levamisole and kinetics of levamisole and aminorex in urine by means of LC-QTOF-HRMS and LC-QqQ-MS.

PubMed

Hess, Cornelius; Ritke, Natalie; Broecker, Sebastian; Madea, Burkhard; Musshoff, Frank

2013-05-01

The antihelminthic drug Levamisole can enhance cocaine effects by conversion into the amphetamine-like drug aminorex. We describe an LC-MS method for the determination of levamisole and its metabolite aminorex in human urine. Selectivity is given, calibration curves were linear within the calibration range 2.5-250 ng/mL; limits of the method were LoD 0.51 ng/mL, LoQ 1.02 ng/mL for levamisole and LoD 0.65 ng/mL, LoQ 0.76 ng/mL for aminorex. Precision data was in accordance with the guidelines (intraday precision for aminorex ranged between 5.75 and 11.0 % for levamisole between 8.36 and 10.9 %; interday precision for levamisole 10.9-16.9 % and for aminorex 7.64-12.7 %; accuracy data for levamisole -1.96 to -14.3 % and for aminorex-11.9 to-18.5 %). The validated method was successfully applied to study the urinary excretion of levamisole after the administration of 100 mg of levamisole orally. Levamisole and aminorex could be detected in post-administration urine samples. Levamisole could be detected up to 39 h after ingestion, while aminorex was detectable up to 54 h. Maximum aminorex concentrations were 45 ng/mL urine. Further metabolites of levamisole after oral ingestion by means of liquid chromatography hybrid quadrupole time-of-flight high-resolution mass spectrometry (LC-QTOF-HRMS) were identified. Only 0.5 % of the ingested drug was quantified as unchanged levamisole in urine. Besides aminorex, five isomers of aminorex and 4 hydroxy-metabolites of aminorex or its isomers were found. Furthermore, levamisole is also hydroxylated and eliminated free or conjugated with sulfate or glucuronide into urine.

A novel fast method for aqueous derivatization of THC, OH-THC and THC-COOH in human whole blood and urine samples for routine forensic analyses.

PubMed

Stefanelli, Fabio; Pesci, Federica Giorgia; Giusiani, Mario; Chericoni, Silvio

2018-04-01

A novel aqueous in situ derivatization procedure with propyl chloroformate (PCF) for the simultaneous, quantitative analysis of Δ 9 -tetrahydrocannabinol (THC), 11-hydroxy-Δ 9 -tetrahydrocannabinol (OH-THC) and 11-nor-Δ 9 -tetrahydrocannabinol-carboxylic acid (THC-COOH) in human blood and urine is proposed. Unlike current methods based on the silylating agent [N,O-bis(trimethylsilyl)trifluoroacetamide] added in an anhydrous environment, this new proposed method allows the addition of the derivatizing agent (propyl chloroformate, PCF) directly to the deproteinized blood and recovery of the derivatives by liquid-liquid extraction. This novel method can be also used for hydrolyzed urine samples. It is faster than the traditional method involving a derivatization with trimethyloxonium tetrafluoroborate. The analytes are separated, detected and quantified by gas chromatography-mass spectrometry in selected ion monitoring mode (SIM). The method was validated in terms of selectivity, capacity of identification, limits of detection (LOD) and quantification (LOQ), carryover, linearity, intra-assay precision, inter-assay precision and accuracy. The LOD and LOQ in hydrolyzed urine were 0.5 and 1.3 ng/mL for THC and 1.2 and 2.6 ng/mL for THC-COOH, respectively. In blood, the LOD and LOQ were 0.2 and 0.5 ng/mL for THC, 0.2 and 0.6 ng/mL for OH-THC, and 0.9 and 2.4 ng/mL for THC-COOH, respectively. This method was applied to 35 urine samples and 50 blood samples resulting to be equivalent to the previously used ones with the advantage of a simpler method and faster sample processing time. We believe that this method will be a more convenient option for the routine analysis of cannabinoids in toxicological and forensic laboratories. Copyright © 2017 John Wiley & Sons, Ltd.

Quantitative analysis of substituted N,N-dimethyl-tryptamines in the presence of natural type XII alkaloids.

PubMed

Ivanova, Bojidarka; Spiteller, Michael

2012-10-01

This paper reports the qualitative and quantitative analysis (QA) of mixtures of hallucinogens, N,N-dimethyltryptamine (DMT) (1), 5-methoxy- (la) and 5-hydroxy-N,N-dimethyltryptamine (1b) in the presence of beta-carbolines (indole alkaloids of type XII) ((2), (3) and (5)}. The validated electronic absorption spectroscopic (EAs) protocol achieved a concentration limit of detection (LOD) of 7.2.10(-7) mol/L {concentration limit of quantification (LOQ) of 24.10(-7) mol/L) using bands (lambda max within 260+/-0.23-262+/-0.33 nm. Metrology, including accuracy, measurement repeatability, measurement precision, trueness of measurement, and reproducibility of the measurements are presented using N,N-dimethyltryptamine (DMA) as standard. The analytical quantities of mixtures of alkaloids 4, 6 and 7 are: lambda max 317+/-0.45, 338+/-0.69 and 430+/-0.09 for 4 (LOD, 8.6.10(-7) mol/L; LOQ, 28.66(6), mol/L), as well as 528+/-0.75 nm for 6 and 7 (LOD, 8.2.10(-7) mol/L; LOQ, 27.33(3), mol/L), respectively. The partially validated protocols by high performance liquid chromatography (HPLC), electrospray ionization (ESI), mass spectrometry (MS), both in single and tandem operation (MS/MS) mode, as well as matrix/assisted laser desorption/ionization (MALDI) MS are elaborated. The Raman spectroscopic (RS) protocol for analysis of psychoactive substances, characterized by strong fluorescence RS profile was developed, with the detection limits being discussed. The known synergistic effect leading to increase the psychoactive and hallucinogenic properties and the reported acute poisoning cases from 1-7, make the present study emergent, since as well the current lack of analytical data and the herein metrology obtained contributed to the elaboration of highly selective and precise analytical protocols, which would be of interest in the field of criminal forensic analysis.

Spectrophotometric method development and validation for determination of chlorpheniramine maleate in bulk and controlled release tablets.

PubMed

Ashfaq, Maria; Sial, Ali Akber; Bushra, Rabia; Rehman, Atta-Ur; Baig, Mirza Tasawur; Huma, Ambreen; Ahmed, Maryam

2018-01-01

Spectrophotometric technique is considered to be the simplest and operator friendly among other available analytical methods for pharmaceutical analysis. The objective of the study was to develop a precise, accurate and rapid UV-spectrophotometric method for the estimation of chlorpheniramine maleate (CPM) in pure and solid pharmaceutical formulation. Drug absorption was measured in various solvent systems including 0.1N HCl (pH 1.2), acetate buffer (pH 4.5), phosphate buffer (pH 6.8) and distil water (pH 7.0). Method validation was performed as per official guidelines of ICH, 2005. High drug absorption was observed in 0.1N HCl medium with λ max of 261nm. The drug showed the good linearity from 20 to 60μg/mL solution concentration with the correlation coefficient linear regression equation Y= 0.1853 X + 0.1098 presenting R 2 value of 0.9998. The method accuracy was evaluated by the percent drug recovery, presents more than 99% drug recovery at three different levels assessed. The % RSD value <1 was computed for inter and intraday analysis indicating the high accuracy and precision of the developed technique. The developed method is robust because it shows no any significant variation in with minute changes. The LOD and LOQ values were assessed to be 2.2μg/mL and 6.6μg/mL respectively. The investigated method proved its sensitivity, precision and accuracy hence could be successfully used to estimate the CPM content in bulk and pharmaceutical matrix tablets.

Researches on High Accuracy Prediction Methods of Earth Orientation Parameters

NASA Astrophysics Data System (ADS)

Xu, X. Q.

2015-09-01

The Earth rotation reflects the coupling process among the solid Earth, atmosphere, oceans, mantle, and core of the Earth on multiple spatial and temporal scales. The Earth rotation can be described by the Earth's orientation parameters, which are abbreviated as EOP (mainly including two polar motion components PM_X and PM_Y, and variation in the length of day ΔLOD). The EOP is crucial in the transformation between the terrestrial and celestial reference systems, and has important applications in many areas such as the deep space exploration, satellite precise orbit determination, and astrogeodynamics. However, the EOP products obtained by the space geodetic technologies generally delay by several days to two weeks. The growing demands for modern space navigation make high-accuracy EOP prediction be a worthy topic. This thesis is composed of the following three aspects, for the purpose of improving the EOP forecast accuracy. (1) We analyze the relation between the length of the basic data series and the EOP forecast accuracy, and compare the EOP prediction accuracy for the linear autoregressive (AR) model and the nonlinear artificial neural network (ANN) method by performing the least squares (LS) extrapolations. The results show that the high precision forecast of EOP can be realized by appropriate selection of the basic data series length according to the required time span of EOP prediction: for short-term prediction, the basic data series should be shorter, while for the long-term prediction, the series should be longer. The analysis also showed that the LS+AR model is more suitable for the short-term forecasts, while the LS+ANN model shows the advantages in the medium- and long-term forecasts. (2) We develop for the first time a new method which combines the autoregressive model and Kalman filter (AR+Kalman) in short-term EOP prediction. The equations of observation and state are established using the EOP series and the autoregressive coefficients respectively, which are used to improve/re-evaluate the AR model. Comparing to the single AR model, the AR+Kalman method performs better in the prediction of UT1-UTC and ΔLOD, and the improvement in the prediction of the polar motion is significant. (3) Following the successful Earth Orientation Parameter Prediction Comparison Campaign (EOP PCC), the Earth Orientation Parameter Combination of Prediction Pilot Project (EOPC PPP) was sponsored in 2010. As one of the participants from China, we update and submit the short- and medium-term (1 to 90 days) EOP predictions every day. From the current comparative statistics, our prediction accuracy is on the medium international level. We will carry out more innovative researches to improve the EOP forecast accuracy and enhance our level in EOP forecast.

Development and validation of a gas chromatography/ion trap-mass spectrometry method for simultaneous quantification of cocaine and its metabolites benzoylecgonine and norcocaine: application to the study of cocaine metabolism in human primary cultured renal cells.

PubMed

Valente, Maria João; Carvalho, Félix; Bastos, M Lourdes; Carvalho, Márcia; de Pinho, Paula Guedes

2010-11-15

Acute renal failure is a common finding in cocaine abusers. While cocaine metabolism may contribute to its nephrotoxic mechanisms, its pharmacokinetics in kidney cells is hitherto to be clarified. Primary cultures of human proximal tubular cells (HPTCs) provide a well-characterized in vitro model, phenotypically representative of HPTCs in vivo. Thus, the present work describes the first sensitive gas chromatography/ion trap-mass spectrometry (GC/IT-MS) method for measurement of cocaine and its metabolites benzoylecgonine (BE) and norcocaine (NCOC) using a primary culture of HPTCs as cellular matrix, following solid phase extraction (SPE) and derivatization with N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA). The application of this methodology also enables the identification of two other cocaine metabolites: ecgonine methyl ester (EME) and anhydroecgonine methyl ester (AEME). The validation of the method was performed through the evaluation of selectivity, linearity, precision and accuracy, limit of detection (LOD), and limit of quantification (LOQ). Its applicability was demonstrated through the quantification of cocaine, BE and NCOC in primary cultured HPTCs after incubation, at physiological conditions, with 1 mM cocaine for 72 h. The developed GC/IT-MS method was found to be linear (r² > 0.99). The intra-day precision varied between 3.6% and 13.5% and the values of accuracy between 92.7% and 111.9%. The LOD values for cocaine, BE and NCOC were 0.97±0.09, 0.40±0.04 and 20.89±1.81 ng/mL, respectively, and 3.24±0.30, 1.34±0.14 and 69.62±6.05 ng/mL as LOQ values. Copyright © 2010 Elsevier B.V. All rights reserved.

Development and validation of an ultra-performance liquid chromatography quadrupole time of flight mass spectrometry method for rapid quantification of free amino acids in human urine.

PubMed

Joyce, Richard; Kuziene, Viktorija; Zou, Xin; Wang, Xueting; Pullen, Frank; Loo, Ruey Leng

2016-01-01

An ultra-performance liquid chromatography quadrupole time of flight mass spectrometry (UPLC-qTOF-MS) method using hydrophilic interaction liquid chromatography was developed and validated for simultaneous quantification of 18 free amino acids in urine with a total acquisition time including the column re-equilibration of less than 18 min per sample. This method involves simple sample preparation steps which consisted of 15 times dilution with acetonitrile to give a final composition of 25 % aqueous and 75 % acetonitrile without the need of any derivatization. The dynamic range for our calibration curve is approximately two orders of magnitude (120-fold from the lowest calibration curve point) with good linearity (r (2) ≥ 0.995 for all amino acids). Good separation of all amino acids as well as good intra- and inter-day accuracy (<15 %) and precision (<15 %) were observed using three quality control samples at a concentration of low, medium and high range of the calibration curve. The limits of detection (LOD) and lower limit of quantification of our method were ranging from approximately 1-300 nM and 0.01-0.5 µM, respectively. The stability of amino acids in the prepared urine samples was found to be stable for 72 h at 4 °C, after one freeze thaw cycle and for up to 4 weeks at -80 °C. We have applied this method to quantify the content of 18 free amino acids in 646 urine samples from a dietary intervention study. We were able to quantify all 18 free amino acids in these urine samples, if they were present at a level above the LOD. We found our method to be reproducible (accuracy and precision were typically <10 % for QCL, QCM and QCH) and the relatively high sample throughput nature of this method potentially makes it a suitable alternative for the analysis of urine samples in clinical setting.

Determination of total antioxidant capacity by oxygen radical absorbance capacity (ORAC) using fluorescein as the fluorescence probe: First Action 2012.23.

PubMed

Ou, Boxin; Chang, Tony; Huang, Dejian; Prior, Ronald L

2013-01-01

An improved method for the measurement of oxygen radical absorbance capacity (ORAC) was developed and validated using fluorescein (3',6'-dihydroxyspiro[isobenzofuran-1[3H], 9'[9H]-xanthen]-3-one) as a new fluorescence probe (ORAC(FL)). Randomly methylated beta-cyclodextrin (RMCD) was introduced as the water-solubility enhancer for lipophilic antioxidants. 7% RMCD (w/v) in 50% acetone-H2O mixture sufficiently solubilized vitamin E compounds and other lipophilic phenolic antioxidants in 75 mM phosphate buffer (pH 7.4). Results indicated that fluorescein shows excellent photostability under the plate reader conditions. This ORAC(FL) was validated through linearity, precision, accuracy, and ruggedness. The validation results demonstrated that the ORACFL assay is reliable and robust. The mean of intraday and interday CVs were <15%; for hydrophilic ORAC, LOD and LOQ are 5 and 6.25 microM, respectively; for lipophilic ORAC, LOD and LOQ are 6.25 and 12.5 microM, respectively. It is concluded that unlike other popular methods, the ORAC(FL) assay provides a direct measure of total antioxidant capacity against the peroxyl radicals.

Development and Validation of Stability-Indicating Derivative Spectrophotometric Methods for Determination of Dronedarone Hydrochloride

NASA Astrophysics Data System (ADS)

Chadha, R.; Bali, A.

2016-05-01

Rapid, sensitive, cost effective and reproducible stability-indicating derivative spectrophotometric methods have been developed for the estimation of dronedarone HCl employing peak-zero (P-0) and peak-peak (P-P) techniques, and their stability-indicating potential assessed in forced degraded solutions of the drug. The methods were validated with respect to linearity, accuracy, precision and robustness. Excellent linearity was observed in concentrations 2-40 μg/ml ( r 2 = 0.9986). LOD and LOQ values for the proposed methods ranged from 0.42-0.46 μg/ml and 1.21-1.27 μg/ml, respectively, and excellent recovery of the drug was obtained in the tablet samples (99.70 ± 0.84%).

The Use and Abuse of Limits of Detection in Environmental Analytical Chemistry

PubMed Central

Brown, Richard J. C.

2008-01-01

The limit of detection (LoD) serves as an important method performance measure that is useful for the comparison of measurement techniques and the assessment of likely signal to noise performance, especially in environmental analytical chemistry. However, the LoD is only truly related to the precision characteristics of the analytical instrument employed for the analysis and the content of analyte in the blank sample. This article discusses how other criteria, such as sampling volume, can serve to distort the quoted LoD artificially and make comparison between various analytical methods inequitable. In order to compare LoDs between methods properly, it is necessary to state clearly all of the input parameters relating to the measurements that have been used in the calculation of the LoD. Additionally, the article discusses that the use of LoDs in contexts other than the comparison of the attributes of analytical methods, in particular when reporting analytical results, may be confusing, less informative than quoting the actual result with an accompanying statement of uncertainty, and may act to bias descriptive statistics. PMID:18690384

Simultaneous determination of trace migration of phthalate esters in honey and royal jelly by GC-MS.

PubMed

Zhou, Jinhui; Qi, Yitao; Wu, Hongmei; Diao, Qingyun; Tian, Feifei; Li, Yi

2014-03-01

A simple, rapid, and reliable liquid-liquid extraction coupled to GC-MS method was developed and validated for the quantification of 22 phthalate esters (PAEs) in honey and royal jelly. Instrument parameters for GC-MS were tested to obtain the satisfactory separation between 22 PAEs with high sensitivity. The extraction procedure was optimized in order to achieve the best recovery. The following criteria were used to validate the developed method: linearity, LOD, lower LOQ, precision, accuracy, matrix effect and carry-over. Correlation coefficients were >0.999 by applying the linear regression model based on the least-squares method with a weighting factor (1/x). The intra- and interday precision were within 12.7% in terms of RSD, and the accuracy was within -11.8% in terms of relative error. The mean extraction recoveries ranged between 80.1 and 110.9% for honey and royal jelly. No significant matrix effect and carry-over for PAEs were observed for the analysis of honey and royal jelly samples. A total of 20 real samples were analyzed for a mini-survey using the developed method. Seven PAEs in honey samples and five PAEs in royal jelly samples were found, indicating potential contamination with several PAEs. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development and validation of a liquid chromatography method for the simultaneous determination of eight water-soluble vitamins in multivitamin formulations and human urine.

PubMed

Patil, Suyog S; Srivastava, Ashwini K

2013-01-01

A simple, precise, and rapid RPLC method has been developed without incorporation of any ion-pair reagent for the simultaneous determination of vitamin C (C) and seven B-complex vitamins, viz, thiamine hydrochloride (B1), pyridoxine hydrochloride (B6), nicotinamide (B3), cyanocobalamine (B12), folic acid, riboflavin (B2), and 4-aminobenzoic acid (Bx). Separations were achieved within 12.0 min at 30 degrees C by gradient elution on an RP C18 column using a mobile phase consisting of a mixture of 15 mM ammonium formate buffer and 0.1% triethylamine adjusted to pH 4.0 with formic acid and acetonitrile. Simultaneous UV detection was performed at 275 and 360 nm. The method was validated for system suitability, LOD, LOQ, linearity, precision, accuracy, specificity, and robustness in accordance with International Conference on Harmonization guidelines. The developed method was implemented successfully for determination of the aforementioned vitamins in pharmaceutical formulations containing an individual vitamin, in their multivitamin combinations, and in human urine samples. The calibration curves for all analytes showed good linearity, with coefficients of correlation higher than 0.9998. Accuracy, intraday repeatability (n = 6), and interday repeatability (n = 7) were found to be satisfactory.

Simultaneous quantification and identification of flavonoids, lignans, coumarin and amides in leaves of Zanthoxylum armatum using UPLC-DAD-ESI-QTOF-MS/MS.

PubMed

Bhatt, Vinod; Sharma, Sushila; Kumar, Neeraj; Sharma, Upendra; Singh, Bikram

2017-01-05

The current study presents isolation and characterization of twelve compounds including catechin (1), isovitexin (2), hesperidin (3), psoralin (4), eudesmin (5), kobusin (6), fargesin (7), sesamin (8), asarinin (9), planispine-A (10), α-sanshool (11) and vitexin (12), from the leaves of Zanthoxylum armatum. Further, two rapid and simple ultra performance liquid chromatography-diode array detection (UPLC-DAD) methods were developed for the simultaneous quantitative determination of isolated compounds from Z. armatum leaves. These analytical methods were validated for linearity, precision, accuracy, limit of detection (LOD) and limit of quantification (LOQ). The LOD and LOQ were in the range of 0.06-0.21μg/mL and 0.19-0.69μg/mL, respectively. The validated method was linear (R 2 ≥0.9906), precise in terms of peak area (intra-day RSDs <3.8% and inter-day RSDs <2.7%), and accurate (109.6-92.5%). This is the first report on the isolation and quantification of 1, 2, 4 and 12 in Z. armatum and 3 in Zanthoxylum genus. The methods: were successfully applied to assess the quality of samples collected from different locations of Himachal Pradesh during summer and winter season. The results demonstrated that flavonoids and furofuran lignans were the major constituents in Z. armatum leaves. The developed methods: were further applied for tandem electrospray ionization-mass spectrometry (UPLC-DAD-ESI-MS/MS) and total eighteen compounds were identified including phenolic acid, flavonoids, furofuran lignans, coumarin and isobutyl amides. Copyright © 2016 Elsevier B.V. All rights reserved.

Quantitative analysis of sitagliptin using the (19)F-NMR method: a universal technique for fluorinated compound detection.

PubMed

Zhang, Fen-Fen; Jiang, Meng-Hong; Sun, Lin-Lin; Zheng, Feng; Dong, Lei; Shah, Vishva; Shen, Wen-Bin; Ding, Ya

2015-01-07

To expand the application scope of nuclear magnetic resonance (NMR) technology in quantitative analysis of pharmaceutical ingredients, (19)F nuclear magnetic resonance ((19)F-NMR) spectroscopy has been employed as a simple, rapid, and reproducible approach for the detection of a fluorine-containing model drug, sitagliptin phosphate monohydrate (STG). ciprofloxacin (Cipro) has been used as the internal standard (IS). Influential factors, including the relaxation delay time (d1) and pulse angle, impacting the accuracy and precision of spectral data are systematically optimized. Method validation has been carried out in terms of precision and intermediate precision, linearity, limit of detection (LOD) and limit of quantification (LOQ), robustness, and stability. To validate the reliability and feasibility of the (19)F-NMR technology in quantitative analysis of pharmaceutical analytes, the assay result has been compared with that of (1)H-NMR. The statistical F-test and student t-test at 95% confidence level indicate that there is no significant difference between these two methods. Due to the advantages of (19)F-NMR, such as higher resolution and suitability for biological samples, it can be used as a universal technology for the quantitative analysis of other fluorine-containing pharmaceuticals and analytes.

Protein Quantification by Derivatization-Free High-Performance Liquid Chromatography of Aromatic Amino Acids

PubMed Central

Hesse, Almut

2016-01-01

Amino acid analysis is considered to be the gold standard for quantitative peptide and protein analysis. Here, we would like to propose a simple HPLC/UV method based on a reversed-phase separation of the aromatic amino acids tyrosine (Tyr), phenylalanine (Phe), and optionally tryptophan (Trp) without any derivatization. The hydrolysis of the proteins and peptides was performed by an accelerated microwave technique, which needs only 30 minutes. Two internal standard compounds, homotyrosine (HTyr) and 4-fluorophenylalanine (FPhe) were used for calibration. The limit of detection (LOD) was estimated to be 0.05 µM (~10 µg/L) for tyrosine and phenylalanine at 215 nm. The LOD for a protein determination was calculated to be below 16 mg/L (~300 ng BSA absolute). Aromatic amino acid analysis (AAAA) offers excellent accuracy and a precision of about 5% relative standard deviation, including the hydrolysis step. The method was validated with certified reference materials (CRM) of amino acids and of a pure protein (bovine serum albumin, BSA). AAAA can be used for the quantification of aromatic amino acids, isolated peptides or proteins, complex peptide or protein samples, such as serum or milk powder, and peptides or proteins immobilized on solid supports. PMID:27559481

Capillary electrophoresis method with UV-detection for analysis of free amino acids concentrations in food.

PubMed

Omar, Mei Musa Ali; Elbashir, Abdalla Ahmed; Schmitz, Oliver J

2017-01-01

Simple and inexpensive capillary electrophoresis with UV-detection method (CE-UV) was optimized and validated for determination of six amino acids namely (alanine, asparagine, glutamine, proline, serine and valine) for Sudanese food. Amino acids in the samples were derivatized with 4-chloro-7-nitro-2,1,3-benzoxadiazole (NBD-Cl) prior to CE-UV analysis. Labeling reaction conditions (100mM borate buffer at pH 8.5, labeling reaction time 60min, temperature 70°C and NBD-Cl concentration 40mM) were systematically investigated. The optimal conditions for the separation were 100mM borate buffer at pH 9.7 and detected at 475nm. The method was validated in terms of linearity, limit of detection (LOD), limit of quantification (LOQ), precision (repeatability) (RSD%) and accuracy (recovery). Good linearity was achieved for all amino acids (r(2)>0.9981) in the concentration range of 2.5-40mg/L. The LODs in the range of 0.32-0.56mg/L were obtained. Recoveries of amino acids ranging from 85% to 108%, (n=3) were obtained. The validated method was successfully applied for the determination of amino acids for Sudanese food samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Determination of Oversulphated Chondroitin Sulphate and Dermatan Sulphate in unfractionated heparin by (1)H-NMR - Collaborative study for quantification and analytical determination of LoD.

PubMed

McEwen, I; Mulloy, B; Hellwig, E; Kozerski, L; Beyer, T; Holzgrabe, U; Wanko, R; Spieser, J-M; Rodomonte, A

2008-12-01

Oversulphated Chondroitin Sulphate (OSCS) and Dermatan Sulphate (DS) in unfractionated heparins can be identified by nuclear magnetic resonance spectrometry (NMR). The limit of detection (LoD) of OSCS is 0.1% relative to the heparin content. This LoD is obtained at a signal-to-noise ratio (S/N) of 2000:1 of the heparin methyl signal. Quantification is best obtained by comparing peak heights of the OSCS and heparin methyl signals. Reproducibility of less than 10% relative standard deviation (RSD) has been obtained. The accuracy of quantification was good.

Determination of Alkaloid Contents in Various Tissues of Coptis Chinensis Franch. by Reversed Phase-High Performance Liquid Chromatography and Ultraviolet Spectrophotometry.

PubMed

Yang, Yanfang; Peng, Jingling; Li, Fangping; Liu, Xin; Deng, Meng; Wu, Hezhen

2017-05-01

A simple and intuitive method for optimizing the chemical constituents of Coptis Chinensis Franch. is important to assess its quality and clinical efficacy. An high performance liquid chromatography and ultraviolet spectrophotometry method was developed for the determination of berberine hydrochloride, palmatine chloride, jatrorrhizine hydrochloride, epiberberine, coptisine, columbamine and magnoflorine in various tissues (i.e., phloem, xylem and medulla) and rizhome of C. Chinensis Franch. The transection of rhizome from outside-in includes cork layer, cortex, phloem, cambium, xylem and medulla. Cork layer consists of dead cells, and therefore is not of any research significance. Cortex, phloem and cambium were almost impossible to separate, therefore they were studied as a whole in our experiments. They were collectively referred to as "phloem". The analytes were separated on a Gemini-NX C18 (250 mm × 4.6 mm, 5 μm) reversed phase column using a gradient elution of acetonitrile-0.03 mol/L ammonium acetate solution (containing 0.1% triethylamine and 0.6% ammonium hydroxide) as the mobile phase at a flow rate of 1.0 mL/min and UV detection at 270 nm. The method allowing the simultaneous quantification of seven major active constituents was optimized and validated for linearity, precision, accuracy, limits of detection (LOD) and quantification. The LOD ranged from 0.102 to 0.651 mg/mL (r ≥ 0.9993). Accuracy, precision and recovery were all within the required limits. The average recovery was between 100.14% and 102.75% and the relative standard deviations were <3.34%. At the same time, the absorbance was determined by ultraviolet spectrophotometry at 345 nm wavelength. Based on contents of the seven constituents and clustering result, this investigation suggests that there are significant differences in the distribution of seven alkaloids in the tissues examined. Furthermore, the total alkaloid content in xylem is relatively lower than that in phloem, medulla and rhizome. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Improving data quality in the linked open data: a survey

NASA Astrophysics Data System (ADS)

Hadhiatma, A.

2018-03-01

The Linked Open Data (LOD) is “web of data”, a different paradigm from “web of document” commonly used today. However, the huge LOD still suffers from data quality problems such as completeness, consistency, and accuracy. Data quality problems relate to designing effective methods both to manage and to retrieve information at various data quality levels. Based on review from papers and journals, addressing data quality requires some standards functioning to (1) identification of data quality problems, (2) assessment of data quality for a given context, and (3) correction of data quality problems. However, mostly the methods and strategies dealing with the LOD data quality were not as an integrative approach. Hence, based on those standards and an integrative approach, there are opportunities to improve the LOD data quality in the term of incompleteness, inaccuracy and inconsistency, considering to its schema and ontology, namely ontology refinement. Moreover, the term of the ontology refinement means that it copes not only to improve data quality but also to enrich the LOD. Therefore, it needs (1) a standard for data quality assessment and evaluation which is more appropriate to the LOD; (2) a framework of methods based on statistical relational learning that can improve the correction of data quality problems as well as enrich the LOD.

A novel approach for determination of free fatty acids in vegetable oils by a flow injection system with manual injection.

PubMed

Ayyildiz, H Filiz; Kara, Huseyin; Sherazi, S T H

2011-12-01

A non-aqueous flow injection method for determining free fatty acid (FFA) content in corn and sunflower oil samples was developed. A single-line manifold system was built by modification of an HPLC for flow injection analysis (FIA). Without pre-treatment, oil samples were injected into a n-propanol solution containing KOH and phenolphthalein (PHP). The main parameters, such as flow rate of carrier phase, length, geometry, inner diameters of the coils and reagent concentration were all optimized. The proposed FIA method was validated for precision, accuracy, linear region, limit of detection (LOD) and limit of quantification (LOQ). The intra- and inter-day measurements of the precision of the method were found to be within the limits of acceptance criteria (RSD < 1%), and were rugged when the method was performed by a different analyst. The linear concentration range was calculated as 0.09-1.50 and 0.07-1.40 FFA% for corn and sunflower oils, correspondingly. The LOD and LOQ were found to be 7.53 × 10(-4)-2.28 × 10(-3) oleic acid % and 7.11 × 10(-4)-2.23 × 10(-3) oleic acid % for corn and sunflower oils, respectively. The results were compared with those obtained by the AOCS (Ca-5a-40) method using statistical t and F tests, and a significant difference was not observed between the methods at a 95% confidence level. The proposed method is suitable for quality control of routine applications due to its simplicity, high sample throughput, and economy of solvents and sample, offering considerable promise as a low cost analytical system that needs minimum human intervention over long periods of time.

A newly validated high-performance liquid chromatography method with diode array ultraviolet detection for analysis of the antimalarial drug primaquine in the blood plasma.

PubMed

Carmo, Ana Paula Barbosa do; Borborema, Manoella; Ribeiro, Stephan; De-Oliveira, Ana Cecilia Xavier; Paumgartten, Francisco Jose Roma; Moreira, Davyson de Lima

2017-01-01

Primaquine (PQ) diphosphate is an 8-aminoquinoline antimalarial drug with unique therapeutic properties. It is the only drug that prevents relapses of Plasmodium vivax or Plasmodium ovale infections. In this study, a fast, sensitive, cost-effective, and robust method for the extraction and high-performance liquid chromatography with diode array ultraviolet detection (HPLC-DAD-UV ) analysis of PQ in the blood plasma was developed and validated. After plasma protein precipitation, PQ was obtained by liquid-liquid extraction and analyzed by HPLC-DAD-UV with a modified-silica cyanopropyl column (250mm × 4.6mm i.d. × 5μm) as the stationary phase and a mixture of acetonitrile and 10mM ammonium acetate buffer (pH = 3.80) (45:55) as the mobile phase. The flow rate was 1.0mL·min-1, the oven temperature was 50OC, and absorbance was measured at 264nm. The method was validated for linearity, intra-day and inter-day precision, accuracy, recovery, and robustness. The detection (LOD) and quantification (LOQ) limits were 1.0 and 3.5ng·mL-1, respectively. The method was used to analyze the plasma of female DBA-2 mice treated with 20mg.kg-1 (oral) PQ diphosphate. By combining a simple, low-cost extraction procedure with a sensitive, precise, accurate, and robust method, it was possible to analyze PQ in small volumes of plasma. The new method presents lower LOD and LOQ limits and requires a shorter analysis time and smaller plasma volumes than those of previously reported HPLC methods with DAD-UV detection. The new validated method is suitable for kinetic studies of PQ in small rodents, including mouse models for the study of malaria.

Procedural 3d Modelling for Traditional Settlements. The Case Study of Central Zagori

NASA Astrophysics Data System (ADS)

Kitsakis, D.; Tsiliakou, E.; Labropoulos, T.; Dimopoulou, E.

2017-02-01

Over the last decades 3D modelling has been a fast growing field in Geographic Information Science, extensively applied in various domains including reconstruction and visualization of cultural heritage, especially monuments and traditional settlements. Technological advances in computer graphics, allow for modelling of complex 3D objects achieving high precision and accuracy. Procedural modelling is an effective tool and a relatively novel method, based on algorithmic modelling concept. It is utilized for the generation of accurate 3D models and composite facade textures from sets of rules which are called Computer Generated Architecture grammars (CGA grammars), defining the objects' detailed geometry, rather than altering or editing the model manually. In this paper, procedural modelling tools have been exploited to generate the 3D model of a traditional settlement in the region of Central Zagori in Greece. The detailed geometries of 3D models derived from the application of shape grammars on selected footprints, and the process resulted in a final 3D model, optimally describing the built environment of Central Zagori, in three levels of Detail (LoD). The final 3D scene was exported and published as 3D web-scene which can be viewed with 3D CityEngine viewer, giving a walkthrough the whole model, same as in virtual reality or game environments. This research work addresses issues regarding textures' precision, LoD for 3D objects and interactive visualization within one 3D scene, as well as the effectiveness of large scale modelling, along with the benefits and drawbacks that derive from procedural modelling techniques in the field of cultural heritage and more specifically on 3D modelling of traditional settlements.

Analysis of cocoa flavanols and procyanidins (DP 1-10) in cocoa-containing ingredients and products by rapid resolution liquid chromatography: single-laboratory validation.

PubMed

Machonis, Philip R; Jones, Matthew A; Kwik-Uribe, Catherine

2014-01-01

Recently, a multilaboratory validation (MLV) of AOAC Official Method 2012.24 for the determination of cocoa flavanols and procyanidins (CF-CP) in cocoa-based ingredients and products determined that the method was robust, reliable, and transferrable. Due to the complexity of the CF-CP molecules, this method required a run time exceeding 1 h to achieve acceptable separations. To address this issue, a rapid resolution normal phase LC method was developed, and a single-laboratory validation (SLV) study conducted. Flavanols and procyanidins with a degree of polymerization (DP) up to 10 were eluted in 15 min using a binary gradient applied to a diol stationary phase, detected using fluorescence detection, and reported as a total sum of DP 1-10. Quantification was achieved using (-)-epicatechin-based relative response factors for DP 2-10. Spike recovery samples and seven different types of cocoa-based samples were analyzed to evaluate the accuracy, precision, LOD, LOQ, and linearity of the method. The within-day precision of the reported content for the samples was 1.15-5.08%, and overall precision was 3.97-13.61%. Spike-recovery experiments demonstrated recoveries of over 98%. The results of this SLV were compared to those previously obtained in the MLV and found to be consistent. The translation to rapid resolution LC allowed for an 80% reduction in analysis time and solvent usage, while retaining the accuracy and reliability of the original method. The savings in both cost and time of this rapid method make it well-suited for routine laboratory use.

Theoretically guided analytical method development and validation for the estimation of rifampicin in a mixture of isoniazid and pyrazinamide by UV spectrophotometer

NASA Astrophysics Data System (ADS)

Khan, Mohammad F.; Rita, Shamima A.; Kayser, Md. Shahidulla; Islam, Md. Shariful; Asad, Sharmeen; Bin Rashid, Ridwan; Bari, Md. Abdul; Rahman, Muhammed M.; Al Aman, D. A. Anwar; Setu, Nurul I.; Banoo, Rebecca; Rashid, Mohammad A.

2017-04-01

A simple, rapid, economic, accurate and precise method for the estimation of rifampicin in a mixture of isoniazid and pyrazinamide by UV spectrophotometeric technique (guided by the theoretical investigation of physicochemical properties) was developed and validated. Theoretical investigations revealed that isoniazid and pyrazinamide both were freely soluble in water and slightly soluble in ethyl acetate whereas rifampicin was practically insoluble in water but freely soluble in ethyl acetate. This indicates that ethyl acetate is an effective solvent for the extraction of rifampicin from a water mixture of isoniazid and pyrazinamide. Computational study indicated that pH range of 6.0-8.0 would favor the extraction of rifampicin. Rifampicin is separated from isoniazid and pyrazinamide at pH 7.4 ± 0.1 by extracting with ethyl acetate. The ethyl acetate was then analyzed at λmax of 344.0 nm. The developed method was validated for linearity, accuracy and precision according to ICH guidelines. The proposed method exhibited good linearity over the concentration range of 2.5 - 35.0 µg/mL. The intraday and inter-day precision in terms of % RSD ranged from 1.09 - 1.70% and 1.63 - 2.99%, respectively. The accuracy (in terms of recovery) of the method varied from of 96.7 ± 0.9 to 101.1 ± 0.4%. The LOD and LOQ were found to be 0.83 and 2.52 µg/mL, respectively. In addition, the developed method was successfully applied to assay rifampicin combination (isoniazid and pyrazinamide) brands available in Bangladesh.

Use of experimental design for optimisation of the cold plasma ICP-MS determination of lithium, aluminum and iron in soft drinks and alcoholic beverages.

PubMed

Bianchi, F; Careri, M; Maffini, M; Mangia, A; Mucchino, C

2003-01-01

A sensitive method for the simultaneous determination of (7)Li, (27)Al and (56)Fe by cold plasma ICP-MS was developed and validated. Experimental design was used to investigate the effects of torch position, torch power, lens 2 voltage, and coolant flow. Regression models and desirability functions were applied to find the experimental conditions providing the highest global sensitivity in a multi-elemental analysis. Validation was performed in terms of limits of detection (LOD), limits of quantitation (LOQ), linearity and precision. LODs were 1.4 and 159 ng L(-1) for (7)Li and (56)Fe, respectively; the highest LOD found being that for (27)Al (425 ng L(-1)). Linear ranges of 5 orders of magnitude for Li and 3 orders for Fe were statistically verified for each compound. Precision was evaluated by testing two concentration levels, and good results in terms of both intra-day repeatability and intermediate precision were obtained. RSD values lower than 4.8% at the lowest concentration level were calculated for intra-day repeatability. Commercially available soft drinks and alcoholic beverages contained in different packaging materials (TetraPack, polyethylene terephthalate (PET), commercial cans and glass) were analysed, and all the analytes were detected and quantitated. Copyright 2002 John Wiley & Sons, Ltd.

Quantitation of Pyrantel Pamoate in Pharmaceuticals Using Permanganate by Visible Spectrophotometry

NASA Astrophysics Data System (ADS)

Rajendraprasad, N.; Basavaiah, K.

2014-03-01

Two simple, accurate and precise spectrophotometric methods are developed and validated for the assay of pyrantel pamoate (PP) in pharmaceuticals. The methods employ the oxidative property of potassium permanganate (KMnO4) in acidic and alkaline conditions. In the first method (method A), PP is converted into its free base, pyrantel (PR), and treated with known excess of KMnO4 in acidic condition followed by the measurement of unreacted KMnO4 at 550 nm. Method B is based on the registration of absorbance of green colored chromogen formed due to the reduction of KMnO4 by PP in alkaline condition. The methods obeyed Beer's law over a range of 1-20 μg/ml in inverse manner, and 0.75-15 μg/ml for method A and method B, respectively, with apparent molar absorptivity values of 1.05ṡ104 and 2.85ṡ104 lṡmol-1ṡcm-1. The optical parameters such as limits of detection (LOD), quantification (LOQ), and the Sandell sensitivity values are also reported. The accuracy and precision of the methods are assessed on intra- and inter-day basis. A recovery study by standard addition procedure is also carried out for further assurance of accuracy. The developed methods are successfully applied to determine PP in tablets. The results are more satisfactory as per current ICH guidelines.

Development of a stability-indicating CE assay for the determination of amlodipine enantiomers in commercial tablets.

PubMed

Fakhari, Ali Reza; Nojavan, Saeed; Haghgoo, Soheila; Mohammadi, Ali

2008-11-01

A simple, accurate, precise and sensitive method using CD for separation and stability indicating assay of enantiomers of amlodipine in the commercial tablets has been established. Several types of CD were evaluated and best results were obtained using a fused-silica capillary with phosphate running buffer (100 mM, pH 3.0) containing 5 mM hydroxypropyl-alpha-CD. The method has shown adequate separation for amlodipine enantiomers from its degradation products. The drug was subjected to oxidation, hydrolysis, photolysis and heat to apply stress conditions. The range of quantitation for both enantiomers was 5-150 microg/mL. Intra- and inter-day RSD (n=6) was <4%. The limit of quantification that produced the requisite precision and accuracy was found to be 5 microg/mL for both enantiomers. The LOD for both enantiomers was found to be 0.5 microg/mL. Degradation products produced as a result of stress studies did not interfere with the detection of enantiomers and the assay can thus be considered stability indicating.

Development and validation of a HPTLC method for simultaneous estimation of lornoxicam and thiocolchicoside in combined dosage form.

PubMed

Sahoo, Madhusmita; Syal, Pratima; Hable, Asawaree A; Raut, Rahul P; Choudhari, Vishnu P; Kuchekar, Bhanudas S

2011-07-01

To develop a simple, precise, rapid and accurate HPTLC method for the simultaneous estimation of Lornoxicam (LOR) and Thiocolchicoside (THIO) in bulk and pharmaceutical dosage forms. The separation of the active compounds from pharmaceutical dosage form was carried out using methanol:chloroform:water (9.6:0.2:0.2 v/v/v) as the mobile phase and no immiscibility issues were found. The densitometric scanning was carried out at 377 nm. The method was validated for linearity, accuracy, precision, LOD (Limit of Detection), LOQ (Limit of Quantification), robustness and specificity. The Rf values (±SD) were found to be 0.84 ± 0.05 for LOR and 0.58 ± 0.05 for THIO. Linearity was obtained in the range of 60-360 ng/band for LOR and 30-180 ng/band for THIO with correlation coefficients r(2) = 0.998 and 0.999, respectively. The percentage recovery for both the analytes was in the range of 98.7-101.2 %. The proposed method was optimized and validated as per the ICH guidelines.

Rapid screening of drugs of abuse in human urine by high-performance liquid chromatography coupled with high resolution and high mass accuracy hybrid linear ion trap-Orbitrap mass spectrometry.

PubMed

Li, Xiaowen; Shen, Baohua; Jiang, Zheng; Huang, Yi; Zhuo, Xianyi

2013-08-09

A novel analytical toxicology method has been developed for the analysis of drugs of abuse in human urine by using a high resolution and high mass accuracy hybrid linear ion trap-Orbitrap mass spectrometer (LTQ-Orbitrap-MS). This method allows for the detection of different drugs of abuse, including amphetamines, cocaine, opiate alkaloids, cannabinoids, hallucinogens and their metabolites. After solid-phase extraction with Oasis HLB cartridges, spiked urine samples were analysed by HPLC/LTQ-Orbitrap-MS using an electrospray interface in positive ionisation mode, with resolving power of 30,000 full width at half maximum (FWHM). Gradient elution off of a Hypersil Gold PFP column (50mm×2.1mm) allowed to resolve 65 target compounds and 3 internal standards in a total chromatographic run time of 20min. Validation of this method consisted of confirmation of identity, selectivity, linearity, limit of detection (LOD), lowest limits of quantification (LLOQ), accuracy, precision, extraction recovery and matrix effect. The regression coefficients (r(2)) for the calibration curves (LLOQ - 100ng/mL) in the study were ≥0.99. The LODs for 65 validated compounds were better than 5ng/ml except for 4 compounds. The relative standard deviation (RSD), which was used to estimate repeatability at three concentrations, was always less than 15%. The recovery of extraction and matrix effects were above 50 and 70%, respectively. Mass accuracy was always better than 2ppm, corresponding to a maximum mass error of 0.8 millimass units (mmu). The accurate masses of characteristic fragments were obtained by collisional experiments for a more reliable identification of the analytes. Automated data analysis and reporting were performed using ToxID software with an exact mass database. This procedure was then successfully applied to analyse drugs of abuse in a real urine sample from subject who was assumed to be drug addict. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

Capillary electrophoresis determination of glucosamine in nutraceutical formulations after labeling with anthranilic acid and UV detection.

PubMed

Volpi, Nicola

2009-04-05

A new robust CE method for the determination of the glucosamine (GlcN) content in nutraceutical formulations is described after its derivatization with anthranilic acid (2-aminobenzoic acid, AA). The CE separation of derivatized GlcN with AA was performed on an uncoated fused-silica capillary tube (50 microm I.D.) using an operating pH 7.0 buffer of 150 mM boric acid/50 mM NaH2PO4 and UV detection at 214 nm. The method was validated for specificity, linearity, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ). The detector response for GlcN was linear over the selected concentration range from 240 to 2400 pg (40-400 microg/mL) with a correlation coefficient greater than 0.980. The intra- and inter-day variations (CV%) were between 0.5 and 0.9 for migration time, and between 2.8 and 4.3 for peak area, respectively. The LOD and the LOQ of the method were approximately 200 and 500 pg, respectively. The intra- and inter-day accuracy was estimated to range from 2.8% to 5.1%, while the percent recoveries of GlcN in formulations were calculated to be about 100% after simple centrifugation for 10 min, lyophilization and derivatization with AA. The CE method was applied to the determination of GlcN content, in the form of GlcN-hydrochloride or GlcN-sulfate, of several nutraceutical preparations in the presence of other ingredients, i.e. chondroitin sulfate, vitamin C and/or methylsulfonylmethane (MSM) as well as salts and other agents. The quantitative results obtained were in total conformity with the label claims.

Determination of flurbiprofen in human plasma by gas chromatography with mass spectrometry and its pharmacokinetics.

PubMed

Yilmaz, Bilal; Sahin, Huseyin; Akba, Vedat; Erdem, Ali Fuat

2014-01-01

This paper describes a GCIMS method for the determination of flurbiprofen in human plasma. Flurbiprofen and internal standard ibuprofen were extracted from plasma by using a liquid-liquid extraction method. Derivatization was carried out using N-Methyl-N-(trimethylsilyl)trifluoroacetamide. The calibration curve was linear between the concentration range of 0.10 and 5.0 microg/mL. Intraday and interday precision values for flurbiprofen in plasma were less than 5.49%, and accuracy (relative error) was better than 5.33%. The extraction recoveries of flurbiprofen from human plasma were between 93.6 and 98.6%. The LOD and LOQ of flurbiprofen were 0.03 and 0.10 microg/mL, respectively. This assay was applied to determine the pharmacokinetic parameters of flurbiprofen in healthy Turkish volunteers who had been given 100 mg of flurbiprofen.

Determination of acrylamide in dried fruits and edible seeds using QuEChERS extraction and LC separation with MS detection.

PubMed

De Paola, Eleonora Laura; Montevecchi, Giuseppe; Masino, Francesca; Garbini, Davide; Barbanera, Martino; Antonelli, Andrea

2017-02-15

Acrylamide is a carcinogenic and neurotoxic process contaminant that is generated from food components during heat treatment, while it is absent in raw foodstuffs. Its level in food arouses great concern. A method for acrylamide extraction and determination in dried fruits (dried prunes and raisins) and edible seeds (almonds, hazelnuts, peanuts, pine nuts, pistachios, and walnuts) using a QuEChERS-LC-ESI-MS-Triple Quadrupole approach was set up. Linearity, sensitivity, accuracy, and precision of the method were satisfactory. Dried prunes and peanuts were the only samples appreciably contaminated, 14.7-124.3 and 10.0-42.9μg/kg, respectively, as a consequence of the drying process. In fact, prunes are dried at 70-80°C for a quite long time (24-36h), while peanuts undergo a roasting process at 160-180°C for 25-30min. The relative standard deviations, accuracy, LOD, and LOQ show that the method provides a reliable approach to acrylamide determination in different matrices. Copyright © 2016 Elsevier Ltd. All rights reserved.

QuEChERS-based purification method coupled to ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) to determine six quaternary ammonium compounds (QACs) in dairy products.

PubMed

Xian, Yanping; Dong, Hao; Wu, Yuluan; Guo, Xindong; Hou, Xiangchang; Wang, Bin

2016-12-01

QuEChERS-based purification coupled with UPLC-MS/MS method, was developed for six quaternary ammonium compounds (QACs) determination in dairy products. Powder samples were firstly dispersed by water. Protein in liquid milk was precipitated and sample solution was extracted by acetonitrile. QuEChERS-based purification was used to purify the solution. QACs were finally separated by HILIC column and detected in MRM mode of MS/MS under ESI(+). The stable isotope benzyl-2,3,4,5,6-d5-dimethyltetradecylammonium bromide (C14-BAC-d5) was used as an internal standard. This method was validated in terms of linearity, sensitivity, precision, accuracy. Linear relations were favorable for QACs over the selected concentration ranges of 0.2-50μg/L, with correlation coefficients greater than 0.999. The limits of detection (LODs) were in the range of 0.4-14.5μg/kg. Recoveries were between 91.2% and 115% with RSDs of 2.8-7.5% for intra-day precision and 3.7-6.7% for inter-day precision. This validated method was successfully applied to determine the QACs concentrations in dairy products. Copyright © 2016 Elsevier Ltd. All rights reserved.

Prediction of UT1-UTC, LOD and AAM χ3 by combination of least-squares and multivariate stochastic methods

NASA Astrophysics Data System (ADS)

Niedzielski, Tomasz; Kosek, Wiesław

2008-02-01

This article presents the application of a multivariate prediction technique for predicting universal time (UT1-UTC), length of day (LOD) and the axial component of atmospheric angular momentum (AAM χ 3). The multivariate predictions of LOD and UT1-UTC are generated by means of the combination of (1) least-squares (LS) extrapolation of models for annual, semiannual, 18.6-year, 9.3-year oscillations and for the linear trend, and (2) multivariate autoregressive (MAR) stochastic prediction of LS residuals (LS + MAR). The MAR technique enables the use of the AAM χ 3 time-series as the explanatory variable for the computation of LOD or UT1-UTC predictions. In order to evaluate the performance of this approach, two other prediction schemes are also applied: (1) LS extrapolation, (2) combination of LS extrapolation and univariate autoregressive (AR) prediction of LS residuals (LS + AR). The multivariate predictions of AAM χ 3 data, however, are computed as a combination of the extrapolation of the LS model for annual and semiannual oscillations and the LS + MAR. The AAM χ 3 predictions are also compared with LS extrapolation and LS + AR prediction. It is shown that the predictions of LOD and UT1-UTC based on LS + MAR taking into account the axial component of AAM are more accurate than the predictions of LOD and UT1-UTC based on LS extrapolation or on LS + AR. In particular, the UT1-UTC predictions based on LS + MAR during El Niño/La Niña events exhibit considerably smaller prediction errors than those calculated by means of LS or LS + AR. The AAM χ 3 time-series is predicted using LS + MAR with higher accuracy than applying LS extrapolation itself in the case of medium-term predictions (up to 100 days in the future). However, the predictions of AAM χ 3 reveal the best accuracy for LS + AR.

Development of an Advanced HPLC–MS/MS Method for the Determination of Carotenoids and Fat-Soluble Vitamins in Human Plasma

PubMed Central

Hrvolová, Barbora; Martínez-Huélamo, Miriam; Colmán-Martínez, Mariel; Hurtado-Barroso, Sara; Lamuela-Raventós, Rosa Maria; Kalina, Jiří

2016-01-01

The concentration of carotenoids and fat-soluble vitamins in human plasma may play a significant role in numerous chronic diseases such as age-related macular degeneration and some types of cancer. Although these compounds are of utmost interest for human health, methods for their simultaneous determination are scarce. A new high pressure liquid chromatography (HPLC)-tandem mass spectrometry (MS/MS) method for the quantification of selected carotenoids and fat-soluble vitamins in human plasma was developed, validated, and then applied in a pilot dietary intervention study with healthy volunteers. In 50 min, 16 analytes were separated with an excellent resolution and suitable MS signal intensity. The proposed HPLC–MS/MS method led to improvements in the limits of detection (LOD) and quantification (LOQ) for all analyzed compounds compared to the most often used HPLC–DAD methods, in some cases being more than 100-fold lower. LOD values were between 0.001 and 0.422 µg/mL and LOQ values ranged from 0.003 to 1.406 µg/mL, according to the analyte. The accuracy, precision, and stability met with the acceptance criteria of the AOAC (Association of Official Analytical Chemists) International. According to these results, the described HPLC-MS/MS method is adequately sensitive, repeatable and suitable for the large-scale analysis of compounds in biological fluids. PMID:27754400

Optimization and validation of high-performance liquid chromatography method for analyzing 25-desacetyl rifampicin in human urine

NASA Astrophysics Data System (ADS)

Lily; Laila, L.; Prasetyo, B. E.

2018-03-01

A selective, reproducibility, effective, sensitive, simple and fast High-Performance Liquid Chromatography (HPLC) was developed, optimized and validated to analyze 25-Desacetyl Rifampicin (25-DR) in human urine which is from tuberculosis patient. The separation was performed by HPLC Agilent Technologies with column Agilent Eclipse XDB- Ci8 and amobile phase of 65:35 v/v methanol: 0.01 M sodium phosphate buffer pH 5.2, at 254 nm and flow rate of 0.8ml/min. The mean retention time was 3.016minutes. The method was linear from 2–10μg/ml 25-DR with a correlation coefficient of 0.9978. Standard deviation, relative standard deviation and coefficient variation of 2, 6, 10μg/ml 25-DR were 0-0.0829, 03.1752, 0-0.0317%, respectively. The recovery of 5, 7, 9μg/ml25-DR was 80.8661, 91.3480 and 111.1457%, respectively. Limits of detection (LoD) and quantification (LoQ) were 0.51 and 1.7μg/ml, respectively. The method has fulfilled the validity guidelines of the International Conference on Harmonization (ICH) bioanalytical method which includes parameters of specificity, linearity, precision, accuracy, LoD, and LoQ. The developed method is suitable for pharmacokinetic analysis of various concentrations of 25-DR in human urine.

Degradation Kinetics Study of Alogliptin Benzoate in Alkaline Medium by Validated Stability-Indicating HPTLC Method.

PubMed

Bodiwala, Kunjan Bharatkumar; Shah, Shailesh; Thakor, Jeenal; Marolia, Bhavin; Prajapati, Pintu

2016-11-01

A rapid, sensitive, and stability-indicating high-performance thin-layer chromatographic method was developed and validated to study degradation kinetics of Alogliptin benzoate (ALG) in an alkaline medium. ALG was degraded under acidic, alkaline, oxidative, and thermal stress conditions. The degraded samples were chromatographed on silica gel 60F254-TLC plates, developed using a quaternary-solvent system (chloroform-methanol-ethyl acetate-triethyl amine, 9+1+1+0.5, v/v/v/v), and scanned at 278 nm. The developed method was validated per International Conference on Harmonization guidelines using validation parameters such as specificity, linearity and range, precision, accuracy, LOD, and LOQ. The linearity range for ALG was 100-500 ng/band (correlation coefficient = 0.9997) with an average recovery of 99.47%. The LOD and LOQ for ALG were 9.8 and 32.7 ng/band, respectively. The developed method was successfully applied for the quantitative estimation of ALG in its synthetic mixture with common excipients. Degradation kinetics of ALG in an alkaline medium was studied by degrading it under three different temperatures and three different concentrations of alkali. Degradation of ALG in the alkaline medium was found to follow first-order kinetics. Contour plots have been generated to predict degradation rate constant, half-life, and shelf life of ALG in various combinations of temperature and concentration of alkali using Design Expert software.

Development of an Advanced HPLC-MS/MS Method for the Determination of Carotenoids and Fat-Soluble Vitamins in Human Plasma.

PubMed

Hrvolová, Barbora; Martínez-Huélamo, Miriam; Colmán-Martínez, Mariel; Hurtado-Barroso, Sara; Lamuela-Raventós, Rosa Maria; Kalina, Jiří

2016-10-14

The concentration of carotenoids and fat-soluble vitamins in human plasma may play a significant role in numerous chronic diseases such as age-related macular degeneration and some types of cancer. Although these compounds are of utmost interest for human health, methods for their simultaneous determination are scarce. A new high pressure liquid chromatography (HPLC)-tandem mass spectrometry (MS/MS) method for the quantification of selected carotenoids and fat-soluble vitamins in human plasma was developed, validated, and then applied in a pilot dietary intervention study with healthy volunteers. In 50 min, 16 analytes were separated with an excellent resolution and suitable MS signal intensity. The proposed HPLC-MS/MS method led to improvements in the limits of detection (LOD) and quantification (LOQ) for all analyzed compounds compared to the most often used HPLC-DAD methods, in some cases being more than 100-fold lower. LOD values were between 0.001 and 0.422 µg/mL and LOQ values ranged from 0.003 to 1.406 µg/mL, according to the analyte. The accuracy, precision, and stability met with the acceptance criteria of the AOAC (Association of Official Analytical Chemists) International. According to these results, the described HPLC-MS/MS method is adequately sensitive, repeatable and suitable for the large-scale analysis of compounds in biological fluids.

Pinaverium Bromide: Development and Validation of Spectrophotometric Methods for Assay and Dissolution Studies.

PubMed

Martins, Danielly da Fonte Carvalho; Florindo, Lorena Coimbra; Machado, Anna Karolina Mouzer da Silva; Todeschini, Vítor; Sangoi, Maximiliano da Silva

2017-11-01

This study presents the development and validation of UV spectrophotometric methods for the determination of pinaverium bromide (PB) in tablet assay and dissolution studies. The methods were satisfactorily validated according to International Conference on Harmonization guidelines. The response was linear (r2 > 0.99) in the concentration ranges of 2-14 μg/mL at 213 nm and 10-70 μg/mL at 243 nm. The LOD and LOQ were 0.39 and 1.31 μg/mL, respectively, at 213 nm. For the 243 nm method, the LOD and LOQ were 2.93 and 9.77 μg/mL, respectively. Precision was evaluated by RSD, and the obtained results were lower than 2%. Adequate accuracy was also obtained. The methods proved to be robust using a full factorial design evaluation. For PB dissolution studies, the best conditions were achieved using a United States Pharmacopeia Dissolution Apparatus 2 (paddle) at 50 rpm and with 900 mL 0.1 M hydrochloric acid as the dissolution medium, presenting satisfactory results during the validation tests. In addition, the kinetic parameters of drug release were investigated using model-dependent methods, and the dissolution profiles were best described by the first-order model. Therefore, the proposed methods were successfully applied for the assay and dissolution analysis of PB in commercial tablets.

Accuracy of a composite score using daily SAPS II and LOD scores for predicting hospital mortality in ICU patients hospitalized for more than 72 h.

PubMed

Timsit, J F; Fosse, J P; Troché, G; De Lassence, A; Alberti, C; Garrouste-Orgeas, M; Azoulay, E; Chevret, S; Moine, P; Cohen, Y

2001-06-01

In most databases used to build general severity scores the median duration of intensive care unit (ICU) stay is less than 3 days. Consequently, these scores are not the most appropriate tools for measuring prognosis in studies dealing with ICU patients hospitalized for more than 72 h. To develop a new prognostic model based on a general severity score (SAPS II), an organ dysfunction score (LOD) and evolution of both scores during the first 3 days of ICU stay. Prospective multicenter study. Twenty-eight intensive care units (ICUs) in France. A training data-set was created with four ICUs during an 18-month period (893 patients). Seventy percent of the patients were medical (628) aged 66 years. The median SAPS II was 38. The ICU and hospital mortality rates were 22.7% and 30%, respectively. Forty-seven percent (420 patients) were transferred from hospital wards. In this population, the calibration (Hosmer-Lemeshow chi-square: 37.4, P = 0.001) and the discrimination [area under the ROC curves: 0.744 (95 % CI: 0.714-0.773)] of the original SAPS II were relatively poor. A validation data set was created with a random panel of 24 French ICUs during March 1999 (312 patients). The LOD and SAPS II scores were calculated during the first (SAPS1, LOD1), second (SAPS2, LOD2), and third (SAPS3, LOD3) calendar days. The LOD and SAPS scores alterations were assigned the value "1" when scores increased with time and "0" otherwise. A multivariable logistic regression model was used to select variables measured during the first three calendar days, and independently associated with death. Selected variables were: SAPS II at admission [OR: 1.04 (95 % CI: 1.027-1.053) per point], LOD [OR: 1.16 (95 % CI: 1.085-1.253) per point], transfer from ward [OR: 1.74 (95 % CI: 1.25-2.42)], as well as SAPS3-SAPS2 alterations [OR: 1.516 (95 % CI: 1.04-2.22)], and LOD3-LOD2 alterations [OR: 2.00 (95 % CI: 1.29-3.11)]. The final model has good calibration and discrimination properties in the training data set [area under the ROC curve: 0.794 (95 % CI: 0.766-0.820), Hosmer-Lemeshow C statistic: 5.56, P = 0.7]. In the validation data set, the model maintained good accuracy [area under the ROC curve: 0.826 (95 % CI: 0.780-0.867), Hosmer-Lemeshow C statistic: 7.14, P = 0.5]. The new model using SAPS II and LOD and their evolution during the first calendar days has good discrimination and calibration properties. We propose its use for benchmarking and evaluating the over-risk of death associated with ICU-acquired nosocomial infections.

Estimation of the Length of Day (LOD) from DORIS observations

NASA Astrophysics Data System (ADS)

Štěpánek, Petr; Hugentobler, Urs; Buday, Michal; Filler, Vratislav

2018-07-01

The paper is devoted to the estimation of the Length of the Day (LOD) from DORIS observations and summarizes the first successful experiment with LOD estimation at the level of geodetic precision. This result is confirmed by 9 years of DORIS data (2006.0-2015.0). The mean difference of the non smoothed LOD series with respect to the IERS C04 model reaches a value of tens μs and a standard deviation around 120 μs for the last years of the campaign 2012.0-2015.0. However, the mean difference with respect to the reference model varies over time, reaching negative values from -60 to -20 μs for the years 2006-2011 and positive values from 80 to 120 μs for the years 2012-2014. The time variable mean difference with respect to the changes in DORIS satellite constellation is discussed, as well as the possibility of the bias reduction applying the long-term averages of the cross-track harmonics or adjustment of the geopotential coefficient C20. Moreover, the possibility of LOD adjustment in the standard DORIS solution is discussed with focus on the station coordinates estimation. In addition, the power spectrum of the difference between estimated LOD and the reference model was performed, showing the domination of the annual signal. Also LOD estimated from single-satellite DORIS solutions was analyzed to identify satellite-specific issues. The paper includes a correlation analysis of the orbit parameters, Earth rotation parameters and the geopotential coefficient C20, based on covariance matrices from weekly solutions. High correlation around 0.96 was found for LOD and the sine amplitude of the cross-track harmonic empirical acceleration, which was also confirmed analytically.

Theoretically Guided Analytical Method Development and Validation for the Estimation of Rifampicin in a Mixture of Isoniazid and Pyrazinamide by UV Spectrophotometer

PubMed Central

Khan, Mohammad F.; Rita, Shamima A.; Kayser, Md. Shahidulla; Islam, Md. Shariful; Asad, Sharmeen; Bin Rashid, Ridwan; Bari, Md. Abdul; Rahman, Muhammed M.; Al Aman, D. A. Anwar; Setu, Nurul I.; Banoo, Rebecca; Rashid, Mohammad A.

2017-01-01

A simple, rapid, economic, accurate, and precise method for the estimation of rifampicin in a mixture of isoniazid and pyrazinamide by UV spectrophotometeric technique (guided by the theoretical investigation of physicochemical properties) was developed and validated. Theoretical investigations revealed that isoniazid and pyrazinamide both were freely soluble in water and slightly soluble in ethyl acetate whereas rifampicin was practically insoluble in water but freely soluble in ethyl acetate. This indicates that ethyl acetate is an effective solvent for the extraction of rifampicin from a water mixture of isoniazid and pyrazinamide. Computational study indicated that pH range of 6.0–8.0 would favor the extraction of rifampicin. Rifampicin is separated from isoniazid and pyrazinamide at pH 7.4 ± 0.1 by extracting with ethyl acetate. The ethyl acetate was then analyzed at λmax of 344.0 nm. The developed method was validated for linearity, accuracy and precision according to ICH guidelines. The proposed method exhibited good linearity over the concentration range of 2.5–35.0 μg/mL. The intraday and inter-day precision in terms of % RSD ranged from 1.09 to 1.70% and 1.63 to 2.99%, respectively. The accuracy (in terms of recovery) of the method varied from of 96.7 ± 0.9 to 101.1 ± 0.4%. The LOD and LOQ were found to be 0.83 and 2.52 μg/mL, respectively. In addition, the developed method was successfully applied to determine rifampicin combination (isoniazid and pyrazinamide) brands available in Bangladesh. PMID:28503547

Theoretically Guided Analytical Method Development and Validation for the Estimation of Rifampicin in a Mixture of Isoniazid and Pyrazinamide by UV Spectrophotometer.

PubMed

Khan, Mohammad F; Rita, Shamima A; Kayser, Md Shahidulla; Islam, Md Shariful; Asad, Sharmeen; Bin Rashid, Ridwan; Bari, Md Abdul; Rahman, Muhammed M; Al Aman, D A Anwar; Setu, Nurul I; Banoo, Rebecca; Rashid, Mohammad A

2017-01-01

A simple, rapid, economic, accurate, and precise method for the estimation of rifampicin in a mixture of isoniazid and pyrazinamide by UV spectrophotometeric technique (guided by the theoretical investigation of physicochemical properties) was developed and validated. Theoretical investigations revealed that isoniazid and pyrazinamide both were freely soluble in water and slightly soluble in ethyl acetate whereas rifampicin was practically insoluble in water but freely soluble in ethyl acetate. This indicates that ethyl acetate is an effective solvent for the extraction of rifampicin from a water mixture of isoniazid and pyrazinamide. Computational study indicated that pH range of 6.0-8.0 would favor the extraction of rifampicin. Rifampicin is separated from isoniazid and pyrazinamide at pH 7.4 ± 0.1 by extracting with ethyl acetate. The ethyl acetate was then analyzed at λ max of 344.0 nm. The developed method was validated for linearity, accuracy and precision according to ICH guidelines. The proposed method exhibited good linearity over the concentration range of 2.5-35.0 μg/mL. The intraday and inter-day precision in terms of % RSD ranged from 1.09 to 1.70% and 1.63 to 2.99%, respectively. The accuracy (in terms of recovery) of the method varied from of 96.7 ± 0.9 to 101.1 ± 0.4%. The LOD and LOQ were found to be 0.83 and 2.52 μg/mL, respectively. In addition, the developed method was successfully applied to determine rifampicin combination (isoniazid and pyrazinamide) brands available in Bangladesh.

Determination of catechins and caffeine in camillia sinensis raw materials, extracts, and dietary supplements by HPLC-uv: single-laboratory validation.

PubMed

Roman, Mark C

2013-01-01

A rapid method has been developed to quantify seven catechins and caffeine in green tea (Camillia sinensis) raw material and powdered extract, and dietary supplements containing green tea extract. The method utilizes RP HPLC with a phenyl-based stationary phase and gradient elution. Detection is by UV absorbance. The total run time, including column re-equilibration, is 13 min. Single-laboratory validation (SLV) has been performed on the method to determine the repeatability, accuracy, selectivity, LOD, LOQ, ruggedness, and linearity for (+)-catechin, (-)-epicatechin, (-)-epicatechin gallate, (-)-epigallocatechin, (-)-gallocatechin gallate, (-)-epigallocatechin gallate, and (+)-gallocatechin, as well as caffeine. Repeatability precision and recovery results met AOAC guidelines for SLV studies for all catechins and caffeine down to a level of approximately 20 mg/g. Finished products containing high concentrations of minerals require the use of EDTA to prevent decomposition of the catechins.

Qualitative and quantitative determination of extractives in heartwood of Scots pine (Pinus sylvestris L.) by gas chromatography.

PubMed

Ekeberg, Dag; Flaete, Per-Otto; Eikenes, Morten; Fongen, Monica; Naess-Andresen, Carl Fredrik

2006-03-24

A method for quantitative determination of extractives from heartwood of Scots pine (Pinus sylvestris L.) using gas chromatography (GC) with flame ionization detection (FID) was developed. The limit of detection (LOD) was 0.03 mg/g wood and the linear range (r = 0.9994) was up to 10 mg/g with accuracy within +/- 10% and precision of 18% relative standard deviation. The identification of the extractives was performed using gas chromatography combined with mass spectrometry (GC-MS). The yields of extraction by Soxhlet were tested for solid wood, small particles and fine powder. Small particles were chosen for further analysis. This treatment gave good yields of the most important extractives: pinosylvin, pinosylvin monomethyl ether, resin acids and free fatty acids. The method is used to demonstrate the variation of these extractives across stems and differences in north-south direction.

Determination of pesticides in coconut (Cocos nucifera Linn.) water and pulp using modified QuEChERS and LC-MS/MS.

PubMed

Ferreira, Jordana Alves; Ferreira, Joana Maria Santos; Talamini, Viviane; Facco, Janice de Fátima; Rizzetti, Tiele Medianeira; Prestes, Osmar Damian; Adaime, Martha Bohrer; Zanella, Renato; Bottoli, Carla Beatriz Grespan

2016-12-15

The use of pesticides is directly linked to improvements in productivity and to the preservation of coconut palms. However pesticide analysis is necessary to determine whether pesticide residues in the food products containing coconut are within the maximum residue limits (MRLs), ensuring the quality of these products. This work aimed to develop a method for multiresidue determination of ten pesticides in coconut water and pulp using QuEChERS and LC-MS/MS. The method was effective in terms of selectivity, linearity, matrix effect, accuracy and precision, providing LOD of 3μgkg(-1), LOQ of 10μgkg(-1) and recoveries between 70 and 120% with RSD lower than 20%. The developed method was applied to 36 samples in which residues of carbendazim, carbofuran, cyproconazole and thiabendazole were found below the LOQ in coconut water and pulp. Copyright © 2016 Elsevier Ltd. All rights reserved.

High-performance liquid chromatographic assay for the determination of Aloe Emodin in mouse plasma.

PubMed

Zaffaroni, M; Mucignat, C; Pecere, T; Zagotto, G; Frapolli, R; D'Incalci, M; Zucchetti, M

2003-10-25

An isocratic high-performance liquid chromatography (HPLC) method was developed and validated to determine Aloe Emodin (AE) in mouse plasma. The analysis required 0.3 ml of plasma and involves extraction with dichloromethane. The HPLC separation was carried out on Symmetry Shield RP18, a mobile phase of methanol-water-acetic acid (65:35:0.2) and fluorescence detection at lambda(ex)=410 nm and lambda(em)=510 nm. The retention time of AE was 11.7 min. The assay was linear from 10 to 1,000 ng/ml (r2 > or = 0.999), showed intra- and inter-day precision within 7.8 and 4.7%, and accuracy of 87.3-105.7%. Detection limit (LOD) and quantification limit (LOQ) were 4.5 and 5 ng/ml, respectively. The method was applied to determine for the first time the pharmacokinetic of AE in mice.

a Framework for Architectural Heritage Hbim Semantization and Development

NASA Astrophysics Data System (ADS)

Brusaporci, S.; Maiezza, P.; Tata, A.

2018-05-01

Despite the recognized advantages of the use of BIM in the field of architecture and engineering, the extension of this procedure to the architectural heritage is neither immediate nor critical. The uniqueness and irregularity of historical architecture, on the one hand, and the great quantity of information necessary for the knowledge of architectural heritage, on the other, require appropriate reflections. The aim of this paper is to define a general framework for the use of BIM procedures for architectural heritage. The proposed methodology consists of three different Level of Development (LoD), depending on the characteristics of the building and the objectives of the study: a simplified model with a low geometric accuracy and a minimum quantity of information (LoD 200); a model nearer to the reality but, however, with a high deviation between virtual and real model (LoD 300); a detailed BIM model that reproduce as much as possible the geometric irregularities of the building and is enriched by the maximum quantity of information available (LoD 400).

A Fast and Validated Reversed-Phase HPLC Method for Simultaneous Determination of Simvastatin, Atorvastatin, Telmisartan and Irbesartan in Bulk Drugs and Tablet Formulations

PubMed Central

Alhazmi, Hassan A.; Alnami, Ahmed M.; Arishi, Mohammed A. A.; Alameer, Raad K.; Al Bratty, Mohammed; Rehman, Zia ur; Javed, Sadique A.; Arbab, Ismail A.

2017-01-01

The aim of this study was to develop and validate a fast and simple reversed-phase HPLC method for simultaneous determination of four cardiovascular agents—atorvastatin, simvastatin, telmisartan and irbesartan in bulk drugs and tablet oral dosage forms. The chromatographic separation was accomplished by using Symmetry C18 column (75 mm × 4.6 mm; 3.5 μ) with a mobile phase consisting of ammonium acetate buffer (10 mM; pH 4.0) and acetonitrile in a ratio 40:60 v/v. Flow rate was maintained at 1 mL/min up to 3.5 min, and then suddenly changed to 2 mL/min till the end of the run (7.5 min). The data was acquired using ultraviolet detector monitored at 220 nm. The method was validated for linearity, precision, accuracy and specificity. The developed method has shown excellent linearity (R2 > 0.999) over the concentration range of 1–16 µg/mL. The limits of detection (LODs) and limits of quantification (LOQs) were in the range of 0.189–0.190 and 0.603–0.630 µg/mL, respectively. Inter-day and intra-day accuracy and precision data were recorded in the acceptable limits. The new method has successfully been applied for quantification of all four drugs in their tablet dosage forms with percent recovery within 100 ± 2%. PMID:29257120

A digital enzyme-linked immunosorbent assay for ultrasensitive measurement of amyloid-β 1-42 peptide in human plasma with utility for studies of Alzheimer's disease therapeutics.

PubMed

Song, Linan; Lachno, D Richard; Hanlon, David; Shepro, Adam; Jeromin, Andreas; Gemani, Dipika; Talbot, Jayne A; Racke, Margaret M; Dage, Jeffrey L; Dean, Robert A

2016-12-15

Amyloid-β 1-42 peptide (Aβ 1-42 ) is associated with plaque formation in the brain of patients with Alzheimer's disease (AD). Pharmacodynamic studies of AD therapeutics that lower the concentrations of Aβ 1-42 in peripheral blood require highly sensitive assays for its measurement. A digital enzyme-linked immunosorbent assay (ELISA) using single molecule array (Simoa) technology has been developed that provides improved sensitivity compared with conventional ELISA methods using the same antibody reagents. A sensitive digital ELISA for measurement of Aβ 1-42 using antibodies 3D6 and 21F12 was developed. Assay performance was evaluated by repeated testing of pooled human plasma and buffer diluent quality control samples to determine relative accuracy, intra- and inter-assay precision, limit of detection (LOD), lower limit of quantification (LLOQ), dilutional linearity, and spike recovery. The optimized assay was used to quantify Aβ 1-42 in clinical samples from patients treated with the β-site amyloid precursor protein cleaving enzyme 1 inhibitor LY2886721. The prototype assay measured Aβ 1-42 with an LOD of 0.3 pg/ml and an LLOQ of 2.8 pg/ml in plasma, calibrated using an Aβ 1-42 peptide standard from Fujirebio. Assay precision was acceptable with intra- and inter-assay coefficients of variation both being ≤10%. Dilutional linearity was demonstrated in sample diluent and immunodepleted human plasma. Analyte spike recovery ranged from 51% to 93% with a mean of 80%. This assay was able to quantify Aβ 1-42 in all of the 84 clinical samples tested. A rapid reduction in levels of Aβ 1-42 was detected within 1 h after drug treatment, and a dose-dependent decrease of Aβ 1-42 levels was also observed over the time course of sample collection. This digital ELISA has potential utility in clinical applications for quantification of Aβ 1-42 in plasma where high sensitivity and precision are required.

EOP and scale from continuous VLBI observing: CONT campaigns to future VGOS networks

NASA Astrophysics Data System (ADS)

MacMillan, D. S.

2017-07-01

Continuous (CONT) VLBI campaigns have been carried out about every 3 years since 2002. The basic idea of these campaigns is to acquire state-of-the-art VLBI data over a continuous time period of about 2 weeks to demonstrate the highest accuracy of which the current VLBI system is capable. In addition, these campaigns support scientific studies such as investigations of high-resolution Earth rotation, reference frame stability, and daily to sub-daily site motions. The size of the CONT networks and the observing data rate have increased steadily since 1994. Performance of these networks based on reference frame scale precision and polar motion/LOD comparison with global navigation satellite system (GNSS) earth orientation parameters (EOP) has been substantially better than the weekly operational R1 and R4 series. The precisions of CONT EOP and scale have improved by more than a factor of two since 2002. Polar motion precision based on the WRMS difference between VLBI and GNSS for the most recent CONT campaigns is at the 30 μas level, which is comparable to that of GNSS. The CONT campaigns are a natural precursor to the planned future VLBI observing networks, which are expected to observe continuously. We compare the performance of the most recent CONT campaigns in 2011 and 2014 with the expected performance of the future VLBI global observing system network using simulations. These simulations indicate that the expected future precision of scale and EOP will be at least 3 times better than the current CONT precision.

Determination of Bile Acids in Piglet Bile by Solid Phase Extraction and Liquid Chromatography-Electrospray Tandem Mass Spectrometry.

PubMed

Mi, Si; Lim, David W; Turner, Justine M; Wales, Paul W; Curtis, Jonathan M

2016-03-01

An LC/MS/MS-based method was developed for the determination of individual bile acids (BA) and their conjugates in porcine bile samples. The C18-based solid-phase extraction (SPE) procedure was optimized so that all 19 target BA and their glycine and taurine conjugates were collected with high recoveries for standards (89.1-100.2%). Following this, all 19 compounds were separated and quantified in a single 12 min chromatographic run. The method was validated in terms of linearity, sensitivity, accuracy, precision, and recovery. An LOD in the low ppb range with measured precisions in the range of 0.5-9.3% was achieved. The recoveries for all of the 19 analytes in bile samples were all >80%. The validated method was successfully applied to the profiling of BA and their conjugates in the bile from piglets treated with exogenous glucagon-like peptide-2 (GLP-2) in a preclinical model of neonatal parenteral nutrition-associated liver disease (PNALD). The method developed is rapid and could be easily implemented for routine analysis of BA and their conjugates in other biofluids or tissues.

A preliminary study on identification of Thai rice samples by INAA and statistical analysis

NASA Astrophysics Data System (ADS)

Kongsri, S.; Kukusamude, C.

2017-09-01

This study aims to investigate the elemental compositions in 93 Thai rice samples using instrumental neutron activation analysis (INAA) and to identify rice according to their types and rice cultivars using statistical analysis. As, Mg, Cl, Al, Br, Mn, K, Rb and Zn in Thai jasmine rice and Sung Yod rice samples were successfully determined by INAA. The accuracy and precision of the INAA method were verified by SRM 1568a Rice Flour. All elements were found to be in a good agreement with the certified values. The precisions in term of %RSD were lower than 7%. The LODs were obtained in range of 0.01 to 29 mg kg-1. The concentration of 9 elements distributed in Thai rice samples was evaluated and used as chemical indicators to identify the type of rice samples. The result found that Mg, Cl, As, Br, Mn, K, Rb, and Zn concentrations in Thai jasmine rice samples are significantly different but there was no evidence that Al is significantly different from concentration in Sung Yod rice samples at 95% confidence interval. Our results may provide preliminary information for discrimination of rice samples and may be useful database of Thai rice.

Determination of residual cell culture media components by MEKC.

PubMed

Zhang, Junge; Chakraborty, Utpal; Foley, Joe P

2009-11-01

Folic acid, hypoxanthine, mycophenolic acid, nicotinic acid, riboflavin, and xanthine are widely used as cell culture media components in monoclonal antibody manufacturing. These components are subsequently removed during the downstream purification processes. This article describes a single MEKC method that can simultaneously determine all the listed compounds with acceptable LOD and LOQ. All the analytes were successfully separated by MEKC using running buffer containing 40 mM SDS, 20 mM sodium phosphate, and 20 mM sodium borate at pH 9.0. The MEKC method was compared to the corresponding CZE method using the same running buffer containing no SDS. The effect of SDS concentration on separation, the pH of the running buffer, and the detection wavelength were studied and optimal MEKC conditions were established. Good linearity was obtained with correlation coefficients of more than 0.99 for all analytes. Specificity, accuracy, and precision were also evaluated. The recovery was in the range of 89-112%. The precision results were in the range of 1.7-4.8%. The experimentally determined data demonstrated that the MEKC method is applicable to the determination of the six analytes in in-process samples from monoclonal antibody manufacturing processes.

Comprehensive determination of flavouring additives and nicotine in e-cigarette refill solutions. Part I: Liquid chromatography-tandem mass spectrometry analysis.

PubMed

Aszyk, Justyna; Kubica, Paweł; Kot-Wasik, Agata; Namieśnik, Jacek; Wasik, Andrzej

2017-10-13

Liquid chromatography-tandem mass spectrometry with electrospray ionization (HPLC-ESI-MS/MS) methods were developed for the simultaneous determination of 42 flavouring compounds and nicotine in liquids for e-cigarettes. The chromatographic separation was performed using an Ace ® Ultracore™ SuperC18™ (100×2.1mm, 2.5μm) column in both acidic and alkaline pH conditions to separate all the compounds. A simple "dilute & shoot" approach was used for the sample preparation. The method validation was performed by evaluating key analytical parameters such as linearity, accuracy, selectivity, precision, limit of detection (LOD) and limit of quantification (LOQ). The calibration curves showed good linearity within the specific ranges for the investigated compounds with correlation coefficients greater than 0.990 in each case. The recovery for all the investigated compounds varied from 89% to 110%. The intra- and inter-day precision were within the acceptable limits (±15%) at all tested concentrations. The applicability of the methods was examined by analysing 25 liquid samples from e-cigarettes commercially available on the Polish market. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of phenolic compounds derived from hydrolysable tannins in biological matrices by RP-HPLC.

PubMed

Díez, María Teresa; García del Moral, Pilar; Resines, José Antonio; Arín, María Jesús

2008-08-01

An RP-HPLC method for the determination of four phenolic compounds: gallic acid (GA), pyrogallol (PY), resorcinol (RE) and ellagic acid (EA), derived from hydrolysable tannins is reported. Separation was achieved on a SunFire C18 (250 x 4.6 mm id, 5 microm) column at 40 degrees C with gradient elution. UV detection at 280 nm was applied. The developed method was validated in terms of linearity, accuracy and precision. Satisfactory repeatability and between day precision were noticed with RSD values lower than 3%. Recoveries from different biological samples ranged from 91.50 to 105.25%. The LODs were estimated as 1.70 mg/L for PY, 1.68 mg/L for GA, 1.52 mg/L for RE and 0.98 mg/L for EA with a 20 microL injection volume. The method was applied for the determination of these compounds in oak leaves and in ruminal fluid and urine samples taken from beef cattle fed with oak leaves. The proposed method could be used in ruminant nutrition studies to verify the effect that a diet rich in tannins have on ruminal fermentation and to determine the toxicity of these compounds.

Development and validation of a HPTLC method for simultaneous estimation of lornoxicam and thiocolchicoside in combined dosage form

PubMed Central

Sahoo, Madhusmita; Syal, Pratima; Hable, Asawaree A.; Raut, Rahul P.; Choudhari, Vishnu P.; Kuchekar, Bhanudas S.

2011-01-01

Aim: To develop a simple, precise, rapid and accurate HPTLC method for the simultaneous estimation of Lornoxicam (LOR) and Thiocolchicoside (THIO) in bulk and pharmaceutical dosage forms. Materials and Methods: The separation of the active compounds from pharmaceutical dosage form was carried out using methanol:chloroform:water (9.6:0.2:0.2 v/v/v) as the mobile phase and no immiscibility issues were found. The densitometric scanning was carried out at 377 nm. The method was validated for linearity, accuracy, precision, LOD (Limit of Detection), LOQ (Limit of Quantification), robustness and specificity. Results: The Rf values (±SD) were found to be 0.84 ± 0.05 for LOR and 0.58 ± 0.05 for THIO. Linearity was obtained in the range of 60–360 ng/band for LOR and 30–180 ng/band for THIO with correlation coefficients r2 = 0.998 and 0.999, respectively. The percentage recovery for both the analytes was in the range of 98.7–101.2 %. Conclusion: The proposed method was optimized and validated as per the ICH guidelines. PMID:23781452

Sensitive determination of dopamine levels via surface-enhanced Raman scattering of Ag nanoparticle dimers.

PubMed

Yu, Xiantong; He, XiaoXiao; Yang, Taiqun; Zhao, Litao; Chen, Qichen; Zhang, Sanjun; Chen, Jinquan; Xu, Jianhua

2018-01-01

Dopamine (DA) is an important neurotransmitter in the hypothalamus and pituitary gland, which can produce a direct influence on mammals' emotions in midbrain. Additionally, the level of DA is highly related with some important neurologic diseases such as schizophrenia, Parkinson, and Huntington's diseases, etc. In light of the important roles that DA plays in the disease modulation, it is of considerable significance to develop a sensitive and reproducible approach for monitoring DA. The objective of this study was to develop an efficient approach to quantitatively monitor the level of DA using Ag nanoparticle (NP) dimers and enhanced Raman spectroscopy. Ag NP dimers were synthesized for the sensitive detection of DA via surface-enhanced Raman scattering (SERS). Citrate was used as both the capping agent of NPs and sensing agent to DA, which is self-assembled on the surface of Ag NP dimers by reacting with the surface carboxyl group to form a stable amide bond. To improve accuracy and precision, the multiplicative effects model for surface-enhanced Raman spectroscopy was utilized to analyze the SERS assays. A low limits of detection (LOD) of 20 pM and a wide linear response range from 30 pM to 300 nM were obtained for DA quantitative detection. The SERS enhancement factor was theoretically valued at approximately 10 7 by discrete dipole approximation. DA was self-assembled on the citrate capped surface of Ag NPs dimers through the amide bond. The adsorption energy was estimated to be 256 KJ/mol using the Langmuir isotherm model. The density functional theory was used to simulate the spectral characteristics of SERS during the adsorption of DA on the surface of the Ag dimers. Furthermore, to improve the accuracy and precision of quantitative analysis of SERS assays with a multiplicative effects model for surface-enhanced Raman spectroscopy. A LOD of 20 pM DA-level was obtained, and the linear response ranged from 30 pM to 300 nM for quantitative DA detection. The absolute relative percentage error was 4.22% between the real and predicted DA concentrations. This detection scheme is expected to have good applications in the prevention and diagnosis of certain diseases caused by disorders in the DA level.

Sensitive determination of dopamine levels via surface-enhanced Raman scattering of Ag nanoparticle dimers

PubMed Central

Yu, Xiantong; He, XiaoXiao; Yang, Taiqun; Zhao, Litao; Chen, Qichen; Zhang, Sanjun; Chen, Jinquan; Xu, Jianhua

2018-01-01

Background Dopamine (DA) is an important neurotransmitter in the hypothalamus and pituitary gland, which can produce a direct influence on mammals’ emotions in midbrain. Additionally, the level of DA is highly related with some important neurologic diseases such as schizophrenia, Parkinson, and Huntington’s diseases, etc. In light of the important roles that DA plays in the disease modulation, it is of considerable significance to develop a sensitive and reproducible approach for monitoring DA. Purpose The objective of this study was to develop an efficient approach to quantitatively monitor the level of DA using Ag nanoparticle (NP) dimers and enhanced Raman spectroscopy. Methods Ag NP dimers were synthesized for the sensitive detection of DA via surface-enhanced Raman scattering (SERS). Citrate was used as both the capping agent of NPs and sensing agent to DA, which is self-assembled on the surface of Ag NP dimers by reacting with the surface carboxyl group to form a stable amide bond. To improve accuracy and precision, the multiplicative effects model for surface-enhanced Raman spectroscopy was utilized to analyze the SERS assays. Results A low limits of detection (LOD) of 20 pM and a wide linear response range from 30 pM to 300 nM were obtained for DA quantitative detection. The SERS enhancement factor was theoretically valued at approximately 107 by discrete dipole approximation. DA was self-assembled on the citrate capped surface of Ag NPs dimers through the amide bond. The adsorption energy was estimated to be 256 KJ/mol using the Langmuir isotherm model. The density functional theory was used to simulate the spectral characteristics of SERS during the adsorption of DA on the surface of the Ag dimers. Furthermore, to improve the accuracy and precision of quantitative analysis of SERS assays with a multiplicative effects model for surface-enhanced Raman spectroscopy. Conclusion A LOD of 20 pM DA-level was obtained, and the linear response ranged from 30 pM to 300 nM for quantitative DA detection. The absolute relative percentage error was 4.22% between the real and predicted DA concentrations. This detection scheme is expected to have good applications in the prevention and diagnosis of certain diseases caused by disorders in the DA level. PMID:29713165

An LC-MS/MS method for the simultaneous determination of 15 antipsychotics and two metabolites in hair and its application to rat hair.

PubMed

Sim, Juhyun; Kim, Eunmi; Yang, Wonkyung; Woo, Sanghee; In, Sangwhan

2017-05-01

In recent years, the inappropriate use of antipsychotics by young Korean men has become a social problem. As military service exemptions are given for mental illness, some men pose as mental health patients to avoid military service. In order to verify the authenticity of mental illnesses, we developed simultaneous analytical methods for the detection of 15 antipsychotics and 2 of their metabolites in hair using liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. The target drugs were modafinil, atomoxetine, aripiprazole, benztropine, buspirone, duloxetine, gabapentin, oxcarbazepine, topiramate, escitalopram, paliperidone, ziprasidone, lamotrigine, clonazepam, levetiracetam, and metabolites of oxcarbazepine and clonazepam. To remove possible contaminants on the hair surface, hair samples were washed twice with methanol and distilled water, and then were extracted with methanol overnight at 38°C. Desipramine-d 3 was used as an internal standard. LC-MS/MS analysis was performed on an Agilent 1290 Infinity UHPLC coupled to an AB Sciex Qtrap ® 5500 MS/MS. The total chromatographic run time was 14min. The following validation parameters were evaluated: selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, matrix effect, and recovery. The LOD and LOQ values for all analytes, except modafinil, ranged from 0.2 to 10pg/mg hair and from 0.2 to 20pg/mg hair, respectively. Good linearity was achieved for most of the analytes in the range of 20-200pg/mg hair. The method showed acceptable precision and accuracy, which were less than 15%, as well as satisfactory matrix effects and recoveries. Furthermore, this method was also applied to the analysis of rat hair samples. The study in rats showed that the concentrations of atomoxetine and aripiprazole in pigmented hair were significantly higher than those in non-pigmented hair. However, no significant difference was observed in the concentration of topiramate between pigmented and non-pigmented hair. This method will be useful in monitoring the inappropriate use of antipsychotics in suspects posing as mental health patients. However, further research is necessary before applying this method to authentic hair samples from mental health patients. Copyright © 2017 Elsevier B.V. All rights reserved.

ERP-Variations on Time Scales Between Hours and Months Derived From GNSS Observations

NASA Astrophysics Data System (ADS)

Weber, R.; Englich, S.; Mendes Cerveira, P.

2007-05-01

Current observations gained by the space geodetic techniques, especially VLBI, GPS and SLR, allow for the determination of Earth Rotation Parameters (ERPs - polar motion, UT1/LOD) with unprecedented accuracy and temporal resolution. This presentation focuses on contributions to the ERP recovery provided by satellite navigation systems (primarily GPS). The IGS (International GNSS Service), for example, currently provides daily polar motion with an accuracy of less than 0.1mas and LOD estimates with an accuracy of a few microseconds. To study more rapid variations in polar motion and LOD we established in a first step a high resolution (hourly resolution) ERP-time series from GPS observation data of the IGS network covering the year 2005. The calculations were carried out by means of the Bernese GPS Software V5.0 considering observations from a subset of 113 fairly stable stations out of the IGS05 reference frame sites. From these ERP time series the amplitudes of the major diurnal and semidiurnal variations caused by ocean tides are estimated. After correcting the series for ocean tides the remaining geodetic observed excitation is compared with variations of atmospheric excitation (AAM). To study the sensitivity of the estimates with respect to the applied mapping function we applied both the widely used NMF (Niell Mapping Function) and the VMF1 (Vienna Mapping Function 1). In addition, based on computations covering two months in 2005, the potential improvement due to the use of additional GLONASS data will be discussed.

Effect of sample preparation method on quantification of polymorphs using PXRD.

PubMed

Alam, Shahnwaz; Patel, Sarsvatkumar; Bansal, Arvind Kumar

2010-01-01

The purpose of this study was to improve the sensitivity and accuracy of quantitative analysis of polymorphic mixtures. Various techniques such as hand grinding and mixing (in mortar and pestle), air jet milling and ball milling for micronization of particle and mixing were used to prepare binary mixtures. Using these techniques, mixtures of form I and form II of clopidogrel bisulphate were prepared in various proportions from 0-5% w/w of form I in form II and subjected to x-ray powder diffraction analysis. In order to obtain good resolution in minimum time, step time and step size were varied to optimize scan rate. Among the six combinations, step size of 0.05 degrees with step time of 5 s demonstrated identification of maximum characteristic peaks of form I in form II. Data obtained from samples prepared using both grinding and mixing in ball mill showed good analytical sensitivity and accuracy compared to other methods. Powder x-ray diffraction method was reproducible, precise with LOD of 0.29% and LOQ of 0.91%. Validation results showed excellent correlation between actual and predicted concentration with R2 > 0.9999.

Simultaneous determination of multiclass preservatives including isothiazolinones and benzophenone-type UV filters in household and personal care products by micellar electrokinetic chromatography.

PubMed

Lopez-Gazpio, Josu; Garcia-Arrona, Rosa; Millán, Esmeralda

2015-04-01

In this work, a simple and reliable micellar electrokinetic chromatography method for the separation and quantification of 14 preservatives, including isothiazolinones, and two benzophenone-type UV filters in household, cosmetic and personal care products was developed. The selected priority compounds are widely used as ingredients in many personal care products, and are included in the European Regulation concerning cosmetic products. The electrophoretic separation parameters were optimized by means of a modified chromatographic response function in combination with an experimental design, namely a central composite design. After optimization of experimental conditions, the BGE selected for the separation of the targets consisted of 60 mM SDS, 18 mM sodium tetraborate, pH 9.4 and 10% v/v methanol. The MEKC method was checked in terms of linearity, LODs and quantification, repeatability, intermediate precision, and accuracy, providing appropriate values (i.e. R(2) ≥ 0.992, repeatability RSD values ˂9%, and accuracy 90-115%). Applicability of the validated method was successfully assessed by quantifying preservatives and UV filters in commercial consumer products. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Slurry micro-sampling technique for use in argon-helium microwave induced plasma optical emission spectrometry.

PubMed

Ślachciński, Mariusz

2016-12-01

The Flow Focusing Pneumatic Nebulizer (FFPN) working at low liquid flow rates was evaluated for the elemental analysis in slurried samples by argon-helium microwave induced plasma optical emission spectrometry (MIP-OES). The obtained results achieved were compared with commercially available V-groove Babington type nebulizer (VBPN). A univariate approach and the simplex optimization procedure were used to achieve optimized conditions and derive analytical figures of merit. Analytical performance of the micro nebulization system was characterized by a determination of the limits of detection (LODs), the precision (RSDs) and the wash-out times for Ba, Ca, Cd, Cu, Fe, Mg, Mn, Pb and Sr. The experimental concentration detection limits for simultaneous determination, calculated as the concentration giving a signal equal to three times of the standard deviation of the blank (LOD, 3σ blank criterion, peak height) were 0.9, 0.2, 0.3, 0.2, 0.3, 0.1, 0.2, 0.4, 0.4 and 0.3ngmL -1 for Ba, Ca, Cd, Cu, Fe, Mg, Mn, Pb and Sr, respectively. The method offers relatively good precision (RSD ranged from 5% to 8%) for micro-slurry sampling analysis. Analyses of the certified reference materials (NRCC DOLT-2, GBW 07302 and SRM 2710) were performed in order to determine the accuracy available with the presented nebulization systems. The measured contents of elements in the reference materials were in satisfactory agreement with the certified values. In addition, these elements were determined in two real samples. Slurry concentration up to 3% m/v (particles <20μm), prepared in 10% m/v HCl through the application of ultrasonic agitation, was used with calibration by the standard addition technique. An ultrasonic probe was used to homogenize the slurry in the polypropylene bottle just before its introduction into the nebulizer. The nebulizers exhibited no clogging problems. Copyright © 2016 Elsevier B.V. All rights reserved.

Application of a validated stability-indicating densitometric thin-layer chromatographic method to stress degradation studies on moxifloxacin.

PubMed

Motwani, Sanjay K; Khar, Roop K; Ahmad, Farhan J; Chopra, Shruti; Kohli, K; Talegaonkar, S

2007-01-16

A simple, sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic (HPTLC) method for densitometric determination of moxifloxacin both as a bulk drug and from pharmaceutical formulation was developed and validated as per the International Conference on Harmonization (ICH) guidelines. The method employed TLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase and the mobile phase consisted of n-propanol-ethanol-6M ammonia solution (4:1:2, v/v/v). Densitometric analysis of moxifloxacin was carried out in the absorbance mode at 298 nm. Compact spots for moxifloxacin were found at R(f) value of 0.58+/-0.02. The linear regression analysis data for the calibration plots showed good linear relationship with r=0.9925 in the working concentration range of 100-800 ng spot(-1). The method was validated for precision, accuracy, ruggedness, robustness, specificity, recovery, limit of detection (LOD) and limit of quantitation (LOQ). The LOD and LOQ were 3.90 and 11.83 ng spot(-1), respectively. Drug was subjected to acid and alkali hydrolysis, oxidation, dry heat, wet heat treatment and photodegradation. All the peaks of degradation products were well resolved from the standard drug with significantly different R(f) values. Statistical analysis proves that the developed HPTLC method is reproducible and selective. As the method could effectively separate the drug from its degradation products, it can be employed as stability-indicating one. Moreover, the proposed HPTLC method was utilized to investigate the kinetics of the acidic and alkaline degradation processes at different temperatures. Arrhenius plot was constructed and apparent pseudo-first-order rate constant, half-life and activation energy were calculated. In addition the pH-rate profile for degradation of moxifloxacin in constant ionic strength buffer solutions within the pH range 1.2-10.8 was studied.

Development and validation of an LC-MS/MS analysis for simultaneous determination of delphinidin-3-glucoside, cyanidin-3-glucoside and cyanidin-3-(6-malonylglucoside) in human plasma and urine after blood orange juice administration.

PubMed

Giordano, Lucia; Coletta, Walter; Rapisarda, Paolo; Donati, Maria Benedetta; Rotilio, Domenico

2007-12-01

Blood orange juice has a high content in anthocyanins, especially represented by delphinidin-3-glucoside (D3G), cyanidin-3-glucoside (C3G) and cyanidin-3-(6-malonylglucoside) (CMG). An LC-MS/MS method for the simultaneous determination of D3G and C3G in human plasma and urine was developed and validated. After sample preparation by SPE, chromatographic separation was performed with an RP-C(18) column, using a water/methanol linear gradient. The quantitation of target compounds was determined by multiple reaction monitoring (MRM) mode, using ESI. The method showed good selectivity, sensitivity (LOD = 0.05 and 0.10 ng/mL for C3G in plasma and urine, respectively; LOD = 0.10 ng/mL for D3G in plasma and urine), linearity (0.20-200 ng/mL; r >or= 0.998), intra- and interday precision and accuracy (

Ultrasensitive colorimetric immunoassay for hCG detection based on dual catalysis of Au@Pt core-shell nanoparticle functionalized by horseradish peroxidase

NASA Astrophysics Data System (ADS)

Wang, Weiguo; Zou, Yake; Yan, Jinwu; Liu, Jing; Chen, Huixiong; Li, Shan; Zhang, Lei

2018-03-01

In this paper, an ultrasensitive colorimetric biosensor for human chorionic gonadotrophin (hCG) detection was designed from bottom-up method based on the dual catalysis of the horseradish peroxidase (HRP) and Au@Pt nanoparticles (NPs) relative to H2O2-TEM system. HRP and monoclonal mouse anti-hCG antibody (β-submit, mAb1) were co-immobilized onto the Au@Pt NP surface to improve catalytic efficiency and specificity, which formed a dual functionalized Au@Pt-HRP probe with the mean size of 42.8 nm (D50). The colorimetric immunoassay was developed for the hCG detection, and the Au@Pt-HRP probe featured a higher sensitivity in the concentration range of 0.4-12.8 IU L- 1 with a low limit of detection (LOD) of 0.1 IU L- 1 compared with the LODs of 0.8 IU L- 1 for BA-ELISA and of 2.0 IU L- 1 for Au@Pt, which indicated that the Au@Pt-HRP probe possessed higher catalytic efficiency with 2.8-fold increase over Au@Pt and 33.8-fold increase over HRP. Also, the Au@Pt-HRP probe exhibited good precision and reproducibility, high specificity and acceptable accuracy with CV being less than 15%. The dual functionalized Au@Pt-HRP probe as a type of signal amplified method was firstly applied in the colorimetric immunoassay for the hCG detection.

Analysis of 3-MCPD and 1,3-DCP in Various Foodstuffs Using GC-MS

PubMed Central

Kim, Wooseok; Jeong, Yun A; On, Jiwon; Choi, Ari; Lee, Jee-yeon; Lee, Joon Goo; Lee, Kwang-Geun

2015-01-01

3-Monochloro-1,2-propanediol (3-MCPD) and 1,3-dichloro-2-propanol (1,3-DCP) are not only produced in the manufacturing process of foodstuffs such as hydrolyzed vegetable proteins and soy sauce but are also formed by heat processing in the presence of fat and low water activity. 3-MCPD exists both in free and ester forms, and the ester form has been also detected in various foods. Free 3-MCPD and 1,3-DCP are classified as Group 2B by the International Agency for Research on Cancer. Although there is no data confirming the toxicity of either compound in humans, their toxicity was evidenced in animal experimentation or in vitro. Although few studies have been conducted, free 3-MCPD has been shown to have neurotoxicity, reproductive toxicity, and carcinogenicity. In contrast, 1,3-DCP only has mutagenic activity. The purpose of this study was to analyze 3-MCPD and 1,3-DCP in various foods using gas chromatography -mass spectrometry. 3-MCPD and 1,3-DCP were analyzed using phenyl boronic acid derivatization and the liquid–liquid extraction method, respectively. The analytical method for 3-MCPD and 1,3-DCP was validated in terms of linearity, limit of detection (LOD), limit of quantitation, accuracy and precision. Consequently, the LODs of 3-MCPD and 1,3-DCP in various matrices were identified to be in the ranges of 4.18~10.56 ng/g and 1.06~3.15 ng/g, respectively. PMID:26483891

Evaluation of multi-walled carbon nanotubes as solid-phase extraction adsorbents of pesticides from agricultural, ornamental and forestal soils.

PubMed

Asensio-Ramos, M; Hernández-Borges, J; Borges-Miquel, T M; Rodríguez-Delgado, M A

2009-08-11

A new, simple and cost-effective method based on the use of multi-walled carbon nanotubes (MWCNTs) as solid-phase extraction stationary phases is proposed for the determination of a group of seven organophosphorus pesticides (i.e. ethoprophos, diazinon, chlorpyriphos-methyl, fenitrothion, malathion, chlorpyriphos and phosmet) and one thiadiazine (buprofezin) in different kinds of soil samples (forestal, ornamental and agricultural) using gas chromatography with nitrogen phosphorus detection. Soils were first ultrasound extracted with 10 mL 1:1 methanol/acetonitrile (v/v) and the evaporated extract redissolved in 20 mL water (pH 6.0) was passed through 100 mg of MWCNTs of 10-15 nm o.d., 2-6 nm i.d. and 0.1-10 microm length. Elution was carried out with 20 mL dichloromethane. The method was validated in terms of linearity, precision, recovery, accuracy and selectivity. Matrix-matched calibration was carried out for each type of soil since statistical differences between the calibration curves constructed in pure solvent and in the reconstituted soil extract were found for most of the pesticides under study. Recovery values of spiked samples ranged between 54 and 91% for the three types of soils (limits of detection (LODs) between 2.97 and 9.49 ngg(-1)), except for chlorpyrifos, chlorpyrifos-methyl and buprofezin which ranged between 12 and 54% (LODs between 3.14 and 72.4 ngg(-1)), which are the pesticides with the highest soil organic carbon sorption coefficient (K(OC)) values. Using a one-sample test (Student's t-test) with fortified samples at two concentration levels in each type of soil, no significant differences were observed between the real and the experimental values (accuracy percentages ranged between 87 and 117%). It is the first time that the adsorptive potential of MWCNTs for the extraction of organophosphorus pesticides from soils is investigated.

Quantitative analysis of three chiral pesticide enantiomers by high-performance column liquid chromatography.

PubMed

Wang, Peng; Liu, Donghui; Gu, Xu; Jiang, Shuren; Zhou, Zhiqiang

2008-01-01

Methods for the enantiomeric quantitative determination of 3 chiral pesticides, paclobutrazol, myclobutanil, and uniconazole, and their residues in soil and water are reported. An effective chiral high-performance liquid chromatographic (HPLC)-UV method using an amylose-tris(3,5-dimethylphenylcarbamate; AD) column was developed for resolving the enantiomers and quantitative determination. The enantiomers were identified by a circular dichroism detector. Validation involved complete resolution of each of the 2 enantiomers, plus determination of linearity, precision, and limit of detection (LOD). The pesticide enantiomers were isolated by solvent extraction from soil and C18 solid-phase extraction from water. The 2 enantiomers of the 3 pesticides could be completely separated on the AD column using n-hexane isopropanol mobile phase. The linearity and precision results indicated that the method was reliable for the quantitative analysis of the enantiomers. LODs were 0.025, 0.05, and 0.05 mg/kg for each enantiomer of paclobutrazol, myclobutanil, and uniconazole, respectively. Recovery and precision data showed that the pretreatment procedures were satisfactory for enantiomer extraction and cleanup. This method can be used for optical purity determination of technical material and analysis of environmental residues.

El Nino, La Nina and VLBI Measured LOD

NASA Technical Reports Server (NTRS)

Clark, Thomas A.; Gipson, J. M.; Ma, C.

1998-01-01

VLBI is one of the most important techniques for measuring Earth orientation parameters (EOP), and is unique in its ability to make high accuracy measurements of UT1, and its time derivative, which is related to changes in the length of day, conventionally called LOD. These measurements of EOP give constraints on geophysical models of the solid-Earth, atmosphere and oceans. Changes in EOP are due either to external torques from gravitational forces, or to the exchange of angular momentum between the Earth, atmosphere and oceans. The effect of the external torques is strictly harmonic and nature, and is therefore easy to remove. We analyze an LOD time series derived from VLBI measurements with the goal of comparing this to predictions from AAM, and various ENSO indices. Previous work by ourselves and other investigators demonstrated a high degree of coherence between atmospheric angular momentum (AAM) and EOP. We continue to see this. As the angular momentum of the atmosphere increases, the rate of rotation of the Earth decreases, and vice versa. The signature of the ENSO is particularly strong. At the peak of the 1982-83 El Nino increased LOD by almost 1 ms. This was subsequently followed by a reduction in LOD of 0.75 ms. At its peak, in February of 1998, the 1997-98 El Nino increased LOD by 0.8 msec. As predicted at the 1998 Spring AGU, this has been followed by an abrupt decrease in LOD which is currently -0.4 ms. At this time (August, 1998) the current ENSO continues to develop in new and unexpected ways. We plan to update our analysis with all data available prior to the Fall AGU.

Stir bar sorptive extraction of diclofenac from liquid formulations: a proof of concept study.

PubMed

Kole, Prashant Laxman; Millership, Jeff; McElnay, James C

2011-03-25

A new stir bar sorptive extraction (SBSE) technique coupled with HPLC-UV method for quantification of diclofenac in pharmaceutical formulations has been developed and validated as a proof of concept study. Commercially available polydimethylsiloxane stir bars (Twister™) were used for method development and SBSE extraction (pH, phase ratio, stirring speed, temperature, ionic strength and time) and liquid desorption (solvents, desorption method, stirring time etc) procedures were optimised. The method was validated as per ICH guidelines and was successfully applied for the estimation of diclofenac from three liquid formulations viz. Voltarol(®) Optha single dose eye drops, Voltarol(®) Ophtha multidose eye drops and Voltarol(®) ampoules. The developed method was found to be linear (r=0.9999) over 100-2000ng/ml concentration range with acceptable accuracy and precision (tested over three QC concentrations). The SBSE extraction recovery of the diclofenac was found to be 70% and the LOD and LOQ of the validated method were found to be 16.06 and 48.68ng/ml, respectively. Furthermore, a forced degradation study of a diclofenac formulation leading to the formation of structurally similar cyclic impurity (indolinone) was carried out. The developed extraction method showed comparable results to that of the reference method, i.e. method was capable of selectively extracting the indolinone and diclofenac from the liquid matrix. Data on inter and intra stir bar accuracy and precision further confirmed robustness of the method, supporting the multiple re-use of the stir bars. Copyright © 2010 Elsevier B.V. All rights reserved.

METHODS OF DEALING WITH VALUES BELOW THE LIMIT OF DETECTION USING SAS

EPA Science Inventory

Due to limitations of chemical analysis procedures, small concentrations cannot be precisely measured. These concentrations are said to be below the limit of detection (LOD). In statistical analyses, these values are often censored and substituted with a constant value, such ...

Development and validation of polar RP-HPLC method for screening for ectoine high-yield strains in marine bacteria with green chemistry.

PubMed

Chen, Jun; Chen, Jianwei; Wang, Sijia; Zhou, Guangmin; Chen, Danqing; Zhang, Huawei; Wang, Hong

2018-04-02

A novel, green, rapid, and precise polar RP-HPLC method has been successfully developed and screened for ectoine high-yield strain in marine bacteria. Ectoine is a polar and extremely useful solute which allows microorganisms to survive in extreme environmental salinity. This paper describes a polar-HPLC method employed polar RP-C18 (5 μm, 250 × 4.6 mm) using pure water as the mobile phase and a column temperature of 30 °C, coupled with a flow rate at 1.0 mL/min and detected under a UV detector at wavelength of 210 nm. Our method validation demonstrates excellent linearity (R 2  = 0.9993), accuracy (100.55%), and a limit of detection LOQ and LOD of 0.372 and 0.123 μgmL -1 , respectively. These results clearly indicate that the developed polar RP-HPLC method for the separation and determination of ectoine is superior to earlier protocols.

Establishment of a method for determination of arsenic species in seafood by LC-ICP-MS.

PubMed

Zmozinski, Ariane V; Llorente-Mirandes, Toni; López-Sánchez, José F; da Silva, Márcia M

2015-04-15

An analytical method for determination of arsenic species (inorganic arsenic (iAs), methylarsonic acid (MA), dimethylarsinic acid (DMA), arsenobetaine (AB), trimethylarsine oxide (TMAO) and arsenocholine (AC)) in Brazilian and Spanish seafood samples is reported. This study was focused on extraction and quantification of inorganic arsenic (iAs), the most toxic form. Arsenic speciation was carried out via LC with both anionic and cationic exchange with ICP-MS detection (LC-ICP-MS). The detection limits (LODs), quantification limits (LOQs), precision and accuracy for arsenic species were established. The proposed method was evaluated using eight reference materials (RMs). Arsenobetaine was the main species found in all samples. The total and iAs concentration in 22 seafood samples and RMs ranged between 0.27-35.2 and 0.02-0.71 mg As kg(-1), respectively. Recoveries ranging from 100% to 106% for iAs, based on spikes, were achieved. The proposed method provides reliable iAs data for future risk assessment analysis. Copyright © 2014 Elsevier Ltd. All rights reserved.

Validated reversed phase LC method for quantitative analysis of polymethoxyflavones in citrus peel extracts.

PubMed

Wang, Zhenyu; Li, Shiming; Ferguson, Stephen; Goodnow, Robert; Ho, Chi-Tang

2008-01-01

Polymethoxyflavones (PMFs), which exist exclusively in the citrus genus, have biological activities including anti-inflammatory, anticarcinogenic, and antiatherogenic properties. A validated RPLC method was developed for quantitative analysis of six major PMFs, namely nobiletin, tangeretin, sinensetin, 5,6,7,4'-tetramethoxyflavone, 3,5,6,7,3',4'-hexamethoxyflavone, and 3,5,6,7,8,3',4'-heptamethoxyflavone. The polar embedded LC stationary phase was able to fully resolve the six analogues. The developed method was fully validated in terms of linearity, accuracy, precision, sensitivity, and system suitability. The LOD of the method was calculated as 0.15 microg/mL and the recovery rate was between 97.0 and 105.1%. This analytical method was successfully applied to quantify the individual PMFs in four commercially available citrus peel extracts (CPEs). Each extract shows significant difference in the PMF composition and concentration. This method may provide a simple, rapid, and reliable tool to help reveal the correlation between the bioactivity of the PMF extracts and the individual PMF content.

Simultaneous quantification of coumarins, flavonoids and limonoids in Fructus Citri Sarcodactylis by high performance liquid chromatography coupled with diode array detector.

PubMed

Chu, Jun; Li, Song-Lin; Yin, Zhi-Qi; Ye, Wen-Cai; Zhang, Qing-Wen

2012-07-01

A high performance liquid chromatography coupled with diode array detector (HPLC-DAD) method was developed for simultaneous quantification of eleven major bioactive components including six coumarins, three flavonoids and two limonoids in Fructus Citri Sarcodactylis. The analysis was performed on a Cosmosil 5 C(18)-MS-II column (4.6 mm × 250 mm, 5 μm) with water-acetonitrile gradient elution. The method was validated in terms of linearity, sensitivity, precision, stability and accuracy. It was found that the calibration curves for all analytes showed good linearity (R(2)>0.9993) within the test ranges. The overall limit of detection (LOD) and limit of quantification (LOQ) were less than 3.0 and 10.2 ng. The relative standard deviations (RSDs) for intra- and inter-day repeatability were not more than 4.99% and 4.92%, respectively. The sample was stable for at least 48 h. The spike recoveries of eleven components were 95.1-104.9%. The established method was successfully applied to determine eleven components in three samples from different locations. The results showed that the newly developed HPLC-DAD method was linear, sensitive, precise and accurate, and could be used for quality control of Fructus Citri Sarcodactylis. Copyright © 2012 Elsevier B.V. All rights reserved.

Performance Equivalence and Validation of the Soleris Automated System for Quantitative Microbial Content Testing Using Pure Suspension Cultures.

PubMed

Limberg, Brian J; Johnstone, Kevin; Filloon, Thomas; Catrenich, Carl

2016-09-01

Using United States Pharmacopeia-National Formulary (USP-NF) general method <1223> guidance, the Soleris(®) automated system and reagents (Nonfermenting Total Viable Count for bacteria and Direct Yeast and Mold for yeast and mold) were validated, using a performance equivalence approach, as an alternative to plate counting for total microbial content analysis using five representative microbes: Staphylococcus aureus, Bacillus subtilis, Pseudomonas aeruginosa, Candida albicans, and Aspergillus brasiliensis. Detection times (DTs) in the alternative automated system were linearly correlated to CFU/sample (R(2) = 0.94-0.97) with ≥70% accuracy per USP General Chapter <1223> guidance. The LOD and LOQ of the automated system were statistically similar to the traditional plate count method. This system was significantly more precise than plate counting (RSD 1.2-2.9% for DT, 7.8-40.6% for plate counts), was statistically comparable to plate counting with respect to variations in analyst, vial lots, and instruments, and was robust when variations in the operating detection thresholds (dTs; ±2 units) were used. The automated system produced accurate results, was more precise and less labor-intensive, and met or exceeded criteria for a valid alternative quantitative method, consistent with USP-NF general method <1223> guidance.

Determination of lithium and transition metals in Li1 Ni1/3 Co1/3 Mn1/3 O2 (NCM) cathode material for lithium-ion batteries by capillary electrophoresis.

PubMed

Vortmann-Westhoven, Britta; Lürenbaum, Constantin; Winter, Martin; Nowak, Sascha

2017-02-01

In this work, we present a novel electrophoretic method that was developed for the determination of lithium and transition metals in LiNi 1/3 Co 1/3 Mn 1/3 O 2 cathode material after microwave digestion. The cations in the digested LiNi 1/3 Co 1/3 Mn 1/3 O 2 material were separated by CE and the element content was determined by UV/Vis detection. To characterize the precision of the measurements, the RSDs and concentrations were calculated and compared to those obtained with ICP-optical emission spectrometry (ICP-OES). Furthermore, a certified reference material (BCR 176R-fly ash) was investigated for all techniques. For active material components, the LOD and LOQ were determined. The LODs and LOQs for the metals determined by CE were as follows: lithium (LOD/LOQ): 17.41/62.70 μg/L, cobalt (LOD/LOQ): 348.4/1283 μg/L, manganese (LOD/LOQ): 540.2/2095 μg/L, and nickel (LOD/LOQ): 838.0/2982 μg/L. Recovery rates for lithium were in the range of 95-103%. It could be proven that with the new technique, the results for the determination of the lithium content of active material were comparable with those obtained by ICP-OES and ion chromatography. Furthermore, the recovery rates of the transition metals were determined to be between 96 and 110% by CE and ICP-OES. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Centrifugal multiplexing fixed-volume dispenser on a plastic lab-on-a-disk for parallel biochemical single-end-point assays

PubMed Central

La, Moonwoo; Park, Sang Min; Kim, Dong Sung

2015-01-01

In this study, a multiple sample dispenser for precisely metered fixed volumes was successfully designed, fabricated, and fully characterized on a plastic centrifugal lab-on-a-disk (LOD) for parallel biochemical single-end-point assays. The dispenser, namely, a centrifugal multiplexing fixed-volume dispenser (C-MUFID) was designed with microfluidic structures based on the theoretical modeling about a centrifugal circumferential filling flow. The designed LODs were fabricated with a polystyrene substrate through micromachining and they were thermally bonded with a flat substrate. Furthermore, six parallel metering and dispensing assays were conducted at the same fixed-volume (1.27 μl) with a relative variation of ±0.02 μl. Moreover, the samples were metered and dispensed at different sub-volumes. To visualize the metering and dispensing performances, the C-MUFID was integrated with a serpentine micromixer during parallel centrifugal mixing tests. Parallel biochemical single-end-point assays were successfully conducted on the developed LOD using a standard serum with albumin, glucose, and total protein reagents. The developed LOD could be widely applied to various biochemical single-end-point assays which require different volume ratios of the sample and reagent by controlling the design of the C-MUFID. The proposed LOD is feasible for point-of-care diagnostics because of its mass-producible structures, reliable metering/dispensing performance, and parallel biochemical single-end-point assays, which can identify numerous biochemical. PMID:25610516

Development and practical application of accelerated solvent extraction for the isolation of cocaine/crack biomarkers in meconium samples.

PubMed

Mantovani, Cínthia de Carvalho; Lima, Marcela Bittar; Oliveira, Carolina Dizioli Rodrigues de; Menck, Rafael de Almeida; Diniz, Edna Maria de Albuquerque; Yonamine, Mauricio

2014-04-15

A method using accelerated solvent extraction (ASE) for the isolation of cocaine/crack biomarkers in meconium samples, followed by solid phase extraction (SPE) and the simultaneous quantification by gas chromatography-mass spectrometry (GC-MS) was developed and validated. Initially, meconium samples were submitted to an ASE procedure, which was followed by SPE with Bond Elut Certify I cartridges. The analytes were derivatizated with PFP/PFPA and analyzed by GC-MS. The limits of detection (LOD) were between 11 and 17ng/g for all analytes. The limits of quantification (LOQ) were 30ng/g for anhydroecgonine methyl ester, and 20ng/g for cocaine, benzoylecgonine, ecgonine methyl ester and cocaethylene. Linearity ranged from the LOQ to 1500ng/g for all analytes, with a coefficients of determination greater than 0.991, except for m-hydroxybenzoylecgonine, which was only qualitatively detected. Precision and accuracy were evaluated at three concentration levels. For all analytes, inter-assay precision ranged from 3.2 to 18.1%, and intra-assay precision did not exceed 12.7%. The accuracy results were between 84.5 and 114.2% and the average recovery ranged from 17 to 84%. The method was applied to 342 meconium samples randomly collected in the University Hospital-University of São Paulo (HU-USP), Brazil. Cocaine biomarkers were detected in 19 samples, which represent 5.6% of exposure prevalence. Significantly lower birth weight, length and head circumference were found for the exposed newborns compared with the non-exposed group. This is the first report in which ASE was used as a sample preparation technique to extract cocaine biomarkers from a complex biological matrix such as meconium samples. The advantages of the developed method are the smaller demand for organic solvents and the minor sample handling, which allows a faster and accurate procedure, appropriate to confirm fetal exposure to cocaine/crack. Copyright © 2014 Elsevier B.V. All rights reserved.

The Partition of Multi-Resolution LOD Based on Qtm

NASA Astrophysics Data System (ADS)

Hou, M.-L.; Xing, H.-Q.; Zhao, X.-S.; Chen, J.

2011-08-01

The partition hierarch of Quaternary Triangular Mesh (QTM) determine the accuracy of spatial analysis and application based on QTM. In order to resolve the problem that the partition hierarch of QTM is limited by the level of the computer hardware, the new method that Multi- Resolution LOD (Level of Details) based on QTM will be discussed in this paper. This method can make the resolution of the cells varying with the viewpoint position by partitioning the cells of QTM, selecting the particular area according to the viewpoint; dealing with the cracks caused by different subdivisions, it satisfies the request of unlimited partition in part.

Sensitivity of lod scores to changes in diagnostic status.

PubMed Central

Hodge, S E; Greenberg, D A

1992-01-01

This paper investigates effects on lod scores when one individual in a data set changes diagnostic or recombinant status. First we examine the situation in which a single offspring in a nuclear family changes status. The nuclear-family situation, in addition to being of interest in its own right, also has general theoretical importance, since nuclear families are "transparent"; that is, one can track genetic events more precisely in nuclear families than in complex pedigrees. We demonstrate that in nuclear families log10 [(1-theta)/theta] gives an upper limit on the impact that a single offspring's change in status can have on the lod score at that recombination fraction (theta). These limits hold for a fully penetrant dominant condition and fully informative marker, in either phase-known or phase-unknown matings. Moreover, log10 [(1-theta)/theta] (where theta denotes the value of theta at which Zmax occurs) gives an upper limit on the impact of a single offspring's status change on the maximum lod score (Zmax). In extended pedigrees, in contrast to nuclear families, no comparable limit can be set on the impact of a single individual on the lod score. Complex pedigrees are subject to both stabilizing and destabilizing influences, and these are described. Finally, we describe a "sensitivity analysis," in which, after all linkage analysis is completed, every informative individual in the data set is changed, one at a time, to see the effect which each separate change has on the lod scores. The procedure includes identifying "critical individuals," i.e., those who would have the greatest impact on the lod scores, should their diagnostic status in fact change. To illustrate use of the sensitivity analysis, we apply it to the large bipolar pedigree reported by Egeland et al. and Kelsoe et al. We show that the changes in lod scores observed there, on the order of 1.1-1.2 per person, are not unusual. We recommend that investigators include a sensitivity analysis as a standard part of reporting the results of a linkage analysis. PMID:1570835

Sensitivity of lod scores to changes in diagnostic status.

PubMed

Hodge, S E; Greenberg, D A

1992-05-01

This paper investigates effects on lod scores when one individual in a data set changes diagnostic or recombinant status. First we examine the situation in which a single offspring in a nuclear family changes status. The nuclear-family situation, in addition to being of interest in its own right, also has general theoretical importance, since nuclear families are "transparent"; that is, one can track genetic events more precisely in nuclear families than in complex pedigrees. We demonstrate that in nuclear families log10 [(1-theta)/theta] gives an upper limit on the impact that a single offspring's change in status can have on the lod score at that recombination fraction (theta). These limits hold for a fully penetrant dominant condition and fully informative marker, in either phase-known or phase-unknown matings. Moreover, log10 [(1-theta)/theta] (where theta denotes the value of theta at which Zmax occurs) gives an upper limit on the impact of a single offspring's status change on the maximum lod score (Zmax). In extended pedigrees, in contrast to nuclear families, no comparable limit can be set on the impact of a single individual on the lod score. Complex pedigrees are subject to both stabilizing and destabilizing influences, and these are described. Finally, we describe a "sensitivity analysis," in which, after all linkage analysis is completed, every informative individual in the data set is changed, one at a time, to see the effect which each separate change has on the lod scores. The procedure includes identifying "critical individuals," i.e., those who would have the greatest impact on the lod scores, should their diagnostic status in fact change. To illustrate use of the sensitivity analysis, we apply it to the large bipolar pedigree reported by Egeland et al. and Kelsoe et al. We show that the changes in lod scores observed there, on the order of 1.1-1.2 per person, are not unusual. We recommend that investigators include a sensitivity analysis as a standard part of reporting the results of a linkage analysis.

Determination of Major Phenolic Compounds in Echinacea spp. Raw Materials and Finished Products by High-Performance Liquid Chromatography with Ultraviolet Detection: Single-Laboratory Validation Matrix Extension

PubMed Central

Brown, Paula N.; Chan, Michael; Paley, Lori; Betz, Joseph M.

2013-01-01

A method previously validated to determine caftaric acid, chlorogenic acid, cynarin, echinacoside, and cichoric acid in echinacea raw materials has been successfully applied to dry extract and liquid tincture products in response to North American consumer needs. Single-laboratory validation was used to assess the repeatability, accuracy, selectivity, LOD, LOQ, analyte stability (ruggedness), and linearity of the method, with emphasis on finished products. Repeatability precision for each phenolic compound was between 1.04 and 5.65% RSD, with HorRat values between 0.30 and 1.39 for raw and dry extract finished products. HorRat values for tinctures were between 0.09 and 1.10. Accuracy of the method was determined through spike recovery studies. Recovery of each compound from raw material negative control (ginseng) was between 90 and 114%, while recovery from the finished product negative control (maltodextrin and magnesium stearate) was between 97 and 103%. A study was conducted to determine if cichoric acid, a major phenolic component of Echinacea purpurea (L.) Moench and E. angustifolia DC, degrades during sample preparation (extraction) and HPLC analysis. No significant degradation was observed over an extended testing period using the validated method. PMID:22165004

Determination of major phenolic compounds in Echinacea spp. raw materials and finished products by high-performance liquid chromatography with ultraviolet detection: single-laboratory validation matrix extension.

PubMed

Brown, Paula N; Chan, Michael; Paley, Lori; Betz, Joseph M

2011-01-01

A method previously validated to determine caftaric acid, chlorogenic acid, cynarin, echinacoside, and cichoric acid in echinacea raw materials has been successfully applied to dry extract and liquid tincture products in response to North American consumer needs. Single-laboratory validation was used to assess the repeatability, accuracy, selectivity, LOD, LOQ, analyte stability (ruggedness), and linearity of the method, with emphasis on finished products. Repeatability precision for each phenolic compound was between 1.04 and 5.65% RSD, with HorRat values between 0.30 and 1.39 for raw and dry extract finished products. HorRat values for tinctures were between 0.09 and 1.10. Accuracy of the method was determined through spike recovery studies. Recovery of each compound from raw material negative control (ginseng) was between 90 and 114%, while recovery from the finished product negative control (maltodextrin and magnesium stearate) was between 97 and 103%. A study was conducted to determine if cichoric acid, a major phenolic component of Echinacea purpurea (L.) Moench and E. angustifolia DC, degrades during sample preparation (extraction) and HPLC analysis. No significant degradation was observed over an extended testing period using the validated method.

Dual ultrasonic-assisted dispersive liquid-liquid microextraction coupled with microwave-assisted derivatization for simultaneous determination of 20(S)-protopanaxadiol and 20(S)-protopanaxatriol by ultra high performance liquid chromatography-tandem mass spectrometry.

PubMed

Zhao, Xian-En; Lv, Tao; Zhu, Shuyun; Qu, Fei; Chen, Guang; He, Yongrui; Wei, Na; Li, Guoliang; Xia, Lian; Sun, Zhiwei; Zhang, Shijuan; You, Jinmao; Liu, Shu; Liu, Zhiqiang; Sun, Jing; Liu, Shuying

2016-03-11

This paper, for the first time, reported a speedy hyphenated technique of low toxic dual ultrasonic-assisted dispersive liquid-liquid microextraction (dual-UADLLME) coupled with microwave-assisted derivatization (MAD) for the simultaneous determination of 20(S)-protopanaxadiol (PPD) and 20(S)-protopanaxatriol (PPT). The developed method was based on ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) detection using multiple-reaction monitoring (MRM) mode. A mass spectrometry sensitizing reagent, 4'-carboxy-substituted rosamine (CSR) with high reaction activity and ionization efficiency was synthesized and firstly used as derivatization reagent. Parameters of dual-UADLLME, MAD and UHPLC-MS/MS conditions were all optimized in detail. Low toxic brominated solvents were used as extractant instead of traditional chlorinated solvents. Satisfactory linearity, recovery, repeatability, accuracy and precision, absence of matrix effect and extremely low limits of detection (LODs, 0.010 and 0.015ng/mL for PPD and PPT, respectively) were achieved. The main advantages were rapid, sensitive and environmentally friendly, and exhibited high selectivity, accuracy and good matrix effect results. The proposed method was successfully applied to pharmacokinetics of PPD and PPT in rat plasma. Copyright © 2016 Elsevier B.V. All rights reserved.

Quantitative isomer-specific N-glycan fingerprinting using isotope coded labeling and high performance liquid chromatography-electrospray ionization-mass spectrometry with graphitic carbon stationary phase.

PubMed

Michael, Claudia; Rizzi, Andreas M

2015-02-27

Glycan reductive isotope labeling (GRIL) using (12)C6-/(13)C6-aniline as labeling reagent is reported with the aim of quantitative N-glycan fingerprinting. Porous graphitized carbon (PGC) as stationary phase in capillary scale HPLC coupled to electrospray mass spectrometry with time of flight analyzer was applied for the determination of labeled N-glycans released from glycoproteins. The main benefit of using stable isotope-coding in the context of comparative glycomics lies in the improved accuracy and precision of the quantitative analysis in combined samples and in the potential of correcting for structure-dependent incomplete enzymatic release of oligosaccharides when comparing identical target proteins. The method was validated with respect to mobile phase parameters, reproducibility, accuracy, linearity and limit of detection/quantification (LOD/LOQ) using test glycoproteins. It is shown that the developed method is capable of determining relative amounts of N-glycans (including isomers) comparing two samples in one single HPLC-MS run. The analytical potential and usefulness of GRIL in combination with PGC-ESI-TOF-MS is demonstrated comparing glycosylation in human monoclonal antibodies produced in Chinese hamster ovary cells (CHO) and hybridoma cell lines. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis of molecular imprinted polymers for selective extraction of domperidone from human serum using high performance liquid chromatography with fluorescence detection.

PubMed

Salehi, Simin; Rasoul-Amini, Sara; Adib, Noushin; Shekarchi, Maryam

2016-08-01

In this study a novel method is described for selective quantization of domperidone in biological matrices applying molecular imprinted polymers (MIPs) as a sample clean up procedure using high performance liquid chromatography coupled with a fluorescence detector. MIPs were synthesized with chloroform as the porogen, ethylene glycol dimethacrylate as the crosslinker, methacrylic acid as the monomer, and domperidone as the template molecule. The new imprinted polymer was used as a molecular sorbent for separation of domperidone from serum. Molecular recognition properties, binding capacity and selectivity of MIPs were determined. The results demonstrated exceptional affinity for domperidone in biological fluids. The domperidone analytical method using MIPs was verified according to validation parameters, such as selectivity, linearity (5-80ng/mL, r(2)=0.9977), precision and accuracy (10-40ng/mL, intra-day=1.7-5.1%, inter-day=4.5-5.9%, and accuracy 89.07-98.9%).The limit of detection (LOD) and quantization (LOQ) of domperidone was 0.0279 and 0.092ng/mL, respectively. The simplicity and suitable validation parameters makes this a highly valuable selective bioequivalence method for domperidone analysis in human serum. Copyright © 2016 Elsevier B.V. All rights reserved.

Separation of catechins and methylxanthines in tea samples by capillary electrochromatography.

PubMed

Uysal, Ulku Dilek; Aturki, Zeineb; Raggi, Maria Augusta; Fanali, Salvatore

2009-04-01

In this paper, the simultaneous separation of several polyphenols such as (+)-catechin, (-)-epicatechin, (-)-epigallocatechin, theophylline, caffeine in green and black teas by capillary electrochromatography (CEC) was developed. Several experimental parameters such as stationary phase type, mobile phase composition, buffer and pH, inner diameter of the columns, sample injection, were evaluated to obtain the complete separation of the analysed compounds. Baseline resolution of the studied polyphenols was achieved within 30 min by using a capillary column (id 100 microm) packed with bidentate C(18) particles for 24.5 cm and a mobile phase composed of 5 mM ammonium acetate buffer pH 4 with H(2)O/ACN (80:20, v/v). The applied voltage and the temperature were set at 30 kV and 20 degrees C. Precision, detection and quantification limits, linearity, and accuracy were investigated. A good linearity (R(2) > 0.9992) was achieved over a concentration working range of 2-100 microg/mL for all the analytes. LOD and LOQ were 1 and 2 microg/mL, respectively, for all studied compounds. The CEC method was applied to the analysis of those polyphenols in green and black tea samples after an extraction procedure. Good recovery data from accuracy studies ranged between 90% and 112% for all analytes.

New Spectrophotometric Assay of Pyrantel Pamoate in Pharmaceuticals and Spiked Human Urine Using Three Complexing Agents

NASA Astrophysics Data System (ADS)

Swamy, N.; Prashanth, K. N.; Basavaiah, K.

2015-07-01

Three simple, rapid, inexpensive, and highly sensitive spectrophotometric methods are described for the quantifi cation of pyrantel pamoate (PYP) in pure drug and formulations. The methods are based on the molecular charge-transfer (CT) complexation reaction involving pyrantel base (PYL) as n-donor and iodine as σ-acceptor (I 2 , method A), and 2,4-dinitrophenol (DNP, method B) or picric acid (PA, method C) as π-acceptors. Spectrophotometrically, the CT complexes showed absorption maxima at 380, 420, and 430 nm, for methods A, B, and C, respectively. Under optimum conditions, Beer's law was obeyed over the concentration ranges 0.12-2.9, 0.12-3.75, and 0.12-2.9 μg/ml for methods A, B, and C, respectively. The apparent molar absorptivity of the CT complexes at the respective λmax are calculated to be 2.63 × 10 5 , 6.91 × 10 4 , and 1.73 × 10 5 l/mol· cm respectively and the corresponding Sandell sensitivity values are 0.0009, 0.003, and 0.0012. The limits of detection (LOD) and quantification (LOQ) are calculated to be (0.02 and 0.07), (0.05 and 0.15), and (0.02 and 0.07) μg/ml with methods A, B, and C, respectively. The intra-day and inter-day accuracy expressed as %RE and precision expressed as %RSD are less than 3%. The methods have been applied to the determination of PYP in tablets, suspensions, and spiked human urine. Parallel assay by a reference method and statistical analysis of the results obtained show no significant difference between the proposed methods and the reference method with respect to accuracy and precision, as evident from the Student's t and variation ratio tests. The accuracy of the methods has been further ascertained by recovery tests via the standard addition technique.

Simultaneous in-cell derivatization pressurized liquid extraction for the determination of multiclass preservatives in leave-on cosmetics.

PubMed

Sanchez-Prado, Lucia; Lamas, J Pablo; Lores, Marta; Garcia-Jares, Carmen; Llompart, Maria

2010-11-15

An effective one-step sample preparation methodology for the determination of multiclass preservatives in cosmetics has been developed, applying, for the first time to this kind of matrix, pressurized liquid extraction (PLE) and a very simple, cheap, and fast derivatization procedure: acetylation with acetic anhydride and pyridine. A multifactorial experimental design has been used to evaluate and optimize the main experimental parameters potentially affecting the extraction process. In the final conditions the sample was mixed with Florisil as the dispersing sorbent and extracted with ethyl acetate for 15 min at 120 °C. One of the main goals of this work was to demonstrate the possibility of carrying out direct cosmetic preservative acetylation by simply adding the derivatization reagents into the PLE cell. The extract was then analyzed by GC/MS without any further cleanup or concentration step. The accuracy, precision, linearity, and detection limits (LODs) were evaluated to assess the performance of the proposed method. Quantitative recoveries were obtained, and relative standard deviation values were lower than 10% in all cases. The obtained LODs ranged from 0.000004% to 0.0001% (w/w), values far below the established restrictions in the European Cosmetics Regulation, making this multicomponent analytical method suitable for routine control. Finally, several cosmetic products such as moisturizing and antiwrinkle creams and lotions, hand creams, sunscreen and after-sun creams, baby lotions, and hair care products were analyzed. All the samples contained several of the target cosmetic ingredients, in some cases at quite high concentrations, although the actual European Cosmetics Regulation was fulfilled in all cases.

A high-performance liquid chromatographic-tandem mass spectrometric method for the determination of ethyl glucuronide and ethyl sulfate in urine validated according to forensic guidelines.

PubMed

Albermann, M E; Musshoff, F; Madea, B

2012-01-01

Ethyl glucuronide (EtG) and ethyl sulfate (EtS) are powerful markers for alcohol intake and abuse. Several analytical procedures for the quantification of EtG and EtG in serum and urine have been developed so far. Many of the published methods show limits of detections (LODs) or limits of quantifications (LOQs) for EtG in urine within the range of 0.1 mg/L or higher. Since this is the actual cutoff value for proving abstinence in Germany, problems may occur if urine samples are highly diluted. In this paper, the validation of a highly sensitive, fast and simple LC-MS-MS for the determination of EtG and EtS in urine is described. The calibration curves for EtG and EtS is linear over the whole range (0.025-2.0 mg/L). Very low detection limits can be achieved (LOD: EtG 0.005 mg/L, EtS 0.005 mg/L; and LOQ: EtG 0.019 mg/L, EtS 0.015 mg/L). All data for selectivity, precision and accuracy, recovery, as well as for the processed sample and the freeze/thaw stability, comply with the guidelines of the German Society of Toxicological and Forensic Chemistry. Strong matrix-related effects can be compensated for by using an internal standard. Finally, the applicability of the procedure is proven by analysis of 87 human urine samples and by successful participation in interlaboratory comparison tests. © The Author [2011]. Published by Oxford University Press. All rights reserved.

Development and validation of LC-MS/MS method for the determination of Ochratoxin A and its metabolite Ochratoxin α in poultry tissues and eggs.

PubMed

Paoloni, Angela; Solfrizzo, Michele; Bibi, Rita; Pecorelli, Ivan

2018-05-04

The objective of this study was to develop a liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the determination of Ochratoxin A (OTA) and Ochratoxin α (OTα) in poultry tissues and eggs. The two toxins were extracted by a mixture of acetonitrile/water, purified with a reversed phase C18 solid phase extraction column (SPE) and determined by LC-MS/MS. The LC-MS/MS method performances were evaluated in terms of linearity in solvent and in matrix (ranged from 0.5 to 15.10 µg L -1 for OTA and from 0.60 to 17.85 µg L -1 for OTα), limit of detection (LOD), limit of quantitation (LOQ), specificity, accuracy and precision in repeatability conditions. Recovery experiments were performed by spiking poultry liver, kidney, muscle and eggs around 1 µg kg -1 and 10 µg kg -1 . LODs were 0.27 and 0.26 µg kg -1 while LOQs were fixed at 1.0 and 1.2 µg kg -1 for OTA and OTα, respectively. Main recoveries for OTA ranged from 82 to 109% and for OTα ranged from 55 to 89%. The values of within-laboratory relative standard deviation (RSD r ) were equal to or below 20%. Considering the results obtained and that all analytical performance criteria were fulfilled, the new extraction and purification method developed for OTA and OTα determination in animal tissues and eggs was found appropriate for control laboratories and research activities designed to ensure food safety.

Determination of sulfonamides in animal tissues by modified QuEChERS and liquid chromatography tandem mass spectrometry.

PubMed

Wen, Ching-Hsuan; Lin, Shu-Ling; Fuh, Ming-Ren

2017-03-01

In this study, the salting-out solvent extraction and dispersive solid-phase extraction (dSPE) clean-up steps in QuEChERS (quick, easy, cheap, effective, rugged, and safe) method were optimized to reduce matrix effect and efficiently extract target sulfonamides from a variety of edible animal tissues. The extracted sulfonamides were then analyzed using liquid chromatography tandem mass spectrometry (LC-MS/MS). Good extraction recoveries (74.0-100.3% in five different sources of animal tissues; n=3) with acceptable matrix effect (<10%, except for liver samples) were obtained using the proposed method. For the first time, a commercial ND-lipids cartridge was used to remove hydrophobic matrix components from fat-rich animal tissues in the clean-up step of QuEChERS. In addition, good linearity (0.125-12.5ngg -1 ) was observed using matrix-matched calibration (in beef). Limits of detection (LODs) were estimated at 0.01-0.03ngg -1 in beef, pork, and chicken samples. For beef tripe and pig liver samples, the LODs were in the range of 0.02-0.04ngg -1 . Good intra-day/inter-day precision (1.0-10.5%/0.4-8.0%) and accuracy (95.2-107.2%/97.8-102.1%) were also achieved using the modified QuEChERS for sample pretreatment. The applicability of the modified QuEChERS-LC-MS/MS method was demonstrated by determining the occurrence of target sulfonamides in various edible animal tissues for potential food safety analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of trace labile copper in environmental waters by magnetic nanoparticle solid phase extraction and high-performance chelation ion chromatography.

PubMed

Wei, Z; Sandron, S; Townsend, A T; Nesterenko, P N; Paull, B

2015-04-01

Cobalt magnetic nanoparticles surface functionalised with iminodiacetic acid were evaluated as a nano-particulate solid phase extraction absorbent for copper ions (Cu(2+)) from environmental water samples. Using an external magnetic field, the collector nanoparticles could be separated from the aqueous phase, and adsorbed ions simply decomplexed using dilute HNO3. Effects of pH, buffer concentration, sample and sorbent volume, extraction equilibrium time, and interfering ion concentration on extraction efficiency were investigated. Optimal conditions were then applied to the extraction of Cu(2+) ions from natural water samples, prior to their quantitation using high-performance chelation ion chromatography. The limits of detection (LOD) of the combined extraction and chromatographic method were ~0.1 ng ml(-1), based upon a 100-fold preconcentration factor (chromatographic performance; LOD=9.2 ng ml(-1) Cu(2+)), analytical linear range from 20 to 5000 ng mL(-1), and relative standard deviations=4.9% (c=1000 ng ml(-1), n=7). Accuracy and precision of the combined approach was verified using a certified reference standard estuarine water sample (SLEW-2) and comparison of sample determinations with sector field inductively coupled plasma mass spectrometry. Recoveries from the addition of Cu(2+) to impacted estuarine and rain water samples were 103.5% and 108.5%, respectively. Coastal seawater samples, both with and without prior UV irradiation and dissolved organic matter removal were also investigated using the new methodology. The effect of DOM concentration on copper availability was demonstrated. Copyright © 2015. Published by Elsevier B.V.

Least median of squares and iteratively re-weighted least squares as robust linear regression methods for fluorimetric determination of α-lipoic acid in capsules in ideal and non-ideal cases of linearity.

PubMed

Korany, Mohamed A; Gazy, Azza A; Khamis, Essam F; Ragab, Marwa A A; Kamal, Miranda F

2018-06-01

This study outlines two robust regression approaches, namely least median of squares (LMS) and iteratively re-weighted least squares (IRLS) to investigate their application in instrument analysis of nutraceuticals (that is, fluorescence quenching of merbromin reagent upon lipoic acid addition). These robust regression methods were used to calculate calibration data from the fluorescence quenching reaction (∆F and F-ratio) under ideal or non-ideal linearity conditions. For each condition, data were treated using three regression fittings: Ordinary Least Squares (OLS), LMS and IRLS. Assessment of linearity, limits of detection (LOD) and quantitation (LOQ), accuracy and precision were carefully studied for each condition. LMS and IRLS regression line fittings showed significant improvement in correlation coefficients and all regression parameters for both methods and both conditions. In the ideal linearity condition, the intercept and slope changed insignificantly, but a dramatic change was observed for the non-ideal condition and linearity intercept. Under both linearity conditions, LOD and LOQ values after the robust regression line fitting of data were lower than those obtained before data treatment. The results obtained after statistical treatment indicated that the linearity ranges for drug determination could be expanded to lower limits of quantitation by enhancing the regression equation parameters after data treatment. Analysis results for lipoic acid in capsules, using both fluorimetric methods, treated by parametric OLS and after treatment by robust LMS and IRLS were compared for both linearity conditions. Copyright © 2018 John Wiley & Sons, Ltd.

Using Affordable Data Capturing Devices for Automatic 3d City Modelling

NASA Astrophysics Data System (ADS)

Alizadehashrafi, B.; Abdul-Rahman, A.

2017-11-01

In this research project, many movies from UTM Kolej 9, Skudai, Johor Bahru (See Figure 1) were taken by AR. Drone 2. Since the AR drone 2.0 has liquid lens, while flying there were significant distortions and deformations on the converted pictures of the movies. Passive remote sensing (RS) applications based on image matching and Epipolar lines such as Agisoft PhotoScan have been tested to create the point clouds and mesh along with 3D models and textures. As the result was not acceptable (See Figure 2), the previous Dynamic Pulse Function based on Ruby programming language were enhanced and utilized to create the 3D models automatically in LoD3. The accuracy of the final 3D model is almost 10 to 20 cm. After rectification and parallel projection of the photos based on some tie points and targets, all the parameters were measured and utilized as an input to the system to create the 3D model automatically in LoD3 in a very high accuracy.

Combining presentation high-sensitivity cardiac troponin I and glucose measurements to rule-out an acute myocardial infarction in patients presenting to emergency department with chest pain.

PubMed

Greenslade, J H; Kavsak, P; Parsonage, W; Shortt, C; Than, M; Pickering, J W; Aldous, S; Cullen, L

2015-03-01

The use of high sensitivity troponin (hs-Tn) may enable early rule out of acute myocardial infarction (AMI) for patients presenting to the emergency department (ED) with chest pain. This study evaluated two approaches to the early rule out of AMI; a combination of a presentation hs-Tn <4ng/L and normal glucose at presentation (dual testing) and a presentation hs-Tn troponin below the limit of detection (LoD). We utilised prospectively collected data on adult patients presenting with suspected ACS in two EDs in Australia and New Zealand. Blood samples were taken on presentation and tested for glucose and high sensitivity troponin I. The primary endpoint was index AMI and the secondary endpoint was 30-day acute coronary syndrome (ACS). Sensitivity, specificity, positive and negative predictive values were used to assess the diagnostic accuracy of the dual testing and LoD approaches. Of the 1412 participants, 182 (12.9%) had index AMI. The LoD and the dual testing approach were 100% sensitive for index AMI. The specificity of the dual testing approach (25.2%) was slightly higher than that of the LoD (20.4%). Sensitivity for ACS was similar for the two approaches (96.5% for dual testing and 98.1% for the LoD). The dual testing and LoD approach identified all patients with index AMI and could be used to reduce the proportion of patients requiring lengthy assessment and inpatient admission. Further investigation is still required to rule out unstable angina pectoris in patients identified as low risk. Copyright © 2014 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Quality Analysis of Chlorogenic Acid and Hyperoside in Crataegi fructus

PubMed Central

Weon, Jin Bae; Jung, Youn Sik; Ma, Choong Je

2016-01-01

Background: Crataegi fructus is a herbal medicine for strong stomach, sterilization, and alcohol detoxification. Chlorogenic acid and hyperoside are the major compounds in Crataegi fructus. Objective: In this study, we established novel high-performance liquid chromatography (HPLC)-diode array detection analysis method of chlorogenic acid and hyperoside for quality control of Crataegi fructus. Materials and Methods: HPLC analysis was achieved on a reverse-phase C18 column (5 μm, 4.6 mm × 250 mm) using water and acetonitrile as mobile phase with gradient system. The method was validated for linearity, precision, and accuracy. About 31 batches of Crataegi fructus samples collected from Korea and China were analyzed by using HPLC fingerprint of developed HPLC method. Then, the contents of chlorogenic acid and hyperoside were compared for quality evaluation of Crataegi fructus. Results: The results have shown that the average contents (w/w %) of chlorogenic acid and hyperoside in Crataegi fructus collected from Korea were 0.0438% and 0.0416%, respectively, and the average contents (w/w %) of 0.0399% and 0.0325%, respectively. Conclusion: In conclusion, established HPLC analysis method was stable and could provide efficient quality evaluation for monitoring of commercial Crataegi fructus. SUMMARY Quantitative analysis method of chlorogenic acid and hyperoside in Crataegi fructus is developed by high.performance liquid chromatography.(HPLC).diode array detectionEstablished HPLC analysis method is validated with linearity, precision, and accuracyThe developed method was successfully applied for quantitative analysis of Crataegi fructus sample collected from Korea and China. Abbreviations used: HPLC: High-performance liquid chromatography, GC: Gas chromatography, MS: Mass spectrometer, LOD: Limits of detection, LOQ: Limits of quantification, RSD: Relative standard deviation, RRT: Relative retention time, RPA: Relation peak area. PMID:27076744

A fast liquid chromatography-tandem mass spectrometry method for determining benzodiazepines and analogues in urine. Validation and application to real cases of forensic interest.

PubMed

Salomone, Alberto; Gerace, Enrico; Brizio, Paola; Gennaro, M Carla; Vincenti, Marco

2011-11-01

A fast liquid chromatographic/tandem mass spectrometric method was developed for the simultaneous determination in human urine of seventeen benzodiazepines, four relevant metabolites together plus zolpidem and zopiclone. The sample preparation, optimized to take into account the matrix effect, was based on enzymatic hydrolysis and liquid-liquid extraction. The separation of the twenty-three analytes was achieved in less than eight minutes. The whole methodology was fully validated according to UNI EN ISO/IEC 17025:2005 rules and 2006 SOFT/AAFS guidelines. Selectivity, linearity range, identification (LOD) and quantitation (LOQ) limits, precision, accuracy and recovery were evaluated. For all the species the signal/concentration linearity was satisfactory in the 50-1000 ng/mL concentration range. The limits of detection ranged from 0.5 to 30 ng/mL and LOQs from 1.7 to 100.0 ng/mL. Precisions were in the ranges 5.0-11.8%, 1.5-11.0% and 1.1-4.4% for low (100 ng/mL), medium (300 ng/mL) and high (1000 ng/mL) concentration, respectively. The accuracy, expressed as bias% was within ± 25 % for all the analytes. The recovery values, evaluated at 300 ng/mL concentration, ranged from 56.2% to 98.8%. The present method for the determination of several benzodiazepines, zolpidem and zopiclone in human urine proved to be simple, fast, specific and sensitive. The quantification by LC-MS/MS was successfully applied to 329 forensic cases among driving re-licensing, car accidents and alleged sexual violence cases. Copyright © 2011 Elsevier B.V. All rights reserved.

Quantification of cortisol in human eccrine sweat by liquid chromatography - tandem mass spectrometry.

PubMed

Jia, Min; Chew, Wade M; Feinstein, Yelena; Skeath, Perry; Sternberg, Esther M

2016-03-21

Cortisol has long been recognized as the "stress biomarker" in evaluating stress related disorders. Plasma, urine or saliva are the current source for cortisol analysis. The sampling of these biofluids is either invasive or has reliability problems that could lead to inaccurate results. Sweat has drawn increasing attention as a promising source for non-invasive stress analysis. A sensitive HPLC-MS/MS method was developed for the quantitation of cortisol ((11β)-11,17,21-trihydroxypregn-4-ene-3,20-dione) in human eccrine sweat. At least one unknown isomer that has previously not been reported and could potentially interfere with quantification was separated from cortisol with mixed mode RP HPLC. Detection of cortisol was carried out using atmospheric pressure chemical ionization (APCI) and selected reaction monitoring (SRM) in positive ion mode, using cortisol-9,11,12,12-D4 as internal standard. LOD and LOQ were estimated to be 0.04 ng ml(-1) and 0.1 ng ml(-1), respectively. Linear range of 0.10-25.00 ng ml(-1) was obtained. Intraday precision (2.5%-9.7%) and accuracy (0.5%-2.1%), interday precision (12.3%-18.7%) and accuracy (7.1%-15.1%) were achieved. This method has been successfully applied to the cortisol analysis of human eccrine sweat samples. This is the first demonstration that HPLC-MS/MS can be used for the sensitive and highly specific determination of cortisol in human eccrine sweat in the presence of at least one isomer that has similar hydrophobicity as cortisol. This study demonstrated that human eccrine sweat could be used as a promising source for non-invasive assessment of stress biomarkers such as cortisol and other steroid hormones.

Characterization and application of restricted access carbon nanotubes in online extraction of anticonvulsant drugs from plasma samples followed by liquid chromatography analysis.

PubMed

Dos Santos, Rodrigo Campos; Kakazu, Adriana Kaori; Santos, Mariane Gonçalves; Belinelli Silva, Fábio Antônio; Figueiredo, Eduardo Costa

2017-06-01

Anticonvulsant drugs are often used in the treatment of epilepsy. However, their therapeutic monitoring is often necessary in order to obtain an appropriate dose adjustment, due to the proximity between their therapeutic and toxic ranges. The aim of this study was to carry out the synthesis, characterization and use of restricted access carbon nanotubes (RACNTs) in an online method for the analyses of phenobarbital and carbamazepine and primidone from untreated human blood plasma by column switching liquid chromatography. Therefore, the synthesis of RACNTs was carried out through coating commercial Carbon nanotubes with bovine serum albumin (BSA) to subsequently use them as adsorbents in a column switching system operating in the backflush mode. This material was evaluated through the construction of the kinetic and isotherm curves. The experimental data for the interaction of primidone with RACNTs were adequately adjusted to the chemisorption and Sips models for the kinetic and adsorption studies, respectively. The analytical curves ranged from 2.0 to 40.0mgL -1 , with correlation coefficients higher than 0.99, for all the analytes. The LODs of 0.1, 0.1 and 0.01μgmL -1 were defined for PHB, PRM and CBZ, respectively. The relative standard deviation values ranged from 1.0% to 8.4% for the intra assay precision and from 2.7% to 7.6% for inter assay precision. The relative error values ranged from -13.4% to 7.7% for the intra assay accuracy and from -8.6% to 2.5% for the inter assay accuracy. The method was adequately used in the therapeutic monitoring of anticonvulsant drugs in human plasma samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Camera-based ratiometric fluorescence transduction of nucleic acid hybridization with reagentless signal amplification on a paper-based platform using immobilized quantum dots as donors.

PubMed

Noor, M Omair; Krull, Ulrich J

2014-10-21

Paper-based diagnostic assays are gaining increasing popularity for their potential application in resource-limited settings and for point-of-care screening. Achievement of high sensitivity with precision and accuracy can be challenging when using paper substrates. Herein, we implement the red-green-blue color palette of a digital camera for quantitative ratiometric transduction of nucleic acid hybridization on a paper-based platform using immobilized quantum dots (QDs) as donors in fluorescence resonance energy transfer (FRET). A nonenzymatic and reagentless means of signal enhancement for QD-FRET assays on paper substrates is based on the use of dry paper substrates for data acquisition. This approach offered at least a 10-fold higher assay sensitivity and at least a 10-fold lower limit of detection (LOD) as compared to hydrated paper substrates. The surface of paper was modified with imidazole groups to assemble a transduction interface that consisted of immobilized QD-probe oligonucleotide conjugates. Green-emitting QDs (gQDs) served as donors with Cy3 as an acceptor. A hybridization event that brought the Cy3 acceptor dye in close proximity to the surface of immobilized gQDs was responsible for a FRET-sensitized emission from the acceptor dye, which served as an analytical signal. A hand-held UV lamp was used as an excitation source and ratiometric analysis using an iPad camera was possible by a relative intensity analysis of the red (Cy3 photoluminescence (PL)) and green (gQD PL) color channels of the digital camera. For digital imaging using an iPad camera, the LOD of the assay in a sandwich format was 450 fmol with a dynamic range spanning 2 orders of magnitude, while an epifluorescence microscope detection platform offered a LOD of 30 fmol and a dynamic range spanning 3 orders of magnitude. The selectivity of the hybridization assay was demonstrated by detection of a single nucleotide polymorphism at a contrast ratio of 60:1. This work provides an important framework for the integration of QD-FRET methods with digital imaging for a ratiometric transduction of nucleic acid hybridization on a paper-based platform.

Flowing Liquid Anode Atmospheric Pressure Glow Discharge as an Excitation Source for Optical Emission Spectrometry with the Improved Detectability of Ag, Cd, Hg, Pb, Tl, and Zn.

PubMed

Greda, Krzysztof; Swiderski, Krzysztof; Jamroz, Piotr; Pohl, Pawel

2016-09-06

A novel atmospheric pressure glow discharge generated in contact with a flowing liquid anode (FLA-APGD) was developed as the efficient excitation source for the optical emission spectrometry (OES) detection. Differences in the appearance and the electrical characteristic of the FLA-APGD and a conventional system operated with a flowing liquid cathode (FLC-APGD) were studied in detail and discussed. Under the optimal operating conditions for the FLA-APGD, the emission from the analytes (Ag, Cd, Hg, Pb, Tl, and Zn) was from 20 to 120 times higher as compared to the FLC-APGD. Limits of detections (LODs) established with a novel FLA-APGD system were on average 20 times better than those obtained for the FLC-APGD. A further improvement of the LODs was achieved by reducing the background shift interferences and, as a result, the LODs for Ag, Cd, Hg, Pb, Tl, and Zn were 0.004, 0.040, 0.70, 1.7, 0.035, and 0.45 μg L(-1), respectively. The precision of the FLA-APGD-OES method was evaluated to be within 2-5% (as the relative standard deviation of the repeated measurements). The method found its application in the determination of the content of Ag, Cd, Hg, Pb, Tl, and Zn in a certified reference material (CRM) of Lobster hepatopancreas (TORT-2), four brass samples as well as mineral water and tea leaves samples spiked with the analytes. In the case of brass samples, a reference method, i.e., inductively coupled plasma optical emission spectrometry (ICP-OES) was used. A good agreement between the results obtained with FLA-APGD-OES and the certified values for the CRM TORT-2 as well as the reference values obtained with ICP-OES for the brass samples was revealed, indicating the good accuracy of the proposed method. The recoveries obtained for the spiked samples of mineral water and tea leaves were within the range of 97.5-102%.

High-performance thin-layer chromatography (HPTLC) for the simultaneous quantification of the cyclic lipopeptides Surfactin, Iturin A and Fengycin in culture samples of Bacillus species.

PubMed

Geissler, Mareen; Oellig, Claudia; Moss, Karin; Schwack, Wolfgang; Henkel, Marius; Hausmann, Rudolf

2017-02-15

A high-performance thin-layer chromatography method has been established for the identification and simultaneous quantification of the cyclic lipopeptides Surfactin, Iturin A and Fengycin in Bacillus culture samples. B. subtilis DSM 10 T , B. amyloliquefaciens DSM 7 T and B. methylotrophicus DSM 23117 were used as model strains. Culture samples indicated that a sample pretreatment is necessary in order to run HPTLC analyses. A threefold extraction of the cell-free broth with the solvent chloroform/methanol (2:1, v/v) gave best results, when all three lipopeptides were included in the analysis. For the mobile phase, a two-step development was considered most suitable. The first development is conducted with chloroform/methanol/water (65:25:4, v/v/v) over a migration distance of 60mm and the second development using butanol/ethanol/0.1% acetic acid (1:4:1, v/v/v) over a migration distance of 60mm, as well. The method was validated according to Validation of Analytical Procedures: Methodology (FDA Guidance) with respect to the parameters linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy and recovery rate. A linear range with R 2 >0.99 was obtained for all samples from 30ng/zone up to 600ng/zone. The results indicated that quantification of Surfactin has to be performed after the first development (hR F =44), while Fengycin is quantified after the second development (hR F =36, hR F range=20-40). For Iturin A, the results demonstrated that quantification is in favor after the first (hR F =19) development, but also possible after the second (hR F =59) development. LOD and LOQ for Surfactin and Iturin A after the first development, and Fengycin after the second development were determined to be 16ng/zone and 47ng/zone, 13ng/zone and 39ng/zone, and 27ng/zone and 82ng/zone, respectively. Results further revealed the highly accurate and precise character of the developed method with a good inter- and intraday reproducibility. For the precision and accuracy, expressed as % recovery and relative standard deviation, respectively, the determined values did not exceed ±15% as specified by the FDA Guidance. The recovery assay conducted for samples obtained from two strains with the solvent chloroform/methanol (2:1, v/v), which was determined to be most suitable if all three lipopeptides are of interest, gave recoveries of 96.5% and 99.6%, 68.6% and 71.6%, and 102.5% and 95.2% for Surfactin, Iturin A and Fengycin, respectively. Overall, a suitable and reliable method for the simultaneous quantification of the lipopeptides Surfactin, Iturin A and Fengycin in biological samples using HPTLC was successfully developed and validated. Copyright © 2016 Elsevier B.V. All rights reserved.

Local curvature entropy-based 3D terrain representation using a comprehensive Quadtree

NASA Astrophysics Data System (ADS)

Chen, Qiyu; Liu, Gang; Ma, Xiaogang; Mariethoz, Gregoire; He, Zhenwen; Tian, Yiping; Weng, Zhengping

2018-05-01

Large scale 3D digital terrain modeling is a crucial part of many real-time applications in geoinformatics. In recent years, the improved speed and precision in spatial data collection make the original terrain data more complex and bigger, which poses challenges for data management, visualization and analysis. In this work, we presented an effective and comprehensive 3D terrain representation based on local curvature entropy and a dynamic Quadtree. The Level-of-detail (LOD) models of significant terrain features were employed to generate hierarchical terrain surfaces. In order to reduce the radical changes of grid density between adjacent LODs, local entropy of terrain curvature was regarded as a measure of subdividing terrain grid cells. Then, an efficient approach was presented to eliminate the cracks among the different LODs by directly updating the Quadtree due to an edge-based structure proposed in this work. Furthermore, we utilized a threshold of local entropy stored in each parent node of this Quadtree to flexibly control the depth of the Quadtree and dynamically schedule large-scale LOD terrain. Several experiments were implemented to test the performance of the proposed method. The results demonstrate that our method can be applied to construct LOD 3D terrain models with good performance in terms of computational cost and the maintenance of terrain features. Our method has already been deployed in a geographic information system (GIS) for practical uses, and it is able to support the real-time dynamic scheduling of large scale terrain models more easily and efficiently.

Novel loci interacting epistatically with Bone Morphogenetic Protein Receptor 2 cause familial pulmonary arterial hypertension

PubMed Central

Rodriguez-Murillo, Laura; Subaran, Ryan; Stewart, William C. L.; Pramanik, Sreemanta; Marathe, Sudhir; Barst, Robyn J.; Chung, Wendy K.; Greenberg, David A.

2009-01-01

Background Familial pulmonary arterial hypertension (FPAH) is a rare, autosomal-dominant inherited disease with low penetrance. Mutations in the Bone Morphogenetic Protein Receptor 2 (BMPR2) have been identified in at least 70% of FPAH patients. However, the lifetime penetrance of these BMPR2 mutations is 10-20%, suggesting that genetic and/or environmental modifiers are required for disease expression. Our goal in this study is to identify genetic loci that may influence FPAH expression in BMPR2-mutation-carriers. Methods We performed a genome-wide linkage scan in 15 FPAH families segregating for BMPR2 mutations. We used a dense SNP array and a novel multi-scan linkage procedure that provides increased power and precision for the localization of linked loci. Results We observed linkage evidence in four regions: 3q22 (median LOD=3.43), 3p12 (median LOD = 2.35), 2p22 (median LOD = 2.21), and 13q21 (median LOD = 2.09). When used in conjunction with the nonparametric bootstrap, our approach yields high-resolution to identify candidate gene regions containing putative BMPR2-interacting genes. Imputation of the disease model by LOD score maximization indicates that the 3q22 locus alone predicts most FPAH cases in BMPR2-mutation carriers, providing strong evidence that BMPR2 and the 3q22 locus interact epistatically. Conclusions Our findings suggest that genotypes at loci in the newly-identified regions, especially at 3q22, could improve FPAH risk prediction in FPAH families and suggest other targets for therapeutic intervention. PMID:19864167

Novel loci interacting epistatically with bone morphogenetic protein receptor 2 cause familial pulmonary arterial hypertension.

PubMed

Rodriguez-Murillo, Laura; Subaran, Ryan; Stewart, William C L; Pramanik, Sreemanta; Marathe, Sudhir; Barst, Robyn J; Chung, Wendy K; Greenberg, David A

2010-02-01

Familial pulmonary arterial hypertension (FPAH) is a rare, autosomal-dominant, inherited disease with low penetrance. Mutations in the bone morphogenetic protein receptor 2 (BMPR2) have been identified in at least 70% of FPAH patients. However, the lifetime penetrance of these BMPR2 mutations is 10% to 20%, suggesting that genetic and/or environmental modifiers are required for disease expression. Our goal in this study was to identify genetic loci that may influence FPAH expression in BMPR2 mutation carriers. We performed a genome-wide linkage scan in 15 FPAH families segregating for BMPR2 mutations. We used a dense single-nucleotide polymorphism (SNP) array and a novel multi-scan linkage procedure that provides increased power and precision for the localization of linked loci. We observed linkage evidence in four regions: 3q22 ([median log of the odds (LOD) = 3.43]), 3p12 (median LOD) = 2.35), 2p22 (median LOD = 2.21), and 13q21 (median LOD = 2.09). When used in conjunction with the non-parametric bootstrap, our approach yields high-resolution to identify candidate gene regions containing putative BMPR2-interacting genes. Imputation of the disease model by LOD-score maximization indicates that the 3q22 locus alone predicts most FPAH cases in BMPR2 mutation carriers, providing strong evidence that BMPR2 and the 3q22 locus interact epistatically. Our findings suggest that genotypes at loci in the newly identified regions, especially at 3q22, could improve FPAH risk prediction in FPAH families. We also suggest other targets for therapeutic intervention.

Combining markers with and without the limit of detection

PubMed Central

Dong, Ting; Liu, Catherine Chunling; Petricoin, Emanuel F.; Tang, Liansheng Larry

2014-01-01

In this paper, we consider the combination of markers with and without the limit of detection (LOD). LOD is often encountered when measuring proteomic markers. Because of the limited detecting ability of an equipment or instrument, it is difficult to measure markers at a relatively low level. Suppose that after some monotonic transformation, the marker values approximately follow multivariate normal distributions. We propose to estimate distribution parameters while taking the LOD into account, and then combine markers using the results from the linear discriminant analysis. Our simulation results show that the ROC curve parameter estimates generated from the proposed method are much closer to the truth than simply using the linear discriminant analysis to combine markers without considering the LOD. In addition, we propose a procedure to select and combine a subset of markers when many candidate markers are available. The procedure based on the correlation among markers is different from a common understanding that a subset of the most accurate markers should be selected for the combination. The simulation studies show that the accuracy of a combined marker can be largely impacted by the correlation of marker measurements. Our methods are applied to a protein pathway dataset to combine proteomic biomarkers to distinguish cancer patients from non-cancer patients. PMID:24132938

[Determination of tungsten and cobalt in the air of workplace by ICP-OES].

PubMed

Zhang, J; Ding, C G; Li, H B; Song, S; Yan, H F

2017-08-20

Objective: To establish the inductively coupled plasma optical emission spectrometry (ICP-OES) method for determination of cobalt and tungsten in the air of workplace. Methods: The cobalt and tungsten were collected by filter membrane and then digested by nitric acid, inductively coupled plasma optical emission spectrometry (ICP-OES) was used for the detection of cobalt and tungsten. Results: The linearity of tungsten was good at the range of 0.01-1 000 μg/ml with a correlation coefficient of 0.999 9, the LOD and LOQ were 0.006 7 μg/ml and 0.022 μg/ml, respectively. The recovery was ranged from 98%-101%, the RSD of intra-and inter-batch precision were 1.1%-3.0% and 2.1%-3.8%, respectively. The linearity of cobalt was good at the range of 0.01-100 μg/ml with a correlation coefficient of 0.999 9, the LOD and LOQ were 0.001 2 μg/ml and 0.044 μg/ml, respectively. The recovery was ranged from 95%-97%, the RSD of intra-and inter-batch precision were 1.1%-2.4% and 1.1%-2.9%, respectively. The sampling efficiency of tungsten and cobalt were higher than 94%. Conclusion: The linear range, sensitivity and precision of the method was suitable for the detection of tungsten and cobalt in the air of workplace.

Quantitative Determination of L-DOPA in Seeds of Mucuna Pruriens Germplasm by High Performance Thin Layer Chromatography

PubMed Central

Raina, Archana P.; Khatri, Renu

2011-01-01

Mucuna pruriens Linn. is an important medicinal plant used for treatment of Parkinson's disease and many others in ancient Indian medical system. L-DOPA extracted from seeds of Mucuna is a constituent of more than 200 indigenous drug formulations and is more effective as drug than the synthetic counterpart. A densitometric high performance thin-layer chromatographic (HPTLC) method was developed for quantification of L-DOPA content present in the seeds extract. The method involves separation of L-DOPA on precoated silica gel 60 GF254 HPTLC plates using a solvent system of n-butanol-acetic-acid-water (4:1:1, v/v) as the mobile phase. Quantification was done at 280 nm using absorbance reflectance mode. Linearity was found in the concentration range of 100 to 1000 ng/spot with the correlation coefficient value of 0.9980. The method was validated for accuracy, precision and repeatability. Mean recovery was 100.89%. The LOD and LOQ for L-DOPA determination were found to be 3.41 ng/spot and 10.35 ng/spot respectively. The proposed HPTLC method was found to be precise, specific and accurate for quantitative determination of L-DOPA. It can be used for rapid screening of large germplasm collections of Mucuna pruriens for L-DOPA content. The method was used to study variation in fifteen accessions of Mucuna germplasm collected from different geographical regions. PMID:22707835

Quantitative Determination of L-DOPA in Seeds of Mucuna Pruriens Germplasm by High Performance Thin Layer Chromatography.

PubMed

Raina, Archana P; Khatri, Renu

2011-07-01

Mucuna pruriens Linn. is an important medicinal plant used for treatment of Parkinson's disease and many others in ancient Indian medical system. L-DOPA extracted from seeds of Mucuna is a constituent of more than 200 indigenous drug formulations and is more effective as drug than the synthetic counterpart. A densitometric high performance thin-layer chromatographic (HPTLC) method was developed for quantification of L-DOPA content present in the seeds extract. The method involves separation of L-DOPA on precoated silica gel 60 GF(254) HPTLC plates using a solvent system of n-butanol-acetic-acid-water (4:1:1, v/v) as the mobile phase. Quantification was done at 280 nm using absorbance reflectance mode. Linearity was found in the concentration range of 100 to 1000 ng/spot with the correlation coefficient value of 0.9980. The method was validated for accuracy, precision and repeatability. Mean recovery was 100.89%. The LOD and LOQ for L-DOPA determination were found to be 3.41 ng/spot and 10.35 ng/spot respectively. The proposed HPTLC method was found to be precise, specific and accurate for quantitative determination of L-DOPA. It can be used for rapid screening of large germplasm collections of Mucuna pruriens for L-DOPA content. The method was used to study variation in fifteen accessions of Mucuna germplasm collected from different geographical regions.

A HPLC-DAD method for the simultaneous determination of five marker components in the traditional herbal medicine Bangpungtongsung-san

PubMed Central

Weon, Jin Bae; Yang, Hye Jin; Ma, Jin Yeul; Ma, Choong Je

2011-01-01

Background: Bangpungtongsung-san, one of the traditional herbal medicines, was known to be a prescription for obesity. Objective: For the simultaneous determination of five components (paeoniflorin, 6-gingerol, decursin, geniposide, and glycyrrhizin) in Bangpungtongsung-san, a high-performance liquid chromatography with diode-array detector method was established. Materials and Methods: To develop the method, a reverse phase column, DIONEX C 18 (5 μm, 120 µ, 4.6 mm × 150 mm) was used. The mobile phase consisted of methanol and water using a gradient elution. The UV wavelength was set at 230, 240, and 254 nm. Method validation was accomplished by linearity, precision test, and recovery test. Results: All calibration curves of components showed good linearity (R 2 > 0.9959). The limit of detection (LOD) and limit of quantification (LOQ) ranged from 0.01 to 0.17 μg/ml and 0.04 to 0.53 μg/ml, respectively. The relative standard deviations (RSD) value of precision test, intraday and interday tests were less than 0.43% and 1.26%. In the recovery test, results of accuracy ranged from 95.27% to 107.70% with RSD values less than 2.21%. Conclusion: This developed method was applied to the commercial Bangpungtongsung-san sample and the five marker components were separated effectively without interference of any peaks of components. PMID:21472081

Validation of a Method for Cylindrospermopsin Determination in Vegetables: Application to Real Samples Such as Lettuce (Lactuca sativa L.).

PubMed

Prieto, Ana I; Guzmán-Guillén, Remedios; Díez-Quijada, Leticia; Campos, Alexandre; Vasconcelos, Vitor; Jos, Ángeles; Cameán, Ana M

2018-02-01

Reports on the occurrence of the cyanobacterial toxin cylindrospermopsin (CYN) have increased worldwide because of CYN toxic effects in humans and animals. If contaminated waters are used for plant irrigation, these could represent a possible CYN exposure route for humans. For the first time, a method employing solid phase extraction and quantification by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) of CYN was optimized in vegetables matrices such as lettuce ( Lactuca sativa ). The validated method showed a linear range, from 5 to 500 ng CYN g -1 of fresh weight (f.w.), and detection and quantitation limits (LOD and LOQ) of 0.22 and 0.42 ng CYN g -1 f.w., respectively. The mean recoveries ranged between 85 and 104%, and the intermediate precision from 12.7 to 14.7%. The method showed to be robust for the three different variables tested. Moreover, it was successfully applied to quantify CYN in edible lettuce leaves exposed to CYN-contaminated water (10 µg L -1 ), showing that the tolerable daily intake (TDI) in the case of CYN could be exceeded in elderly high consumers. The validated method showed good results in terms of sensitivity, precision, accuracy, and robustness for CYN determination in leaf vegetables such as lettuce. More studies are needed in order to prevent the risks associated with the consumption of CYN-contaminated vegetables.

Capillary electrophoresis coupled with chloroform-acetonitrile extraction for rapid and highly selective determination of cysteine and homocysteine levels in human blood plasma and urine.

PubMed

Ivanov, Alexander Vladimirovich; Bulgakova, Polina Olegovna; Virus, Edward Danielevich; Kruglova, Maria Petrovna; Alexandrin, Valery Vasil'evich; Gadieva, Viktoriya Aleksandrovna; Luzyanin, Boris Petrovich; Kushlinskii, Nikolai Evgen'evich; Fedoseev, Anatolij Nikolaevich; Kubatiev, Aslan Amirkhanovich

2017-10-01

A rapid and selective method has been developed for highly sensitive determination of total cysteine and homocysteine levels in human blood plasma and urine by capillary electrophoresis (CE) coupled with liquid-liquid extraction. Analytes were first derivatized with 1,1'-thiocarbonyldiimidazole and then samples were purified by chloroform-ACN extraction. Electrophoretic separation was performed using 0.1 M phosphate with 30 mM triethanolamine, pH 2, containing 25 μM CTAB, 2.5 μM SDS, and 2.5% polyethylene glycol 600. Samples were injected into the capillary (with total length 32 cm and 50 μm id) at 2250 mbar*s and subsequent injection was performed for 30 s with 0.5 M KОН. The total analysis time was less than 9 min, accuracy was 98%, and precision was <2.6%. The LOD was 0.2 μM for homocysteine and 0.5 μM for cysteine. The use of liquid-liquid extraction allowed the precision and sensitivity of the CE method to be significantly increased. The validated method was applied to determine total cysteine and homocysteine content in human blood plasma and urine samples obtained from healthy volunteers and patients with kidney disorders. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Enantioseparation and determination of the chiral fungicide furametpyr enantiomers in rice, soil, and water by high-performance liquid chromatography.

PubMed

Dong, Fengshou; Chen, Xiu; Xu, Jun; Liu, Xingang; Chen, Zenglong; Li, Yuanbo; Zhang, Hongjun; Zheng, Yongquan

2013-12-01

The chiral fungicide furametpyr is widely used in the rice field to control rice sheath blight; however, furametpyr enantiomers are treated as just one compound in traditional achiral analysis, which gives only partial information. An effective chiral analytical method was developed for the resolution and determination of the fungicide furametpyr enantiomers in rice, soil, and water samples. Furametpyr enantiomers were excellently separated and determined on a Chiralpak AD-H column with n-hexane/ethanol (90:10, v/v) as mobile phase at a flow rate of 0.8 mL min(-1) with UV detection at 220 nm. The resolution was up to 8.85. The first eluted enantiomer was (+)-furametpyr and the second eluted one was (-)-furametpyr. The effects of mobile-phase composition and column temperature on the enantioseparation were evaluated. The method was validated for linearity, repeatability, accuracy, limit of detection (LOD), and limit of quantification LOQ. LOD was 2.0 µg kg(-1) in water, 0.02 mg kg(-1) in soil, and 0.07 mg kg(-1) in rice with an LOQ of 6.7 µg kg(-1) in water, 0.07 mg kg(-1) in soil, and 0.23 mg kg(-1) in rice. The average recoveries of the pesticide in all matrices ranged from 73.1 to 101.8% for all fortification levels. The precision values associated with the analytical method, expressed as relative standard deviation (RSD) values, were below 14.0% in all matrices. The methodology was successfully applied for the enantioselective analysis of furametpyr enantiomers in real samples. © 2013 Wiley Periodicals, Inc.

Variability of pesticide residues in cauliflower units collected from a field trial and market places in Greece.

PubMed

Prodhan, M D H; Papadakis, Emmanouil-N; Papadopoulou-Mourkidou, Euphemia

2016-09-01

To estimate the variability of pesticide residue levels present in cauliflower units, a total of 142 samples were collected from a field trial of a cooperative farmer, and 120 samples were collected from different market places in Thessaloniki, Greece. The collected samples were extracted using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction technique, and the residues were determined by liquid chromatography-tandem mass spectrometry. The developed method was validated by evaluating the accuracy, precision, linearity, limit of detection (LOD), and limit of quantification (LOQ). The average recoveries for all the analytes, derived from the data of control samples fortified at 0.01, 0.05, 0.1, and 0.2 mg/kg, ranged from 74 to 110% with a relative standard deviation of ≤8%. The correlation coefficient (R(2)) was ≥0.997 for all the analytes using matrix-matched calibration standards. The LOD values ranged from 0.001 to 0.003 mg/kg, and the LOQ was determined at 0.01 mg/kg for all the sought analytes. The matrix effect was found to be at a considerable level, especially for cypermethrin and deltamethrin, amounting to +90% and +145%, respectively. For the field samples, the unit-to-unit variability factors (VFs) calculated for cypermethrin and deltamethrin were 2.38 and 2.32, respectively, while the average VF for the market basket samples was 5.11. In the market basket samples, residues of cypermethrin, deltamethrin, chlorpyrifos, and indoxacarb were found at levels ≥LOQ and their respective VFs were 7.12, 5.67, 5.28, and 2.40.

Analysis of lysergic acid amide in human serum and urine after ingestion of Argyreia nervosa seeds.

PubMed

Paulke, Alexander; Kremer, Christian; Wunder, Cora; Toennes, Stefan W

2012-08-01

The ergot alkaloid lysergic acid amide (LSA) is a secondary plant constituent in a number of plants, but it is mainly present in considerable amounts in Convolvulaceae, like Argyreia nervosa. Due to its close structural similarity to lysergic acid diethylamide, LSA is considered as psychedelic and therefore promoted as so-called "legal high" in various internet forums. During a human behavioral study with orally administered seeds of A. nervosa, blood and urine samples were obtained. The present study describes the validation of a sensitive and robust high performance liquid chromatography method with fluorescence detection, which was applied to the study samples. The limit of detection (LOD) and lower limit of quantification in human serum were 0.05 and 0.17 ng/mL, respectively, and in urine, the LOD was 0.15 ng/mL. Intra- and interday precision and accuracy were below 15 % relative standard deviation with a bias better than ±15 %. No conversion of LSA to its epimer iso-LSA was noted during analyses. The LSA concentrations in the authentic human serum samples were in the range of 0.66 to 3.15 ng/mL approximately 2 h after ingestion. In urine, LSA could be found 1-24 h after ingestion; after 48 h, no LSA could be detected. The LSA epimer iso-LSA was also detected in serum and urine in varying ratios. In conclusion, LSA serum levels in the low nanogram per milliliter range correlated with severe vegetative adverse effects (nausea, weakness, fatigue, tremor, blood pressure elevation) and a psychosis-like state, which led to study termination.

Simultaneous determination of LSD and 2-oxo-3-hydroxy LSD in hair and urine by LC-MS/MS and its application to forensic cases.

PubMed

Jang, Moonhee; Kim, Jihyun; Han, Inhoi; Yang, Wonkyung

2015-11-10

Lysergic acid diethylamide (LSD) is administered in low dosages, which makes its detection in biological matrices a major challenge in forensic toxicology. In this study, two sensitive and reliable methods based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) were established and validated for the simultaneous determination of LSD and its metabolite, 2-oxo-3-hydroxy-LSD (O-H-LSD), in hair and urine. Target analytes in hair were extracted using methanol at 38°C for 15h and analyzed by LC-MS/MS. For urine sample preparation, liquid-liquid extraction was performed. Limits of detection (LODs) in hair were 0.25pg/mg for LSD and 0.5pg/mg for O-H-LSD. In urine, LODs were 0.01 and 0.025ng/ml for LSD and O-H-LSD, respectively. Method validation results showed good linearity and acceptable precision and accuracy. The developed methods were applied to authentic specimens from two legal cases of LSD ingestion, and allowed identification and quantification of LSD and O-H-LSD in the specimens. In the two cases, LSD concentrations in hair were 1.27 and 0.95pg/mg; O-H-LSD was detected in one case, but its concentration was below the limit of quantification. In urine samples collected from the two suspects 8 and 3h after ingestion, LSD concentrations were 0.48 and 2.70ng/ml, respectively, while O-H-LSD concentrations were 4.19 and 25.2ng/ml, respectively. These methods can be used for documenting LSD intake in clinical and forensic settings. Copyright © 2015 Elsevier B.V. All rights reserved.

Ultra high performance liquid chromatography-time of flight mass spectrometry for analysis of avocado fruit metabolites: method evaluation and applicability to the analysis of ripening degrees.

PubMed

Hurtado-Fernández, Elena; Pacchiarotta, Tiziana; Gómez-Romero, María; Schoenmaker, Bart; Derks, Rico; Deelder, André M; Mayboroda, Oleg A; Carrasco-Pancorbo, Alegría; Fernández-Gutiérrez, Alberto

2011-10-21

We have developed an analytical method using UHPLC-UV/ESI-TOF MS for the comprehensive profiling of the metabolites found in the methanolic extracts of 13 different varieties of avocado at two different ripening degrees. Both chromatographic and detection parameters were optimized in order to maximize the number of compounds detected and the sensitivity. After achieving the optimum conditions, we performed a complete analytical validation of the method with respect to its linearity, sensitivity, precision, accuracy and possible matrix effects. The LODs ranged from 1.64 to 730.54 ppb (in negative polarity) for benzoic acid and chrysin, respectively, whilst they were found within the range from 0.51 to 310.23 ppb in positive polarity. The RSDs for repeatability test did not exceed 7.01% and the accuracy ranged from 97.2% to 102.0%. Our method was then applied to the analysis of real avocado samples and advanced data processing and multivariate statistical analysis (PCA, PLS-DA) were carried out to discriminate/classify the examined avocado varieties. About 200 compounds belonging to various structural classes were tentatively identified; we are certain about the identity of around 60 compounds, 20 of which have been quantified in terms of their own commercially available standard. Copyright © 2011 Elsevier B.V. All rights reserved.

Ordered Monolayer Gold Nano-urchin Structures and Their Size Induced Control for High Gas Sensing Performance

PubMed Central

Sabri, Ylias M.; Kandjani, Ahmad Esmaielzadeh; Ippolito, Samuel J.; Bhargava, Suresh K.

2016-01-01

The synthesis of ordered monolayers of gold nano-urchin (Au-NU) nanostructures with controlled size, directly on thin films using a simple electrochemical method is reported in this study. In order to demonstrate one of the vast potential applications, the developed Au-NUs were formed on the electrodes of transducers (QCM) to selectively detect low concentrations of elemental mercury (Hg0) vapor. It was found that the sensitivity and selectivity of the sensor device is enhanced by increasing the size of the nanospikes on the Au-NUs. The Au-NU-12 min QCM (Au-NUs with nanospikes grown on it for a period of 12 min) had the best performance in terms of transducer based Hg0 vapor detection. The sensor had 98% accuracy, 92% recovery, 96% precision (repeatability) and significantly, showed the highest sensitivity reported to date, resulting in a limit of detection (LoD) of only 32 μg/m3 at 75 °C. When compared to the control counterpart, the accuracy and sensitivity of the Au-NU-12 min was enhanced by ~2 and ~5 times, respectively. The results demonstrate the excellent activity of the developed materials which can be applied to a range of applications due to their long range order, tunable size and ability to form directly on thin-films. PMID:27090570

Sensitive determination of cholesterol and its metabolic steroid hormones by UHPLC-MS/MS via derivatization coupled with dual ultrasonic-assisted dispersive liquid-liquid microextraction.

PubMed

Zhao, Xian-En; Yan, Ping; Wang, Renjun; Zhu, Shuyun; You, Jinmao; Bai, Yu; Liu, Huwei

2016-08-01

Quantitative analysis of cholesterol and its metabolic steroid hormones plays a vital role in diagnosing endocrine disorders and understanding disease progression, as well as in clinical medicine studies. Because of their extremely low abundance in body fluids, it remains a challenging task to develop a sensitive detection method. A hyphenated technique of dual ultrasonic-assisted dispersive liquid-liquid microextraction (dual-UADLLME) coupled with microwave-assisted derivatization (MAD) was proposed for cleansing, enrichment and sensitivity enhancement. 4'-Carboxy-substituted rosamine (CSR) was synthesized and used as derivatization reagent. An ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method was developed for determination of cholesterol and its metabolic steroid hormones in the multiple reaction monitoring mode. Parameters of dual-UADLLME, MAD and UHPLC-MS/MS were all optimized. Satisfactory linearity, recovery, repeatability, accuracy and precision, absence of matrix effect and extremely low limits of detection (LODs, 0.08-0.15 pg mL(-1) ) were achieved. Through the combination of dual-UADLLME and MAD, a determination method for cholesterol and its metabolic steroid hormones in human plasma, serum and urine samples was developed and validated with high sensitivity, selectivity, accuracy and perfect matrix effect results. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Spectrophotometric Determination of Mycophenolate Mofetil as Its Charge-Transfer Complexes with Two π-Acceptors

PubMed Central

Vinay, K. B.; Revanasiddappa, H. D.; Raghu, M. S.; Abdulrahman, Sameer. A. M.; Rajendraprasad, N.

2012-01-01

Two simple, selective, and rapid spectrophotometric methods are described for the determination of mycophenolate mofetil (MPM) in pure form and in tablets. Both methods are based on charge-transfer complexation reaction of MPM with p-chloranilic acid (p-CA) or 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) in dioxane-acetonitrile medium resulting in coloured product measurable at 520 nm (p-CA) or 580 nm (DDQ). Beer's law is obeyed over the concentration ranges of 40–400 and 12–120 μg mL−1 MPM for p-CA and DDQ, respectively, with correlation coefficients (r) of 0.9995 and 0.9947. The apparent molar absorptivity values are calculated to be 1.06 × 103 and 3.87 × 103 L mol−1 cm−1, respectively, and the corresponding Sandell's sensitivities are 0.4106 and 0.1119 μg cm−1. The limits of detection (LOD) and quantification (LOQ) are also reported for both methods. The described methods were successfully applied to the determination of MPM in tablets. Statistical comparison of the results with those of the reference method showed excellent agreement. No interference was observed from the common excipients present in tablets. Both methods were validated statistically for accuracy and precision. The accuracy and reliability of the methods were further ascertained by recovery studies via standard addition procedure. PMID:22567572

Ordered Monolayer Gold Nano-urchin Structures and Their Size Induced Control for High Gas Sensing Performance

NASA Astrophysics Data System (ADS)

Sabri, Ylias M.; Kandjani, Ahmad Esmaielzadeh; Ippolito, Samuel J.; Bhargava, Suresh K.

2016-04-01

The synthesis of ordered monolayers of gold nano-urchin (Au-NU) nanostructures with controlled size, directly on thin films using a simple electrochemical method is reported in this study. In order to demonstrate one of the vast potential applications, the developed Au-NUs were formed on the electrodes of transducers (QCM) to selectively detect low concentrations of elemental mercury (Hg0) vapor. It was found that the sensitivity and selectivity of the sensor device is enhanced by increasing the size of the nanospikes on the Au-NUs. The Au-NU-12 min QCM (Au-NUs with nanospikes grown on it for a period of 12 min) had the best performance in terms of transducer based Hg0 vapor detection. The sensor had 98% accuracy, 92% recovery, 96% precision (repeatability) and significantly, showed the highest sensitivity reported to date, resulting in a limit of detection (LoD) of only 32 μg/m3 at 75 °C. When compared to the control counterpart, the accuracy and sensitivity of the Au-NU-12 min was enhanced by ~2 and ~5 times, respectively. The results demonstrate the excellent activity of the developed materials which can be applied to a range of applications due to their long range order, tunable size and ability to form directly on thin-films.

Synthesis and application of a new thiazolylazo reagent for cloud point extraction and determination of cobalt in pharmaceutical preparations.

PubMed

Yamaki, Regina Terumi; Nunes, Luana Sena; de Oliveira, Hygor Rodrigues; Araújo, André S; Bezerra, Marcos Almeida; Lemos, Valfredo Azevedo

2011-01-01

The synthesis and characterization of the reagent 2-(5-bromothiazolylazo)-4-chlorophenol and its application in the development of a preconcentration procedure for cobalt determination using flame atomic absorption spectrometry after cloud point extraction is presented. This procedure is based on cobalt complexing and entrapment of the metal chelates into micelles of a surfactant-rich phase of Triton X-114. The preconcentration procedure was optimized by using a response surface methodology through the application of the Box-Behnken matrix. Under optimum conditions, the procedure determined the presence of cobalt with an LOD of 2.8 microg/L and LOQ of 9.3 microg/L. The enrichment factor obtained was 25. The precision was evaluated as the RSD, which was 5.5% for 10 microg/L cobalt and 6.9% for 30 microg/L. The accuracy of the procedure was assessed by comparing the results with those found using inductively coupled plasma-optical emission spectrometry. After validation, the procedure was applied to the determination of cobalt in pharmaceutical preparation samples containing cobalamin (vitamin B12).

Simultaneous determination of eight flavonoids in the flowers of Matricaria chamomilla by high performance liquid chromatography.

PubMed

Xie, Xiao-Yu; Chen, Fang-Fang; Shi, Yan-Ping

2014-01-01

An HPLC method was developed for simultaneous determination of five flavones (apigenin, three apigenin 7-O-glucoside acylated derivatives, and luteolin) and three methoxylated flavonols in Matricaria chamomilla. Full validation of the assay was carried out including linearity, LODs, LOQs, precision, repeatability, stability, and accuracy. The results demonstrated that the method developed was simple, accurate, and reliable. Five batches of M. chamomilla samples were determined using the developed method, and total contents of the eight flavonoids ranged from 1.843 to 2.134 mg/g. Among them, the content of apigenin was the highest with values of 0.538 to 0.618 mg/g. In addition, the extract solution from M. chamomilla exhibited a significant dose-dependent inhibition of 2,2-diphenyl-1-picrylhydrazyl (DPPH) activity, with a 50% inhibition (SC50) at a concentration of 3.06 +/- 0.09 mg/mL, and the flavonoids apigenin-7-O-(6"-acetyl)-glucoside, luteolin, apigenin, eupatolitin, and chrysosplenol D played an important role in the antioxidant activities of the extract solution from M. chamomilla.

Semi-preparative HPLC preparation and HPTLC quantification of tetrahydroamentoflavone as marker in Semecarpus anacardium and its polyherbal formulations.

PubMed

Aravind, S G; Arimboor, Ranjith; Rangan, Meena; Madhavan, Soumya N; Arumughan, C

2008-11-04

Application of modern scientific knowledge coupled with sensitive analytical technique is important for the quality evaluation and standardization of polyherbal formulations. Semecarpus anacardium, an important medicinal plant with wide medicinal properties, is frequently used in a large number of traditional herbal preparations. Tetrahydroamentoflavone (THA), a major bioactive biflavonoid was selected as a chemical marker of S. anacardium and RP-semi-preparative HPLC conditions were optimized for the isolation of tetrahydroamentoflavone. HPTLC analytical method was developed for the fingerprinting of S. anacardium flavonoids and quantification of tetrahydroamentoflavone. The method was validated in terms of their linearity, LOD, LOQ, precision and accuracy and compared with RP-HPLC-DAD method. The methods were demonstrated for the chemical fingerprinting of S. anacardium plant parts and some commercial polyherbal formulations and the amount of tetrahydroamentoflavone was quantified. HPTLC analysis showed that S. anacardium seed contained approximately 10 g kg(-1) of tetrahydroamentoflavone. The methods were able to identify and quantify tetrahydroamentoflavone from complex mixtures of phytochemicals and could be extended to the marker-based standardization of polyherbal formulations, containing S. anacardium.

Periodic modulation-based stochastic resonance algorithm applied to quantitative analysis for weak liquid chromatography-mass spectrometry signal of granisetron in plasma

NASA Astrophysics Data System (ADS)

Xiang, Suyun; Wang, Wei; Xiang, Bingren; Deng, Haishan; Xie, Shaofei

2007-05-01

The periodic modulation-based stochastic resonance algorithm (PSRA) was used to amplify and detect the weak liquid chromatography-mass spectrometry (LC-MS) signal of granisetron in plasma. In the algorithm, the stochastic resonance (SR) was achieved by introducing an external periodic force to the nonlinear system. The optimization of parameters was carried out in two steps to give attention to both the signal-to-noise ratio (S/N) and the peak shape of output signal. By applying PSRA with the optimized parameters, the signal-to-noise ratio of LC-MS peak was enhanced significantly and distorted peak shape that often appeared in the traditional stochastic resonance algorithm was corrected by the added periodic force. Using the signals enhanced by PSRA, this method extended the limit of detection (LOD) and limit of quantification (LOQ) of granisetron in plasma from 0.05 and 0.2 ng/mL, respectively, to 0.01 and 0.02 ng/mL, and exhibited good linearity, accuracy and precision, which ensure accurate determination of the target analyte.

Simultaneous Determination of Ursodeoxycholic Acid and Chenodeoxycholic Acid in Pharmaceutical Dosage Form by HPLC-UV Detection.

PubMed

Khairy, Mostafa A; Mansour, Fotouh R

2017-01-01

A reversed-phase HPLC method was developed for the simultaneous determination of ursodeoxycholic acid (UDCA) and the epimeric isomer, chenodeoxycholic acid (CDCA), in their synthetic mixtures and in tablet dosage form. The proposed HPLC method uses a C18 column and mobile phase consisting of an acetonitrile-phosphate buffer mixture (pH 2.3, 100 mM; 50 + 50, v/v) at a flow rate of 2.0 mL/min with UV detection at 210 nm. The method was validated according to the International Conference on Harmonization guidelines; and linearity, range, accuracy, precision, robustness, and system suitability were studied. The LOD and LOQ were also calculated and found to be 1.23 and 3.73 μg/mL for UDCA and 0.83 and 2.52 μg/mL for CDCA, respectively. The method was adapted for UHPLC, in which baseline separation was achieved in <2.5 min. The assay results of Ursomix tablets by the developed method were statistically compared with those obtained by the reference method using t- and F-tests, and no significant differences were observed.

Water-Soluble Dried Blood Spot in Protein Analysis: A Proof-of-Concept Study.

PubMed

Rosting, Cecilie; Gjelstad, Astrid; Halvorsen, Trine Grønhaug

2015-08-04

In the present work human chorionic gonadotropin (hCG) was used as a model protein in a proof-of-concept study combining water-soluble dried blood spot (DBS) material in liquid chromatography-tandem mass spectrometry (LC-MS/MS)-based protein analysis. A water-soluble material consisting of commercially available carboxymethyl cellulose (CMC) was evaluated as sampling material for this purpose. The material dissolved readily at physiological pH. Different sample preparation methods were evaluated, and in the final method, 15 μL of whole blood was deposited and dried on CMC before the whole spot was dissolved prior to cleanup by immunoaffinity extraction, tryptic digest, and preconcentration by solid-phase extraction (SPE). The results indicated complete dissolution of hCG from the spots, acceptable limit of detection (LOD) (0.1 IU/mL), linearity (R(2) = 0.959), accuracy (16%), and precision (≤22%). Long-term stability (45 days) of hCG in dried spots at reduced temperatures (≤8 °C) was also demonstrated. The analyte recovery was comparable to the commercially available nonsolvable cellulose material (FTA DMPK-C card).

Spectrofluorimetric Method for Estimation of Curcumin in Rat Blood Plasma: Development and Validation

NASA Astrophysics Data System (ADS)

Trivedi, J.; Variya, B.; Gandhi, H.; Rathod, S. P.

2016-01-01

Curcumin is a medicinally important phytoconstituent of curcuminoids. The present study describes development of a simple method for estimation of curcumin in rat plasma. This method involves the use of spectrofluorimetry for evaluation of curcumin at 257 (Ex) and 504 nm (Em). Sample preparation involves only two steps: extraction of curcumin and drying the extract. Following this procedure, the samples are reconstituted with ethyl acetate, and relative fluorescence intensity is measured using a spectrofluorimeter. The method was validated as per CDER guidelines. The linearity of the method was found to be in the range of 100-500 ng/mL with accuracy and precision lying within 2% RSD. The LOD and LOQ were found to be 15.3 and 46.1 ng/mL, respectively. The method was applied for pharmacokinetic evaluation in rats, and AUC, Cmax, and Tmax were found to be 5580 ± 1006 h × ng/mL, 1526 ± 209 ng/mL, and 2.97 ± 0.28 h, respectively, with a plasma half-life of 1.14 ± 0.27 h.

Simultaneous determination of atorvastatin calcium, ezetimibe, and fenofibrate in a tablet formulation by HPLC.

PubMed

Patel, Archita; Macwana, Chhaya; Parmar, Vishal; Patel, Samir

2012-01-01

An accurate, simple, reproducible, and sensitive HPLC method was developed and validated for the simultaneous determination of atorvastatin calcium, ezetimibe, and fenofibrate in a tablet formulation. The analyses were performed on an RP C18 column, 150 x 4.60 mm id, 5 pm particle size. The mobile phase methanol-acetonitrile-water (76 + 13 + 11, v/v/v), was pumped at a constant flow rate of 1 mL/min. UV detection was performed at 253 nm. Retention times of atorvastatin calcium, ezetimibe, and fenofibrate were found to be 2.25, 3.68, and 6.41 min, respectively. The method was validated in terms of linearity, precision, accuracy, LOD, LOQ, and robustness. The response was linear in the range 2-10 microg/mL (r2 = 0.998) for atorvastatin calcium, 2-10 microg/mL (r2 = 0.998) for ezetimibe, and 40-120 microg/mL (r2 = 0.998) for fenofibrate. The developed method can be used for routine quality analysis of the drugs in the tablet formulation.

Multiresidue analysis of 22 sulfonamides and their metabolites in animal tissues using quick, easy, cheap, effective, rugged, and safe extraction and high resolution mass spectrometry (hybrid linear ion trap-Orbitrap).

PubMed

Abdallah, H; Arnaudguilhem, C; Jaber, F; Lobinski, R

2014-08-15

A new high performance liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) method was developed for a simultaneous multi-residue analysis of 22 sulfonamides (SAs) and their metabolites in edible animal (pig, beef, sheep and chicken) tissues. Sample preparation was optimized on the basis of the "QuEChERS" protocol. The analytes were identified using their LC retention times and accurate mass; the identification was further confirmed by multi-stage high mass accuracy (<5ppm) mass spectrometry. The performance of the method was evaluated according to the EU guidelines for the validation of screening methods for the analysis of veterinary drugs residues. Acceptable values were obtained for: linearity (R(2)<0.99), limit of detection (LOD, 3-26μg/kg), limit of quantification (LOQ, 11-88μg/kg), accuracy (recovery 88-112%), intra- and inter-day precision 1-14 and 1-17%, respectively, decision limit (CCα) and detection capability (CCβ) around the maximum residue limits (MRL) of SAs (100μg/kg). The method was validated by analysis of a reference material FAPAS-02188 "Pig kidney" with ǀ Z-scoreǀ<0.63. The method was applied to various matrices (kidney, liver, muscle) originated from pig, beef, sheep, and chicken) allowing the simultaneous quantification of target sulfonamides at concentration levels above the MRL/2 and the identification of untargeted compounds such as N(4)-acetyl metabolites using multi-stage high mass accuracy mass spectrometry. Copyright © 2014 Elsevier B.V. All rights reserved.

High Frequency Variations in Earth Orientation Derived From GNSS Observations

NASA Astrophysics Data System (ADS)

Weber, R.; Englich, S.; Snajdrova, K.; Boehm, J.

2006-12-01

Current observations gained by the space geodetic techniques, especially VLBI, GPS and SLR, allow for the determination of Earth Orientation Parameters (EOPs - polar motion, UT1/LOD, nutation offsets) with unprecedented accuracy and temporal resolution. This presentation focuses on contributions to the EOP recovery provided by satellite navigation systems (primarily GPS). The IGS (International GNSS Service), for example, currently provides daily polar motion with an accuracy of less than 0.1mas and LOD estimates with an accuracy of a few microseconds. To study more rapid variations in polar motion and LOD we established in a first step a high resolution (hourly resolution) ERP-time series from GPS observation data of the IGS network covering the period from begin of 2005 till March 2006. The calculations were carried out by means of the Bernese GPS Software V5.0 considering observations from a subset of 79 fairly stable stations out of the IGb00 reference frame sites. From these ERP time series the amplitudes of the major diurnal and semidiurnal variations caused by ocean tides are estimated. After correcting the series for ocean tides the remaining geodetic observed excitation is compared with variations of atmospheric excitation (AAM). To study the sensitivity of the estimates with respect to the applied mapping function we applied both the widely used NMF (Niell Mapping Function) and the VMF1 (Vienna Mapping Function 1). In addition, based on computations covering two months in 2005, the potential improvement due to the use of additional GLONASS data will be discussed. Finally, satellite techniques are also able to provide nutation offset rates with respect to the most recent nutation model. Based on GPS observations from 2005 we established nutation rate time series and subsequently derived the amplitudes of several nutation waves with periods less than 30 days. The results are compared to VLBI estimates processed by means of the OCCAM 6.1 software.

Validation of an enzyme-linked immunosorbent assay screening method and a liquid chromatography-tandem mass spectrometry confirmation method for the identification and quantification of ketamine and norketamine in urine samples from Malaysia.

PubMed

Harun, Norlida; Anderson, Robert A; Miller, Eleanor I

2009-01-01

An ELISA and a liquid chromatography-tandem mass spectrometry (LC-MS-MS) confirmation method were developed and validated for the identification and quantitation of ketamine and its major metabolite norketamine in urine samples. The Neogen ketamine microplate ELISA was optimized with respect to sample and enzyme conjugate volumes and the sample preincubation time before addition of the enzyme conjugate. The ELISA kit was validated to include an assessment of the dose-response curve, intra- and interday precision, limit of detection (LOD), and cross-reactivity. The sensitivity and specificity were calculated by comparison to the results from the validated LC-MS-MS confirmation method. An LC-MS-MS method was developed and validated with respect to LOD, lower limit of quantitation (LLOQ), linearity, recovery, intra- and interday precision, and matrix effects. The ELISA dose-response curve was a typical S-shaped binding curve, with a linear portion of the graph observed between 25 and 500 ng/mL for ketamine. The cross-reactivity of 200 ng/mL norketamine to ketamine was 2.1%, and no cross-reactivity was detected with 13 common drugs tested at 10,000 ng/mL. The ELISA LOD was calculated to be 5 ng/mL. Both intra- (n = 10) and interday (n = 50) precisions were below 5.0% at 25 ng/mL. The LOD for ketamine and norketamine was calculated statistically to be 0.6 ng/mL. The LLOQ values were also calculated statistically and were 1.9 ng/mL and 2.1 ng/mL for ketamine and norketamine, respectively. The test linearity was 0-1200 ng/mL with correlation coefficient (R(2)) > 0.99 for both analytes. Recoveries at 50, 500, and 1000 ng/mL range from 97.9% to 113.3%. Intra- (n = 5) and interday (n = 25) precisions between extracts for ketamine and norketamine were excellent (< 10%). Matrix effects analysis showed an average ion suppression of 5.7% for ketamine and an average ion enhancement of 13.0% for norketamine for urine samples collected from six individuals. A comparison of ELISA and LC-MS-MS results demonstrated a sensitivity, specificity, and efficiency of 100%. These results indicated that a cutoff value of 25 ng/mL ketamine in the ELISA screen is particularly suitable and reliable for urine testing in a forensic toxicology setting. Furthermore, both ketamine and norketamine were detected in all 34 urine samples collected from individuals socializing in pubs by the Royal Malaysian Police. Ketamine concentrations detected by LC-MS-MS ranged from 22 to 31,670 ng/mL, and norketamine concentrations ranged from 25 to 10,990 ng/mL. The concentrations of ketamine and norketamine detected in the samples are most ikely indicative of ketamine abuse.

3D Visualization of Urban Area Using Lidar Technology and CityGML

NASA Astrophysics Data System (ADS)

Popovic, Dragana; Govedarica, Miro; Jovanovic, Dusan; Radulovic, Aleksandra; Simeunovic, Vlado

2017-12-01

3D models of urban areas have found use in modern world such as navigation, cartography, urban planning visualization, construction, tourism and even in new applications of mobile navigations. With the advancement of technology there are much better solutions for mapping earth’s surface and spatial objects. 3D city model enables exploration, analysis, management tasks and presentation of a city. Urban areas consist of terrain surfaces, buildings, vegetation and other parts of city infrastructure such as city furniture. Nowadays there are a lot of different methods for collecting, processing and publishing 3D models of area of interest. LIDAR technology is one of the most effective methods for collecting data due the large amount data that can be obtained with high density and geometrical accuracy. CityGML is open standard data model for storing alphanumeric and geometry attributes of city. There are 5 levels of display (LoD0, LoD1, LoD2, LoD3, LoD4). In this study, main aim is to represent part of urban area of Novi Sad using LIDAR technology, for data collecting, and different methods for extraction of information’s using CityGML as a standard for 3D representation. By using series of programs, it is possible to process collected data, transform it to CityGML and store it in spatial database. Final product is CityGML 3D model which can display textures and colours in order to give a better insight of the cities. This paper shows results of the first three levels of display. They consist of digital terrain model and buildings with differentiated rooftops and differentiated boundary surfaces. Complete model gives us a realistic view of 3D objects.

Use of ceric ammonium sulphate and two dyes, methyl orange and indigo carmine, in the determination of lansoprazole in pharmaceuticals.

PubMed

Basavaiah, Kanakapura; Ramakrishna, Veeraiah; Kumar, Urdigere Rangachar Anil

2007-06-01

Two spectrophotometric methods are proposed for the assay of lansoprazole (LPZ) in bulk drug and in dosage forms using ceric ammonium sulphate (CAS) and two dyes, methyl orange and indigo carmine, as reagents. The methods involve addition of a known excess of CAS to LPZ in acid medium, followed by determination of residual CAS by reacting with a fixed amount of either methyl orange, measuring the absorbance at 520 nm (method A), or indigo carmine, measuring the absorbance at 610 nm (method B). In both methods, the amount of CAS reacted corresponds to the amount of LPZ and the measured absorbance was found to increase linearly with the concentration of LPZ, which is corroborated by the correlation coefficients of 0.9979 and 0.9954 for methods A and B, respectively. The systems obey Beer's law for 0.5-7.0 microg mL(-1) and 0.25-3.0 microg mL(-1) for methods A and B, respectively. The apparent molar absorptivities were calculated to be 3.0 x 10(4) and 4.4 x 10(4) L mol(-1) cm(-1) for methods A and B, respectively. The limits of detection (LOD) and quantification (LOQ) were calculated to be 0.08 and 0.25 microg mL(-1) for method A, and 0.09 and 0.27 microg mLs(-1) for method B, respectively. The intra-day and inter-day precision and accuracy of the methods were evaluated according to the current ICH guidelines. Both methods were of comparable accuracy (er < or = 2 %). Also, both methods are equally precise as shown by the relative standard deviation values < 1.5%. No interference was observed from common pharmaceutical adjuvants. The accuracy of the methods was further ascertained by performing recovery studies using the standard addition method. The methods were successfully applied to the assay of LPZ in capsule preparations and the results were statistically compared with those of the literature UV-spectrophotometric method by applying Student's t-test and F-test.

Improving Semantic Updating Method on 3d City Models Using Hybrid Semantic-Geometric 3d Segmentation Technique

NASA Astrophysics Data System (ADS)

Sharkawi, K.-H.; Abdul-Rahman, A.

2013-09-01

Cities and urban areas entities such as building structures are becoming more complex as the modern human civilizations continue to evolve. The ability to plan and manage every territory especially the urban areas is very important to every government in the world. Planning and managing cities and urban areas based on printed maps and 2D data are getting insufficient and inefficient to cope with the complexity of the new developments in big cities. The emergence of 3D city models have boosted the efficiency in analysing and managing urban areas as the 3D data are proven to represent the real world object more accurately. It has since been adopted as the new trend in buildings and urban management and planning applications. Nowadays, many countries around the world have been generating virtual 3D representation of their major cities. The growing interest in improving the usability of 3D city models has resulted in the development of various tools for analysis based on the 3D city models. Today, 3D city models are generated for various purposes such as for tourism, location-based services, disaster management and urban planning. Meanwhile, modelling 3D objects are getting easier with the emergence of the user-friendly tools for 3D modelling available in the market. Generating 3D buildings with high accuracy also has become easier with the availability of airborne Lidar and terrestrial laser scanning equipments. The availability and accessibility to this technology makes it more sensible to analyse buildings in urban areas using 3D data as it accurately represent the real world objects. The Open Geospatial Consortium (OGC) has accepted CityGML specifications as one of the international standards for representing and exchanging spatial data, making it easier to visualize, store and manage 3D city models data efficiently. CityGML able to represents the semantics, geometry, topology and appearance of 3D city models in five well-defined Level-of-Details (LoD), namely LoD0 to LoD4. The accuracy and structural complexity of the 3D objects increases with the LoD level where LoD0 is the simplest LoD (2.5D; Digital Terrain Model (DTM) + building or roof print) while LoD4 is the most complex LoD (architectural details with interior structures). Semantic information is one of the main components in CityGML and 3D City Models, and provides important information for any analyses. However, more often than not, the semantic information is not available for the 3D city model due to the unstandardized modelling process. One of the examples is where a building is normally generated as one object (without specific feature layers such as Roof, Ground floor, Level 1, Level 2, Block A, Block B, etc). This research attempts to develop a method to improve the semantic data updating process by segmenting the 3D building into simpler parts which will make it easier for the users to select and update the semantic information. The methodology is implemented for 3D buildings in LoD2 where the buildings are generated without architectural details but with distinct roof structures. This paper also introduces hybrid semantic-geometric 3D segmentation method that deals with hierarchical segmentation of a 3D building based on its semantic value and surface characteristics, fitted by one of the predefined primitives. For future work, the segmentation method will be implemented as part of the change detection module that can detect any changes on the 3D buildings, store and retrieve semantic information of the changed structure, automatically updates the 3D models and visualize the results in a userfriendly graphical user interface (GUI).

Simultaneous determination of four neuroprotective compounds of Tilia amurensis by high performance liquid chromatography coupled with diode array detector

PubMed Central

Lee, Bohyung; Weon, Jin Bae; Yun, Bo-Ra; Lee, Jiwoo; Eom, Min Rye; Ma, Choong Je

2014-01-01

Background: Tilia amurensis consists of various compounds, such as flavonoids and terpenoids. Objective: A simple and reliable high performance liquid chromatography (HPLC) coupled with the diode array detector (DAD) method has been established for simultaneous determination of epicatechin, nudiposide, lyoniside, and scopoletin isolated from Tilia amurensis. Materials and Methods: Optimum separations were obtained with a SHISEIDO C18 column by gradient eluton, with 0.1% Trifluoroacetic acid (TFA) water-methanol as the mobile phase. The gradient elution system was completed within 40 minutes. The flow rate and detection wavelength were 1 mL/minute, 205 nm, 250 nm, and 280 nm, respectively. Results: Validation of the analytical method was evaluated by linearity, precision, and the accuracy test. The calibration curve was linear over the established range with R2 > 0.997. The limit of detection (LOD) and limit of quantification (LOQ) ranged from 0.01-15.20 μg/mL and 0.03-46.06 μg/mL. The method exhibited an intraday and interday precision range of 96.25-105.66% and 93.52-109.92%, respectively (RSD <2.80%). The recoveries and relative standard deviation (RSD) of the four compounds in Tilia amurensis were in the range of 90.42-104.84% and 0.2-2.58%. Conclusion: This developed method was accurate and reliable for the quality evaluation of the four compounds isolated from Tilia amurensis. PMID:25210303

Simultaneous determination of four 5-hydroxy polymethoxyflavones by reversed-phase high performance liquid chromatography with electrochemical detection.

PubMed

Dong, Ping; Qiu, Peiju; Zhu, Yi; Li, Shiming; Ho, Chi-Tang; McClements, David Julian; Xiao, Hang

2010-01-29

Accumulating evidence has suggested the potential health-promoting effects of 5-hydroxy polymethoxyflavones (5-OH-PMFs) naturally existing in citrus genus. However, research efforts are hampered by the lack of reliable and sensitive methods for their determination in plant materials and biological samples. Using reversed-phase high performance liquid chromatography (HPLC) equipped with electrochemical (EC) detection, we have developed a fast and highly sensitive method for quantification of four 5-OH-PMFs, namely 5-hydroxy-6,7,8,3',4'-pentamethoxyflavone, 5-hydroxy-3,6,7,8,3',4'-hexamethoxyflavone, 5-hydroxy-6,7,4'-trimethoxyflavone, and 5-hydroxy-6,7,8,4'-tetramethoxyflavone. The method was fully validated in terms of linearity, accuracy and precision. The limit of detection (LOD) was determined as being between 0.65 and 1.8ng/mL (ppb), demonstrating an over 160 times higher sensitivity in comparison with the previously reported method using UV detection. The recovery rate of the method was between 96.17% and 110.82%, and the precision for the retention times and peak areas was all below 13%. The method was successfully used to quantify 5-OH-PMFs with a wide range of abundance in the citrus products and preparations, such as orange juice, citrus peel, and dried tangerine peel. The quantification method for 5-OH-PMFs developed herein could be useful for the nutritional and pharmacological studies of these compounds in future. Copyright (c) 2009 Elsevier B.V. All rights reserved.

Validation of a Method for Cylindrospermopsin Determination in Vegetables: Application to Real Samples Such as Lettuce (Lactuca sativa L.)

PubMed Central

Prieto, Ana I.; Díez-Quijada, Leticia; Campos, Alexandre; Vasconcelos, Vitor

2018-01-01

Reports on the occurrence of the cyanobacterial toxin cylindrospermopsin (CYN) have increased worldwide because of CYN toxic effects in humans and animals. If contaminated waters are used for plant irrigation, these could represent a possible CYN exposure route for humans. For the first time, a method employing solid phase extraction and quantification by ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) of CYN was optimized in vegetables matrices such as lettuce (Lactuca sativa). The validated method showed a linear range, from 5 to 500 ng CYN g−1 of fresh weight (f.w.), and detection and quantitation limits (LOD and LOQ) of 0.22 and 0.42 ng CYN g−1 f.w., respectively. The mean recoveries ranged between 85 and 104%, and the intermediate precision from 12.7 to 14.7%. The method showed to be robust for the three different variables tested. Moreover, it was successfully applied to quantify CYN in edible lettuce leaves exposed to CYN-contaminated water (10 µg L−1), showing that the tolerable daily intake (TDI) in the case of CYN could be exceeded in elderly high consumers. The validated method showed good results in terms of sensitivity, precision, accuracy, and robustness for CYN determination in leaf vegetables such as lettuce. More studies are needed in order to prevent the risks associated with the consumption of CYN-contaminated vegetables. PMID:29389882

Quantitative determination of insulin entrapment efficiency in triblock copolymeric nanoparticles by high-performance liquid chromatography.

PubMed

Xu, Xiongliang; Fu, Yao; Hu, Haiyan; Duan, Yourong; Zhang, Zhirong

2006-04-11

A rapid and effective isocratic chromatographic procedure was described in this paper for the determination of insulin entrapment efficiency (EE) in triblock copolymeric nanoparticles using reversed-phase high-performance liquid chromatography (RP-HPLC) with an ultraviolet/visible detector at low flow rate. The method has been developed on a Shimadzu Shim-pack VP-ODS column (150 mm x 4.6 mm, 5 microm, Chiyoda-Ku, Tokyo, Japan) using a mixture of 0.2 M sodium sulfate anhydrous solution adjusted to pH 2.3 with phosphoric acid and acetonitrile (73:27, v/v) as mobile phase at the flow rate of 0.8 ml min(-1) and a 214 nm detection. The method was validated in terms of selectivity, linearity, precision, accuracy, solution stability, limit of detection (LOD) and limit of quantification (LOQ). The calibration curve was linear in the concentration range of 2.0-500.0 microg ml(-1), and the limits of detection and quantitation were 8 and 20 ng, respectively. The mean recovery of insulin from spiked samples, in a concentration range of 8-100 microg ml(-1), was 98.96% (R.S.D.= 2.51%, n = 9). The intra- and inter-assay coefficients of variation were less than 2.24%. The proposed method has the advantages of simple pretreatment, rapid isolation, high specificity and precision, which can be used for direct analysis of insulin in commercially available raw materials, formulations of nanoparticles, and drug release as well as stability studies.

Validated Spectrophotometric and RP-HPLC-DAD Methods for the Determination of Ursodeoxycholic Acid Based on Derivatization with 2-Nitrophenylhydrazine.

PubMed

El-Kafrawy, Dina S; Belal, Tarek S; Mahrous, Mohamed S; Abdel-Khalek, Magdi M; Abo-Gharam, Amira H

2017-05-01

This work describes the development, validation, and application of two simple, accurate, and reliable methods for the determination of ursodeoxycholic acid (UDCA) in bulk powder and in pharmaceutical dosage forms. The carboxylic acid group in UDCA was exploited for the development of these novel methods. Method 1 is the colorimetric determination of the drug based on its reaction with 2-nitrophenylhydrazine hydrochloride in the presence of a water-soluble carbodiimide coupler [1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride] and pyridine to produce an acid hydrazide derivative, which ionizes to yield an intense violet color with maximum absorption at 553 nm. Method 2 uses reversed-phase HPLC with diode-array detection for the determination of UDCA after precolumn derivatization using the same reaction mentioned above. The acid hydrazide reaction product was separated using a Pinnacle DB C8 column (4.6 × 150 mm, 5 μm particle size) and a mobile phase consisting of 0.01 M acetate buffer (pH 3)-methanol-acetonitrile (30 + 30 + 40, v/v/v) isocratically pumped at a flow rate of 1 mL/min. Ibuprofen was used as the internal standard (IS). The peaks of the reaction product and IS were monitored at 400 nm. Different experimental parameters for both methods were carefully optimized. Analytical performance of the developed methods were statistically validated for linearity, range, precision, accuracy, specificity, robustness, LOD, and LOQ. Calibration curves showed good linear relationships for concentration ranges 32-192 and 60-600 μg/mL for methods 1 and 2, respectively. The proposed methods were successfully applied for the assay of UDCA in bulk form, capsules, and oral suspension with good accuracy and precision. Assay results were statistically compared with a reference pharmacopeial HPLC method, and no significant differences were observed between proposed and reference methods.

Comparison of analytical performances of inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectrometry for trace analysis of bismuth and bismuth oxide

NASA Astrophysics Data System (ADS)

Medvedev, Nickolay S.; Shaverina, Anastasiya V.; Tsygankova, Alphiya R.; Saprykin, Anatoly I.

2018-04-01

The paper presents а comparison of analytical performances of inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) for trace analysis of high purity bismuth and bismuth oxide. Matrix effects in the ICP-MS and ICP-AES methods were studied as a function of Bi concentration, ICP power and nebulizer flow rate. For ICP-MS the strong dependence of the matrix effects versus the atomic mass of analytes was observed. For ICP-AES the minimal matrix effects were achieved for spectral lines of analytes with low excitation potentials. The optimum degree of sample dilution providing minimum values of the limits of detection (LODs) was chosen. Both methods let us to reach LODs from n·10-7 to n·10-4 wt% for more than 50 trace elements. For most elements the LODs of ICP-MS were lower in comparison to ICP-AES. Validation of accuracy of the developed techniques was performed by "added-found" experiments and by comparison of the results of ICP-MS and ICP-AES analysis of high-purity bismuth oxide.

A comparison of LOD and UT1-UTC forecasts by different combined prediction techniques

NASA Astrophysics Data System (ADS)

Kosek, W.; Kalarus, M.; Johnson, T. J.; Wooden, W. H.; McCarthy, D. D.; Popiński, W.

Stochastic prediction techniques including autocovariance, autoregressive, autoregressive moving average, and neural networks were applied to the UT1-UTC and Length of Day (LOD) International Earth Rotation and Reference Systems Servive (IERS) EOPC04 time series to evaluate the capabilities of each method. All known effects such as leap seconds and solid Earth zonal tides were first removed from the observed values of UT1-UTC and LOD. Two combination procedures were applied to predict the resulting LODR time series: 1) the combination of the least-squares (LS) extrapolation with a stochastic predition method, and 2) the combination of the discrete wavelet transform (DWT) filtering and a stochastic prediction method. The results of the combination of the LS extrapolation with different stochastic prediction techniques were compared with the results of the UT1-UTC prediction method currently used by the IERS Rapid Service/Prediction Centre (RS/PC). It was found that the prediction accuracy depends on the starting prediction epochs, and for the combined forecast methods, the mean prediction errors for 1 to about 70 days in the future are of the same order as those of the method used by the IERS RS/PC.

Quantitation of polymorphic impurity in entecavir polymorphic mixtures using powder X-ray diffractometry and Raman spectroscopy.

PubMed

Kang, Yanlei; Shao, Zhanying; Wang, Qiang; Hu, Xiurong; Yu, Dongdong

2018-05-26

Entecavir was used for the treatment of chronic hepatitis B through inhibiting hepatitis B virus. The anhydrous form of entecavir (ENT-A) often appeared as impurity polymorph in the manufacturing process of entecavir monohydrate (ENT-H) such as granulation, drying and compression. Since different crystal forms might affect drug bioavailability and therapeutic effect, it was vital to control the ENT-A content of the drug product. The work aimed to develop useful methods to assess ENT-A weight percentage in ENT-H. Powder X-ray diffractometry (PXRD) and Raman spectrometric methods were applied. Binary mixtures with different ratios of pure ENT-H and pure ENT-A were scanned using PXRD and Raman to obtain spectra. Then peak heights and peak areas versus weight percentage were used to construct calibration curves. The best linear regression analysis data for PXRD and Raman method were found to be R 2  = 0.9923 and R 2  = 0.9953, in the weight ratio range of 2.1-20.2% w/w% of ENT-A in binary mixtures. Limit of detection (LOD) of ENT-A was 0.38% and limit of quantitation (LOQ) was 1.15% for PXRD method. LOD and LOQ for Raman method were 0.48% and 1.16%. The results showed that PXRD and Raman methods: both were precise and accurate, and could be used for measurement of ENT-A content in the selected weight percentage range. Partial least squares (PLS) algorithm with four data pre-processing methods: including multiplicative scatter correlation (MSC), standard normal variate (SNV), first and second derivatives were applied and evaluated using prediction errors. The best performance of PLS was R 2  = 0.9958 with RMSEC (0.44%) and RMSEP (0.65%). Multivariate analysis for Raman spectra showed similar good results with univariate analysis, and would be an advantageous method when there were overlapped peaks in the spectra. In summary, the proposed PXRD and Raman method could be developed for the quality control of ENT-H. And Raman was a more promising method in industrial practice due to its slightly better precision, accuracy and time-saving advantage. Copyright © 2018 Elsevier B.V. All rights reserved.

Improved LIBS limit of detection of Be, Mg, Si, Mn, Fe and Cu in aluminum alloy samples using a portable Echelle spectrometer with ICCD camera

NASA Astrophysics Data System (ADS)

Mohamed, Walid Tawfik Y.

2008-02-01

Laser-induced breakdown spectroscopy (LIBS) is a laser-based technique that can provide non-intrusive, qualitative and quantitative measurement of metals in various environments. LIBS uses the plasma generated by a high-energy laser beam to prepare and excite the sample in one step. In the present work, LIBS has been applied to perform elemental analysis of six trace elements simultaneously in aluminum alloy targets. The plasma is generated by focusing a pulsed Nd:YAG laser on the target in air at atmospheric pressure. LIBS limit of detection (LOD) is affected by many experimental parameters such as interferences, self-absorption, spectral overlap and matrix effect. We aimed to improve the LIBS LOD by optimizing these experimental parameters as possible. In doing so, a portable Echelle spectrometer with intensified CCD camera was used to detect the LIBS plasma emission. This advanced Echelle spectrometer provides a constant spectral resolution (CSR) of 7500 corresponding to 4 pixels FWHM over a wavelength range 200-1000 nm displayable in a single spectrum. Then, the calibration curves for iron, beryllium, magnesium, silicon, manganese and copper as minor elements were achieved with linear regression coefficients between 98-99% on average in aluminum standard sample alloys. New LOD values were achieved in the ppm range with high precision (RSD 3-8%). From the application view point, improving LIBS LOD is very important in the on-line industrial process control to follow-up multi-elements for the correct alloying in metals.

Rapid Development and Validation of Improved Reversed-Phase High-performance Liquid Chromatography Method for the Quantification of Mangiferin, a Polyphenol Xanthone Glycoside in Mangifera indica

PubMed Central

Naveen, P.; Lingaraju, H. B.; Prasad, K. Shyam

2017-01-01

Mangiferin, a polyphenolic xanthone glycoside from Mangifera indica, is used as traditional medicine for the treatment of numerous diseases. The present study was aimed to develop and validate a reversed-phase high-performance liquid chromatography (RP-HPLC) method for the quantification of mangiferin from the bark extract of M. indica. RP-HPLC analysis was performed by isocratic elution with a low-pressure gradient using 0.1% formic acid: acetonitrile (87:13) as a mobile phase with a flow rate of 1.5 ml/min. The separation was done at 26°C using a Kinetex XB-C18 column as stationary phase and the detection wavelength at 256 nm. The proposed method was validated for linearity, precision, accuracy, limit of detection, limit of quantification, and robustness by the International Conference on Harmonisation guidelines. In linearity, the excellent correlation coefficient more than 0.999 indicated good fitting of the curve and also good linearity. The intra- and inter-day precision showed < 1% of relative standard deviation of peak area indicated high reliability and reproducibility of the method. The recovery values at three different levels (50%, 100%, and 150%) of spiked samples were found to be 100.47, 100.89, and 100.99, respectively, and low standard deviation value < 1% shows high accuracy of the method. In robustness, the results remain unaffected by small variation in the analytical parameters, which shows the robustness of the method. Liquid chromatography–mass spectrometry analysis confirmed the presence of mangiferin with M/Z value of 421. The assay developed by HPLC method is a simple, rapid, and reliable for the determination of mangiferin from M. indica. SUMMARY The present study was intended to develop and validate an RP-HPLC method for the quantification of mangiferin from the bark extract of M. indica. The developed method was validated for linearity, precision, accuracy, limit of detection, limit of quantification and robustness by International Conference on Harmonization guidelines. This study proved that the developed assay by HPLC method is a simple, rapid and reliable for the quantification of the mangiferin from M. indica. Abbreviations Used: M. indica: Mangifera indica, RP-HPLC: Reversed-phase high-performance liquid chromatography, M/Z: Mass to charge ratio, ICH: International conference on harmonization, % RSD: Percentage of relative standard deviation, ppm: Parts per million, LOD: Limit of detection, LOQ: Limit of quantification. PMID:28539748

Rapid Development and Validation of Improved Reversed-Phase High-performance Liquid Chromatography Method for the Quantification of Mangiferin, a Polyphenol Xanthone Glycoside in Mangifera indica.

PubMed

Naveen, P; Lingaraju, H B; Prasad, K Shyam

2017-01-01

Mangiferin, a polyphenolic xanthone glycoside from Mangifera indica , is used as traditional medicine for the treatment of numerous diseases. The present study was aimed to develop and validate a reversed-phase high-performance liquid chromatography (RP-HPLC) method for the quantification of mangiferin from the bark extract of M. indica . RP-HPLC analysis was performed by isocratic elution with a low-pressure gradient using 0.1% formic acid: acetonitrile (87:13) as a mobile phase with a flow rate of 1.5 ml/min. The separation was done at 26°C using a Kinetex XB-C18 column as stationary phase and the detection wavelength at 256 nm. The proposed method was validated for linearity, precision, accuracy, limit of detection, limit of quantification, and robustness by the International Conference on Harmonisation guidelines. In linearity, the excellent correlation coefficient more than 0.999 indicated good fitting of the curve and also good linearity. The intra- and inter-day precision showed < 1% of relative standard deviation of peak area indicated high reliability and reproducibility of the method. The recovery values at three different levels (50%, 100%, and 150%) of spiked samples were found to be 100.47, 100.89, and 100.99, respectively, and low standard deviation value < 1% shows high accuracy of the method. In robustness, the results remain unaffected by small variation in the analytical parameters, which shows the robustness of the method. Liquid chromatography-mass spectrometry analysis confirmed the presence of mangiferin with M/Z value of 421. The assay developed by HPLC method is a simple, rapid, and reliable for the determination of mangiferin from M. indica . The present study was intended to develop and validate an RP-HPLC method for the quantification of mangiferin from the bark extract of M. indica . The developed method was validated for linearity, precision, accuracy, limit of detection, limit of quantification and robustness by International Conference on Harmonization guidelines. This study proved that the developed assay by HPLC method is a simple, rapid and reliable for the quantification of the mangiferin from M. indica . Abbreviations Used: M. indica : Mangifera indica , RP-HPLC: Reversed-phase high-performance liquid chromatography, M/Z: Mass to charge ratio, ICH: International conference on harmonization, % RSD: Percentage of relative standard deviation, ppm: Parts per million, LOD: Limit of detection, LOQ: Limit of quantification.

Spectrofluorimetric method for the determination of sulpiride in pharmaceutical preparations and human plasma through derivatization with 2-cyanoacetamide.

PubMed

Shah, Jasmin; Jan, M Rasul; Khan, M Naeem; Shah, Sultan

2013-01-01

A sensitive and accurate spectrofluorimetric method has been developed for the determination of sulpiride in pharmaceutical preparations and human plasma. The developed method is based on the derivatization reaction of 2-cyanoacetamide with sulpiride in 30% ammonical solution. The fluorescent derivatized reaction product exhibited maximum fluorescence intensity at 379 nm after excitation at 330 nm. The optimum conditions for derivatization reactions were studied and the fluorescence intensity versus concentration plot was found to be linear over the concentration range 0.2-20.0 µg/mL with a correlation coefficient of 0.9985. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.82 and 2.73 ng/mL, respectively. The proposed method was validated according to ICH guidelines. The effects of common excipients and co-administered drugs were also studied. The accuracy of the method was checked using the standard addition method and percent recoveries were found to be in the range of 99.00-101.25% for pharmaceutical preparations and 97.00-97.80% for spiked human plasma. The method was successfully applied to commercial formulations and the results obtained for the proposed method were compared with a high-performance liquid chromatography reference method and statistically evaluated using the Student's t-test for accuracy and the variance ratio F-test for precision. A reaction pathway was also proposed. Copyright © 2012 John Wiley & Sons, Ltd.

Development and validation of a single LC-MS/MS assay following SPE for simultaneous hair analysis of amphetamines, opiates, cocaine and metabolites.

PubMed

Imbert, L; Dulaurent, S; Mercerolle, M; Morichon, J; Lachâtre, G; Gaulier, J-M

2014-01-01

The two major challenges in hair analysis are the limited amount of samples usually available and the low targeted concentrations. To overcome these limitations, a liquid chromatography-electrospray-tandem mass spectrometry method (LC-ESI-MS/MS) allowing the simultaneous analysis of 17 amphetamines (amphetamine, BDB, m-CPP, dexfenfluramine, DOB, DOM, ephedrine, MBDB, MDA, MDEA, MDMA, methamphetamine, methylphenidate, 4-MTA, norephedrine, norfenfluramine and PMA), 5 opiates (morphine, codeine, heroin, ethylmorphine, and 6AM), cocaine and 5 metabolites [ecgonine methyl ester (EME), benzoylecgonine (BZE), anhydroecgonine methyl ester (AME), cocaethylene, and norcocaine] has been developed. The validation procedure included linearity, intra-day and inter-day variability and accuracy for 5 days (5 replicates at 3 concentration levels). Proficiency studies were used to check the accuracy of the method. As a result, all amphetamines, opiates and cocaine derivatives were satisfactory identified by 2 MRM transitions in 15 min. Calibration curves were performed by a quadratic 1/X weighted regression. The calibration model fits from 0.05 to 10 ng/mg. The limits of detection (LODs) range between 0.005 and 0.030 ng/mg. Precision has been checked by intra-day and inter-day RSD, and associated relative bias, which were lower than 25% for the limits of quantifications (LOQs) and lower than 20% for the other levels tested. This method was routinely applied to hair samples: two positive results of adult drug addicts are presented. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

A sensitive detection assay based on signal amplification technology for Alzheimer's disease's early biomarker in exosome.

PubMed

Zhou, Jie; Meng, Lingchang; Ye, Weiran; Wang, Qiaolei; Geng, Shizhen; Sun, Chong

2018-08-31

Alzheimer's disease (AD) considered as the third health "killer" has seriously threatened the health of the elderly. However, the modern diagnostic strategies of AD present several disadvantages: the low accuracy and specificity resulting in some false-negative diagnoses, and the poor sensitivity leading to a delayed treatment. In view of this situation, a enzyme-free and target-triggered signal amplification strategy, based on graphene oxide (GO) and entropy-driven strand displacement reaction (ESDR) principle, was proposed. In this strategy, when the hairpin structure probes (H)specially binds with beta-amyloid-(1-42) oligomers (Aβ42 oligomers), it's structure will be opened, causing the bases complementary to FAM-labeled replacement probes R (R1 and R2) exposed. At this time, R1 and R2 will hybridize with H, resulting in the bound Aβ42 oligomers released. The released Aβ42 oligomers would participate in the next cycle reaction, making the signal amplified. As a quencher, GO could absorb the free single-stranded DNA R1 and R2 and quench their fluorescence; however, the DNA duplex still exists free and keeps its signal-on. Through the detection of Aβ42 oligomers in exosomes, this ultrasensitive detection method with the advantages of low limit of detection (LOD, 20 pM), great accuracy, excellent precision and convenience provides an excellent prospect for AD's early diagnosis. Copyright © 2018 Elsevier B.V. All rights reserved.

Application of ultra-high pressure liquid chromatography linear ion-trap orbitrap to qualitative and quantitative assessment of pesticide residues.

PubMed

Farré, M; Picó, Y; Barceló, D

2014-02-07

The analysis of pesticides residues using a last generation high resolution and high mass accuracy hybrid linear ion trap-Orbitrap mass spectrometer (LTQ-Orbitrap-MS) was explored. Pesticides were extracted from fruits, fish, bees and sediments by QuEChERS and from water by solid-phase with Oasis HLB cartridges. Ultra-high pressure liquid chromatography (UHPLC)-LTQ-Orbitrap mass spectrometer acquired full scan MS data for quantification, and data dependent (dd) MS(2) and MS(3) product ion spectra for identification and/or confirmation. The regression coefficients (r(2)) for the calibration curves (two order of magnitude up to the lowest calibration level) in the study were ≥0.99. The LODs for 54 validated compounds were ≤2ngmL(-1) (analytical standards). The relative standard deviation (RSD), which was used to estimate precision, was always lower than 22%. The recovery of extraction and matrix effects ranged from 58 to 120% and from -92 to 52%, respectively. Mass accuracy was always ≤4ppm, corresponding to a maximum mass error of 1.6millimass units (mmu). This procedure was then successfully applied to pesticide residues in a set of the above-mentioned food and environmental samples. In addition to target analytes, this method enables the simultaneous detection/identification of non-target pesticides, pharmaceuticals, drugs of abuse, mycotoxins, and their metabolites. Copyright © 2013 Elsevier B.V. All rights reserved.

S-193 scatterometer backscattering cross section precision/accuracy for Skylab 2 and 3 missions

NASA Technical Reports Server (NTRS)

Krishen, K.; Pounds, D. J.

1975-01-01

Procedures for measuring the precision and accuracy with which the S-193 scatterometer measured the background cross section of ground scenes are described. Homogeneous ground sites were selected, and data from Skylab missions were analyzed. The precision was expressed as the standard deviation of the scatterometer-acquired backscattering cross section. In special cases, inference of the precision of measurement was made by considering the total range from the maximum to minimum of the backscatter measurements within a data segment, rather than the standard deviation. For Skylab 2 and 3 missions a precision better than 1.5 dB is indicated. This procedure indicates an accuracy of better than 3 dB for the Skylab 2 and 3 missions. The estimates of precision and accuracy given in this report are for backscattering cross sections from -28 to 18 dB. Outside this range the precision and accuracy decrease significantly.

Comparison of Methods for Analyzing Left-Censored Occupational Exposure Data

PubMed Central

Huynh, Tran; Ramachandran, Gurumurthy; Banerjee, Sudipto; Monteiro, Joao; Stenzel, Mark; Sandler, Dale P.; Engel, Lawrence S.; Kwok, Richard K.; Blair, Aaron; Stewart, Patricia A.

2014-01-01

The National Institute for Environmental Health Sciences (NIEHS) is conducting an epidemiologic study (GuLF STUDY) to investigate the health of the workers and volunteers who participated from April to December of 2010 in the response and cleanup of the oil release after the Deepwater Horizon explosion in the Gulf of Mexico. The exposure assessment component of the study involves analyzing thousands of personal monitoring measurements that were collected during this effort. A substantial portion of these data has values reported by the analytic laboratories to be below the limits of detection (LOD). A simulation study was conducted to evaluate three established methods for analyzing data with censored observations to estimate the arithmetic mean (AM), geometric mean (GM), geometric standard deviation (GSD), and the 95th percentile (X0.95) of the exposure distribution: the maximum likelihood (ML) estimation, the β-substitution, and the Kaplan–Meier (K-M) methods. Each method was challenged with computer-generated exposure datasets drawn from lognormal and mixed lognormal distributions with sample sizes (N) varying from 5 to 100, GSDs ranging from 2 to 5, and censoring levels ranging from 10 to 90%, with single and multiple LODs. Using relative bias and relative root mean squared error (rMSE) as the evaluation metrics, the β-substitution method generally performed as well or better than the ML and K-M methods in most simulated lognormal and mixed lognormal distribution conditions. The ML method was suitable for large sample sizes (N ≥ 30) up to 80% censoring for lognormal distributions with small variability (GSD = 2–3). The K-M method generally provided accurate estimates of the AM when the censoring was <50% for lognormal and mixed distributions. The accuracy and precision of all methods decreased under high variability (GSD = 4 and 5) and small to moderate sample sizes (N < 20) but the β-substitution was still the best of the three methods. When using the ML method, practitioners are cautioned to be aware of different ways of estimating the AM as they could lead to biased interpretation. A limitation of the β-substitution method is the absence of a confidence interval for the estimate. More research is needed to develop methods that could improve the estimation accuracy for small sample sizes and high percent censored data and also provide uncertainty intervals. PMID:25261453

Molecularly imprinted polymer-sol-gel tablet toward micro-solid phase extraction: II. Determination of amphetamine in human urine samples by liquid chromatography-tandem mass spectrometry.

PubMed

El-Beqqali, Aziza; Andersson, Lars I; Jeppsson, Amin Dadoun; Abdel-Rehim, Mohamed

2017-09-15

Amphetamine selective molecularly imprinted sol-gel polymer tablets, MIP-tablets, for solid-phase microextraction of biofluid samples were prepared. An acetonitrile solution of deuterated amphetamine template and silane precursor, 3-(propylmethacrylate) trimethoxysilane, was soaked into the pores of polyethylene tablet substrates and polymerized by an acid-catalysed sol-gel process. Application of the resultant MIP-tablets to extract amphetamine from human urine samples followed by LC-MS/MS analysis was investigated. The extraction protocol was optimised with respect to pH of sample, addition of sodium chloride, extraction time, desorption solvent and desorption time. The final analysis method determined amphetamine in human urine with a limit of detection (LOD) of 1.0ng/mL and a lower limit of quantification (LLOQ) of 5ng/mL. Validation demonstrated accuracy of the method was 91.0-104.0% and inter-assay precision was 4.8-8.5% (RSD). Extraction recovery was 80%. The MIP-tablets could be re-used and the same tablet could be employed for more than twenty extractions. Copyright © 2017 Elsevier B.V. All rights reserved.

Top-Down Nanofabrication and Characterization of 20 nm Silicon Nanowires for Biosensing Applications

PubMed Central

M. N, M. Nuzaihan; Hashim, U.; Md Arshad, M. K.; Ruslinda, A. Rahim; Rahman, S. F. A.; Fathil, M. F. M.; Ismail, Mohd. H.

2016-01-01

A top-down nanofabrication approach is used to develop silicon nanowires from silicon-on-insulator (SOI) wafers and involves direct-write electron beam lithography (EBL), inductively coupled plasma-reactive ion etching (ICP-RIE) and a size reduction process. To achieve nanometer scale size, the crucial factors contributing to the EBL and size reduction processes are highlighted. The resulting silicon nanowires, which are 20 nm in width and 30 nm in height (with a triangular shape) and have a straight structure over the length of 400 μm, are fabricated precisely at the designed location on the device. The device is applied in biomolecule detection based on the changes in drain current (Ids), electrical resistance and conductance of the silicon nanowires upon hybridization to complementary target deoxyribonucleic acid (DNA). In this context, the scaled-down device exhibited superior performances in terms of good specificity and high sensitivity, with a limit of detection (LOD) of 10 fM, enables for efficient label-free, direct and higher-accuracy DNA molecules detection. Thus, this silicon nanowire can be used as an improved transducer and serves as novel biosensor for future biomedical diagnostic applications. PMID:27022732

Separation and determination of impurities in paracetamol, codeine and pitophenone in the presence of fenpiverinium in combined suppository dosage form.

PubMed

Vojta, Jiří; Hanzlík, Pavel; Jedlička, Aleš; Coufal, Pavel

2015-01-01

A new HPLC method for separation and determination of impurities in paracetamol, codeine phosphate hemihydrate and pitophenone hydrochloride in the presence of fenpiverinium bromide in combined suppository dosage form was developed and validated. The separation of paracetamol and its impurities 4-aminophenol, 4-nitrophenol, 4-chloracetanilid; codeine and its impurities methylcodeine, morphine, codeine dimer and 10-hydroxycodeine; pitophenone and its impurities 2-[4-[2-(1-piperidinyl)ethoxy]benzoyl] benzoic acid, 2-[4-[2-(1-piperidinyl)ethoxy]benzoyl]benzoic acid 2-(1-piperidinyl)-ethyl ester, methyl ester of 2-(4-hydroxybenzoyl) benzoic acid and fenpiverinium was achieved by using ion-pair reversed phase liquid chromatography with UV detection. Validation parameters such as the precision, accuracy, linearity, limit of detection (LOD), limit of quantification (LOQ) and robustness were verified for all the mentioned impurities of codeine phosphate hemihydrate and 4-aminophenol and 2-[4-[2-(1-piperidinyl)ethoxy]benzoyl] benzoic acid as the main degradation products of paracetamol and pitophenone hydrochloride, respectively. The described method was found to be useful for analysis of the stability samples and therefore suitable for routine purity testing of the drug product. Copyright © 2014 Elsevier B.V. All rights reserved.

Validated spectrofluorimetric method for the determination of clonazepam in pharmaceutical preparations.

PubMed

Ibrahim, Fawzia; El-Enany, Nahed; Shalan, Shereen; Elsharawy, Rasha

2016-05-01

A simple, highly sensitive and validated spectrofluorimetric method was applied in the determination of clonazepam (CLZ). The method is based on reduction of the nitro group of clonazepam with zinc/CaCl2, and the product is then reacted with 2-cyanoacetamide (2-CNA) in the presence of ammonia (25%) yielding a highly fluorescent product. The produced fluorophore exhibits strong fluorescence intensity at ʎ(em) = 383 nm after excitation at ʎ(ex) = 333 nm. The method was rectilinear over a concentration range of 0.1-0.5 ng/mL with a limit of detection (LOD) of 0.0057 ng/mL and a limit of quantification (LOQ) of 0.017 ng/mL. The method was fully validated and successfully applied to the determination of CLZ in its tablets with a mean percentage recovery of 100.10 ± 0.75%. Method validation according to ICH Guidelines was evaluated. Statistical analysis of the results obtained using the proposed method was successfully compared with those obtained using a reference method, and there was no significance difference between the two methods in terms of accuracy and precision. Copyright © 2015 John Wiley & Sons, Ltd.

Gradient RP-HPLC method for the determination of potential impurities in atazanavir sulfate.

PubMed

Chitturi, Sreenivasa Rao; Somannavar, Yallappa Somappa; Peruri, Badarinadh Gupta; Nallapati, Sreenivas; Sharma, Hemant Kumar; Budidet, Shankar Reddy; Handa, Vijay Kumar; Vurimindi, Hima Bindu

2011-04-28

This paper proposes a simple and selective RP-HPLC method for the determination of process impurities and degradation products (degradants) of atazanavir sulfate (ATV) drug substance. Chromatographic separation was achieved on Ascentis(®) Express C8, (150mm×4.6mm, 2.7μm) column thermostated at 30°C under gradient elution by a binary mixture of potassium dihydrogen phosphate (pH 3.5, 0.02M) and ACN at a flow rate of 1.0ml/min. A photodiode array (PDA) detector set at 250nm was used for detection. Stress testing (forced degradation) of ATV was carried out under acidic, alkaline, oxidative, photolytic, thermal and humidity conditions. In presence of alkali, ATV transformed into cyclized products and the order of degradation reaction is determined by the method of initial rates. The unknown process impurities and alkaline degradants are isolated by preparative LC and characterized by ESI-MS/MS, (1)H NMR, and FT-IR spectral data. The developed method is validated with respect to sensitivity (lod and loq), linearity, precision, accuracy and robustness and can be implemented for routine quality control analysis and stability testing of ATV. Copyright © 2011 Elsevier B.V. All rights reserved.

Fast and solvent-free quantitation of boar taint odorants in pig fat by stable isotope dilution analysis-dynamic headspace-thermal desorption-gas chromatography/time-of-flight mass spectrometry.

PubMed

Fischer, Jochen; Haas, Torsten; Leppert, Jan; Lammers, Peter Schulze; Horner, Gerhard; Wüst, Matthias; Boeker, Peter

2014-09-01

Boar taint is a specific off-odour of boar meat products, known to be caused by at least three unpleasant odorants, with very low odour thresholds. Androstenone is a boar pheromone produced in the testes, whereas skatole and indole originate from the microbial breakdown of tryptophan in the intestinal tract. A new procedure, applying stable isotope dilution analysis (SIDA) and dynamic headspace-thermal desorption-gas chromatography/time-of-flight mass spectrometry (dynHS-TD-GC/TOFMS) for the simultaneous quantitation of these boar taint compounds in pig fat was elaborated and validated in this paper. The new method is characterised by a simple and solvent-free dynamic headspace sampling. The deuterated compounds d3-androstenone, d3-skatole and d6-indole were used as internal standards to eliminate matrix effects. The method validation performed revealed low limits of detection (LOD) and quantitation (LOQ) with high accuracy and precision, thus confirming the feasibility of the new dynHS-TD-GC/TOFMS approach for routine analysis. Copyright © 2014 Elsevier Ltd. All rights reserved.

Quantitative Determination of α-Arbutin, β-Arbutin, Kojic Acid, Nicotinamide, Hydroquinone, Resorcinol, 4-Methoxyphenol, 4-Ethoxyphenol, and Ascorbic Acid from Skin Whitening Products by HPLC-UV.

PubMed

Wang, Yan-Hong; Avonto, Cristina; Avula, Bharathi; Wang, Mei; Rua, Diego; Khan, Ikhlas A

2015-01-01

An HPLC-UV method was developed for the quantitative analysis of nine skin whitening agents in a single injection. These compounds are α-arbutin, β-arbutin, kojic acid, nicotinamide, resorcinol, ascorbic acid, hydroquinone, 4-methoxyphenol, and 4-ethoxyphenol. The separation was achieved on a reversed-phase C18 column within 30 min. The mobile phase was composed of water and methanol, both containing 0.1% acetic acid (v/v). The stability of the analytes was evaluated at different pH values between 2.3 and 7.6, and the extraction procedure was validated for different types of skin whitening product matrixes, which included two creams, a soap bar, and a capsule. The best solvent system for sample preparation was 20 mM NaH2PO4 containing 10% methanol at pH 2.3. The analytical method was validated for accuracy, precision, LOD, and LOQ. The developed HPLC-UV method was applied for the quantitation of the nine analytes in 59 skin whitening products including creams, lotions, sera, foams, gels, mask sheets, soap bars, tablets, and capsules.

Analysis of volatile compounds in gluten-free bread crusts with an optimised and validated SPME-GC/QTOF methodology.

PubMed

Pico, Joana; Antolín, Beatriz; Román, Laura; Gómez, Manuel; Bernal, José

2018-04-01

The aroma of bread crust, as one of the first characteristics perceived, is essential for bread acceptance. However, gluten-free bread crusts exhibit weak aroma. A SPME-GC/QTOF methodology was optimised with PCA and RSM and validated for the quantification of 44 volatile compounds in bread crust, extracting 0.75 g of crust at 60 °C for 51 min. LODs ranged between 3.60 and 1760 μg Kg -1 , all the R 2 were higher than 0.99 and %RSD for precision and %Er for accuracy were lower than 9% and 12%, respectively. A commercial wheat bread crust was quantified, and furfural was the most abundant compound. Bread crusts of wheat starch and of japonica rice, basmati rice and teff flours were also quantified. Teff flour and wheat starch crusts were very suitable for improving gluten-free bread crust aroma, due to their similar content in 2-acetyl-1-pyrroline and 4-hydroxy-2,5-dimethyl-3(2H)-furanone compared to wheat flour crust and also for their high content in pyrazines. Copyright © 2018 Elsevier Ltd. All rights reserved.

Ultrafast UPLC-ESI-MS and HPLC with monolithic column for determination of principal flavor compounds in vanilla pods.

PubMed

Sharma, Upendra K; Sharma, Nandini; Sinha, Arun K; Kumar, Neeraj; Gupta, Ajai P

2009-10-01

In this study, two novel chromatographic methods based on monolithic column high-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC) were developed for the ultrafast determination of principal flavor compounds namely vanillin, vanillic acid, p-hydroxybenzoic acid, and p-hydroxybenzaldehyde in ethanolic extracts of Vanilla planifolia pods. Good separation was achieved within 2.5 min using Chromolith RP18e column (100 mm x 4.6 mm) for HPLC and Acquity BEH C-18 (100 mm x 2.1 mm, 1.7 microm) column for UPLC. Both methods were compared in terms of total analysis time, mobile phase consumption, sensitivity, and validation parameters like precision, accuracy, LOD, and LOQ. Further, system suitability test data including resolution, capacity factor, theoretical plates, and tailing factor was determined for both the methods by ten replicate injections. Monolithic column based HPLC gave better results for most of the selected parameters while UPLC was found to be more eco-friendly with low mobile phase consumption and better sensitivity. Both methods may be used conveniently for the high throughput analysis of large number of samples in comparison to traditional particulate column.

Reusable split-aptamer-based biosensor for rapid detection of cocaine in serum by using an all-fiber evanescent wave optical biosensing platform.

PubMed

Tang, Yunfei; Long, Feng; Gu, Chunmei; Wang, Cheng; Han, Shitong; He, Miao

2016-08-24

A rapid, facile, and sensitive assay of cocaine in biological fluids is important to prevent illegal abuse of drugs. A two-step structure-switching aptasensor has been developed for cocaine detection based on evanescent wave optical biosensing platform. In the proposed biosensing platform, two tailored aptamer probes were used to construct the molecular structure switching. In the existence of cocaine, two fragments of cocaine aptamer formed a three-way junction quickly, and the fluorophore group of one fragment was effectively quenched by the quencher group of the other one. The tail of the three-way junction hybridized with the cDNA sequences immobilized on the optical fiber biosensor. Fluorescence was excited by evanescent wave, and the fluorescence signal was proportional to cocaine concentration. Cocaine was detected in 450 s (300 s for incubation and 150 s for detection and regeneration) with a limit of detection (LOD) of 165.2 nM. The proposed aptasensor was evaluated in human serum samples, and it exhibited good recovery, precision, and accuracy without complicated sample pretreatments. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of Oxytetracycline from Salmon Muscle and Skin by Derivative Spectrophotometry.

PubMed

Toral, M Inés; Sabay, Tamara; Orellana, Sandra L; Richter, Pablo

2015-01-01

A method was developed for the identification and quantification of oxytetracycline residues present in salmon muscle and skin using UV-Vis derivative spectrophotometry. With this method, it was possible to reduce the number of steps in the procedure typically required for instrumental analysis of a sample. The spectral variables, order of the derivative, scale factor, smoothing factor, and analytical wavelength were optimized using standard solutions of oxytetracycline dissolved in 900 mg/L oxalic acid in methanol. The matrix effect was significant; therefore, quantification for oxytetracycline residues was carried out using drug-free salmon muscle and skin samples fortified with oxytetracycline. The LOD and LOQ were found to be 271 and 903 μg/kg, respectively. The precision and accuracy of the method were validated using drug-free salmon muscle and skin tissues fortified at three different concentrations (8, 16, and 32 mg/kg) on 3 different days. The recoveries at all fortified concentrations were between 90 and 105%, and RSDs in all cases were less than 6.5%. This method can be used to screen out compliant samples and thereby reduce the number of suspect positive samples that will require further confirmatory analysis.

Microemulsion Liquid Chromatographic Method for Simultaneous Determination of Simvastatin and Ezetimibe in Their Combined Dosage Forms

PubMed Central

Hammouda, Mohammed E. A.; Abu El-Enin, Mohamed A.; El-Sherbiny, Dina T.; El-Wasseef, Dalia R.; El-Ashry, Saadia M.

2013-01-01

A rapid HPLC procedure using a microemulsion as an eluent was developed and validated for analytical quality control of antihyperlipidemic mixture containing simvastatin (SIM) and ezetimibe (EZT) in their pharmaceutical preparations. The separation was performed on a column packed with cyano bonded stationary phase adopting UV detection at 238 nm using a flow rate of 1 mL/min. The optimized microemulsion mobile phase consisted of 0.2 M sodium dodecyl sulphate, 1% octanol, 10% n-propanol, and 0.3% triethylamine in 0.02 M phosphoric acid at pH 5.0. The developed method was validated in terms of specificity, linearity, lower limit of quantification (LOQ), lower limit of detection (LOD), precision, and accuracy. The proposed method is rapid (8.5 min), reproducible (RSD < 2.0%) and achieves satisfactory resolution between SIM and EZT (resolution factor = 2.57). The mean recoveries of the analytes in pharmaceutical preparations were in agreement with those obtained from a reference method, as revealed by statistical analysis of the obtained results using Student's t-test and the variance ratio F-test. PMID:24282651

A New Green Method for the Quantitative Analysis of Enrofloxacin by Fourier-Transform Infrared Spectroscopy.

PubMed

Rebouças, Camila Tavares; Kogawa, Ana Carolina; Salgado, Hérida Regina Nunes

2018-05-18

Background: A green analytical chemistry method was developed for quantification of enrofloxacin in tablets. The drug, a second-generation fluoroquinolone, was first introduced in veterinary medicine for the treatment of various bacterial species. Objective: This study proposed to develop, validate, and apply a reliable, low-cost, fast, and simple IR spectroscopy method for quantitative routine determination of enrofloxacin in tablets. Methods: The method was completely validated according to the International Conference on Harmonisation guidelines, showing accuracy, precision, selectivity, robustness, and linearity. Results: It was linear over the concentration range of 1.0-3.0 mg with correlation coefficients >0.9999 and LOD and LOQ of 0.12 and 0.36 mg, respectively. Conclusions: Now that this IR method has met performance qualifications, it can be adopted and applied for the analysis of enrofloxacin tablets for production process control. The validated method can also be utilized to quantify enrofloxacin in tablets and thus is an environmentally friendly alternative for the routine analysis of enrofloxacin in quality control. Highlights: A new green method for the quantitative analysis of enrofloxacin by Fourier-Transform Infrared spectroscopy was validated. It is a fast, clean and low-cost alternative for the evaluation of enrofloxacin tablets.

Accuracy and Precision of Silicon Based Impression Media for Quantitative Areal Texture Analysis

PubMed Central

Goodall, Robert H.; Darras, Laurent P.; Purnell, Mark A.

2015-01-01

Areal surface texture analysis is becoming widespread across a diverse range of applications, from engineering to ecology. In many studies silicon based impression media are used to replicate surfaces, and the fidelity of replication defines the quality of data collected. However, while different investigators have used different impression media, the fidelity of surface replication has not been subjected to quantitative analysis based on areal texture data. Here we present the results of an analysis of the accuracy and precision with which different silicon based impression media of varying composition and viscosity replicate rough and smooth surfaces. Both accuracy and precision vary greatly between different media. High viscosity media tested show very low accuracy and precision, and most other compounds showed either the same pattern, or low accuracy and high precision, or low precision and high accuracy. Of the media tested, mid viscosity President Jet Regular Body and low viscosity President Jet Light Body (Coltène Whaledent) are the only compounds to show high levels of accuracy and precision on both surface types. Our results show that data acquired from different impression media are not comparable, supporting calls for greater standardisation of methods in areal texture analysis. PMID:25991505

Accuracy assessment of BDS precision orbit determination and the influence analysis of site distribution

NASA Astrophysics Data System (ADS)

Chen, Ming; Guo, Jiming; Li, Zhicai; Zhang, Peng; Wu, Junli; Song, Weiwei

2017-04-01

BDS precision orbit determination is a key content of the BDS application, but the inadequate ground stations and the poor distribution of the network are the main reasons for the low accuracy of BDS precise orbit determination. In this paper, the BDS precise orbit determination results are obtained by using the IGS MGEX stations and the Chinese national reference stations，the accuracy of orbit determination of GEO, IGSO and MEO is 10.3cm, 2.8cm and 3.2cm, and the radial accuracy is 1.6cm,1.9cm and 1.5cm.The influence of ground reference stations distribution on BDS precise orbit determination is studied. The results show that the Chinese national reference stations contribute significantly to the BDS orbit determination, the overlap precision of GEO/IGSO/MEO satellites were improved by 15.5%, 57.5% and 5.3% respectively after adding the Chinese stations.Finally, the results of ODOP(orbit distribution of precision) and SLR are verified. Key words: BDS precise orbit determination; accuracy assessment；Chinese national reference stations；reference stations distribution；orbit distribution of precision

Determination of cocaine and its derivatives in hair samples by liquid phase microextraction (LPME) and gas chromatography-mass spectrometry (GC-MS).

PubMed

Pego, A M F; Roveri, F L; Kuninari, R Y; Leyton, V; Miziara, I D; Yonamine, M

2017-05-01

Hair testing is a recognized approach when it comes to accessing historical drug use. According to the World Drug Report of United Nations Office on Drugs and Crime (UNODC) 2015, Brazil is the largest cocaine (COC) market in South America. New analytical methodologies to detect crack/cocaine analytes in hair samples are highly desirable. Here, a method consisting of a liquid-phase microextraction (LPME) as a clean-up step, followed by gas chromatography-mass spectrometry (GC-MS) analysis has been proposed. The new validated method consisted of a washing step; an overnight incubation with methanol and a quick derivatization with butylchloroformate. Once derivatized, the samples were then submitted to the LPME procedure. Limits of detection (LoD) and quantitation (LoQ) obtained were of 0.1 and 0.5ng/mg for COC 0.4 and 0.5ng/mg for anhydroecgonine methyl ester (AEME); 0.03 and 0.05 for cocaethylene (CE), respectively and 0.05ng/mg for both LoD and LoQ for benzoylecgonine (BZE). All calibration curves were linear over the scope applied, from LoQ up to 20ng/mg, with a r 2 >0.99. Precision and accuracy assays showed acceptable %RSD values, according to international guidelines. Twelve postmortem head hair samples stemming from the Institute of Legal Medicine of Sao Paulo (IML-SP) have been analyzed, from which seven have shown to be positive for COC (0.75->20ng/mg) and BZE (0.1->20ng/mg). Apart from COC's main metabolite, four samples were also positive for CE (0.1-3.9ng/mg) and three samples for AEME (0.5-4.9ng/mg). To conclude, the LPME technique together with GC-MS analysis have shown promising results and were able to meet the demand of the laboratory of analyzing postmortem hair samples to look for all four analytes. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

Determination of novel brominated flame retardants and polybrominated diphenyl ethers in serum using gas chromatography-mass spectrometry with two simplified sample preparation procedures.

PubMed

Gao, Le; Li, Jian; Wu, Yandan; Yu, Miaohao; Chen, Tian; Shi, Zhixiong; Zhou, Xianqing; Sun, Zhiwei

2016-11-01

Two simple and efficient pretreatment procedures have been developed for the simultaneous extraction and cleanup of six novel brominated flame retardants (NBFRs) and eight common polybrominated diphenyl ethers (PBDEs) in human serum. The first sample pretreatment procedure was a quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based approach. An acetone/hexane mixture was employed to isolate the lipid and analytes from the serum with a combination of MgSO 4 and NaCl, followed by a dispersive solid-phase extraction (d-SPE) step using C18 particles as a sorbent. The second sample pretreatment procedure was based on solid-phase extraction. The sample extraction and cleanup were conducted directly on an Oasis HLB SPE column using 5 % aqueous isopropanol, concentrated sulfuric acid, and 10 % aqueous methanol, followed by elution with dichloromethane. The NBFRs and PBDEs were then detected using gas chromatography-negative chemical ionization mass spectrometry (GC-NCI MS). The methods were assessed for repeatability, accuracy, selectivity, limits of detection (LODs), and linearity. The results of spike recovery experiments in fetal bovine serum showed that average recoveries ranged from 77.9 % to 128.8 % with relative standard deviations (RSDs) from 0.73 % to 12.37 % for most of the analytes. The LODs for the analytes in fetal bovine serum ranged from 0.3 to 50.8 pg/mL except for decabromodiphenyl ethane. The proposed method was successfully applied to the determination of the 14 brominated flame retardants in human serum. The two pretreatment procedures described here are simple, accurate, and precise, and are suitable for the routine analysis of human serum. Graphical Abstract Workflow of a QuEChERS-based approach (top) and an SPE-based approach (bottom) for the detection of PBDEs and NBFRs in serum.

Quantitative high-throughput determination of endogenous retinoids in human plasma using triple-stage liquid chromatography/tandem mass spectrometry.

PubMed

Gundersen, Thomas E; Bastani, Nasser E; Blomhoff, Rune

2007-01-01

A high-throughput ultrasensitive analytical method based on liquid chromatography with positive ion atmospheric pressure chemical ionization (APCI) coupled to tandem mass spectrometric detection (LC/MS/MS) was developed for the determination of all-trans-4-oxo-retinoic acid (at4oxoRA), 13-cis-4-oxo-retinoic acid (13c4oxoRA), 13-cis-retinoic acid (13cRA), all-trans-retinoic acid (atRA) and all-trans-retinol (atROH) in human plasma. A stable isotope of atRA was used as internal standard (IS). The analytes and IS were isolated from 100 microL plasma by acetonitrile mono-phase extraction (MPE) performed in black 96-well microtiterplates. A 100 microL injection was focused on-column and chromatographed on an Agilent ZORBAX SB-C18 rapid-resolution high-throughput (RRHT) column with 1.8-microm particles (4.6 mmx50 mm) maintained at 60 degrees C. The initial mobile phase composition was acetonitrile/water/formic acid (10:90:0.1, v/v/v) delivered at 1.8 mL/min. Elution was accomplished by a fast gradient to acetonitrile/methanol/formic acid (90:10:0.1, v/v/v). The method had a chromatographic total run time of 7 min. An Applied Biosystems 4000 Q TRAP linear tandem mass spectrometer equipped with a heated nebulizer (APCI) ionization source was operated in multiple reaction monitoring (MRM) mode with the precursor-to-product ion transitions m/z 315.4-->297 (4-oxo-retinoic acids), 301.2-->205 (retinoic acids), 305.0-->209 (IS) and 269.2-->93 (retinol) used for quantification. The assay was fully validated and found to have acceptable accuracy, precision, linearity, sensitivity and selectivity. The mean extraction recoveries from spiked plasma samples were 80-105% for the various retinoids at three different levels. The intra-day accuracy of the assay was within 8% of nominal and intra-day precision was better than 8% coefficient of variance (CV) for retinoic acids. Inter-day precision results for quality control samples run over a 12-day period alongside clinical samples showed mean precision better than 12.5% CV. The limit of quantification was in the range of 0.1-0.2 ng/mL and the mass limit of detection (mLOD) was in the range 1-4 pg on column for the retinoic acids. The assay has been successfully applied to the analysis of 1700 plasma samples. Copyright (c) 2007 John Wiley & Sons, Ltd.

Performance evaluation of the Aptima HSV-1 and 2 assay for the detection of HSV in cutaneous and mucocutaneous lesion specimens.

PubMed

Sam, Soya S; Caliendo, Angela M; Ingersoll, Jessica; Abdul-Ali, Deborah; Kraft, Colleen S

Timely and precise laboratory diagnosis of Herpes simplex viruses (HSV) is required to guide clinical management. The study evaluated limit of detection (LOD) and performance characteristics of the Aptima HSV 1 & 2 assay in comparison to four assays. The multi-center study compared qualitative detection of HSV-1 and 2 by the Aptima HSV-1 and 2 assay (Hologic) to ELVIS culture, Lyra Direct (Quidel), AmpliVue (Quidel) and a laboratory developed test (LDT). LOD was performed using VTM and STM diluted viral concentrations and clinical performance was evaluated using 505 swab specimens. The Aptima LOD studies performed showed a lower detection limit for STM specimens as 1450 copies/mL and 430 copies/mL for HSV1 and HSV-2 respectively; the LOD for VTM specimens was 9370 copies/mL and 8045 copies/mL for HSV-1 and HSV-2 respectively. When the assays were analyzed based on the positive consensus result established the Aptima had 95% of percent positive agreement (PPA) and 100% negative percent agreement (NPA) for the HSV-1. For the HSV-2, the PPA and NPA for Aptima were 96% and 100% respectively. AmpliVue had 1.8% invalid rate, while Lyra had no invalid results but an inhibition rate of 0.8%. Aptima and LDT did not have any invalid or inhibited results. The results indicate that the Aptima HSV-1 & 2 assay is sensitive and the performance characteristics of the Aptima assay is comparable to the assays analyzed for the detection and differentiation of HSV-1 and 2 from cutaneous and mucocutaneous lesions. Copyright © 2017 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Campbell, Keri R.; Judge, Elizabeth J.; Barefield, James E.

We show the analysis of light water reactor simulated used nuclear fuel using laser-induced breakdown spectroscopy (LIBS) is explored using a simplified version of the main oxide phase. The main oxide phase consists of the actinides, lanthanides, and zirconium. The purpose of this study is to develop a rapid, quantitative technique for measuring zirconium in a uranium dioxide matrix without the need to dissolve the material. A second set of materials including cerium oxide is also analyzed to determine precision and limit of detection (LOD) using LIBS in a complex matrix. Two types of samples are used in this study:more » binary and ternary oxide pellets. The ternary oxide, (U,Zr,Ce)O 2 pellets used in this study are a simplified version the main oxide phase of used nuclear fuel. The binary oxides, (U,Ce)O 2 and (U,Zr)O 2 are also examined to determine spectral emission lines for Ce and Zr, potential spectral interferences with uranium and baseline LOD values for Ce and Zr in a UO 2 matrix. In the spectral range of 200 to 800 nm, 33 cerium lines and 25 zirconium lines were identified and shown to have linear correlation values (R 2) > 0.97 for both the binary and ternary oxides. The cerium LOD in the (U,Ce)O 2 matrix ranged from 0.34 to 1.08 wt% and 0.94 to 1.22 wt% in (U,Ce,Zr)O 2 for 33 of Ce emission lines. The zirconium limit of detection in the (U,Zr)O 2 matrix ranged from 0.84 to 1.15 wt% and 0.99 to 1.10 wt% in (U,Ce,Zr)O 2 for 25 Zr lines. Finally, the effect of multiple elements in the plasma and the impact on the LOD is discussed.« less

Evidence for bivariate linkage of obesity and HDL-C levels in the Framingham Heart Study.

PubMed

Arya, Rector; Lehman, Donna; Hunt, Kelly J; Schneider, Jennifer; Almasy, Laura; Blangero, John; Stern, Michael P; Duggirala, Ravindranath

2003-12-31

Epidemiological studies have indicated that obesity and low high-density lipoprotein (HDL) levels are strong cardiovascular risk factors, and that these traits are inversely correlated. Despite the belief that these traits are correlated in part due to pleiotropy, knowledge on specific genes commonly affecting obesity and dyslipidemia is very limited. To address this issue, we first conducted univariate multipoint linkage analysis for body mass index (BMI) and HDL-C to identify loci influencing variation in these phenotypes using Framingham Heart Study data relating to 1702 subjects distributed across 330 pedigrees. Subsequently, we performed bivariate multipoint linkage analysis to detect common loci influencing covariation between these two traits. We scanned the genome and identified a major locus near marker D6S1009 influencing variation in BMI (LOD = 3.9) using the program SOLAR. We also identified a major locus for HDL-C near marker D2S1334 on chromosome 2 (LOD = 3.5) and another region near marker D6S1009 on chromosome 6 with suggestive evidence for linkage (LOD = 2.7). Since these two phenotypes have been independently mapped to the same region on chromosome 6q, we used the bivariate multipoint linkage approach using SOLAR. The bivariate linkage analysis of BMI and HDL-C implicated the genetic region near marker D6S1009 as harboring a major gene commonly influencing these phenotypes (bivariate LOD = 6.2; LODeq = 5.5) and appears to improve power to map the correlated traits to a region, precisely. We found substantial evidence for a quantitative trait locus with pleiotropic effects, which appears to influence both BMI and HDL-C phenotypes in the Framingham data.

Quantitative Analysis of Heavy Metals in Water Based on LIBS with an Automatic Device for Sample Preparation

NASA Astrophysics Data System (ADS)

Hu, Li; Zhao, Nanjing; Liu, Wenqing; Meng, Deshuo; Fang, Li; Wang, Yin; Yu, Yang; Ma, Mingjun

2015-08-01

Heavy metals in water can be deposited on graphite flakes, which can be used as an enrichment method for laser-induced breakdown spectroscopy (LIBS) and is studied in this paper. The graphite samples were prepared with an automatic device, which was composed of a loading and unloading module, a quantitatively adding solution module, a rapid heating and drying module and a precise rotating module. The experimental results showed that the sample preparation methods had no significant effect on sample distribution and the LIBS signal accumulated in 20 pulses was stable and repeatable. With an increasing amount of the sample solution on the graphite flake, the peak intensity at Cu I 324.75 nm accorded with the exponential function with a correlation coefficient of 0.9963 and the background intensity remained unchanged. The limit of detection (LOD) was calculated through linear fitting of the peak intensity versus the concentration. The LOD decreased rapidly with an increasing amount of sample solution until the amount exceeded 20 mL and the correlation coefficient of exponential function fitting was 0.991. The LOD of Pb, Ni, Cd, Cr and Zn after evaporating different amounts of sample solution on the graphite flakes was measured and the variation tendency of their LOD with sample solution amounts was similar to the tendency for Cu. The experimental data and conclusions could provide a reference for automatic sample preparation and heavy metal in situ detection. supported by National Natural Science Foundation of China (No. 60908018), National High Technology Research and Development Program of China (No. 2013AA065502) and Anhui Province Outstanding Youth Science Fund of China (No. 1108085J19)

The neglected tool in the Bayesian ecologist's shed: a case study testing informative priors' effect on model accuracy

PubMed Central

Morris, William K; Vesk, Peter A; McCarthy, Michael A; Bunyavejchewin, Sarayudh; Baker, Patrick J

2015-01-01

Despite benefits for precision, ecologists rarely use informative priors. One reason that ecologists may prefer vague priors is the perception that informative priors reduce accuracy. To date, no ecological study has empirically evaluated data-derived informative priors' effects on precision and accuracy. To determine the impacts of priors, we evaluated mortality models for tree species using data from a forest dynamics plot in Thailand. Half the models used vague priors, and the remaining half had informative priors. We found precision was greater when using informative priors, but effects on accuracy were more variable. In some cases, prior information improved accuracy, while in others, it was reduced. On average, models with informative priors were no more or less accurate than models without. Our analyses provide a detailed case study on the simultaneous effect of prior information on precision and accuracy and demonstrate that when priors are specified appropriately, they lead to greater precision without systematically reducing model accuracy. PMID:25628867

The neglected tool in the Bayesian ecologist's shed: a case study testing informative priors' effect on model accuracy.

PubMed

Morris, William K; Vesk, Peter A; McCarthy, Michael A; Bunyavejchewin, Sarayudh; Baker, Patrick J

2015-01-01

Despite benefits for precision, ecologists rarely use informative priors. One reason that ecologists may prefer vague priors is the perception that informative priors reduce accuracy. To date, no ecological study has empirically evaluated data-derived informative priors' effects on precision and accuracy. To determine the impacts of priors, we evaluated mortality models for tree species using data from a forest dynamics plot in Thailand. Half the models used vague priors, and the remaining half had informative priors. We found precision was greater when using informative priors, but effects on accuracy were more variable. In some cases, prior information improved accuracy, while in others, it was reduced. On average, models with informative priors were no more or less accurate than models without. Our analyses provide a detailed case study on the simultaneous effect of prior information on precision and accuracy and demonstrate that when priors are specified appropriately, they lead to greater precision without systematically reducing model accuracy.

Cumulative detection probabilities and range accuracy of a pulsed Geiger-mode avalanche photodiode laser ranging system

NASA Astrophysics Data System (ADS)

Luo, Hanjun; Ouyang, Zhengbiao; Liu, Qiang; Chen, Zhiliang; Lu, Hualan

2017-10-01

Cumulative pulses detection with appropriate cumulative pulses number and threshold has the ability to improve the detection performance of the pulsed laser ranging system with GM-APD. In this paper, based on Poisson statistics and multi-pulses cumulative process, the cumulative detection probabilities and their influence factors are investigated. With the normalized probability distribution of each time bin, the theoretical model of the range accuracy and precision is established, and the factors limiting the range accuracy and precision are discussed. The results show that the cumulative pulses detection can produce higher target detection probability and lower false alarm probability. However, for a heavy noise level and extremely weak echo intensity, the false alarm suppression performance of the cumulative pulses detection deteriorates quickly. The range accuracy and precision is another important parameter evaluating the detection performance, the echo intensity and pulse width are main influence factors on the range accuracy and precision, and higher range accuracy and precision is acquired with stronger echo intensity and narrower echo pulse width, for 5-ns echo pulse width, when the echo intensity is larger than 10, the range accuracy and precision lower than 7.5 cm can be achieved.

Extraction optimization and UHPLC method development for determination of the 20-hydroxyecdysone in Sida tuberculata leaves.

PubMed

da Rosa, Hemerson S; Koetz, Mariana; Santos, Marí Castro; Jandrey, Elisa Helena Farias; Folmer, Vanderlei; Henriques, Amélia Teresinha; Mendez, Andreas Sebastian Loureiro

2018-04-01

Sida tuberculata (ST) is a Malvaceae species widely distributed in Southern Brazil. In traditional medicine, ST has been employed as hypoglycemic, hypocholesterolemic, anti-inflammatory and antimicrobial. Additionally, this species is chemically characterized by flavonoids, alkaloids and phytoecdysteroids mainly. The present work aimed to optimize the extractive technique and to validate an UHPLC method for the determination of 20-hydroxyecdsone (20HE) in the ST leaves. Box-Behnken Design (BBD) was used in method optimization. The extractive methods tested were: static and dynamic maceration, ultrasound, ultra-turrax and reflux. In the Box-Behnken three parameters were evaluated in three levels (-1, 0, +1), particle size, time and plant:solvent ratio. In validation method, the parameters of selectivity, specificity, linearity, limits of detection and quantification (LOD, LOQ), precision, accuracy and robustness were evaluated. The results indicate static maceration as better technique to obtain 20HE peak area in ST extract. The optimal extraction from surface response methodology was achieved with the parameters granulometry of 710 nm, 9 days of maceration and plant:solvent ratio 1:54 (w/v). The UHPLC-PDA analytical developed method showed full viability of performance, proving to be selective, linear, precise, accurate and robust for 20HE detection in ST leaves. The average content of 20HE was 0.56% per dry extract. Thus, the optimization of extractive method in ST leaves increased the concentration of 20HE in crude extract, and a reliable method was successfully developed according to validation requirements and in agreement with current legislation. Copyright © 2018 Elsevier Inc. All rights reserved.

Validation of a QuEChERS-based gas chromatographic method for analysis of pesticide residues in Cassia angustifolia (senna).

PubMed

Tripathy, Vandana; Saha, Ajoy; Patel, Dilipkumar J; Basak, B B; Shah, Paresh G; Kumar, Jitendra

2016-08-02

A simple multi-residue method based on modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach was established for the determination of 17 organochlorine (OC), 15 organophosphorous (OP) and 7 synthetic pyrethroid (SP) pesticides in an economically important medicinal plant of India, Senna (Cassia angustifolia), by gas chromatography coupled to electron capture and flame thermionic detectors (GC/ECD/FTD) and confirmation of residues was done on gas chromatograph coupled with mass spectrometry (GC-MS). The developed method was validated by testing the following parameters: linearity, limit of detection (LOD), limit of quantification (LOQ), matrix effect, accuracy-precision and measurement uncertainty; the validation study clearly demonstrated the suitability of the method for its intended application. All pesticides showed good linearity in the range 0.01-1.0 μg mL(-1) for OCs and OPs and 0.05-2.5 μg mL(-1) for SPs with correlation coefficients higher than 0.98. The method gave good recoveries for most of the pesticides (70-120%) with intra-day and inter-day precision < 20% in most of the cases. The limits of detection varied from 0.003 to 0.03 mg kg(-1), and the LOQs were determined as 0.01-0.049 mg kg(-1). The expanded uncertainties were <30%, which was distinctively less than a maximum default value of ±50%. The proposed method was successfully applied to determine pesticide residues in 12 commercial market samples obtained from different locations in India.

Simultaneous determination of five major compounds in the traditional medicine Pyeongwee-San by high performance liquid chromatography-diode array detection and liquid chromatography-mass spectrometry/mass spectrometry.

PubMed

Lee, Bohyoung; Weon, Jin Bae; Yun, Bo-Ra; Lee, Jiwoo; Eom, Min Rye; Ma, Choong Je

2014-01-01

Pyeongwee-San (PWS) has been widely used for treating acute gastritis, chronic, and gastritis. In this paper, simultaneous determination of five compounds (naringin, hesperidin, glycyrrhizin, atractylenolide III, and magnolol) from traditional medicine PWS using the high performance liquid chromatography (HPLC) was established for quality control. Optimum separations were obtained with a SHISEIDO C18 reverse-phase column by gradient elution with 0.1% Trifluoroacetic acid (TFA) water-acetonitrile as the mobile phase. The flow rate was 1 mL/min and detection wavelength was set at 205 nm and 250 nm. Validation of the analytical method was evaluated by linearity, precision, and accuracy test. The calibration curves were linear over the established range with R (2) > 0.9978. The limit of detection (LOD) and limit of quantification (LOQ) ranged from 0.09 to 0.43 and 0.27 to 1.29 μg/mL. The method exhibited intra-day and inter-day precision range between 0.01-1.86% and 0.04-0.35% respectively. The recoveries of five compounds in PWS were in the range between 93.18-106.40%, and 0.20-1.51%. The application of this method was identified through the successful analysis of five compounds in 12 batches of PWS. In addition, identification of five compounds was confirmed by a liquid chromatography method and mass spectrometry. The HPLC method was could be accomplished to the quality control and stable experiment for the preparations consisted of five major compounds.

Multimycotoxin LC-MS/MS Analysis in Tea Beverages after Dispersive Liquid-Liquid Microextraction (DLLME).

PubMed

Pallarés, Noelia; Font, Guillermina; Mañes, Jordi; Ferrer, Emilia

2017-11-29

The aim of the present study was to develop a multimycotoxin liquid chromatography tandem mass spectrometry (LC-MS/MS) method with a dispersive liquid-liquid microextraction procedure (DLLME) for the analysis of AFs, 3aDON, 15aDON, NIV, HT-2, T-2, ZEA, OTA, ENNs, and BEA in tea beverages and to evaluate their mycotoxin contents. The proposed method was characterized in terms of linearity, limits of detection (LODs), limits of quantification (LOQs), recoveries, repeatability (intraday precision), reproducibility (interday precision), and matrix effects to check suitability. The results show LODs in the range of 0.05-10 μg/L, LOQs in the range of 0.2-33 μg/L, and recoveries in the range of 65-127% (RSD < 20%). The method developed in this study was applied to 44 commercial samples of black tea, red tea, green tea, and green mint tea. The results show that, of the analyzed mycotoxins, AFB2, AFG2, 15aDON, AFG1, and ENB were detected in the samples. AFB2 (14.4-32.2 μg/L) and 15aDON (60.5-61 μg/L) presented the highest levels. Green mint tea contained the highest concentration of mycotoxins. The risk assessment study shows that the population is not much exposed to mycotoxins through the consumption of tea beverages.

Mineral element analyses of switchgrass biomass: comparison of the accuracy and precision of laboratories

USDA-ARS?s Scientific Manuscript database

Mineral concentration of plant biomass can affect its use in thermal conversion to energy. The objective of this study was to compare the precision and accuracy of university and private laboratories that conduct mineral analyses of plant biomass on a fee basis. Accuracy and precision of the laborat...

Thickness dependence of polydopamine thin films on detection sensitivity of surface plasmon-enhanced fluorescence biosensors

NASA Astrophysics Data System (ADS)

Toma, Mana; Tawa, Keiko

2018-03-01

A bioinspired polydopamine (PDA) coating is a good candidate for the rapid and cheap chemical modification of biosensor surfaces. Herein, we report the effect of PDA thickness on the detection sensitivity of a fluorescence biosensor utilizing surface plasmon-enhanced fluorescence. The thickness of PDA films was tuned by the incubation time of the dopamine solution and varied from 1 to 17 nm. The detection sensitivity was evaluated as the limit of detection (LOD) of a fluorescently labelled target analyte by a model immunoassay. The LOD was determined to be 1.6 pM for the thickest PDA film and was improved to 1.0 pM by reducing the thickness to the range from 1 to 5 nm, corresponding to the incubation time of 10 to 60 min. The experimental results indicate that the PDA coating is suitable for the surface functionalization of biosensors in mass production as it does not require precise control of the incubation time.

Determination of acrylamide and acrylic acid by isocratic liquid chromatography with pulsed electrochemical detection.

PubMed

Casella, Innocenzo G; Pierri, Marianna; Contursi, Michela

2006-02-24

The electrochemical behaviour of the polycrystalline platinum electrode towards the oxidation/reduction of short-chain unsaturated aliphatic molecules such as acrylamide and acrylic acid was investigated in acidic solutions. Analytes were separated by reverse phase liquid chromatographic and quantified using a pulsed amperometric detection. A new two-step waveform, is introduced for detection of acrylamide and acrylic acid. Detection limits (LOD) of 20 nM (1. 4 microg/kg) and 45 nM (3.2 microg/kg) were determined in water solutions containing acrylamide and acrylic acid, respectively. Compared to the classical three-step waveform, the proposed two-step waveform shows favourable analytical performance in terms of LOD, linear range, precision and improved long-term reproducibility. The proposed analytical method combined with clean-up procedure accomplished by Carrez clearing reagent and subsequent extraction with a strong cation exchanger cartridges (SPE), was successfully used for the quantification of low concentrations of acrylamide in foodstuffs such as coffee and potato fries.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wahyuni, Wulan Tri, E-mail: wulantriws@gmail.com; Department of Chemistry, FMIPA, Universitas Indonesia, Kampus UI Depok; Ivandini, Tribidasari A.

Biomolecule modified magnetic beads has been widely used in separation and sensing process. This study used streptavidin modified magnetic beads to immobilize biotin modified zanamivir. Biotin-streptavidin affinity facilitates immobilization of zanamivir on magnetic beads. Then interaction of zanamivir and neuraminidase was adopted as basic for enzyme detection. Detection of neuraminidase was performed at gold modified BDD using cyclic voltammetry technique. The measurement was carried out based on alteration of electrochemical signals of working electrode as neuraminidase response. The result showed that zanamivir was successfully immobilized on magnetic beads. The optimum amount of magnetic beads for zanamivir immobilization was 120 ug.more » Linear responses of neuraminidase were detected in concentration range of 0-15 mU. Detection limit (LOD) of measurement was 2.32 mU (R2 = 0.959) with precision as % RSD of 1.41%. Measurement of neuraminidase on magnetic beads could be also performed in the presence of mucin matrix. The linearity range was 0-8 mU with LOD of 0.64 mU (R2 = 0.950) and % RSD of 7.25%.« less

Students as Toolmakers: Refining the Results in the Accuracy and Precision of a Trigonometric Activity

ERIC Educational Resources Information Center

Igoe, D. P.; Parisi, A. V.; Wagner, S.

2017-01-01

Smartphones used as tools provide opportunities for the teaching of the concepts of accuracy and precision and the mathematical concept of arctan. The accuracy and precision of a trigonometric experiment using entirely mechanical tools is compared to one using electronic tools, such as a smartphone clinometer application and a laser pointer. This…

Effect of genomic drift of influenza PCR tests.

PubMed

Stellrecht, Kathleen A; Nattanmai, Seela M; Butt, Jumshan; Maceira, Vincente P; Espino, Alvin A; Castro, Allan J; Landes, Allen; Dresser, Nicolas; Butt, Shafiq A

2017-08-01

Nucleic acid amplification assays have become the method of choice for influenza (Flu) testing due to superior accuracy and faster turnaround time. Although assays are designed to detect highly conserved genomic targets, mutations can influence test sensitivity. Most of the circulating viruses in the United States during the 2014-2015 season were associated with significant genetic drift; however, the effect on testing was unknown. We compared the performance of Prodesse ProFlu+/ProFAST+ (PFlu/PFAST), FilmArray Respiratory Panel (RP), cobas ® Influenza A/B test (cIAB), and Xpert ® Flu (Xpt) in a retrospective analysis of consecutive nasopharyngeal specimens received for a two-week period during the winter of 2015. Furthermore, limits of detection (LOD) were determined with six isolates of Flu. Of the 275 specimens, 63 were positive for FluA by PFAST, 60 were positive by RP, 58 were positive by cIAB and 52 were positive by Xpt. Only a subset of 135 specimens was tested by PFlu, of which 32 were positive. The sensitivity/specificity for PFAST, RP, cIAB, Xpt and PFlu was 100/99.1%, 96.7/99.5%, 91.8/99.1%, 85.2%/100%, and 75.6%/98.9%, respectively. LOD analyses demonstrated assay performance variations were strain associated. Specifically, PFlu's and cIAB's LODs were higher with A/Texas/50/2012-like and A/Switzerland/9715293/2013-like strains, while Xpt's highest LOD was with the Swiss strain. Strain-associated assay performance variation is known to occur with other Flu test methods; hence, it is not surprising that such variation would be observed with molecular tests. Careful monitoring and reporting for strain-associated variances are warranted for all test methods. Copyright © 2017 Elsevier B.V. All rights reserved.

[18F]FDOPA PET as an Endophenotype for Parkinson’s Disease Linkage Studies

PubMed Central

Racette, Brad A.; Good, Laura; Antenor, Jo Ann; McGee-Minnich, Lori; Moerlein, Stephen M.; Videen, Tom O.; Perlmutter, Joel S.

2008-01-01

Parkinson Disease (PD) is a late onset disorder with age-dependent penetrance that may confound genetic studies since affected individuals may not demonstrate clinical manifestations at the time of evaluation. The use of endophenotypes, biologic surrogates for clinical disease diagnoses, may permit more accurate classification of at-risk subjects. Positron emission tomography (PET) measurements of 6-[18F]fluorodopa ([18F]FDOPA) uptake indicate nigrostriatal neuronal integrity and may provide a useful endophenotype for PD linkage studies. We performed [18F]FDOPA PET in 11 members of a large, multi-incident Amish family with PD, 24 normals and 48 people with clinically definite idiopathic PD (PD controls). Clinical diagnoses in the Amish were clinically definite PD in four, clinically probable in one, clinically possible in five, and normal in one. Abnormal [18F]FDOPA posterior putamen uptake was defined as less than three standard deviations below the normal mean. The criteria were applied to the Amish sample to determine a PET endophenotype for each. We performed genetic simulations using SLINK to model the effect phenoconversion with the PET endophenotype had on logarithm of odds (LOD) scores. PET endophenotype confirmed the status of two clinically definite subjects. Two clinically definite Amish PD subjects had normal PETs. Two possible PD were converted to “PET definite PD”. The remainder had normal PETs. The average maximum LOD score with the pre-PET was 6.14±0.84. Simulating phenoconversion of subjects with unknown phenotypes increased the LOD score to 7.36±1.23. The [18F]FDOPA PET endophenotype permits phenoconversion in multi-incident PD families and may increase LOD score accuracy and power of an informative pedigree. PMID:16528749

Are Currently Available Wearable Devices for Activity Tracking and Heart Rate Monitoring Accurate, Precise, and Medically Beneficial?

PubMed Central

El-Amrawy, Fatema

2015-01-01

Objectives The new wave of wireless technologies, fitness trackers, and body sensor devices can have great impact on healthcare systems and the quality of life. However, there have not been enough studies to prove the accuracy and precision of these trackers. The objective of this study was to evaluate the accuracy, precision, and overall performance of seventeen wearable devices currently available compared with direct observation of step counts and heart rate monitoring. Methods Each participant in this study used three accelerometers at a time, running the three corresponding applications of each tracker on an Android or iOS device simultaneously. Each participant was instructed to walk 200, 500, and 1,000 steps. Each set was repeated 40 times. Data was recorded after each trial, and the mean step count, standard deviation, accuracy, and precision were estimated for each tracker. Heart rate was measured by all trackers (if applicable), which support heart rate monitoring, and compared to a positive control, the Onyx Vantage 9590 professional clinical pulse oximeter. Results The accuracy of the tested products ranged between 79.8% and 99.1%, while the coefficient of variation (precision) ranged between 4% and 17.5%. MisFit Shine showed the highest accuracy and precision (along with Qualcomm Toq), while Samsung Gear 2 showed the lowest accuracy, and Jawbone UP showed the lowest precision. However, Xiaomi Mi band showed the best package compared to its price. Conclusions The accuracy and precision of the selected fitness trackers are reasonable and can indicate the average level of activity and thus average energy expenditure. PMID:26618039

Are Currently Available Wearable Devices for Activity Tracking and Heart Rate Monitoring Accurate, Precise, and Medically Beneficial?

PubMed

El-Amrawy, Fatema; Nounou, Mohamed Ismail

2015-10-01

The new wave of wireless technologies, fitness trackers, and body sensor devices can have great impact on healthcare systems and the quality of life. However, there have not been enough studies to prove the accuracy and precision of these trackers. The objective of this study was to evaluate the accuracy, precision, and overall performance of seventeen wearable devices currently available compared with direct observation of step counts and heart rate monitoring. Each participant in this study used three accelerometers at a time, running the three corresponding applications of each tracker on an Android or iOS device simultaneously. Each participant was instructed to walk 200, 500, and 1,000 steps. Each set was repeated 40 times. Data was recorded after each trial, and the mean step count, standard deviation, accuracy, and precision were estimated for each tracker. Heart rate was measured by all trackers (if applicable), which support heart rate monitoring, and compared to a positive control, the Onyx Vantage 9590 professional clinical pulse oximeter. The accuracy of the tested products ranged between 79.8% and 99.1%, while the coefficient of variation (precision) ranged between 4% and 17.5%. MisFit Shine showed the highest accuracy and precision (along with Qualcomm Toq), while Samsung Gear 2 showed the lowest accuracy, and Jawbone UP showed the lowest precision. However, Xiaomi Mi band showed the best package compared to its price. The accuracy and precision of the selected fitness trackers are reasonable and can indicate the average level of activity and thus average energy expenditure.

Sensitivity, accuracy, and precision issues in opto-electronic holography based on fiber optics and high-spatial- and high-digitial-resolution cameras

NASA Astrophysics Data System (ADS)

Furlong, Cosme; Yokum, Jeffrey S.; Pryputniewicz, Ryszard J.

2002-06-01

Sensitivity, accuracy, and precision characteristics in quantitative optical metrology techniques, and specifically in optoelectronic holography based on fiber optics and high-spatial and high-digital resolution cameras, are discussed in this paper. It is shown that sensitivity, accuracy, and precision dependent on both, the effective determination of optical phase and the effective characterization of the illumination-observation conditions. Sensitivity, accuracy, and precision are investigated with the aid of National Institute of Standards and Technology (NIST) traceable gages, demonstrating the applicability of quantitative optical metrology techniques to satisfy constantly increasing needs for the study and development of emerging technologies.

LOD map--A visual interface for navigating multiresolution volume visualization.

PubMed

Wang, Chaoli; Shen, Han-Wei

2006-01-01

In multiresolution volume visualization, a visual representation of level-of-detail (LOD) quality is important for us to examine, compare, and validate different LOD selection algorithms. While traditional methods rely on ultimate images for quality measurement, we introduce the LOD map--an alternative representation of LOD quality and a visual interface for navigating multiresolution data exploration. Our measure for LOD quality is based on the formulation of entropy from information theory. The measure takes into account the distortion and contribution of multiresolution data blocks. A LOD map is generated through the mapping of key LOD ingredients to a treemap representation. The ordered treemap layout is used for relative stable update of the LOD map when the view or LOD changes. This visual interface not only indicates the quality of LODs in an intuitive way, but also provides immediate suggestions for possible LOD improvement through visually-striking features. It also allows us to compare different views and perform rendering budget control. A set of interactive techniques is proposed to make the LOD adjustment a simple and easy task. We demonstrate the effectiveness and efficiency of our approach on large scientific and medical data sets.

Accuracy of active chirp linearization for broadband frequency modulated continuous wave ladar.

PubMed

Barber, Zeb W; Babbitt, Wm Randall; Kaylor, Brant; Reibel, Randy R; Roos, Peter A

2010-01-10

As the bandwidth and linearity of frequency modulated continuous wave chirp ladar increase, the resulting range resolution, precisions, and accuracy are improved correspondingly. An analysis of a very broadband (several THz) and linear (<1 ppm) chirped ladar system based on active chirp linearization is presented. Residual chirp nonlinearity and material dispersion are analyzed as to their effect on the dynamic range, precision, and accuracy of the system. Measurement precision and accuracy approaching the part per billion level is predicted.

Analytical Validation of Accelerator Mass Spectrometry for Pharmaceutical Development: the Measurement of Carbon-14 Isotope Ratio.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Keck, B D; Ognibene, T; Vogel, J S

2010-02-05

Accelerator mass spectrometry (AMS) is an isotope based measurement technology that utilizes carbon-14 labeled compounds in the pharmaceutical development process to measure compounds at very low concentrations, empowers microdosing as an investigational tool, and extends the utility of {sup 14}C labeled compounds to dramatically lower levels. It is a form of isotope ratio mass spectrometry that can provide either measurements of total compound equivalents or, when coupled to separation technology such as chromatography, quantitation of specific compounds. The properties of AMS as a measurement technique are investigated here, and the parameters of method validation are shown. AMS, independent of anymore » separation technique to which it may be coupled, is shown to be accurate, linear, precise, and robust. As the sensitivity and universality of AMS is constantly being explored and expanded, this work underpins many areas of pharmaceutical development including drug metabolism as well as absorption, distribution and excretion of pharmaceutical compounds as a fundamental step in drug development. The validation parameters for pharmaceutical analyses were examined for the accelerator mass spectrometry measurement of {sup 14}C/C ratio, independent of chemical separation procedures. The isotope ratio measurement was specific (owing to the {sup 14}C label), stable across samples storage conditions for at least one year, linear over 4 orders of magnitude with an analytical range from one tenth Modern to at least 2000 Modern (instrument specific). Further, accuracy was excellent between 1 and 3 percent while precision expressed as coefficient of variation is between 1 and 6% determined primarily by radiocarbon content and the time spent analyzing a sample. Sensitivity, expressed as LOD and LLOQ was 1 and 10 attomoles of carbon-14 (which can be expressed as compound equivalents) and for a typical small molecule labeled at 10% incorporated with {sup 14}C corresponds to 30 fg equivalents. AMS provides an sensitive, accurate and precise method of measuring drug compounds in biological matrices.« less

Improved accuracy and precision of tracer kinetic parameters by joint fitting to variable flip angle and dynamic contrast enhanced MRI data.

PubMed

Dickie, Ben R; Banerji, Anita; Kershaw, Lucy E; McPartlin, Andrew; Choudhury, Ananya; West, Catharine M; Rose, Chris J

2016-10-01

To improve the accuracy and precision of tracer kinetic model parameter estimates for use in dynamic contrast enhanced (DCE) MRI studies of solid tumors. Quantitative DCE-MRI requires an estimate of precontrast T1 , which is obtained prior to fitting a tracer kinetic model. As T1 mapping and tracer kinetic signal models are both a function of precontrast T1 it was hypothesized that its joint estimation would improve the accuracy and precision of both precontrast T1 and tracer kinetic model parameters. Accuracy and/or precision of two-compartment exchange model (2CXM) parameters were evaluated for standard and joint fitting methods in well-controlled synthetic data and for 36 bladder cancer patients. Methods were compared under a number of experimental conditions. In synthetic data, joint estimation led to statistically significant improvements in the accuracy of estimated parameters in 30 of 42 conditions (improvements between 1.8% and 49%). Reduced accuracy was observed in 7 of the remaining 12 conditions. Significant improvements in precision were observed in 35 of 42 conditions (between 4.7% and 50%). In clinical data, significant improvements in precision were observed in 18 of 21 conditions (between 4.6% and 38%). Accuracy and precision of DCE-MRI parameter estimates are improved when signal models are fit jointly rather than sequentially. Magn Reson Med 76:1270-1281, 2016. © 2015 Wiley Periodicals, Inc. © 2015 Wiley Periodicals, Inc.

Quantitative analysis of flavonoids and phenolic acids in Arnica montana L. by micellar electrokinetic capillary chromatography.

PubMed

Ganzera, Markus; Egger, Christoph; Zidorn, Christian; Stuppner, Hermann

2008-05-05

Arnica montana preparations have been used in Europe for centuries to treat skin disorders. Among the biologically active ingredients in the flower heads of the plant are sequiterpenes, flavonoids and phenolic acids. For the simultaneous determination of compounds belonging to the latter two groups a micellar electrokinetic capillary chromatography (MEKC) method was developed and validated. By using an electrolyte solution containing 50 mM borax, 25 mM sodium dodecyl sulfate and 30% of acetonitrile the separation of seven flavonoids and four caffeic acid derivatives was feasible in less than 20 min. The optimized system was validated for repeatability (sigma(rel) < or = 4.4%), precision (inter-day sigma(rel) < or = 8.13%, intra-day sigma(rel) < or = 4.32%), accuracy (recovery rates from 96.8 to 102.4%), sensitivity (limit of detection (LOD) < or = 4.5 microg mL(-1)) and linearity (R(2) > or = 0.9996), and then successfully applied to assay several plant samples. In all of them the most dominant flavonoid was found to be quercetin 3-O-glucuronic acid, whereas 3,5-dicaffeoylquinic acid was the major phenolic acid; the total content of flavonoids and phenolic acids varied in the samples from 0.60 to 1.70%, and 1.03 to 2.24%, respectively.

A rapid UPLC method for simultaneous determination of eleven components in 'Ge-Gen-Qin-Lian' decoction.

PubMed

An, Rui; You, Lisha; Zhang, Yizhu; Wang, Xinhong; Ma, Yuemin

2014-10-01

'Ge-Gen-Qin-Lian' Decoction derived from 'Shang-Han-Lun' compiled by Zhang Zhongjing. It is widely used in the treatment of acute gastroenteritis, bacillary dysentery, virus diarrhea. This paper describes a sensitive and specific assay for the determination of the 11-marker compounds using ultra performance liquid chromatography (UPLC). To develop an UPLC method for simultaneous determination of 11 bioactive compounds in 'Ge-Gen-Qin-Lian' preparations. The chromatography analysis was performed on an Agilent Proshell 120 EC-C18 column (4.6 × 50 mm, 2.7 μm) at 30°C with a gradient elution of methanol, 0.5% formic acid and 0.5% ammonium acetate at a flow rate 1.0 ml/min and UV detected at 270 nm. All calibration curves showed good linear regression (r ≥ 0.9993) within tested ranges. Limits of detection (LOD) and limits of quantification (LOQ) fell in the range between 0.0691-1.04 μg/ml and 0.23-3.43 μg/ml, respectively. The mean recovery of each herbal medicine ranged from 96.60 to 102.11%. The method was validated for repeatability, precision, stability, accuracy, and selectivity. The validated method was successfully applied to simultaneous analysis of these active components in 'Ge-Gen-Qin-Lian' decoction.

Screening method for the determination of tetracyclines and fluoroquinolones in animal drinking water by liquid chromatography with diode array detector.

PubMed

Patyra, E; Kowalczyk, E; Grelik, A; Przeniosło-Siwczyńska, M; Kwiatek, K

2015-01-01

A liquid chromatography - diode array detector (HPLC-DAD) procedure has been developed for the determination of oxytetracycline (OTC), tetracycline (TC), chlorotetracycline (CTC), doxycycline (DC), enrofloxacin (ENR), ciprofloxacin (CIP), sarafloxacin (SAR) and flumequine (FLU) residues in animal drinking water. This method was applied to animal drinking water. Solid-phase extraction (SPE) clean-up on an Oasis HLB cartridge allowed an extract suitable for liquid chromatographic analysis to be obtained. Chromatographic separation was carried out on a C18 analytical column, using gradient elution with 0.1% trifluoroacetic acid - acetonitrile - methanol at 30°C. The flow-rate was 0.7 mL/min and the eluate was analysed at 330 nm. The whole procedure was evaluated according to the requirements of the Commission Decision 2002/657/EC, determining specificity, decision limit (CCα), detection capacity (CCβ), limit of detection (LOD), limit of quantification (LOQ), precision and accuracy during validation of the method. The recoveries of TCs and FQs from spiked samples at the levels of 10, 100 and 1000 μg/L were higher than 82%. The developed method based on HPLC-DAD has been applied for the determination of four tetracyclines and four fluoroquinolones in animal drinking water samples.

Microfluidic chip based nano liquid chromatography coupled to tandem mass spectrometry for the determination of abused drugs and metabolites in human hair.

PubMed

Zhu, Kevin Y; Leung, K Wing; Ting, Annie K L; Wong, Zack C F; Ng, Winki Y Y; Choi, Roy C Y; Dong, Tina T X; Wang, Tiejie; Lau, David T W; Tsim, Karl W K

2012-03-01

A microfluidic chip based nano-HPLC coupled to tandem mass spectrometry (nano-HPLC-Chip-MS/MS) has been developed for simultaneous measurement of abused drugs and metabolites: cocaine, benzoylecgonine, cocaethylene, norcocaine, morphine, codeine, 6-acetylmorphine, phencyclidine, amphetamine, methamphetamine, MDMA, MDA, MDEA, and methadone in the hair of drug abusers. The microfluidic chip was fabricated by laminating polyimide films and it integrated an enrichment column, an analytical column and a nanospray tip. Drugs were extracted from hairs by sonication, and the chromatographic separation was achieved in 15 min. The drug identification and quantification criteria were fulfilled by the triple quardropule tandem mass spectrometry. The linear regression analysis was calibrated by deuterated internal standards with all of the R(2) at least over 0.993. The limit of detection (LOD) and the limit of quantification (LOQ) were from 0.1 to 0.75 and 0.2 to 1.25 pg/mg, respectively. The validation parameters including selectivity, accuracy, precision, stability, and matrix effect were also evaluated here. In conclusion, the developed sample preparation method coupled with the nano-HPLC-Chip-MS/MS method was able to reveal the presence of drugs in hairs from the drug abusers, with the enhanced sensitivity, compared with the conventional HPLC-MS/MS.

Performance of a pentafluorophenylpropyl stationary phase for the electrospray ionization high-performance liquid chromatography-mass spectrometry-mass spectrometry assay of cocaine and its metabolite ecgonine methyl ester in human urine.

PubMed

Needham, S R; Jeanville, P M; Brown, P R; Estape, E S

2000-10-01

A pentafluorophenylpropyl (PFPP) bonded silica column has been used for the high-performance liquid chromatography-electrospray ionization-mass spectrometry-mass spectrometry assay (HPLC-ESI-MS-MS) of cocaine (COC) and its metabolite, ecgonine methyl ester (EME) in human urine. COC and EME were used as model basic solutes to demonstrate that a PFPP phase yields excellent results for the assay and validation of drugs in biological fluids. The assay was linear over three orders of magnitude (1.0-1000 ng/ml) and precision and accuracy of the assay was 4 and 15%, respectively. The limit of detection (LOD) for COC and EME was 1.6 and 2.8 pg on column, respectively. In addition, only a simple 1:10 dilution of the urine was necessary for the sample preparation procedure thus saving time on a laborious extraction step. The major advantage of the PFPP phase was the enhancement of the ESI-MS signal by providing good retention and good peak shape of COC and EME with a mobile phase of 90% acetonitrile. The MS signal for COC was a factor of 12 times greater on the PFPP phase than on the C18 phase.

A Liquid Chromatography – Tandem Mass Spectrometry Approach for the Identification of Mebendazole Residue in Pork, Chicken, and Horse

PubMed Central

Lee, Ji Sun; Cho, Soo Hee; Lim, Chae Mi; Chang, Moon Ik; Joo, Hyun Jin; Park, Hyun Jin

2017-01-01

A confirmatory and quantitative method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the determination of mebendazole and its hydrolyzed and reduced metabolites in pork, chicken, and horse muscles was developed and validated in this study. Anthelmintic compounds were extracted with ethyl acetate after sample mixture was made alkaline followed by liquid chromatographic separation using a reversed phase C18 column. Gradient elution was performed with a mobile phase consisting of water containing 10 mM ammonium formate and methanol. This confirmatory method was validated according to EU requirements. Evaluated validation parameters included specificity, accuracy, precision (repeatability and within-laboratory reproducibility), analytical limits (decision limit and detection limit), and applicability. Most parameters were proved to be conforming to the EU requirements. The decision limit (CCα) and detection capability (CCβ) for all analytes ranged from 15.84 to 17.96 μgkg-1. The limit of detection (LOD) and the limit of quantification (LOQ) for all analytes were 0.07 μgkg-1 and 0.2 μgkg-1, respectively. The developed method was successfully applied to monitoring samples collected from the markets in major cities and proven great potential to be used as a regulatory tool to determine mebendazole residues in animal based foods. PMID:28085912

Estimating Building Age with 3d GIS

NASA Astrophysics Data System (ADS)

Biljecki, F.; Sindram, M.

2017-10-01

Building datasets (e.g. footprints in OpenStreetMap and 3D city models) are becoming increasingly available worldwide. However, the thematic (attribute) aspect is not always given attention, as many of such datasets are lacking in completeness of attributes. A prominent attribute of buildings is the year of construction, which is useful for some applications, but its availability may be scarce. This paper explores the potential of estimating the year of construction (or age) of buildings from other attributes using random forest regression. The developed method has a two-fold benefit: enriching datasets and quality control (verification of existing attributes). Experiments are carried out on a semantically rich LOD1 dataset of Rotterdam in the Netherlands using 9 attributes. The results are mixed: the accuracy in the estimation of building age depends on the available information used in the regression model. In the best scenario we have achieved predictions with an RMSE of 11 years, but in more realistic situations with limited knowledge about buildings the error is much larger (RMSE = 26 years). Hence the main conclusion of the paper is that inferring building age with 3D city models is possible to a certain extent because it reveals the approximate period of construction, but precise estimations remain a difficult task.

A Stability-Indicating HPLC-DAD Method for Determination of Stiripentol: Development, Validation, Kinetics, Structure Elucidation and Application to Commercial Dosage Form

PubMed Central

Darwish, Hany W.; Abdelhameed, Ali S.; Bakheit, Ahmed H.; Khalil, Nasr Y.; Al-Majed, Abdulrahman A.

2014-01-01

A rapid, simple, sensitive, and accurate isocratic reversed-phase stability-indicating high performance liquid chromatography method has been developed and validated for the determination of stiripentol and its degradation product in its bulk form and pharmaceutical dosage form. Chromatographic separation was achieved on a Symmetry C18 column and quantification was achieved using photodiode array detector (DAD). The method was validated in accordance with the ICH requirements showing specificity, linearity (r 2 = 0.9996, range of 1–25 μg/mL), precision (relative standard deviation lower than 2%), accuracy (mean recovery 100.08 ± 1.73), limits of detection and quantitation (LOD = 0.024 and LOQ = 0.081 μg/mL), and robustness. Stiripentol was subjected to various stress conditions and it has shown marked stability under alkaline hydrolytic stress conditions, thermal, oxidative, and photolytic conditions. Stiripentol degraded only under acidic conditions, forming a single degradation product which was well resolved from the pure drug with significantly different retention time values. This degradation product was characterized by 1H-NMR and 13C-NMR spectroscopy as well as ion trap mass spectrometry. The results demonstrated that the method would have a great value when applied in quality control and stability studies for stiripentol. PMID:25371844

High performance liquid chromatography with photo diode array for separation and analysis of naproxen and esomeprazole in presence of their chiral impurities: Enantiomeric purity determination in tablets.

PubMed

Ragab, Marwa A A; El-Kimary, Eman I

2017-05-12

A stereoselective high performance liquid chromatographic method with diode array detection (HPLC-DAD) was introduced for S-naproxen and esomeprazole determination in tablets. The separation was achieved on a Kromasil Cellucoat chiral column using a mobile phase consisting of hexane: isopropanol: trifluoroacetic acid (TFA) (90:9.9:0.1 v/v/v). The proposed system was found to be suitable for the enantioseparation of naproxen and omeprazole biologically active isomers. After optimization of the chromatographic conditions, resolution values of 3.84 and 2.17 could be obtained for naproxen and omeprazole isomers, respectively. The method was fully validated for the determination of S-isomers of each drug in their dosage form. Also, the enentiomeric purity was determined in commercial tablet containing S-naproxen and esomeprazole. The enantiomeric purity was calculated for each drug and the chiral impurities (R-isomers) could be determined at 1% level. The method was validated and good results with respect to linearity, precision, accuracy, selectivity and robustness were obtained. The limits of detection (LOD) and quantification (LOQ) were 2.00, 6.50 and 0.10, 0.35μgmL -1 for S-naproxen and esomeprazole, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of an Ion-Pairing Reagent and HPLC-UV Method for the Detection and Quantification of Six Water-Soluble Vitamins in Animal Feed.

PubMed

Kim, Ho Jin

2016-01-01

A novel and simple method for detecting six water-soluble vitamins in animal feed using high performance liquid chromatography equipped with a photodiode array detector (HPLC/PDA) and ion-pairing reagent was developed. The chromatographic peaks of the six water-soluble vitamins were successfully identified by comparing their retention times and UV spectra with reference standards. The mobile phase was composed of buffers A (5 mM PICB-6 in 0.1% CH3COOH) and B (5 mM PICB-6 in 65% methanol). All peaks were detected using a wavelength of 270 nm. Method validation was performed in terms of linearity, sensitivity, selectivity, accuracy, and precision. The limits of detection (LODs) for the instrument employed in these experiments ranged from 25 to 197 μg/kg, and the limits of quantification (LOQs) ranged from 84 to 658 μg/kg. Average recoveries of the six water-soluble vitamins ranged from 82.3% to 98.9%. Method replication resulted in intraday and interday peak area variation of <5.6%. The developed method was specific and reliable and is therefore suitable for the routine analysis of water-soluble vitamins in animal feed.

Application of a newly developed and validated high-performance thin-layer chromatographic method to control honey adulteration.

PubMed

Puscas, Anitta; Hosu, Anamaria; Cimpoiu, Claudia

2013-01-11

Honey is a saturated solution of sugars, used for a long time as a natural source of sugars and is an important ingredient in traditional medicine due to its antimicrobial, anti-inflammatory and antioxidant effects. Therefore, methods for quality control of honey and detection of its adulteration are very important. For this reason, the aim of this study is to develop and validate a new, simple and economical analytical method for detecting the adulteration of some Romanian honeys based on high-performance thin-layer chromatography (HPTLC) combined with image analysis. The proposed method involved the chromatographic separations of glucose, fructose and sucrose on silica gel HPTLC plates, developed twice with ethyl acetate-pyridine-water-acetic acid, 6:3:1:0.5 (v/v/v/v), followed by dipping in an immersion solution. The documentation of plates was performed using TLC visualization device and the images of plates were processed using a digital processor. The developed HPTLC method was validated for selectivity, linearity and range, LOD and LOQ, precision, robustness and accuracy. The method was then applied for quantitative determination of glucose, fructose and sucrose from different types of Romanian honeys, commercially available. Copyright © 2012 Elsevier B.V. All rights reserved.

UHPLC-MS/MS method for the quantitation of penicillin G and metabolites in citrus fruit using internal standards.

PubMed

Canzani, Daniele; Hsieh, Kevin; Standland, Matthew; Hammack, Walter; Aldeek, Fadi

2017-02-15

Penicillin G has been applied to citrus trees as a potential treatment in the fight against Huanglongbing (HLB). Here, we have developed and validated a method to identify and quantitate penicillin G and two of its metabolites, penillic acid and penilloic acid, in citrus fruit using ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). This method improves upon a previous method by incorporating isotopically labeled internal standards, namely, penillic acid-D 5 , and penilloic acid-D 5 . These standards greatly enhanced the accuracy and precision of our measurements by compensating for recovery losses, degradation, and matrix effects. When 2g of citrus fruit sample is extracted, the limits of detection (LOD) were determined to be 0.1ng/g for penicillin G and penilloic acid, and 0.25ng/g for penillic acid. At fortification levels of 0.1, 0.25, 1, and 10ng/g, absolute recoveries for penillic and penilloic acids were generally between 50-70%. Recoveries corrected with the isotopically labeled standards were approximately 90-110%. This method will be useful for the identification and quantitation of drug residues and their degradation products using isotopically labeled standards and UHPLC-MS/MS. Published by Elsevier B.V.

Exploring the Impact of Visual Complexity Levels in 3d City Models on the Accuracy of Individuals' Orientation and Cognitive Maps

NASA Astrophysics Data System (ADS)

Rautenbach, V.; Çöltekin, A.; Coetzee, S.

2015-08-01

In this paper we report results from a qualitative user experiment (n=107) designed to contribute to understanding the impact of various levels of complexity (mainly based on levels of detail, i.e., LoD) in 3D city models, specifically on the participants' orientation and cognitive (mental) maps. The experiment consisted of a number of tasks motivated by spatial cognition theory where participants (among other things) were given orientation tasks, and in one case also produced sketches of a path they `travelled' in a virtual environment. The experiments were conducted in groups, where individuals provided responses on an answer sheet. The preliminary results based on descriptive statistics and qualitative sketch analyses suggest that very little information (i.e., a low LoD model of a smaller area) might have a negative impact on the accuracy of cognitive maps constructed based on a virtual experience. Building an accurate cognitive map is an inherently desired effect of the visualizations in planning tasks, thus the findings are important for understanding how to develop better-suited 3D visualizations such as 3D city models. In this study, we specifically discuss the suitability of different levels of visual complexity for development planning (urban planning), one of the domains where 3D city models are most relevant.

Performance of search strategies to retrieve systematic reviews of diagnostic test accuracy from the Cochrane Library.

PubMed

Huang, Yuansheng; Yang, Zhirong; Wang, Jing; Zhuo, Lin; Li, Zhixia; Zhan, Siyan

2016-05-06

To compare the performance of search strategies to retrieve systematic reviews of diagnostic test accuracy from The Cochrane Library. Databases of CDSR and DARE in the Cochrane Library were searched for systematic reviews of diagnostic test accuracy published between 2008 and 2012 through nine search strategies. Each strategy consists of one group or combination of groups of searching filters about diagnostic test accuracy. Four groups of diagnostic filters were used. The Strategy combing all the filters was used as the reference to determine the sensitivity, precision, and the sensitivity x precision product for another eight Strategies. The reference Strategy retrieved 8029 records, of which 832 were eligible. The strategy only composed of MeSH terms about "accuracy measures" achieved the highest values in both precision (69.71%) and product (52.45%) with a moderate sensitivity (75.24%). The combination of MeSH terms and free text words about "accuracy measures" contributed little to increasing the sensitivity. Strategies composed of filters about "diagnosis" had similar sensitivity but lower precision and product to those composed of filters about "accuracy measures". MeSH term "exp'diagnosis' " achieved the lowest precision (9.78%) and product (7.91%), while its hyponym retrieved only half the number of records at the expense of missing 53 target articles. The precision was negatively correlated with sensitivities among the nine strategies. Compared to the filters about "diagnosis", the filters about "accuracy measures" achieved similar sensitivities but higher precision. When combining both terms, sensitivity of the strategy was enhanced obviously. The combination of MeSH terms and free text words about the same concept seemed to be meaningless for enhancing sensitivity. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

A solid-phase microextraction-gas chromatographic approach combined with triple quadrupole mass spectrometry for the assay of carbamate pesticides in water samples.

PubMed

Cavaliere, Brunella; Monteleone, Marcello; Naccarato, Attilio; Sindona, Giovanni; Tagarelli, Antonio

2012-09-28

A simple and sensitive method was developed for the quantification of five carbamate pesticides in water samples using solid phase microextraction (SPME) combined with gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS). The performance of five SPME fibers was tested in univariate mode whereas the other variables affecting the efficiency of SPME analysis were optimized by the multivariate approach of design of experiment (DoE) and, in particular, a central composite design (CCD) was applied. The optimum working conditions in terms of response values were achieved by performing analysis with polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber in immersion mode for 45min at room temperature with addition of NaCl (10%). The multivariate chemometric approach was also used to explore the chromatographic behavior of the carbamates and to evaluate the importance of each variable investigated. An overall appraisement of results shows that the factor which gave a statistically significant effect on the response was only the injection temperature. Identification and quantification of carbamates was performed by using a gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS) system in multiple reaction monitoring (MRM) acquisition. Since the choice of internal standard represented a crucial step in the development of method to achieve good reproducibility and robustness for the entire analytical protocol, three compounds (2,3,5-trimethacarb, 4-bromo-3,5-dimethylphenyl-n-methylcarbamate (BDMC) and carbaryl-d7) were evaluated as internal standards. Both precision and accuracy of the proposed protocol tested at concentration of 0.08, 5 and 3 μg l⁻¹ offered values ranging from 70.8% and 115.7% (except for carbaryl at 3 μg l⁻¹) and from 1.0% and 9.0% for accuracy and precision, respectively. Moreover, LOD and LOQ values ranging from 0.04 to 1.7 ng l⁻¹ and from 0.64 to 2.9 ng l⁻¹, respectively, can be considered very satisfactory. Copyright © 2012 Elsevier B.V. All rights reserved.

Spectrophotometric and spectrofluorimetric determination of indacaterol maleate in pure form and pharmaceutical preparations: application to content uniformity.

PubMed

El-Ashry, S M; El-Wasseef, D R; El-Sherbiny, D T; Salem, Y A

2015-09-01

Two simple, rapid, sensitive and precise spectrophotometric and spectrofluorimetric methods were developed for the determination of indacaterol maleate in bulk powder and capsules. Both methods were based on the direct measurement of the drug in methanol. In the spectrophotometric method (Method I) the absorbance was measured at 259 nm. The absorbance-concentration plot was rectilinear over the range 1.0-10.0 µg mL(-1) with a lower detection limit (LOD) of 0.078 µg mL(-1) and lower quantification limit (LOQ) of 0.238 µg mL(-1). Meanwhile in the spectrofluorimetric method (Method II) the native fluorescence was measured at 358 nm after excitation at 258 nm. The fluorescence-concentration plot was rectilinear over the range of 1.0-40.0 ng mL(-1) with an LOD of 0.075 ng mL(-1) and an LOQ of 0.226 ng mL(-1). The proposed methods were successfully applied to the determination of indacaterol maleate in capsules with average percent recoveries ± RSD% of 99.94 ± 0.96 for Method I and 99.97 ± 0.81 for Method II. In addition, the proposed methods were extended to a content uniformity test according to the United States Pharmacopoeia (USP) guidelines and were accurate, precise for the capsules studied with acceptance value 3.98 for Method I and 2.616 for Method II. Copyright © 2015 John Wiley & Sons, Ltd.

Determination of acetanilide herbicides in cereal crops using accelerated solvent extraction, solid-phase extraction and gas chromatography-electron capture detector.

PubMed

Zhang, Yaping; Yang, Jun; Shi, Ronghua; Su, Qingde; Yao, Li; Li, Panpan

2011-07-01

A method was developed to determine eight acetanilide herbicides from cereal crops based on accelerated solvent extraction (ASE) and solid-phase extraction (SPE) followed by gas chromatography-electron capture detector (GC-ECD) analysis. During the ASE process, the effect of four parameters (temperature, static time, static cycles and solvent) on the extraction efficiency was considered and compared with shake-flask extraction method. After extraction with ASE, four SPE tubes (graphitic carbon black/primary secondary amine (GCB/PSA), GCB, Florisil and alumina-N) were assayed for comparison to obtain the best clean-up efficiency. The results show that GCB/PSA cartridge gave the best recoveries and cleanest chromatograms. The analytical process was validated by the analysis of spiked blank samples. Performance characteristics such as linearity, limit of detection (LOD), limit of quantitation (LOQ), precision and recovery were studied. At 0.05 mg/kg spiked level, recoveries and precision values for rice, wheat and maize were 82.3-115.8 and 1.1-13.6%, respectively. For all the herbicides, LOD and LOQ ranged from 0.8 to 1.7 μg/kg and from 2.4 to 5.3 μg/kg, respectively. The proposed analytical methodology was applied for the analysis of the targets in samples; only three herbicides, propyzamid, metolachlor and diflufenican, were detected in two samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Water vapor δ(2) H, δ(18) O and δ(17) O measurements using an off-axis integrated cavity output spectrometer - sensitivity to water vapor concentration, delta value and averaging-time.

PubMed

Tian, Chao; Wang, Lixin; Novick, Kimberly A

2016-10-15

High-precision analysis of atmospheric water vapor isotope compositions, especially δ(17) O values, can be used to improve our understanding of multiple hydrological and meteorological processes (e.g., differentiate equilibrium or kinetic fractionation). This study focused on assessing, for the first time, how the accuracy and precision of vapor δ(17) O laser spectroscopy measurements depend on vapor concentration, delta range, and averaging-time. A Triple Water Vapor Isotope Analyzer (T-WVIA) was used to evaluate the accuracy and precision of δ(2) H, δ(18) O and δ(17) O measurements. The sensitivity of accuracy and precision to water vapor concentration was evaluated using two international standards (GISP and SLAP2). The sensitivity of precision to delta value was evaluated using four working standards spanning a large delta range. The sensitivity of precision to averaging-time was assessed by measuring one standard continuously for 24 hours. Overall, the accuracy and precision of the δ(2) H, δ(18) O and δ(17) O measurements were high. Across all vapor concentrations, the accuracy of δ(2) H, δ(18) O and δ(17) O observations ranged from 0.10‰ to 1.84‰, 0.08‰ to 0.86‰ and 0.06‰ to 0.62‰, respectively, and the precision ranged from 0.099‰ to 0.430‰, 0.009‰ to 0.080‰ and 0.022‰ to 0.054‰, respectively. The accuracy and precision of all isotope measurements were sensitive to concentration, with the higher accuracy and precision generally observed under moderate vapor concentrations (i.e., 10000-15000 ppm) for all isotopes. The precision was also sensitive to the range of delta values, although the effect was not as large compared with the sensitivity to concentration. The precision was much less sensitive to averaging-time than the concentration and delta range effects. The accuracy and precision performance of the T-WVIA depend on concentration but depend less on the delta value and averaging-time. The instrument can simultaneously and continuously measure δ(2) H, δ(18) O and δ(17) O values in water vapor, opening a new window to better understand ecological, hydrological and meteorological processes. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Offline solid-phase extraction for preconcentration of pharmaceuticals and personal care products in environmental water and their simultaneous determination using the reversed phase high-performance liquid chromatography method.

PubMed

G Archana; Dhodapkar, Rita; Kumar, Anupama

2016-09-01

The present study reports a precise and simple offline solid-phase extraction (SPE) coupled with reversed-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous determination of five representative and commonly present pharmaceuticals and personal care products (PPCPs), a new class of emerging pollutants in the aquatic environment. The target list of analytes including ciprofloxacin, acetaminophen, caffeine benzophenone and irgasan were separated by a simple HPLC method. The column used was a reversed-phase C18 column, and the mobile phase was 1 % acetic acid and methanol (20:80 v/v) under isocratic conditions, at a flow rate of 1 mL min(-1). The analytes were separated and detected within 15 min using the photodiode array detector (PDA). The linearity of the calibration curves were obtained with correlation coefficients 0.98-0.99.The limit of detection (LOD), limit of quantification (LOQ), precision, accuracy and ruggedness demonstrated the reproducibility, specificity and sensitivity of the developed method. Prior to the analysis, the SPE was performed using a C18 cartridge to preconcentrate the targeted analytes from the environmental water samples. The developed method was applied to evaluate and fingerprint PPCPs in sewage collected from a residential engineering college campus, polluted water bodies such as Nag river and Pili river and the influent and effluent samples from a sewage treatment plant (STP) situated at Nagpur city, in the peak summer season. This method is useful for estimation of pollutants present in microquantities in the surface water bodies and treated sewage as compared to nanolevel pollutants detected by mass spectrometry (MS) detectors.

Stability indicating RP-HPLC method development and validation for the simultaneous determination of aminexil and minoxidil in pharmaceutical dosage form.

PubMed

Siddiraju, S; Sahithi, M

2015-03-01

The objective of the present work is to develop stability indicating high-performance liquid chromatographic method for the simultaneous determination of aminexil and minoxidil in pharmaceutical dosage form. The chromatographic separation was achieved with BDS Hypersil C18 column (250 mm×4.6 mm×5 μ) as stationary phase and phosphate buffer and acetonitrile (78:22) as mobile phase. The method was employed by using a flow rate of 1.1 mL/min kept at 30°C. The detection wavelength was kept at 238 nm by using photo-diode array detector. The retention times of the aminexil and minoxidil were found to be 2.3 min and 3.9 min, respectively. The method developed was validated in accordance with ICH guidelines with respect to the stability indicating capacity of the method including system suitability, accuracy, precision, linearity, range, limit of detection, limit of quantification and robustness. The linearity responses of aminexil and minoxidil were found to be in the concentration ranges of 18.75-112.5 μg/mL and 25-150 μg/mL, respectively. The LOD and LOQ values for aminexil were found to be 0.31 and 0.92 μg/mL and minoxidil were found to be 0.03 and 0.10 μg/mL respectively. The percentage recoveries for both the drugs were found in the range of 98-101%. This method is accurate, precise and sensitive; hence, it can be employed for routine quality control of aminexil and minoxidil in pharmaceutical industries and drug testing laboratories. Copyright © 2014 Elsevier Masson SAS. All rights reserved.

Determination of triazine herbicides and their metabolites in multiple medicinal parts of traditional Chinese medicines using streamlined pretreatment and UFLC-ESI-MS/MS.

PubMed

Liu, Congmin; Dou, Xiaowen; Zhang, Lei; Li, Qian; Qin, Jia'an; Duan, Yaping; Yang, Meihua

2018-01-01

A rapid, sensitive, and reliable ultra-fast liquid chromatography combined with electrospray ionization tandem mass spectrometry (UFLC-ESI-MS/MS) method was established and applied to simultaneous determination of 31 triazine herbicides and their metabolites in multiple medicinal parts of traditional Chinese medicines (TCMs). A streamlined pretreatment approach using one-step extraction and dilution was proposed, which provided high-throughput processing, excellent recovery, and negligible interference. Afterwards, multiple-reaction monitoring (MRM) and information-dependent acquisition (IDA) triggered enhanced product ion spectra (EPI) was adopted to identify and quantify the targets in a single analysis. The optimized method was then validated according to the guidelines of the European Commission for the following parameters: Matrix effects, specificity, accuracy, precision, linearity, range, and stability. The LOD and LOQ for the 31 triazine herbicides were 0.1-10 μg kg -1 and 0.5-25 μg kg -1 , respectively. Recoveries at three concentration levels were within 67.9-120.3% with an associated precision RSD <20%. Using the proposed approach, trazines herbicides were determined from 44 commercially available TCMs. The detection rate of triazine herbicides residues was 15.9% of the total samples. Among them, atrazine, simeton, and simetryn were found in the radix, herba, and seed TCMs with values far below the referenced maximum residue limits (MRLs), but no residues were detected in either the flos or fructus. Taken together, this method has the potential to provide a means for triazines screening in extensive matrices, thereby laying the foundation for pesticide registration on TCMs. Moreover, it has the potential to guide further triazine residue control in TCMs. Copyright © 2017 Elsevier Ltd. All rights reserved.

Low gas flow inductively coupled plasma optical emission spectrometry for the analysis of food samples after microwave digestion.

PubMed

Nowak, Sascha; Gesell, Monika; Holtkamp, Michael; Scheffer, Andy; Sperling, Michael; Karst, Uwe; Buscher, Wolfgang

2014-11-01

In this work, the recently introduced low flow inductively coupled plasma optical emission spectrometry (ICP-OES) with a total argon consumption below 0.7 L/min is applied for the first time to the field of food analysis. One goal is the investigation of the performance of this low flow plasma compared to a conventional ICP-OES system when non-aqueous samples with a certain matrix are introduced into the system. For this purpose, arsenic is determined in three different kinds of fish samples. In addition several nutrients (K, Na, Mg, Ca) and trace metals (Co, Cu, Mn, Cd, Pb, Zn, Fe, and Ni) are determined in honey samples (acacia) after microwave digestion. The precision of the measurements is characterized by relative standard deviations (RSD) and compared to the corresponding precision values achieved using the conventional Fassel-type torch of the ICP. To prove the accuracy of the low flow ICP-OES method, the obtained data from honey samples are validated by a conventional ICP-OES. For the measurements concerning arsenic in fish, the low flow ICP-OES values are validated by conventional Fassel-type ICP-OES. Furthermore, a certified reference material was investigated with the low gas flow setup. Limits of detection (LOD), according to the 3σ criterion, were determined to be in the low microgram per liter range for all analytes. Recovery rates in the range of 96-106% were observed for the determined trace metal elements. It was proven that the low gas flow ICP-OES leads to results that are comparable with those obtained with the Fassel-type torch for the analysis of food samples. Copyright © 2014 Elsevier B.V. All rights reserved.

A rapid and accurate quantification method for real-time dynamic analysis of cellular lipids during microalgal fermentation processes in Chlorella protothecoides with low field nuclear magnetic resonance.

PubMed

Wang, Tao; Liu, Tingting; Wang, Zejian; Tian, Xiwei; Yang, Yi; Guo, Meijin; Chu, Ju; Zhuang, Yingping

2016-05-01

The rapid and real-time lipid determination can provide valuable information on process regulation and optimization in the algal lipid mass production. In this study, a rapid, accurate and precise quantification method of in vivo cellular lipids of Chlorella protothecoides using low field nuclear magnetic resonance (LF-NMR) was newly developed. LF-NMR was extremely sensitive to the algal lipids with the limits of the detection (LOD) of 0.0026g and 0.32g/L in dry lipid samples and algal broth, respectively, as well as limits of quantification (LOQ) of 0.0093g and 1.18g/L. Moreover, the LF-NMR signal was specifically proportional to the cellular lipids of C. protothecoides, thus the superior regression curves existing in a wide detection range from 0.02 to 0.42g for dry lipids and from 1.12 to 8.97gL(-1) of lipid concentration for in vivo lipid quantification were obtained with all R(2) higher than 0.99, irrespective of the lipid content and fatty acids profile variations. The accuracy of this novel method was further verified to be reliable by comparing lipid quantification results to those obtained by GC-MS. And the relative standard deviation (RSD) of LF-NMR results were smaller than 2%, suggesting the precision of this method. Finally, this method was successfully used in the on-line lipid monitoring during the algal lipid fermentation processes, making it possible for better understanding of the lipid accumulation mechanism and dynamic bioprocess control. Copyright © 2016 Elsevier B.V. All rights reserved.

Ion-pair in-tube solid-phase microextraction and capillary liquid chromatography using a titania-based column: application to the specific lauralkonium chloride determination in water.

PubMed

Prieto-Blanco, M C; Moliner-Martínez, Y; López-Mahía, P; Campíns-Falcó, P

2012-07-27

A quick, miniaturized and on-line method has been developed for the determination in water of the predominant homologue of benzalkonium chloride, dodecyl dimethyl benzyl ammonium chloride or lauralkonium chloride (C(12)-BAK). The method is based on the formation of an ion-pair in both in-tube solid-phase microextraction (IT-SPME) and capillary liquid chromatography. The IT-SPME optimization required the study of the length and nature of the stationary phase of capillary and the processed sample volume. Because to the surfactant character of the analyte both, the extracting and replacing solvents, have played a decisive role in the IT-SPME optimized procedure. Conditioning the capillary with the mobile phase which contains the counter ion (acetate), using an organic additive (tetrabutylammonium chloride) added to the sample and a mixture water/methanol as replacing solvent (processed just before the valve is switched to the inject position), allowed to obtain good precision of the retention time and a narrow peak for C(12)-BAK. A reversed-phase capillary based TiO(2) column and a mobile phase containing ammonium acetate at pH 5.0 for controlling the interactions of cationic surfactant with titania surface were proposed. The optimized procedure provided adequate linearity, accuracy and precision at the concentrations interval of 1.5-300 μg L(-1) .The limit of detection (LOD) was 0.5 μg L(-1) using diode array detection (DAD). The applicability of proposed IT-SPME-capillary LC method has been assessed in several water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Application of statistical experimental design to the optimisation of microextraction by packed sorbent for the analysis of nonsteroidal anti-inflammatory drugs in human urine by ultra-high pressure liquid chromatography.

PubMed

Magiera, Sylwia; Gülmez, Şefika; Michalik, Aleksandra; Baranowska, Irena

2013-08-23

A new approach based on microextraction by packed sorbent (MEPS) and a reversed-phase ultra-high pressure liquid chromatography (UHPLC) method was developed and validated for the determination and quantification of nonsteroidal anti-inflammatory drugs (NSAIDs) (acetylsalicylic acid, ketoprofen, diclofenac, naproxen and ibuprofen) in human urine. The important factors that could influence the extraction were previously screened using the Plackett-Burman design approach. The optimal MEPS extraction conditions were obtained using C18 phase as a sorbent, small sample volume (20μL) and a short time period (approximately 5min) for the entire sample preparation step. The analytes were separated on a core-shell column (Poroshell 120 EC-C18; 100mm×3.0mm; 2.7μm) using a binary mobile phase composed of aqueous 0.1% trifluoroacetic acid and acetonitrile in the gradient elution mode (4.5min of analysis time). The analytical method was fully validated based on linearity, limits of detection (LOD), limits of quantification (LOQ), inter- and intra-day precision and accuracy, and extraction yield. Under optimised conditions, excellent linearity (R(2)>0.9991), limits of detection (1.07-16.2ngmL(-1)) and precision (0.503-9.15% RSD) were observed for the target drugs. The average absolute recoveries of the analysed compounds extracted from the urine samples were 89.4-107%. The proposed method was also applied to the analysis of NSAIDs in human urine. The new approach offers an attractive alternative for the analysis of selected drugs from urine samples, providing several advantages including fewer sample preparation steps, faster sample throughput and ease of performance compared to traditional methodologies. Copyright © 2013 Elsevier B.V. All rights reserved.

Screening approach by ultra-high performance liquid chromatography-tandem mass spectrometry for the blood quantification of thirty-four toxic principles of plant origin. Application to forensic toxicology.

PubMed

Carlier, Jérémy; Guitton, Jérôme; Romeuf, Ludovic; Bévalot, Fabien; Boyer, Baptiste; Fanton, Laurent; Gaillard, Yvan

2015-01-15

Plant poisonings have left their mark on history and still cause many deaths, whether intentional or accidental. The means to show toxicological evidence of such poisonings should be implemented with great care. This article presents a technique for measuring thirty-nine toxic principles of plant origin in the blood, covering a large amount of toxins from local or exotic plants: α-lobeline, α-solanine, aconitine, ajmaline, atropine, brucine, cephalomannine, colchicine, convallatoxin, cymarine, cytisine, digitoxin, digoxin, emetine, gelsemine, ibogaine, jervine, kavain, lanatoside C, lupanine, mitragynine, neriifolin, oleandrin, ouabain, paclitaxel, physostigmine, pilocarpine, podophyllotoxin, proscillaridin A, reserpine, retrorsine, ricinine, scopolamine, senecionine, sparteine, strophanthidin, strychnine, veratridine and yohimbine. Analysis was carried out using an original ultra-high performance liquid chromatography separation coupled with tandem mass spectrometry detection. Extraction was a standard solid phase extraction performed on Oasis(®) HLB cartridge. Thirty-four of the thirty-nine compounds were put through a validation procedure. The assay was linear in the calibration curve range from 0.5 or 5 μg/L to 1000 μg/L according to the compounds. The method is sensitive (LOD from 0.1 to 1.6 μg/L). The within-day precision of the assay was less than 22.5% at the LLOQ, and the between-day precision was less than 21.5% for 10 μg/L for all the compounds included. The assay accuracy was in the range of 87.4 to 119.8% for the LLOQ. The extraction recovery and matrix effect ranged from 30 to 106% and from -30 to 14%, respectively. It has proven useful and effective in several difficult forensic cases. Copyright © 2014 Elsevier B.V. All rights reserved.

Increased reliability of nuclear magnetic resonance protein structures by consensus structure bundles.

PubMed

Buchner, Lena; Güntert, Peter

2015-02-03

Nuclear magnetic resonance (NMR) structures are represented by bundles of conformers calculated from different randomized initial structures using identical experimental input data. The spread among these conformers indicates the precision of the atomic coordinates. However, there is as yet no reliable measure of structural accuracy, i.e., how close NMR conformers are to the "true" structure. Instead, the precision of structure bundles is widely (mis)interpreted as a measure of structural quality. Attempts to increase precision often overestimate accuracy by tight bundles of high precision but much lower accuracy. To overcome this problem, we introduce a protocol for NMR structure determination with the software package CYANA, which produces, like the traditional method, bundles of conformers in agreement with a common set of conformational restraints but with a realistic precision that is, throughout a variety of proteins and NMR data sets, a much better estimate of structural accuracy than the precision of conventional structure bundles. Copyright © 2015 Elsevier Ltd. All rights reserved.

Field comparison of several commercially available radon detectors.

PubMed Central

Field, R W; Kross, B C

1990-01-01

To determine the accuracy and precision of commercially available radon detectors in a field setting, 15 detectors from six companies were exposed to radon and compared to a reference radon level. The detectors from companies that had already passed National Radon Measurement Proficiency Program testing had better precision and accuracy than those detectors awaiting proficiency testing. Charcoal adsorption detectors and diffusion barrier charcoal adsorption detectors performed very well, and the latter detectors displayed excellent time averaging ability. Alternatively, charcoal liquid scintillation detectors exhibited acceptable accuracy but poor precision, and bare alpha registration detectors showed both poor accuracy and precision. The mean radon level reported by the bare alpha registration detectors was 68 percent lower than the radon reference level. PMID:2368851

Determination of bisphenols in beverages by mixed-mode solid-phase extraction and liquid chromatography coupled to tandem mass spectrometry.

PubMed

Regueiro, Jorge; Wenzl, Thomas

2015-11-27

Facing growing restrictions on the use of bisphenol A in food contact materials, several bisphenol analogs are arising as major alternatives to replace this chemical in most of its applications. This work reports a simple and robust method based on mixed-mode solid-phase extraction and stable-isotope dilution liquid chromatography-tandem mass spectrometry for the analysis of bisphenol A and its main analogs - bisphenol S, 4,4'-sulfonylbis(2-methylphenol), bisphenol F, bisphenol E, bisphenol B, bisphenol Z, bisphenol AF, bisphenol AP, tetrabromobisphenol A and bisphenol P - in alcoholic and non-alcoholic beverages. Mixed-mode solid-phase extraction, combining cationic exchange and reversed-phase mechanisms, was optimized to provide a selective extraction and purification of the target analytes. Derivatization of bisphenols with pyridine-3-sulfonyl chloride allowed increasing their ionization efficiency by electrospray ionization. Validation of the proposed method was performed in terms of selectivity, matrix effects, linearity, precision, measurement uncertainty, trueness and limits of detection. Satisfactory repeatability and intermediate precision were obtained; the related relative standard deviations were ≤9% and ≤12%, respectively. The relative expanded uncertainty (k=2) was below 20% for all bisphenol analogs and the trueness of the method was demonstrated by recovery experiments. Limits of detection (LOD) ranged from 1.6ngL(-1) to 27.9ngL(-1) for all compounds. Finally, several canned and non-canned beverages were analyzed to demonstrate the applicability of the method. Only bisphenol A and three bisphenol F isomers were detected in any of the samples. Bisphenol A concentration ranged from

Precision and accuracy of manual water-level measurements taken in the Yucca Mountain area, Nye County, Nevada, 1988-90

USGS Publications Warehouse

Boucher, M.S.

1994-01-01

Water-level measurements have been made in deep boreholes in the Yucca Mountain area, Nye County, Nevada, since 1983 in support of the U.S. Department of Energy's Yucca Mountain Project, which is an evaluation of the area to determine its suitability as a potential storage area for high-level nuclear waste. Water-level measurements were taken either manually, using various water-level measuring equipment such as steel tapes, or they were taken continuously, using automated data recorders and pressure transducers. This report presents precision range and accuracy data established for manual water-level measurements taken in the Yucca Mountain area, 1988-90. Precision and accuracy ranges were determined for all phases of the water-level measuring process, and overall accuracy ranges are presented. Precision ranges were determined for three steel tapes using a total of 462 data points. Mean precision ranges of these three tapes ranged from 0.014 foot to 0.026 foot. A mean precision range of 0.093 foot was calculated for the multiconductor cable, using 72 data points. Mean accuracy values were calculated on the basis of calibrations of the steel tapes and the multiconductor cable against a reference steel tape. The mean accuracy values of the steel tapes ranged from 0.053 foot, based on three data points to 0.078, foot based on six data points. The mean accuracy of the multiconductor cable was O. 15 foot, based on six data points. Overall accuracy of the water-level measurements was calculated by taking the square root of the sum of the squares of the individual accuracy values. Overall accuracy was calculated to be 0.36 foot for water-level measurements taken with steel tapes, without accounting for the inaccuracy of borehole deviations from vertical. An overall accuracy of 0.36 foot for measurements made with steel tapes is considered satisfactory for this project.

The power and robustness of maximum LOD score statistics.

PubMed

Yoo, Y J; Mendell, N R

2008-07-01

The maximum LOD score statistic is extremely powerful for gene mapping when calculated using the correct genetic parameter value. When the mode of genetic transmission is unknown, the maximum of the LOD scores obtained using several genetic parameter values is reported. This latter statistic requires higher critical value than the maximum LOD score statistic calculated from a single genetic parameter value. In this paper, we compare the power of maximum LOD scores based on three fixed sets of genetic parameter values with the power of the LOD score obtained after maximizing over the entire range of genetic parameter values. We simulate family data under nine generating models. For generating models with non-zero phenocopy rates, LOD scores maximized over the entire range of genetic parameters yielded greater power than maximum LOD scores for fixed sets of parameter values with zero phenocopy rates. No maximum LOD score was consistently more powerful than the others for generating models with a zero phenocopy rate. The power loss of the LOD score maximized over the entire range of genetic parameters, relative to the maximum LOD score calculated using the correct genetic parameter value, appeared to be robust to the generating models.

Laser-induced breakdown spectroscopy of light water reactor simulated used nuclear fuel: Main oxide phase

DOE PAGES

Campbell, Keri R.; Judge, Elizabeth J.; Barefield, James E.; ...

2017-04-22

We show the analysis of light water reactor simulated used nuclear fuel using laser-induced breakdown spectroscopy (LIBS) is explored using a simplified version of the main oxide phase. The main oxide phase consists of the actinides, lanthanides, and zirconium. The purpose of this study is to develop a rapid, quantitative technique for measuring zirconium in a uranium dioxide matrix without the need to dissolve the material. A second set of materials including cerium oxide is also analyzed to determine precision and limit of detection (LOD) using LIBS in a complex matrix. Two types of samples are used in this study:more » binary and ternary oxide pellets. The ternary oxide, (U,Zr,Ce)O 2 pellets used in this study are a simplified version the main oxide phase of used nuclear fuel. The binary oxides, (U,Ce)O 2 and (U,Zr)O 2 are also examined to determine spectral emission lines for Ce and Zr, potential spectral interferences with uranium and baseline LOD values for Ce and Zr in a UO 2 matrix. In the spectral range of 200 to 800 nm, 33 cerium lines and 25 zirconium lines were identified and shown to have linear correlation values (R 2) > 0.97 for both the binary and ternary oxides. The cerium LOD in the (U,Ce)O 2 matrix ranged from 0.34 to 1.08 wt% and 0.94 to 1.22 wt% in (U,Ce,Zr)O 2 for 33 of Ce emission lines. The zirconium limit of detection in the (U,Zr)O 2 matrix ranged from 0.84 to 1.15 wt% and 0.99 to 1.10 wt% in (U,Ce,Zr)O 2 for 25 Zr lines. Finally, the effect of multiple elements in the plasma and the impact on the LOD is discussed.« less

Simultaneous Determination of Four Compounds, Campesterol, Emodin8-O-β-D-Glucopyranoside, Quercetin, and Isoquercitrin in Reynoutria sachalinensis by High-performance Liquid Chromatography-Diode Array Detector

PubMed Central

Eom, Min Rye; Weon, Jin Bae; Jung, Youn Sik; Ryu, Ga Hee; Yang, Woo Seung; Ma, Choong Je

2017-01-01

Background: Reynoutria sachalinensis is a well-known and used herbal medicine to treatment of arthralgia, jaundice, amenorrhea, coughs, carbuncles, and sores. Objective: We have developed high-performance liquid chromatography analysis method for simultaneous determination of isolated four compounds, campesterol, emodin8-O-β-D-glucopyranoside, quercetin, and isoquercitrin from R. sachalinensis is. Materials and Methods: The four compounds were separated on Shiseido C18 column (S-5 μm, 4.6 mm I.D. ×250 mm) at a column temperature of 25°C. The mobile phase composed of water and methanol with gradient elution system, and flow rate is 1.0 ml/min. The detection wavelength was set at 205 nm. Results: Validation of this analytical method was evaluated by linearity, precision, and accuracy test. This established method had good linearity (R2 > 0.997). The relative standard deviation values of intra- and inter-day testing were indicated that <2%, and accuracy is 91.66%–103.31% at intraday and 91.69%–103.31% at intraday. The results of recovery test were 92.60%–108.99%. Conclusion: In these results, developed method was accurate and reliable to the quality evaluation of campesterol, emodin 8-O-β-D-glucopyranoside, quercetin, and isoquercitrin isolated from R. sachalinensis. SUMMARY We have developed high-performance liquid analysis method for simultaneous determination of 4 compounds of Reynoutria sachalinensis. Abbreviations used: HPLC: High-performance liquid chromatography, DAD: Diode array detector, LOD: Limit of detection, LOQ: Limit of quantitation, ICH: International Conference on Harmonisation. PMID:28808389

Clinical evaluation of the FreeStyle Precision Pro system.

PubMed

Brazg, Ronald; Hughes, Kristen; Martin, Pamela; Coard, Julie; Toffaletti, John; McDonnell, Elizabeth; Taylor, Elizabeth; Farrell, Lausanne; Patel, Mona; Ward, Jeanne; Chen, Ting; Alva, Shridhara; Ng, Ronald

2013-06-05

A new version of international standard (ISO 15197) and CLSI Guideline (POCT12) with more stringent accuracy criteria are near publication. We evaluated the glucose test performance of the FreeStyle Precision Pro system, a new blood glucose monitoring system (BGMS) designed to enhance accuracy for point-of-care testing (POCT). Precision, interference and system accuracy with 503 blood samples from capillary, venous and arterial sources were evaluated in a multicenter study. Study results were analyzed and presented in accordance with the specifications and recommendations of the final draft ISO 15197 and the new POCT12. The FreeStyle Precision Pro system demonstrated acceptable precision (CV <5%), no interference across a hematocrit range of 15-65%, and, except for xylose, no interference from 24 of 25 potentially interfering substances. It also met all accuracy criteria specified in the final draft ISO 15197 and POCT12, with 97.3-98.9% of the individual results of various blood sample types agreeing within ±12 mg/dl of the laboratory analyzer values at glucose concentrations <100mg/dl and within ±12.5% of the laboratory analyzer values at glucose concentrations ≥100 mg/dl. The FreeStyle Precision Pro system met the tighter accuracy requirements, providing a means for enhancing accuracy for point-of-care blood glucose monitoring. Copyright © 2013 Elsevier B.V. All rights reserved.

Dynamic interpretation of geoid anomalies

NASA Technical Reports Server (NTRS)

Hager, Bradford H.

1988-01-01

The NASA Geodynamics program has as two of its missions precise determination of spatial variations in earth's geopotential (or geoid) and highly accurate monitoring of polar motion, including changes in the length of day (LOD). For the past several years, data sets provided by NASA, along with data and models from other areas of geophysic were used to place fundamental contraints on the large scale dynamics of earth and her sister planet Venus. The main approach was using fluid mechanical models of mantle flow to predict the long-wavelength variations in the geoid.

Impact of laparoscopic ovarian drilling on serum anti-mullerian hormone levels in patients with anovulatory Polycystic Ovarian syndrome.

PubMed

Paramu, Sobhana

2016-12-01

Anti-mullerian hormone (AMH) is a marker of the activity of recruitable ovarian follicles. It is useful in the prediction of ovarian reserve. Women with polycystic ovarian syndrome (PCOS) have elevated circulating and intrafollicular AMH levels. Laparoscopic ovarian drilling (LOD) in patients with PCOS destroys ovarian androgen-producing tissue and reduces their peripheral conversion to estrogens. Identifying factors that determine the response of patients with PCOS to LOD will help in selecting the patients who would likely benefit from this treatment. AMH is one such marker that can predict the response to LOD. To evaluate the effect of LOD on serum AMH levels among PCOS responders and non-responders and the usefulness of AMH as a tool in predicting the response to LOD, and to whether there was loss of ovarian function after LOD. This is a prospective cohort study including 30 clomiphene-resistant women with anovulatory PCOS undergoing LOD. Statistical analysis was performed to evaluate the effect of LOD on serum levels of AMH on these women. A significant fall in the levels of AMH was observed after LOD in both responders and non-responders (p<0.001). Women with AMH >8.3 ng/mL showed a significantly lower ovulation rate (33.3%). LOD was not associated with a risk of diminished ovarian reserve. LOD is an effective first-line treatment for women with PCOS who are clomiphene resistant. LOD has no negative effect on ovarian reserve. AMH is a useful marker in predicting the outcome of LOD.

Enrichment and low-level determination of glyphosate, aminomethylphosphonic acid and glufosinate in drinking water after cleanup by cation exchange resin.

PubMed

Küsters, Markus; Gerhartz, Michael

2010-04-01

For the determination of glyphosate, aminomethylphosphonic acid and glufosinate in drinking water, different procedures of enrichment and cleanup were examined using anion exchange or SPE. In many cases interactions of, e.g. alkaline earth metal ions especially calcium could be observed during enrichment and cleanup resulting in loss of analytes. For that reason, a novel cleanup and enrichment procedure for the determination of these phosphonic acid herbicides has been developed in drinking water using cation-exchange resin. In summary, the cleanup procedure with cation-exchange resin developed in this study avoids interactions as described above and is applicable to calcium-rich drinking water samples. After derivatization with 9-fluorenylmethylchloroformate followed by LC with fluorescence detection, LOD of 12, 14 and 12 ng/L and mean recoveries from real-world drinking water samples of 98+/-9, 100+/-16 and 101+/-11% were obtained for glyphosate, aminomethylphosphonic acid and glufosinate, respectively. The low LODs and the high precision permit the analysis of these phosphonic acid herbicides according to the guidelines of the European Commission.

Precise Orbit Determination for ALOS

NASA Technical Reports Server (NTRS)

Nakamura, Ryo; Nakamura, Shinichi; Kudo, Nobuo; Katagiri, Seiji

2007-01-01

The Advanced Land Observing Satellite (ALOS) has been developed to contribute to the fields of mapping, precise regional land coverage observation, disaster monitoring, and resource surveying. Because the mounted sensors need high geometrical accuracy, precise orbit determination for ALOS is essential for satisfying the mission objectives. So ALOS mounts a GPS receiver and a Laser Reflector (LR) for Satellite Laser Ranging (SLR). This paper deals with the precise orbit determination experiments for ALOS using Global and High Accuracy Trajectory determination System (GUTS) and the evaluation of the orbit determination accuracy by SLR data. The results show that, even though the GPS receiver loses lock of GPS signals more frequently than expected, GPS-based orbit is consistent with SLR-based orbit. And considering the 1 sigma error, orbit determination accuracy of a few decimeters (peak-to-peak) was achieved.

A Dynamic Precision Evaluation Method for the Star Sensor in the Stellar-Inertial Navigation System.

PubMed

Lu, Jiazhen; Lei, Chaohua; Yang, Yanqiang

2017-06-28

Integrating the advantages of INS (inertial navigation system) and the star sensor, the stellar-inertial navigation system has been used for a wide variety of applications. The star sensor is a high-precision attitude measurement instrument; therefore, determining how to validate its accuracy is critical in guaranteeing its practical precision. The dynamic precision evaluation of the star sensor is more difficult than a static precision evaluation because of dynamic reference values and other impacts. This paper proposes a dynamic precision verification method of star sensor with the aid of inertial navigation device to realize real-time attitude accuracy measurement. Based on the gold-standard reference generated by the star simulator, the altitude and azimuth angle errors of the star sensor are calculated for evaluation criteria. With the goal of diminishing the impacts of factors such as the sensors' drift and devices, the innovative aspect of this method is to employ static accuracy for comparison. If the dynamic results are as good as the static results, which have accuracy comparable to the single star sensor's precision, the practical precision of the star sensor is sufficiently high to meet the requirements of the system specification. The experiments demonstrate the feasibility and effectiveness of the proposed method.

TLS for generating multi-LOD of 3D building model

NASA Astrophysics Data System (ADS)

Akmalia, R.; Setan, H.; Majid, Z.; Suwardhi, D.; Chong, A.

2014-02-01

The popularity of Terrestrial Laser Scanners (TLS) to capture three dimensional (3D) objects has been used widely for various applications. Development in 3D models has also led people to visualize the environment in 3D. Visualization of objects in a city environment in 3D can be useful for many applications. However, different applications require different kind of 3D models. Since a building is an important object, CityGML has defined a standard for 3D building models at four different levels of detail (LOD). In this research, the advantages of TLS for capturing buildings and the modelling process of the point cloud can be explored. TLS will be used to capture all the building details to generate multi-LOD. This task, in previous works, involves usually the integration of several sensors. However, in this research, point cloud from TLS will be processed to generate the LOD3 model. LOD2 and LOD1 will then be generalized from the resulting LOD3 model. Result from this research is a guiding process to generate the multi-LOD of 3D building starting from LOD3 using TLS. Lastly, the visualization for multi-LOD model will also be shown.

Determination of trace amount of cadmium using dispersive liquid-liquid microextraction-slotted quartz tube-flame atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Fırat, Merve; Bakırdere, Sezgin; Fındıkoğlu, Maral Selin; Kafa, Emine Betül; Yazıcı, Elif; Yolcu, Melda; Büyükpınar, Çağdaş; Chormey, Dotse Selali; Sel, Sabriye; Turak, Fatma

2017-03-01

This study was performed to develop a sensitive analytical method for the determination of cadmium by slotted quartz tube-flame atomic absorption spectrometry (SQT-FAAS) after dispersive liquid-liquid microextraction (DLLME). The parameters affecting the cadmium complex formation and its extraction output were optimized to obtain high extraction efficiency. These included the pH and amount of the buffer solution, and the concentration of the ligand. The DLLME method was comprehensively optimized based on the type and amount of extraction solvent, dispersive solvent and salt. The type and period of mixing needed for a more effective extraction was also investigated. In order to further improve the sensitivity for the determination of cadmium, the flame atomic absorption spectrometry was fitted with a slotted quartz tube to increase the residence time of cadmium atoms in the pathway of incident light from a hollow cathode lamp. The limits of detection and quantitation (LOD and LOQ) for the FAAS were found to be 42 and 140 μg L- 1, respectively. Under the optimum conditions, LOD and LOQ of the FAAS after DLLME were calculated as 1.3 and 4.4 μg L- 1, respectively. Combining both optimized parameters of the DLLME and SQT-FAAS gave 0.5 and 1.5 μg L- 1 as LOD and LOQ, respectively. Accuracy of the method was also checked using a wastewater certified reference material (EU-L-2), and the result was in good agreement with the certified value.

Formulation of an aloe-based product according to Iranian traditional medicine and development of its analysis method.

PubMed

Moein, Elham; Hajimehdipoor, Homa; Toliyat, Tayebeh; Choopani, Rasool; Hamzeloo-Moghadam, Maryam

2017-08-29

Currently, people are more interested to traditional medicine. The traditional formulations should be converted to modern drug delivery systems to be more acceptable for the patients. In the present investigation, a poly herbal medicine "Ayarij-e-Faiqra" (AF) based on Iranian traditional medicine (ITM) has been formulated and its quality control parameters have been developed. The main ingredients of AF including barks of Cinnamomum zeylanicum Blume and Cinnamomum cassia J. Presl, the rhizomes of Nardostachys jatamansi DC., the fruits of Piper cubeba L.f., the flowers of Rosa damascena Herrm., the oleo gum resin of Pistacia terebinthus L. and Aloe spp. dried juice were powdered and used for preparing seven tablet formulations of the herbal mixture. Flowability of the different formulated powders was examined and the best formulations were selected (F6&F7). The tablets were prepared from the selected formulations compared according to the physical characteristics and finally, F7 was selected and coated. Physicochemical characters of core and coated AF tablets were determined and the HPLC method for quantitation of aloin as a marker of tablets was selected and verified according to selectivity, linearity, precision, recovery, LOD and LOQ. The results showed that core and coated AF tablets were in agreement with USP requirements for herbal drugs. They had acceptable appearance, disintegration time, friability, hardness, dissolution behavior, weight variation and content uniformity. The amount of aloin in tablets was found 123.1 mg/tab. The HPLC method for aloin determination in AF tablets was verified according to selectivity, linearity (5-500 μg/ml, r 2 :0.9999), precision (RSD: 1.62%), recovery (108.0%), LOD & LOQ (0.0053 & 0.0161 μg/ml). The formulated tablets could be a good substitute for powder and capsules of AF in ITM clinics with a feasible and precise method for its quality control. Ayarij-e-Faiqra formulation.

Determination of Bortezomib in API Samples Using HPLC: Assessment of Enantiomeric and Diastereomeric Impurities.

PubMed

Kamalzadeh, Zahra; Babanezhad, Esmaeil; Ghaffari, Solmaz; Mohseni Ezhiyeh, Alireza; Mohammadnejad, Mahdieh; Naghibfar, Mehdi; Bararjanian, Morteza; Attar, Hossein

2017-08-01

A new, normal phase high performance liquid chromatography (NP-HPLC) method was developed for separation of Bortezomib (BZB) enantiomers and quantitative determination of (1S,2R)-enantiomer of BZB in active pharmaceutical ingredient (API) samples. The developed method was validated based on International Conference on Harmonisation (ICH) guidelines and it was proved to be accurate, precise and robust. The obtained resolution (RS) between the enantiomers was more than 2. The calibration curve for (1S,2R)-enantiomer was found to be linear in the concentration range of 0.24-5.36 mg/L with regression coefficient (R2) of 0.9998. Additionally, the limit of detection (LOD) and limit of quantification (LOQ) were 0.052 and 0.16 mg/L, respectively. Also, in this study, a precise, sensitive and robust gradient reversed-phase HPLC (RP-HPLC) method was developed and validated for determination of BZB in API samples. The detector response was linear over the concentration range of 0.26-1110.5 mg/L. The values of R2, LOD and LOQ were 0.9999, 0.084 and 0.25 mg/L, respectively. For both NP-HPLC and RP-HPLC methods, all of the RSD (%) values obtained in the precision study were <1.0%. System suitability parameters in terms of tailing factor (TF), number of theoretical plates (N) and RS were TF < 2.0, N > 2,000 and RS > 2.0. The performance of two common integration methods of valley to valley and drop perpendicular for drawing the baseline between two adjacent peaks were investigated for the determination of diastereomeric impurity (Imp-D) in the BZB-API samples. The results showed that the valley to valley method outperform the drop perpendicular method for calculation of Imp-D peak areas. Therefore, valley to valley method was chosen for peak integration. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Airborne Topographic Mapper Calibration Procedures and Accuracy Assessment

NASA Technical Reports Server (NTRS)

Martin, Chreston F.; Krabill, William B.; Manizade, Serdar S.; Russell, Rob L.; Sonntag, John G.; Swift, Robert N.; Yungel, James K.

2012-01-01

Description of NASA Airborn Topographic Mapper (ATM) lidar calibration procedures including analysis of the accuracy and consistancy of various ATM instrument parameters and the resulting influence on topographic elevation measurements. The ATM elevations measurements from a nominal operating altitude 500 to 750 m above the ice surface was found to be: Horizontal Accuracy 74 cm, Horizontal Precision 14 cm, Vertical Accuracy 6.6 cm, Vertical Precision 3 cm.

Meteorological interpretation of transient LOD changes

NASA Astrophysics Data System (ADS)

Masaki, Y.

2008-04-01

The Earth’s spin rate is mainly changed by zonal winds. For example, seasonal changes in global atmospheric circulation and episodic changes accompanied with El Nĩ os are clearly detected n in the Length-of-day (LOD). Sub-global to regional meteorological phenomena can also change the wind field, however, their effects on the LOD are uncertain because such LOD signals are expected to be subtle and transient. In our previous study (Masaki, 2006), we introduced atmospheric pressure gradients in the upper atmosphere in order to obtain a rough picture of the meteorological features that can change the LOD. In this presentation, we compare one-year LOD data with meteorological elements (winds, temperature, pressure, etc.) and make an attempt to link transient LOD changes with sub-global meteorological phenomena.

Flow injection analysis of organic peroxide explosives using acid degradation and chemiluminescent detection of released hydrogen peroxide.

PubMed

Mahbub, Parvez; Zakaria, Philip; Guijt, Rosanne; Macka, Mirek; Dicinoski, Greg; Breadmore, Michael; Nesterenko, Pavel N

2015-10-01

The applicability of acid degradation of organic peroxides into hydrogen peroxide in a pneumatically driven flow injection system with chemiluminescence reaction with luminol and Cu(2+) as a catalyst (FIA-CL) was investigated for the fast and sensitive detection of organic peroxide explosives (OPEs). The target OPEs included hexamethylene triperoxide diamine (HMTD), triacetone triperoxide (TATP) and methylethyl ketone peroxide (MEKP). Under optimised conditions maximum degradations of 70% and 54% for TATP and HMTD, respectively were achieved at 162 µL min(-1), and 9% degradation for MEKP at 180 µL min(-1). Flow rates were precisely controlled in this single source pneumatic pressure driven multi-channel FIA system by model experiments on mixing of easily detectable component solutions. The linear range for detection of TATP, HMTD and H2O2 was 1-200 µM (r(2)=0.98-0.99) at both flow rates, while that for MEKP was 20-200 µM (r(2)=0.97) at 180 µL min(-1). The detection limits (LODs) obtained were 0.5 µM for TATP, HMTD and H2O2 and 10 µM for MEKP. The detection times varied from 1.5 to 3 min in this FIA-CL system. Whilst the LOD for H2O2 was comparable with those reported by other investigators, the LODs and analysis times for TATP and HMTD were superior, and significantly, this is the first time the detection of MEKP has been reported by FIA-CL. Copyright © 2015 Elsevier B.V. All rights reserved.

A study comparing precision of the maximum multipoint heterogeneity LOD statistic to three model-free multipoint linkage methods.

PubMed

Finch, S J; Chen, C H; Gordon, D; Mendell, N R

2001-12-01

This study compared the performance of the maximum lod (MLOD), maximum heterogeneity lod (MHLOD), maximum non-parametric linkage score (MNPL), maximum Kong and Cox linear extension (MKC(lin)) of NPL, and maximum Kong and Cox exponential extension (MKC(exp)) of NPL as calculated in Genehunter 1.2 and Genehunter-Plus. Our performance measure was the distance between the marker with maximum value for each linkage statistic and the trait locus. We performed a simulation study considering: 1) four modes of transmission, 2) 100 replicates for each model, 3) 58 pedigrees (with 592 subjects) per replicate, 4) three linked marker loci each having three equally frequent alleles, and 5) either 0% unlinked families (linkage homogeneity) or 50% unlinked families (linkage heterogeneity). For each replicate, we obtained the Haldane map position of the location at which each of the five statistics is maximized. The MLOD and MHLOD were obtained by maximizing over penetrances, phenocopy rate, and risk-allele frequencies. For the models simulated, MHLOD appeared to be the best statistic both in terms of identifying a marker locus having the smallest mean distance from the trait locus and in terms of the strongest negative correlation between maximum linkage statistic and distance of the identified position and the trait locus. The marker loci with maximum value of the Kong and Cox extensions of the NPL statistic also were closer to the trait locus than the marker locus with maximum value of the NPL statistic. Copyright 2001 Wiley-Liss, Inc.

Electrothermal vaporization of mineral acid solutions in inductively coupled plasma mass spectrometry: comparison with sample nebulization

NASA Astrophysics Data System (ADS)

Mora, Juan; Gras, Luis; van Veen, Eric H.; de Loos-Vollebregt, Margaretha T. C.

1999-06-01

The analytical behaviour of an electrothermal vaporization (ETV) device for the introduction of mineral acid solutions in inductively coupled plasma mass spectrometry (ICP-MS) was evaluated. Water, nitric acid, hydrochloric acid, perchloric acid and sulphuric acid in concentrations within the 0.05-1.0 mol l-1 range were studied. For all the acids tested, increasing the acid concentration increases the ion signal and deteriorates the precision. The magnitude of the signal enhancement depends on the analyte and on the acid considered. Acid solutions give rise to ion signals that are between 2 and 10 times higher than those with water. Among the acids tested, sulphuric acid provides the highest signals. The addition of palladium reduces matrix effects due to the acids and increases the signal in ETV ICP-MS. In comparison with conventional sample nebulization (CS), the ETV sample introduction system provides higher sensitivities (between 2 and 20 times higher) at the same acid concentration. The magnitude of this improvement is similar to that obtained with a microwave desolvation system (MWDS). The ETV sample introduction system gives rise to the lowest background signals from matrix-induced species. Due to this fact, the limits of detection (LODs) obtained for the isotopes affected by any interference are lower for ETV sample introduction than those obtained with the CS and the MWDS. For the isotopes that do not suffer from matrix-induced spectral interferences, the ETV gives rise to LODs higher than those obtained with the CS. For these isotopes the lowest LODs are obtained with MWDS.

A Note on "Accuracy" and "Precision"

ERIC Educational Resources Information Center

Stallings, William M.; Gillmore, Gerald M.

1971-01-01

Advocates the use of precision" rather than accuracy" in defining reliability. These terms are consistently differentiated in certain sciences. Review of psychological and measurement literature reveals, however, interchangeable usage of the terms in defining reliability. (Author/GS)

40 CFR 92.105 - General equipment specifications.

Code of Federal Regulations, 2011 CFR

2011-07-01

... accuracy and precision of 0.1 percent of absolute pressure at point or better. (2) Gauges and transducers used to measure any other pressures shall have an accuracy and precision of 1 percent of absolute...

Development and validation of an automated and marker-free CT-based spatial analysis method (CTSA) for assessment of femoral hip implant migration: In vitro accuracy and precision comparable to that of radiostereometric analysis (RSA).

PubMed

Scheerlinck, Thierry; Polfliet, Mathias; Deklerck, Rudi; Van Gompel, Gert; Buls, Nico; Vandemeulebroucke, Jef

2016-01-01

We developed a marker-free automated CT-based spatial analysis (CTSA) method to detect stem-bone migration in consecutive CT datasets and assessed the accuracy and precision in vitro. Our aim was to demonstrate that in vitro accuracy and precision of CTSA is comparable to that of radiostereometric analysis (RSA). Stem and bone were segmented in 2 CT datasets and both were registered pairwise. The resulting rigid transformations were compared and transferred to an anatomically sound coordinate system, taking the stem as reference. This resulted in 3 translation parameters and 3 rotation parameters describing the relative amount of stem-bone displacement, and it allowed calculation of the point of maximal stem migration. Accuracy was evaluated in 39 comparisons by imposing known stem migration on a stem-bone model. Precision was estimated in 20 comparisons based on a zero-migration model, and in 5 patients without stem loosening. Limits of the 95% tolerance intervals (TIs) for accuracy did not exceed 0.28 mm for translations and 0.20° for rotations (largest standard deviation of the signed error (SD(SE)): 0.081 mm and 0.057°). In vitro, limits of the 95% TI for precision in a clinically relevant setting (8 comparisons) were below 0.09 mm and 0.14° (largest SD(SE): 0.012 mm and 0.020°). In patients, the precision was lower, but acceptable, and dependent on CT scan resolution. CTSA allows detection of stem-bone migration with an accuracy and precision comparable to that of RSA. It could be valuable for evaluation of subtle stem loosening in clinical practice.

Successional stage of biological soil crusts: an accurate indicator of ecohydrological condition

USGS Publications Warehouse

Belnap, Jayne; Wilcox, Bradford P.; Van Scoyoc, Matthew V.; Phillips, Susan L.

2013-01-01

Biological soil crusts are a key component of many dryland ecosystems. Following disturbance, biological soil crusts will recover in stages. Recently, a simple classification of these stages has been developed, largely on the basis of external features of the crusts, which reflects their level of development (LOD). The classification system has six LOD classes, from low (1) to high (6). To determine whether the LOD of a crust is related to its ecohydrological function, we used rainfall simulation to evaluate differences in infiltration, runoff, and erosion among crusts in the various LODs, across a range of soil depths and with different wetting pre-treatments. We found large differences between the lowest and highest LODs, with runoff and erosion being greatest from the lowest LOD. Under dry antecedent conditions, about 50% of the water applied ran off the lowest LOD plots, whereas less than 10% ran off the plots of the two highest LODs. Similarly, sediment loss was 400 g m-2 from the lowest LOD and almost zero from the higher LODs. We scaled up the results from these simulations using the Rangeland Hydrology and Erosion Model. Modelling results indicate that erosion increases dramatically as slope length and gradient increase, especially beyond the threshold values of 10 m for slope length and 10% for slope gradient. Our findings confirm that the LOD classification is a quick, easy, nondestructive, and accurate index of hydrological condition and should be incorporated in field and modelling assessments of ecosystem health.

S193 radiometer brightness temperature precision/accuracy for SL2 and SL3

NASA Technical Reports Server (NTRS)

Pounds, D. J.; Krishen, K.

1975-01-01

The precision and accuracy with which the S193 radiometer measured the brightness temperature of ground scenes is investigated. Estimates were derived from data collected during Skylab missions. Homogeneous ground sites were selected and S193 radiometer brightness temperature data analyzed. The precision was expressed as the standard deviation of the radiometer acquired brightness temperature. Precision was determined to be 2.40 K or better depending on mode and target temperature.

Research on the impact factors of GRACE precise orbit determination by dynamic method

NASA Astrophysics Data System (ADS)

Guo, Nan-nan; Zhou, Xu-hua; Li, Kai; Wu, Bin

2018-07-01

With the successful use of GPS-only-based POD (precise orbit determination), more and more satellites carry onboard GPS receivers to support their orbit accuracy requirements. It provides continuous GPS observations in high precision, and becomes an indispensable way to obtain the orbit of LEO satellites. Precise orbit determination of LEO satellites plays an important role for the application of LEO satellites. Numerous factors should be considered in the POD processing. In this paper, several factors that impact precise orbit determination are analyzed, namely the satellite altitude, the time-variable earth's gravity field, the GPS satellite clock error and accelerometer observation. The GRACE satellites provide ideal platform to study the performance of factors for precise orbit determination using zero-difference GPS data. These factors are quantitatively analyzed on affecting the accuracy of dynamic orbit using GRACE observations from 2005 to 2011 by SHORDE software. The study indicates that: (1) with the altitude of the GRACE satellite is lowered from 480 km to 460 km in seven years, the 3D (three-dimension) position accuracy of GRACE satellite orbit is about 3˜4 cm based on long spans data; (2) the accelerometer data improves the 3D position accuracy of GRACE in about 1 cm; (3) the accuracy of zero-difference dynamic orbit is about 6 cm with the GPS satellite clock error products in 5 min sampling interval and can be raised to 4 cm, if the GPS satellite clock error products with 30 s sampling interval can be adopted. (4) the time-variable part of earth gravity field model improves the 3D position accuracy of GRACE in about 0.5˜1.5 cm. Based on this study, we quantitatively analyze the factors that affect precise orbit determination of LEO satellites. This study plays an important role to improve the accuracy of LEO satellites orbit determination.

Simultaneous HPLC-F analysis of three recent antiepileptic drugs in human plasma.

PubMed

Mercolini, Laura; Mandrioli, Roberto; Amore, Mario; Raggi, Maria Augusta

2010-09-21

An original high-performance liquid chromatographic method with fluorescence detection is presented for the simultaneous determination of the three antiepileptic drugs gabapentin, vigabatrin and topiramate in human plasma. After pre-column derivatisation with dansyl chloride, the analytes were separated on a Hydro-RP column with a mobile phase composed of phosphate buffer (55%) and acetonitrile (45%) and detected at lambda(em)=500 nm, exciting at 300 nm. An original pre-treatment procedure on biological samples, based on solid-phase extraction with MCX cartridges for gabapentin and vigabatrin, and with Plexa cartridges for topiramate, gave high extraction yields (>91%), satisfactory precision (RSD<6.4%) and good selectivity. Linearity was found in the 0.2-50.0 microg mL(-1) range for gabapentin, in the 1.0-100.0 microg mL(-1) range for vigabatrin and in the 1.0-50.0 microg mL(-1) range for topiramate, with limits of detection (LODs) between 0.1 and 0.3 microg mL(-1). After validation, the method was successfully applied to some plasma samples from patients undergoing therapy with one or more of these drugs. Accuracy results were satisfactory (recovery >91%). Therefore, the method seems to be suitable for the therapeutic drug monitoring (TDM) of patients treated with gabapentin, vigabatrin and topiramate. Copyright 2010 Elsevier B.V. All rights reserved.

Validation and evaluation of an HPLC methodology for the quantification of the potent antimitotic compound (+)-discodermolide in the Caribbean marine sponge Discodermia dissoluta.

PubMed

Valderrama, Katherine; Castellanos, Leonardo; Zea, Sven

2010-08-01

The sponge Discodermia dissoluta is the source of the potent antimitotic compound (+)-discodermolide. The relatively abundant and shallow populations of this sponge in Santa Marta, Colombia, allow for studies to evaluate the natural and biotechnological supply options of (+)-discodermolide. In this work, an RP-HPLC-UV methodology for the quantification of (+)-discodermolide from sponge samples was tested and validated. Our protocol for extracting this compound from the sponge included lyophilization, exhaustive methanol extraction, partitioning using water and dichloromethane, purification of the organic fraction in RP-18 cartridges and then finally retrieving the (+)-discodermolide in the methanol-water (80:20 v/v) fraction. This fraction was injected into an HPLC system with an Xterra RP-18 column and a detection wavelength of 235 nm. The calibration curve was linear, making it possible to calculate the LODs and quantification in these experiments. The intra-day and inter-day precision showed relative standard deviations lower than 5%. The accuracy, determined as the percentage recovery, was 99.4%. Nine samples of the sponge from the Bahamas, Bonaire, Curaçao and Santa Marta had concentrations of (+)-discodermolide ranging from 5.3 to 29.3 microg/g(-1) of wet sponge. This methodology is quick and simple, allowing for the quantification in sponges from natural environments, in situ cultures or dissociated cells.

A Localized Surface Plasmon Resonance Sensing Method for Simultaneous Determination of Atenolol and Amiloride in Pharmaceutical Dosage Forms and Urine Samples

PubMed Central

2018-01-01

This contribution describes a simple, fast, and sensitive application of localized surface plasmon resonance effect of silver nanoparticles for simultaneous determination of antihypertensive drugs' mixture atenolol and amiloride in both pharmaceutical dosage forms and in biological samples (urine). Silver nanoparticles were prepared by chemical reduction of silver nitrate using hydroxylamine HCL in an alkaline medium. Application of silver-hydroxylamine nanoparticles (SH NPs) provides many advantages including reproducibility, sensitivity, and cost effective way of analyte determination. Amiloride has four amino groups which act as attachment points on the surface of silver nanoparticles resulting in a synergistic effect on the absorption intensity of atenolol, leading to increase the sensitivity of the determination of both compounds. This method shows excellent advantages comparing with the previously reported methods, including accuracy, precision, and selectivity. The linear range of atenolol is 1 × 10−5–1 × 10−4 mol·L−1 and of amiloride is 1 × 10−6–1 × 10−5 mol·L−1. The limit of detection (LOD) values of atenolol and amiloride are 0.89 × 10−5 and 0.42 × 10−6 mol·L−1, respectively. PMID:29576886

Method for the determination of catechin and epicatechin enantiomers in cocoa-based ingredients and products by high-performance liquid chromatography: single-laboratory validation.

PubMed

Machonis, Philip R; Jones, Matthew A; Schaneberg, Brian T; Kwik-Uribe, Catherine L

2012-01-01

A single-laboratory validation study was performed for an HPLC method to identify and quantify the flavanol enantiomers (+)- and (-)-epicatechin and (+)- and (-)-catechin in cocoa-based ingredients and products. These compounds were eluted isocratically with an ammonium acetate-methanol mobile phase applied to a modified beta-cyclodextrin chiral stationary phase and detected using fluorescence. Spike recovery experiments using appropriate matrix blanks, along with cocoa extract, cocoa powder, and dark chocolate, were used to evaluate accuracy, repeatability, specificity, LOD, LOQ, and linearity of the method as performed by a single analyst on multiple days. In all samples analyzed, (-)-epicatechin was the predominant flavanol and represented 68-91% of the total monomeric flavanols detected. For the cocoa-based products, within-day (intraday) precision for (-)-epicatechin was between 1.46-3.22%, for (+)-catechin between 3.66-6.90%, and for (-)-catechin between 1.69-6.89%; (+)-epicatechin was not detected in these samples. Recoveries for the three sample types investigated ranged from 82.2 to 102.1% at the 50% spiking level, 83.7 to 102.0% at the 100% spiking level, and 80.4 to 101.1% at the 200% spiking level. Based on performance results, this method may be suitable for routine laboratory use in analysis of cocoa-based ingredients and products.

Validated spectrofluorimetric method for determination of two phosphodiesterase inhibitors tadalafil and vardenafil in pharmaceutical preparations and spiked human plasma.

PubMed

Abu El-Enin, Mohammed Abu Bakr; Al-Ghaffar Hammouda, Mohammed El-Sayed Abd; El-Sherbiny, Dina Tawfik; El-Wasseef, Dalia Rashad; El-Ashry, Saadia Mahmoud

2016-02-01

A valid, sensitive and rapid spectrofluorimetric method has been developed and validated for determination of both tadalafil (TAD) and vardenafil (VAR) either in their pure form, in their tablet dosage forms or spiked in human plasma. This method is based on measurement of the native fluorescence of both drugs in acetonitrile at λem 330 and 470 nm after excitation at 280 and 275 nm for tadalafil and vardenafil, respectively. Linear relationships were obtained over the concentration range 4-40 and 10-250 ng/mL with a minimum detection of 1 and 3 ng/mL for tadalafil and vardenafil, respectively. Various experimental parameters affecting the fluorescence intensity were carefully studied and optimized. The developed method was applied successfully for the determination of tadalafil and vardenafil in bulk drugs and tablet dosage forms. Moreover, the high sensitivity of the proposed method permitted their determination in spiked human plasma. The developed method was validated in terms of specificity, linearity, lower limit of quantification (LOQ), lower limit of detection (LOD), precision and accuracy. The mean recoveries of the analytes in pharmaceutical preparations were in agreement with those obtained from the comparison methods, as revealed by statistical analysis of the obtained results using Student's t-test and the variance ratio F-test. Copyright © 2015 John Wiley & Sons, Ltd.

Ionic liquid phase microextraction combined with fluorescence spectrometry for preconcentration and quantitation of carvedilol in pharmaceutical preparations and biological media.

PubMed

Zeeb, Mohsen; Mirza, Behrooz

2015-04-30

Carvedilol belongs to a group of medicines termed non-selective beta-adrenergic blocking agents. In the presented approach, a practical and environmentally friendly microextraction method based on the application of ionic liquids (ILs) was followed by fluorescence spectrometry for trace determination of carvedilol in pharmaceutical and biological media. A rapid and simple ionic liquid phase microextraction was utilized for preconcentration and extraction of carvedilol. A hydrophobic ionic liquid (IL) was applied as a microextraction solvent. In order to disperse the IL through the aqueous media and extract the analyte of interest, IL was injected into the sample solution and a proper temperature was applied and then for aggregating the IL-phase, the sample was cooled in an ice water-bath. The aqueous media was centrifuged and IL-phase collected at the bottom of the test tube was introduced to the micro-cell of spectrofluorimeter, in order to determine the concentration of the enriched analyte. Main parameters affecting the accuracy and precision of the proposed approach were investigated and optimized values were obtained. A linear response range of 10-250 μg I(-1) and a limit of detection (LOD) of 1.7 μg I(-1) were obtained. Finally, the presented method was utilized for trace determination of carvedilol in commercial pharmaceutical preparations and biological media.

Development of a microchip-pulsed electrochemical method for rapid determination of L-DOPA and tyrosine in Mucuna pruriens.

PubMed

Li, Xinchun; Chen, Zuanguang; Yang, Fan; Pan, Jianbin; Li, Yinbao

2013-05-01

L-3,4-dihydroxyphenylalanine (L-DOPA) is a well-recognized therapeutic compound to Parkinson's disease. Tyrosine is a precursor for the biosynthesis of L-DOPA, both of which are widely found in traditional medicinal material, Mucuna pruriens. In this paper, we described a validated novel analytical method based on microchip capillary electrophoresis with pulsed electrochemical detection for the simultaneous measurement of L-DOPA and tyrosine in M. pruriens. This protocol adopted end-channel amperometric detection using platinum disk electrode on a homemade glass/polydimethylsiloxane electrophoresis microchip. The background buffer consisted of 10 mM borate (pH 9.5) and 0.02 mM cetyltrimethylammonium bromide, which can produce an effective resolution for the two analytes. In the optimal condition, sufficient electrophoretic separation and sensitive detection for the target analytes can be realized within 60 s. Both tyrosine and L-DOPA yielded linear response in the concentration range of 5.0-400 μM (R(2) > 0.99), and the LOD were 0.79 and 1.1 μM, respectively. The accuracy and precision of the established method were favorable. The present method shows several merits such as facile apparatus, high speed, low cost and minimal pollution, and provides a means for the pharmacologically active ingredients assay in M. pruriens. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of homovanillic acid (HVA) in human plasma by HPLC with coulometric detection and a new SPE procedure.

PubMed

Saracino, M A; Mandrioli, R; Mercolini, L; Ferranti, A; Zaimovic, A; Leonardi, C; Raggi, M A

2006-09-11

A sensitive high-performance liquid chromatographic method has been developed for the determination of homovanillic acid (HVA), the main metabolite of dopamine, in human plasma. Analyses were carried out on a reversed-phase column (C8, 250 mm x 4.6 mm i.d., 5 microm) using a mobile phase composed of 10% methanol and 90% aqueous citrate buffer, containing octanesulfonic acid and EDTA at pH 4.8. Coulometric detection was used, setting the guard cell at +0.100 V, the first analytical cell at -0.200 V and the second analytical cell at +0.500 V. A careful solid-phase extraction procedure, based on strong anion exchange (SAX) cartridges (100 mg, 1 mL), was implemented for the pre-treatment of plasma samples. Extraction yield was satisfactory, being the mean value 98.0%. The calibration curve was linear over the concentration range of 0.2-25.0 ng mL(-1) of homovanillic acid. The limit of quantitation (LOQ) was 0.2 ng mL(-1) and the limit of detection (LOD) was 0.1 ng mL(-1). The method was successfully applied to plasma samples from former alcohol, cocaine and heroin addicts. Results were satisfactory in terms of precision and accuracy. Hence, the method is suitable for the determination of homovanillic acid in human plasma.

An improved HPLC-DAD method for quantitative comparisons of triterpenes in Ganoderma lucidum and its five related species originating from Vietnam.

PubMed

Ha, Do Thi; Loan, Le Thi; Hung, Tran Manh; Han, Le Vu Ngoc; Khoi, Nguyen Minh; Dung, Le Viet; Min, Byung Sun; Nguyen, Nguyen Phuong Dai

2015-01-09

An HPLC-DAD method for the quality control of wild and cultivated Ganoderma lucidum (Linhzhi) and related species samples was developed and validated. The quantitative determination of G. lucidum and its related species using 14 triterpene constituents, including nine ganoderma acids (compounds 4-12), four alcohols (compounds 13-16), and one sterol (ergosterol, 17) were reported. The standard curves were linear over the concentration range of 7.5-180 µg/mL. The LOD and LOQ values for the analyses varied from 0.34 to 1.41 µg/mL and from 1.01 to 4.23 µg/mL, respectively. The percentage recovery of each reference compound was found to be from 97.09% to 100.79%, and the RSD (%) was less than 2.35%. The precision and accuracy ranged from 0.81%-3.20% and 95.38%-102.19% for intra-day, and from 0.43%-3.67% and 96.63%-103.09% for inter-day, respectively. The study disclosed in detail significant differences between the quantities of analyzed compounds in different samples. The total triterpenes in wild Linhzhi samples were significantly higher than in cultivated ones. The total constituent contents of the five related Linhzhi samples were considerably lower than that in the G. lucidum specimens, except for G. australe as its constituent content outweighed wild Linhzhi's content by 4:1.

Development, validation and application of a SDME/GC-FID methodology for the multiresidue determination of organophosphate and pyrethroid pesticides in water.

PubMed

Pinheiro, Anselmo de Souza; de Andrade, Jailson B

2009-10-15

A single-drop microextraction (SDME) procedure was developed for the analysis of organophosphorus and pyrethroid pesticides in water by gas chromatography (GC) with flame ionization detection (GC-FID). The significant parameters that affect SDME performance, such as the selection of microextraction solvent, solvent volume, extraction time, and stirring rate, were studied and optimized using a tool screening factorial design. The limits of detection (LODs) in water for the four investigated compounds were between 0.3 and 3.0 microgL(-1), with relative standard deviations ranging from 7.7 to 18.8%. Linear response data were obtained in the concentration range of 0.9-6.0 microg L(-1) (lambda-cyhalothrin), 3.0-60.0 microg L(-1) (methyl parathion), 9.0-60.0 microg L(-1) (ethion), and 9.0-30.0 microg L(-1) (permethrin), with correlation coefficients ranging from 0.9337 to 0.9977. The relative recoveries for the spiked water ranged from 73.0 to 104%. Environmental water samples (n=26) were successfully analyzed using the proposed method and methyl parathion presented concentration up to 2.74 microg L(-1). The SDME method, coupled with GC-FID analysis, provided good precision, accuracy, and reproducibility over a wide linear range. Other highlights of the method include its ease of use and its requirement of only small volumes of both organic solvent and sample.

A rapid UPLC method for simultaneous determination of eleven components in ‘Ge-Gen-Qin-Lian’ decoction

PubMed Central

An, Rui; You, Lisha; Zhang, Yizhu; Wang, Xinhong; Ma, Yuemin

2014-01-01

Background: ‘Ge-Gen-Qin-Lian’ Decoction derived from ‘Shang-Han-Lun’ compiled by Zhang Zhongjing. It is widely used in the treatment of acute gastroenteritis, bacillary dysentery, virus diarrhea. This paper describes a sensitive and specific assay for the determination of the 11-marker compounds using ultra performance liquid chromatography (UPLC). Objective: To develop an UPLC method for simultaneous determination of 11 bioactive compounds in ‘Ge-Gen-Qin-Lian’ preparations. Materials and Methods: The chromatography analysis was performed on an Agilent Proshell 120 EC-C18 column (4.6 × 50 mm, 2.7 μm) at 30°C with a gradient elution of methanol, 0.5% formic acid and 0.5% ammonium acetate at a flow rate 1.0 ml/min and UV detected at 270 nm. Results: All calibration curves showed good linear regression (r ≥ 0.9993) within tested ranges. Limits of detection (LOD) and limits of quantification (LOQ) fell in the range between 0.0691-1.04 μg/ml and 0.23–3.43 μg/ml, respectively. The mean recovery of each herbal medicine ranged from 96.60 to 102.11%. Conclusion: The method was validated for repeatability, precision, stability, accuracy, and selectivity. The validated method was successfully applied to simultaneous analysis of these active components in ‘Ge-Gen-Qin-Lian’ decoction. PMID:25422547

Magnetic nano graphene oxide as solid phase extraction adsorbent coupled with liquid chromatography to determine pseudoephedrine in urine samples.

PubMed

Taghvimi, Arezou; Hamishehkar, Hamed; Ebrahimi, Mahmoud

2016-01-15

This paper reports on a method based on magnetic solid phase extraction (MSPE) for the determination of pseudoephedrine. Magnetic nanographene oxide (MNGO) was applied as a new adsorbent for the extraction of pseudoephedrine from urine samples. Synthesis of MNGO was characterized by Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), powder X-ray diffraction (XRD), and vibrating sample magnetometer (VSM). The main factors influencing extraction efficiency, including the amounts of sample volume, amount of adsorbent, type and amount of extraction organic solvent, time of extraction and desorption, pH, ionic strength of extraction medium, and agitation rate, were investigated and optimized. Under optimized extraction conditions, a good linearity was observed in the range of 100-2000ng/mL with a correlation coefficient of 0.9908 (r(2)). Limit of detection (LOD) and limit of quantification (LOQ) were 25 and 82.7ng/mL, respectively. Inter-day and intra-day precision and accuracy were 6.01 and 0.34 (%), and 8.70 and 0.29 (%), respectively. The method was applied for the determination of pseudoephedrine in urine samples of volunteers receiving pseudoephedrine with the recovery of 96.42. It was concluded that the proposed method can be applied in diagnostic clinics. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of Sodium, Potassium, Magnesium, and Calcium Minerals Level in Fresh and Boiled Broccoli and Cauliflower by Atomic Absorption Spectrometry

NASA Astrophysics Data System (ADS)

Nerdy

2018-01-01

Vegetables from the cabbage family vegetables consumed by many people, which is known healthful, by eaten raw, boiled, or cooked (stir fry or soup). Vegetables like broccoli and cauliflower contain vitamins, minerals, and fiber. This study aims to determine the decrease percentage of sodium, potassium, magnesium, and calcium minerals level caused by boiled broccoli and cauliflower by atomic absorption spectrometry. Boiled broccoli and cauliflower prepared by given boiled treatment in boiling water for 3 minutes. Fresh and boiled broccoli and cauliflower carried out dry destruction, followed by quantitative analysis of sodium, potassium, magnesium, and calcium minerals respectively at a wavelength of 589.0 nm; 766.5 nm; 285.2 nm; and 422.7 nm, using atomic absorption spectrometry methods. After the determination of the sodium, potassium, magnesium, and calcium minerals level followed by validation of analytical methods with accuracy, precision, linearity, range, limit of detection (LOD), and limit of quantitation (LOQ) parameters. Research results show a decrease in the sodium, potassium, magnesium, and calcium minerals level in boiled broccoli and cauliflower compared with fresh broccoli and cauliflower. Validation of analytical methods gives results that spectrometry methods used for determining sodium, potassium, magnesium, and calcium minerals level are valid. It concluded that the boiled gives the effect of decreasing the minerals level significantly in broccoli and cauliflower.

RP-HPLC ANALYSIS OF ACIDIC AND BASIC DRUGS IN SYSTEMS WITH DIETHYLAMINE AS ELUENTS ADDITIVE.

PubMed

Petruczynik, Anna; Wroblewski, Karol; Strozek, Szymon; Waksmundzka-Hajnos, Monika

2016-11-01

The chromatographic behavior of some basic and acidic drugs was studied on Cl 8, Phenyl-Hexyl and Polar RP columns with methanol or acetonitrile as organic modifiers of aqueous mobile phases containing addition of diethylamine. Diethylamine plays a double function of silanol blocker reagent in analysis of basic drugs and ion-pair reagent in analysis of acidic drugs. Most symmetrical peaks and highest system efficiency were obtained on Phenyl-Hexyl and Polar RP columns in tested mobile phase systems compared to results obtained on C18 column. A new rapid, simple, specific and accurate reverse phase liquid chromatographic method was developed for the simultaneous determination of atorvastatin - antihyperlipidemic drug and amlodipine - calcium channel blocker in one pharmaceutical formulation. Atorvastatin is an acidic compounds while amlodipine is a basic substance. The chromatographic separation was carried out on Phenyl-Hexyl column by gradient elution mode with acetonitrile as organic modifier, acetate buffer at pH 3.5 and Q.025 M/L diethylamine. The proposed method was validated for specificity, precision, accuracy, linearity, and robustness. The linearity range of atorvastatin and amlodipine for 5 - 100 μg/mL was obtained with limits of-detection (LOD) 3.2750 gg/mL and 3.2102 μg/mL, respectively. The proposed method made use of DAD as a tool for peak identity and purity confirmation.

Spectrophotometric Determination of Rifampicin in Bulk Drug and Pharmaceutical Formulations Based on Redox and Complexation Reactions

NASA Astrophysics Data System (ADS)

Swamy, N.; Basavaiah, K.

2017-09-01

Two spectrophotometric methods were developed and validated for the determination of rifampicin (RIF) in bulk form, formulations, and spiked human urine. The first method is based on the reduction of the Folin-Ciocalteu (FC) reagent by RIF to form a blue colored chromogen with λmax at 760 nm (the FCR method). In the second method, iron(III) is reduced by RIF in a neutral medium, and the resulting iron(II) is complexed with ferricyanide to form a Prussian blue peaking at 750 nm (the FFC method). Under optimum conditions, Beer's law enabled the determination of the drug in the concentration ranges 1-35 and 2.5-50 μg/mL with apparent molar absorptivities of 2.72 × 104 and 1.63×104 L/(mol × cm) for the FCR and FFC methods, respectively. The Sandell sensitivity, limits of detection (LOD), and quantification (LOQ) values were also reported for both methods. The precision of the methods, with % RSD of < 2%, was satisfactory, and the accuracy was higher than 2% (RE). The proposed methods were successfully applied to the determination of drug in capsules without interference from common additives and spiked human urine without interference from endogenous substances. A statistical analysis indicated that there was no significant difference between the results obtained by the developed methods and the official method.

Development of a new HPLC method for the simultaneous determination of ticarcillin and clavulanic acid in pharmaceutical formulations.

PubMed

Tsou, Tai-Li; Lee, Chiu-Wey; Wang, Hsian-Jenn; Cheng, Ya-Chung; Liu, Yu-Tien; Chen, Su-Hwei

2009-01-01

A new HPLC method has been developed and validated for the simultaneous determination of ticarcillin (TIC) and clavulanic acid (CA) in pharmaceutical formulations. The HPLC separation was achieved on a beta-cyclodextrin column (Cyclobond I, 250 x 4.6 mm, 5 microm) with methanol-16 mM pH 6.0 ammonium acetate buffer (50 + 50, v/v) mobile phase at a flow rate of 0.8 mL/min. Detection was at 220 nm. Validation of the method was performed by evaluating specificity, robustness, accuracy, and precision. The calibration curves were linear in the range of 1-100 microg/mL for CA and 2-200 microg/mL for TIC. The LOQs based on the standard regression lines were 0.42 and 1.42 microg/mL for CA and TIC, respectively, and the LOD were 0.14 and 0.47 microg/mL, respectively. Total recoveries of synthetic mixtures (CA:TIC = 1:10, 1:15, and 1:30) were 99.25-100.99% for CA and 99.54-100.82% for TIC. Compared with the U.S. Pharmacopeia method, the proposed method has the advantage of a relatively low flow rate and short analysis time. The proposed method was successfully applied for the simultaneous determination of these two drugs in sterilized H20 and 5% dextrose injection solutions.

HPLC/ELSD analysis of amidated bile acids: an effective and rapid way to assist continuous flow chemistry processes.

PubMed

Sardella, Roccaldo; Gioiello, Antimo; Ianni, Federica; Venturoni, Francesco; Natalini, Benedetto

2012-10-15

The employment of the flow N-acyl amidation of natural bile acids (BAs) required the in-line connection with suitable analytical tools enabling the determination of reaction yields as well as of the purity grade of the synthesized glyco- and tauro-conjugated derivatives. In this framework, a unique HPLC method was successfully established and validated for ursodeoxycholic (UDCA), chenodeoxycholic (CDCA), deoxycholic (DCA) and cholic (CA) acids, as well as the corresponding glyco- and tauro-conjugated forms. Because of the shared absence of relevant chromophoric moieties in the sample structure, an evaporative light scattering detector (ELSD) was profitably utilized for the analysis of such steroidal species. For each of the investigated compounds, all the runs were contemporarily carried out on the acidic free and the two relative conjugated variants. The different ELSD response of the free and the corresponding conjugated BAs, imposed to build-up separate calibration curves. In all the cases, very good precision (RSD% values ranging from 1.04 to 6.40% in the long-period) and accuracy (Recovery% values ranging from 96.03 to 111.14% in the long-period) values along with appreciably low LOD and LOQ values (the former being within the range 1-27 ng mL(-1) and the latter within the range 2-44 ng mL(-1)) turned out. Copyright © 2012 Elsevier B.V. All rights reserved.

A stability indicating HPLC method for determination of mebeverine in the presence of its degradation products and kinetic study of its degradation in oxidative condition

PubMed Central

Souri, E.; Aghdami, A. Negahban; Adib, N.

2014-01-01

An HPLC method for determination of mebeverine hydrochloride (MH) in the presence of its degradation products was developed. The degradation of MH was studied under hydrolysis, oxidative and photolysis stress conditions. Under alkaline, acidic and oxidative conditions, degradation of MH was observed. The separation was performed using a Symmetry C18 column and a mixture of 50 mM KH2PO4, acetonitrile and tetrahydrfuran (THF) (63:35:2; v/v/v) as the mobile phase. No interference peaks from degradation products in acidic, alkaline and oxidative conditions were observed. The linearity, accuracy and precision of the method were studied. The method was linear over the range of 1-100 μg/ml MH (r2>0.999) and the CV values for intra-day and inter-day variations were in the range of 1.0-1.8%. The limit of quantification (LOQ) and the limit of detection (LOD) of the method were 1.0 and 0.2 μg/ml, respectively. Determination of MH in pharmaceutical dosage forms was performed using the developed method. Furthermore the kinetics of the degradation of MH in the presence of hydrogen peroxide was investigated. The proposed method could be a suitable method for routine quality control studies of mebeverine dosage forms. PMID:25657790

A stability indicating HPLC method for determination of mebeverine in the presence of its degradation products and kinetic study of its degradation in oxidative condition.

PubMed

Souri, E; Aghdami, A Negahban; Adib, N

2014-01-01

An HPLC method for determination of mebeverine hydrochloride (MH) in the presence of its degradation products was developed. The degradation of MH was studied under hydrolysis, oxidative and photolysis stress conditions. Under alkaline, acidic and oxidative conditions, degradation of MH was observed. The separation was performed using a Symmetry C18 column and a mixture of 50 mM KH2PO4, acetonitrile and tetrahydrfuran (THF) (63:35:2; v/v/v) as the mobile phase. No interference peaks from degradation products in acidic, alkaline and oxidative conditions were observed. The linearity, accuracy and precision of the method were studied. The method was linear over the range of 1-100 μg/ml MH (r(2)>0.999) and the CV values for intra-day and inter-day variations were in the range of 1.0-1.8%. The limit of quantification (LOQ) and the limit of detection (LOD) of the method were 1.0 and 0.2 μg/ml, respectively. Determination of MH in pharmaceutical dosage forms was performed using the developed method. Furthermore the kinetics of the degradation of MH in the presence of hydrogen peroxide was investigated. The proposed method could be a suitable method for routine quality control studies of mebeverine dosage forms.

Earthquake triggering, Earth's rotation variations, Meton's cycle and torques acting on the Earth.

NASA Astrophysics Data System (ADS)

Ostrihansky, L.

2012-04-01

In contrast to unsuccessful searching (lasting over 150 years) of correlation of earthquakes with biweekly tides the author found correlation of earthquakes with sidereal 13.66 days Earth's rotation variations expressed as the length of a day (LOD) measured daily by the International Earth's Rotation Service. After short mention about earthquakes Denali Fault Alaska 3rd November 2002, M 7.9, triggered on LOD maximum and Great Sumatra earthquake 26th December 2004 triggered on LOD minimum and the full Moon, the main object of this paper are earthquakes of period 2010-VI. 2011: Haiti M 7.0 Jan. 12, 2010 on LOD minimum, Maule Chile M 8.8 Feb. 12, 2010 on LOD maximum, Sumatra and Andaman Sea region 6 earthquakes revealed from 7 on LOD minimum, New Zealand, Christchurch M 7.1 Sep. 9, 2010 on LOD minimum and Christchurch M 6.3 Feb. 21, 2011 on LOD maximum and Japan Near coast of Honshu M 9.1 March 11, 2011 on LOD minimum. I found that LOD minimums coincide with full or new Moon only twice in a year in solstices and also twice in the year with LOD maximums in equinoxes. To prove that determined coincidences of earthquakes and LOD extremes stated above are not accidental events, histograms were constructed of earthquake occurrence and their position on LOD graph deeply in the past, in some cases from the time the IERS started to measure the Earth's rotation variations in 1962. Evaluation of histograms and the Schuster's test has proven that maxima of earthquakes are triggered always in both Earth's rotation deceleration and acceleration. Backward overview of the past earthquakes revealed that the Great Sumatra earthquake Dec. 26, 2004 had its equivalent in the shape of LOD graph, full Moon position, character of aftershocks, 19 years ago in difference only one day of Dec. 27, 1985 M 6.6, proving that not only sidereal 13.66 days variations but also the 19 years Meton's cycle is the period of the earthquakes occurrence.

Precision and accuracy of luminescence lifetime-based phosphor thermometry: A case study of Eu(III):YSZ

NASA Astrophysics Data System (ADS)

Heeg, B.; Jenkins, T. P.

2013-09-01

Laser induced phosphor thermometry as a reliable technique requires an analysis of factors controlling or contributing to the precision and accuracy of a measurement. In this paper, we discuss several critical design parameters in the development of luminescence lifetime-based phosphor thermometry instrumentation for use at elevated temperatures such as encountered in hot sections of gas turbine engines. As precision is predominantly governed by signal and background photon shot noise and detector noise, a brief summary is presented of how these noise contributions may affect the measurement. Accuracy, on the other hand, is governed by a range of effects including, but not limited to, detector response characteristics, laser-induced effects, the photo-physics of the sensor materials, and also the method of data reduction. The various possible outcomes of measurement precision and accuracy are discussed with luminescence lifetime measurements on Eu(III):YSZ sensor coatings.

Validation of a method to detect cocaine and its metabolites in nails by gas chromatography-mass spectrometry.

PubMed

Valente-Campos, Simone; Yonamine, Mauricio; de Moraes Moreau, Regina Lucia; Silva, Ovandir Alves

2006-06-02

The objective of the present work was to compare previously published methods and provide validation data to detect simultaneously cocaine (COC), benzoylecgonine (BE) and norcocaine (NCOC) in nail. Finger and toenail samples (5mg) were cut in very small pieces and submitted to an initial procedure for external decontamination. Methanol (3 ml) was used to release analytes from the matrix. A cleanup step was performed simultaneously by solid-phase extraction (SPE) and the residue was derivatized with pentafluoropropionic anhydride/pentafluoropropanol (PFPA/PFP). Gas chromatography-mass spectrometry (GC-MS) was used to detect the analytes in selected ion monitoring mode (SIM). Confidence parameters of validation of the method were: recovery, intra- and inter-assay precision, as well as limit of detection (LOD) of the analytes. The limits of detection were: 3.5 ng/mg for NCOC and 3.0 ng/mg for COC and BE. Good intra-assay precision was observed for all detected substances (coefficient of variation (CV)<11%). The inter-assay precision for norcocaine and benzoylecgonine were <4%. For intra- and inter-assay precision deuterated internal standards were used. Toenail and fingernail samples from eight declared cocaine users were submitted to the validated method.

Atmospheric and Oceanic Excitations to LOD Change on Quasi-biennial Time Scales

NASA Astrophysics Data System (ADS)

Ma, Li-Hua; Liao, De-Chun; Han, Yan-Ben

2006-12-01

We use wavelet transform to study the time series of the Earth's rotation rate (length-of-day, LOD), the axial components of atmospheric angular momentum (AAM) and oceanic angular momentum (OAM) in the period 1962--2005, and discuss the quasi-biennial oscillations (QBO) of LOD change. The results show that the QBO of LOD change varies remarkably in amplitude and phase. It was weak before 1978, then became much stronger and reached maximum values during the strong El Nino events in around 1983 and 1997. Results from analyzing the axial AAM indicate that the QBO signals in axial AAM are extremely consistent with the QBOs of LOD change. During 1963--2003, the QBO variance in the axial AAM can explain about 99.0% of that of the LOD, in other words, all QBO signals of LOD change are almost excited by the axial AAM, while the weak QBO signals of the axial OAM are quite different from those of the LOD and the axial AAM in both time-dependent characteristics and magnitudes. The combined effects of the axial AAM and OAM can explain about 99.1% of the variance of QBO in LOD change during this period.

An LOD with improved breakdown voltage in full-frame CCD devices

NASA Astrophysics Data System (ADS)

Banghart, Edmund K.; Stevens, Eric G.; Doan, Hung Q.; Shepherd, John P.; Meisenzahl, Eric J.

2005-02-01

In full-frame image sensors, lateral overflow drain (LOD) structures are typically formed along the vertical CCD shift registers to provide a means for preventing charge blooming in the imager pixels. In a conventional LOD structure, the n-type LOD implant is made through the thin gate dielectric stack in the device active area and adjacent to the thick field oxidation that isolates the vertical CCD columns of the imager. In this paper, a novel LOD structure is described in which the n-type LOD impurities are placed directly under the field oxidation and are, therefore, electrically isolated from the gate electrodes. By reducing the electrical fields that cause breakdown at the silicon surface, this new structure permits a larger amount of n-type impurities to be implanted for the purpose of increasing the LOD conductivity. As a consequence of the improved conductance, the LOD width can be significantly reduced, enabling the design of higher resolution imaging arrays without sacrificing charge capacity in the pixels. Numerical simulations with MEDICI of the LOD leakage current are presented that identify the breakdown mechanism, while three-dimensional solutions to Poisson's equation are used to determine the charge capacity as a function of pixel dimension.

[Assessment of precision and accuracy of digital surface photogrammetry with the DSP 400 system].

PubMed

Krimmel, M; Kluba, S; Dietz, K; Reinert, S

2005-03-01

The objective of the present study was to evaluate the precision and accuracy of facial anthropometric measurements obtained through digital 3-D surface photogrammetry with the DSP 400 system in comparison to traditional 2-D photogrammetry. Fifty plaster casts of cleft infants were imaged and 21 standard anthropometric measurements were obtained. For precision assessment the measurements were performed twice in a subsample. Accuracy was determined by comparison of direct measurements and indirect 2-D and 3-D image measurements. Precision of digital surface photogrammetry was almost as good as direct anthropometry and clearly better than 2-D photogrammetry. Measurements derived from 3-D images showed better congruence to direct measurements than from 2-D photos. Digital surface photogrammetry with the DSP 400 system is sufficiently precise and accurate for craniofacial anthropometric examinations.

Evaluation and selection of anatomic sites for magnetic resonance imaging-guided mild hyperthermia therapy: a healthy volunteer study.

PubMed

V V N Kothapalli, Satya; Altman, Michael B; Zhu, Lifei; Partanen, Ari; Cheng, Galen; Gach, H Michael; Straube, William; Zoberi, Imran; Hallahan, Dennis E; Chen, Hong

2018-01-04

Since mild hyperthermia therapy (MHT) requires maintaining the temperature within a narrow window (e.g. 40-43 °C) for an extended duration (up to 1 h), accurate and precise temperature measurements are essential for ensuring safe and effective treatment. This study evaluated the precision and accuracy of MR thermometry in healthy volunteers at different anatomical sites for long scan times. A proton resonance frequency shift method was used for MR thermometry. Eight volunteers were subjected to a 5-min scanning protocol, targeting chest wall, bladder wall, and leg muscles. Six volunteers were subjected to a 30-min scanning protocol and three volunteers were subjected to a 60-min scanning protocol, both targeting the leg muscles. The precision and accuracy of the MR thermometry were quantified. Both the mean precision and accuracy <1 °C were used as criteria for acceptable thermometry. Drift-corrected MR thermometry measurements based on 5-min scans of the chest wall, bladder wall, and leg muscles had accuracies of 1.41 ± 0.65, 1.86 ± 1.20, and 0.34 ± 0.44 °C, and precisions of 2.30 ± 1.21, 1.64 ± 0.56, and 0.48 ± 0.05 °C, respectively. Measurements based on 30-min scans of the leg muscles had accuracy and precision of 0.56 ± 0.05 °C and 0.42 ± 0.50 °C, respectively, while the 60-min scans had accuracy and precision of 0.49 ± 0.03 °C and 0.56 ± 0.05 °C, respectively. Respiration, cardiac, and digestive-related motion pose challenges to MR thermometry of the chest wall and bladder wall. The leg muscles had satisfactory temperature accuracy and precision per the chosen criteria. These results indicate that extremity locations may be preferable targets for MR-guided MHT using the existing MR thermometry technique.

The variants of an LOD of a 3D building model and their influence on spatial analyses

NASA Astrophysics Data System (ADS)

Biljecki, Filip; Ledoux, Hugo; Stoter, Jantien; Vosselman, George

2016-06-01

The level of detail (LOD) of a 3D city model indicates the model's grade and usability. However, there exist multiple valid variants of each LOD. As a consequence, the LOD concept is inconclusive as an instruction for the acquisition of 3D city models. For instance, the top surface of an LOD1 block model may be modelled at the eaves of a building or at its ridge height. Such variants, which we term geometric references, are often overlooked and are usually not documented in the metadata. Furthermore, the influence of a particular geometric reference on the performance of a spatial analysis is not known. In response to this research gap, we investigate a variety of LOD1 and LOD2 geometric references that are commonly employed, and perform numerical experiments to investigate their relative difference when used as input for different spatial analyses. We consider three use cases (estimation of the area of the building envelope, building volume, and shadows cast by buildings), and compute the deviations in a Monte Carlo simulation. The experiments, carried out with procedurally generated models, indicate that two 3D models representing the same building at the same LOD, but modelled according to different geometric references, may yield substantially different results when used in a spatial analysis. The outcome of our experiments also suggests that the geometric reference may have a bigger influence than the LOD, since an LOD1 with a specific geometric reference may yield a more accurate result than when using LOD2 models.

Accurate time delay technology in simulated test for high precision laser range finder

NASA Astrophysics Data System (ADS)

Chen, Zhibin; Xiao, Wenjian; Wang, Weiming; Xue, Mingxi

2015-10-01

With the continuous development of technology, the ranging accuracy of pulsed laser range finder (LRF) is higher and higher, so the maintenance demand of LRF is also rising. According to the dominant ideology of "time analog spatial distance" in simulated test for pulsed range finder, the key of distance simulation precision lies in the adjustable time delay. By analyzing and comparing the advantages and disadvantages of fiber and circuit delay, a method was proposed to improve the accuracy of the circuit delay without increasing the count frequency of the circuit. A high precision controllable delay circuit was designed by combining the internal delay circuit and external delay circuit which could compensate the delay error in real time. And then the circuit delay accuracy could be increased. The accuracy of the novel circuit delay methods proposed in this paper was actually measured by a high sampling rate oscilloscope actual measurement. The measurement result shows that the accuracy of the distance simulated by the circuit delay is increased from +/- 0.75m up to +/- 0.15m. The accuracy of the simulated distance is greatly improved in simulated test for high precision pulsed range finder.

Isotope ratios of trace elements in samples from human nutrition studies determined by TIMS and ICP-MS: precision and accuracy compared.

PubMed

Turnlund, Judith R; Keyes, William R

2002-09-01

Stable isotopes are used with increasing frequency to trace the metabolic fate of minerals in human nutrition studies. The precision of the analytical methods used must be sufficient to permit reliable measurement of low enrichments and the accuracy should permit comparisons between studies. Two methods most frequently used today are thermal ionization mass spectrometry (TIMS) and inductively coupled plasma mass spectrometry (ICP-MS). This study was conducted to compare the two methods. Multiple natural samples of copper, zinc, molybdenum, and magnesium were analyzed by both methods to compare their internal and external precision. Samples with a range of isotopic enrichments that were collected from human studies or prepared from standards were analyzed to compare their accuracy. TIMS was more precise and accurate than ICP-MS. However, the cost, ease, and speed of analysis were better for ICP-MS. Therefore, for most purposes, ICP-MS is the method of choice, but when the highest degrees of precision and accuracy are required and when enrichments are very low, TIMS is the method of choice.

Presentation accuracy of the web revisited: animation methods in the HTML5 era.

PubMed

Garaizar, Pablo; Vadillo, Miguel A; López-de-Ipiña, Diego

2014-01-01

Using the Web to run behavioural and social experiments quickly and efficiently has become increasingly popular in recent years, but there is some controversy about the suitability of using the Web for these objectives. Several studies have analysed the accuracy and precision of different web technologies in order to determine their limitations. This paper updates the extant evidence about presentation accuracy and precision of the Web and extends the study of the accuracy and precision in the presentation of multimedia stimuli to HTML5-based solutions, which were previously untested. The accuracy and precision in the presentation of visual content in classic web technologies is acceptable for use in online experiments, although some results suggest that these technologies should be used with caution in certain circumstances. Declarative animations based on CSS are the best alternative when animation intervals are above 50 milliseconds. The performance of procedural web technologies based on the HTML5 standard is similar to that of previous web technologies. These technologies are being progressively adopted by the scientific community and have promising futures, which makes their use advisable to utilizing more obsolete technologies.

Precision, accuracy, and efficiency of four tools for measuring soil bulk density or strength.

Treesearch

Richard E. Miller; John Hazard; Steven Howes

2001-01-01

Monitoring soil compaction is time consuming. A desire for speed and lower costs, however, must be balanced with the appropriate precision and accuracy required of the monitoring task. We compared three core samplers and a cone penetrometer for measuring soil compaction after clearcut harvest on a stone-free and a stony soil. Precision (i.e., consistency) of each tool...

Hardware accuracy counters for application precision and quality feedback

DOE Office of Scientific and Technical Information (OSTI.GOV)

de Paula Rosa Piga, Leonardo; Majumdar, Abhinandan; Paul, Indrani

Methods, devices, and systems for capturing an accuracy of an instruction executing on a processor. An instruction may be executed on the processor, and the accuracy of the instruction may be captured using a hardware counter circuit. The accuracy of the instruction may be captured by analyzing bits of at least one value of the instruction to determine a minimum or maximum precision datatype for representing the field, and determining whether to adjust a value of the hardware counter circuit accordingly. The representation may be output to a debugger or logfile for use by a developer, or may be outputmore » to a runtime or virtual machine to automatically adjust instruction precision or gating of portions of the processor datapath.« less

Distribution and magnitude of type I error of model-based multipoint lod scores: implications for multipoint mod scores.

PubMed

Xing, Chao; Elston, Robert C

2006-07-01

The multipoint lod score and mod score methods have been advocated for their superior power in detecting linkage. However, little has been done to determine the distribution of multipoint lod scores or to examine the properties of mod scores. In this paper we study the distribution of multipoint lod scores both analytically and by simulation. We also study by simulation the distribution of maximum multipoint lod scores when maximized over different penetrance models. The multipoint lod score is approximately normally distributed with mean and variance that depend on marker informativity, marker density, specified genetic model, number of pedigrees, pedigree structure, and pattern of affection status. When the multipoint lod scores are maximized over a set of assumed penetrances models, an excess of false positive indications of linkage appear under dominant analysis models with low penetrances and under recessive analysis models with high penetrances. Therefore, caution should be taken in interpreting results when employing multipoint lod score and mod score approaches, in particular when inferring the level of linkage significance and the mode of inheritance of a trait.

Bullet trajectory reconstruction - Methods, accuracy and precision.

PubMed

Mattijssen, Erwin J A T; Kerkhoff, Wim

2016-05-01

Based on the spatial relation between a primary and secondary bullet defect or on the shape and dimensions of the primary bullet defect, a bullet's trajectory prior to impact can be estimated for a shooting scene reconstruction. The accuracy and precision of the estimated trajectories will vary depending on variables such as, the applied method of reconstruction, the (true) angle of incidence, the properties of the target material and the properties of the bullet upon impact. This study focused on the accuracy and precision of estimated bullet trajectories when different variants of the probing method, ellipse method, and lead-in method are applied on bullet defects resulting from shots at various angles of incidence on drywall, MDF and sheet metal. The results show that in most situations the best performance (accuracy and precision) is seen when the probing method is applied. Only for the lowest angles of incidence the performance was better when either the ellipse or lead-in method was applied. The data provided in this paper can be used to select the appropriate method(s) for reconstruction and to correct for systematic errors (accuracy) and to provide a value of the precision, by means of a confidence interval of the specific measurement. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

Application of high-precision two-way ranging to Galileo Earth-1 encounter navigation

NASA Technical Reports Server (NTRS)

Pollmeier, V. M.; Thurman, S. W.

1992-01-01

The application of precision two-way ranging to orbit determination with relatively short data arcs is investigated for the Galileo spacecraft's approach to its first Earth encounter (December 8, 1990). Analysis of previous S-band (2.3-GHz) ranging data acquired from Galileo indicated that under good signal conditions submeter precision and 10-m ranging accuracy were achieved. It is shown that ranging data of sufficient accuracy, when acquired from multiple stations, can sense the geocentric angular position of a distant spacecraft. A range data filtering technique, in which explicit modeling of range measurement bias parameters for each station pass is utilized, is shown to largely remove the systematic ground system calibration errors and transmission media effects from the Galileo range measurements, which would otherwise corrupt the angle-finding capabilities of the data. The accuracy of the Galileo orbit solutions obtained with S-band Doppler and precision ranging were found to be consistent with simple theoretical calculations, which predicted that angular accuracies of 0.26-0.34 microrad were achievable. In addition, the navigation accuracy achieved with precision ranging was marginally better than that obtained using delta-differenced one-way range (delta DOR), the principal data type that was previously used to obtain spacecraft angular position measurements operationally.

Study on high-precision measurement of long radius of curvature

NASA Astrophysics Data System (ADS)

Wu, Dongcheng; Peng, Shijun; Gao, Songtao

2016-09-01

It is hard to get high-precision measurement of the radius of curvature (ROC), because of many factors that affect the measurement accuracy. For the measurement of long radius of curvature, some factors take more important position than others'. So, at first this paper makes some research about which factor is related to the long measurement distance, and also analyse the uncertain of the measurement accuracy. At second this article also study the influence about the support status and the adjust error about the cat's eye and confocal position. At last, a 1055micrometer radius of curvature convex is measured in high-precision laboratory. Experimental results show that the proper steady support (three-point support) can guarantee the high-precision measurement of radius of curvature. Through calibrating the gain of cat's eye and confocal position, is useful to ensure the precise position in order to increase the measurement accuracy. After finish all the above process, the high-precision long ROC measurement is realized.

Determination of cocaine, benzoylecgonine and cocaethylene in human hair by solid-phase microextraction and gas chromatography-mass spectrometry.

PubMed

de Toledo, Fernanda Crossi Pereira; Yonamine, Mauricio; de Moraes Moreau, Regina Lucia; Silva, Ovandir Alves

2003-12-25

The present work describes a highly precise and sensitive method developed to detect cocaine (COC), benzoylecgonine (BE, its main metabolite) and cocaethylene (CE, transesterification product of the coingestion of COC with ethanol) in human head hair samples. The method was based on an alkylchloroformate derivatization of benzoylecgonine and the extraction of the analytes by solid-phase microextraction (SPME). Gas chromatography-mass spectrometry (GC-MS) was used to identify and quantify the analytes in selected ion monitoring mode (SIM). The limits of quantification and detection (LOQ and LOD) were: 0.1 ng/mg for COC and CE, and 0.5 ng/mg for BE. Good inter- and intra-assay precision was observed. The dynamic range of the assay was 0.1-50 ng/mg. The method is not time consuming and was shown to be easy to perform.

The power to detect linkage in complex disease by means of simple LOD-score analyses.

PubMed Central

Greenberg, D A; Abreu, P; Hodge, S E

1998-01-01

Maximum-likelihood analysis (via LOD score) provides the most powerful method for finding linkage when the mode of inheritance (MOI) is known. However, because one must assume an MOI, the application of LOD-score analysis to complex disease has been questioned. Although it is known that one can legitimately maximize the maximum LOD score with respect to genetic parameters, this approach raises three concerns: (1) multiple testing, (2) effect on power to detect linkage, and (3) adequacy of the approximate MOI for the true MOI. We evaluated the power of LOD scores to detect linkage when the true MOI was complex but a LOD score analysis assumed simple models. We simulated data from 14 different genetic models, including dominant and recessive at high (80%) and low (20%) penetrances, intermediate models, and several additive two-locus models. We calculated LOD scores by assuming two simple models, dominant and recessive, each with 50% penetrance, then took the higher of the two LOD scores as the raw test statistic and corrected for multiple tests. We call this test statistic "MMLS-C." We found that the ELODs for MMLS-C are >=80% of the ELOD under the true model when the ELOD for the true model is >=3. Similarly, the power to reach a given LOD score was usually >=80% that of the true model, when the power under the true model was >=60%. These results underscore that a critical factor in LOD-score analysis is the MOI at the linked locus, not that of the disease or trait per se. Thus, a limited set of simple genetic models in LOD-score analysis can work well in testing for linkage. PMID:9718328

The power to detect linkage in complex disease by means of simple LOD-score analyses.

PubMed

Greenberg, D A; Abreu, P; Hodge, S E

1998-09-01

Maximum-likelihood analysis (via LOD score) provides the most powerful method for finding linkage when the mode of inheritance (MOI) is known. However, because one must assume an MOI, the application of LOD-score analysis to complex disease has been questioned. Although it is known that one can legitimately maximize the maximum LOD score with respect to genetic parameters, this approach raises three concerns: (1) multiple testing, (2) effect on power to detect linkage, and (3) adequacy of the approximate MOI for the true MOI. We evaluated the power of LOD scores to detect linkage when the true MOI was complex but a LOD score analysis assumed simple models. We simulated data from 14 different genetic models, including dominant and recessive at high (80%) and low (20%) penetrances, intermediate models, and several additive two-locus models. We calculated LOD scores by assuming two simple models, dominant and recessive, each with 50% penetrance, then took the higher of the two LOD scores as the raw test statistic and corrected for multiple tests. We call this test statistic "MMLS-C." We found that the ELODs for MMLS-C are >=80% of the ELOD under the true model when the ELOD for the true model is >=3. Similarly, the power to reach a given LOD score was usually >=80% that of the true model, when the power under the true model was >=60%. These results underscore that a critical factor in LOD-score analysis is the MOI at the linked locus, not that of the disease or trait per se. Thus, a limited set of simple genetic models in LOD-score analysis can work well in testing for linkage.

Opto-mechanical system design of test system for near-infrared and visible target

NASA Astrophysics Data System (ADS)

Wang, Chunyan; Zhu, Guodong; Wang, Yuchao

2014-12-01

Guidance precision is the key indexes of the guided weapon shooting. The factors of guidance precision including: information processing precision, control system accuracy, laser irradiation accuracy and so on. The laser irradiation precision is an important factor. This paper aimed at the demand of the precision test of laser irradiator，and developed the laser precision test system. The system consists of modified cassegrain system, the wide range CCD camera, tracking turntable and industrial PC, and makes visible light and near infrared target imaging at the same time with a Near IR camera. Through the analysis of the design results, when it exposures the target of 1000 meters that the system measurement precision is43mm, fully meet the needs of the laser precision test.

An Improved Method of AGM for High Precision Geolocation of SAR Images

NASA Astrophysics Data System (ADS)

Zhou, G.; He, C.; Yue, T.; Huang, W.; Huang, Y.; Li, X.; Chen, Y.

2018-05-01

In order to take full advantage of SAR images, it is necessary to obtain the high precision location of the image. During the geometric correction process of images, to ensure the accuracy of image geometric correction and extract the effective mapping information from the images, precise image geolocation is important. This paper presents an improved analytical geolocation method (IAGM) that determine the high precision geolocation of each pixel in a digital SAR image. This method is based on analytical geolocation method (AGM) proposed by X. K. Yuan aiming at realizing the solution of RD model. Tests will be conducted using RADARSAT-2 SAR image. Comparing the predicted feature geolocation with the position as determined by high precision orthophoto, results indicate an accuracy of 50m is attainable with this method. Error sources will be analyzed and some recommendations about improving image location accuracy in future spaceborne SAR's will be given.

Earth's rotation variations and earthquakes 2010-2011

NASA Astrophysics Data System (ADS)

Ostřihanský, L.

2012-01-01

In contrast to unsuccessful searching (lasting over 150 years) for correlation of earthquakes with biweekly tides, the author found correlation of earthquakes with sidereal 13.66 days Earth's rotation variations expressed as length of a day (LOD) measured daily by International Earth's Rotation Service. After short mention about earthquakes M 8.8 Denali Fault Alaska 3 November 2002 triggered on LOD maximum and M 9.1 Great Sumatra earthquake 26 December 2004 triggered on LOD minimum and the full Moon, the main object of this paper are earthquakes of period 2010-June 2011: M 7.0 Haiti (12 January 2010 on LOD minimum, M 8.8 Maule Chile 12 February 2010 on LOD maximum, map constructed on the Indian plate revealing 6 earthquakes from 7 on LOD minimum in Sumatra and Andaman Sea region, M 7.1 New Zealand Christchurch 9 September 2010 on LOD minimum and M 6.3 Christchurch 21 February 2011 on LOD maximum, and M 9.1 Japan near coast of Honshu 11 March 2011 on LOD minimum. It was found that LOD minimums coincide with full or new Moon only twice in a year in solstices. To prove that determined coincidences of earthquakes and LOD extremes stated above are not accidental events, histograms were constructed of earthquake occurrences and their position on LOD graph deeply in the past, in some cases from the time the IERS (International Earth's Rotation Service) started to measure the Earth's rotation variations in 1962. Evaluations of histograms and the Schuster's test have proven that majority of earthquakes are triggered in both Earth's rotation deceleration and acceleration. Because during these coincidences evident movements of lithosphere occur, among others measured by GPS, it is concluded that Earth's rotation variations effectively contribute to the lithospheric plates movement. Retrospective overview of past earthquakes revealed that the Great Sumatra earthquake 26 December 2004 had its equivalent in the shape of LOD graph, full Moon position, and character of aftershocks 19 years earlier in difference only one day to 27 December 1985 earthquake, proving that not only sidereal 13.66 days variations but also that the 19 years Metons cycle is the period of the earthquakes occurrence. Histograms show the regular change of earthquake positions on branches of LOD graph and also the shape of histogram and number of earthquakes on LOD branches from the mid-ocean ridge can show which side of the ridge moves quicker.

Laser-induced breakdown spectroscopic detection of trace level heavy metal in solutions on a laser-pretreated metallic target.

PubMed

Niu, Sheng; Zheng, Lijuan; Khan, Abdul Qayyum; Feng, Guang; Zeng, Heping

2018-03-01

A fast and sensitive analysis for trace level heavy metals in aqueous solution was realized by using an improved laser induced breakdown spectroscopy (LIBS) methodology. Solutions containing heavy metal elements, Ni, Cr, and Cd, were concentrated in a laser-pretreated area (25 × 20mm 2 ) of a polished aluminum target surface, wherein pretreated grooves enabled homogeneous distribution of the metallic solutions in the well-defined area, and laser ablation of the aluminum target produced unique plasma excitation of various metallic ions. For 1-mL solutions deposited, we obtained an analytical precision of about 7% relative standard deviation (RSD), and limits of detection (LODs) of 22, 19, and 184μg/L for Ni, Cr, and Cd, respectively. Moreover, the laser-pretreated metallic microstructure allowed more solution deposited with the help of a hot plate, which supported improvement of LODs to sub-μg/L level for Cr and Ni and μg/L level for Cd with about 20-mL solution engaged in the enrichment processes. The applicability of the proposed methodology was validated on certified reference materials and real river water. Copyright © 2017 Elsevier B.V. All rights reserved.

Precision and accuracy of suggested maxillary and mandibular landmarks with cone-beam computed tomography for regional superimpositions: An in vitro study.

PubMed

Lemieux, Genevieve; Carey, Jason P; Flores-Mir, Carlos; Secanell, Marc; Hart, Adam; Lagravère, Manuel O

2016-01-01

Our objective was to identify and evaluate the accuracy and precision (intrarater and interrater reliabilities) of various anatomic landmarks for use in 3-dimensional maxillary and mandibular regional superimpositions. We used cone-beam computed tomography reconstructions of 10 human dried skulls to locate 10 landmarks in the maxilla and the mandible. Precision and accuracy were assessed with intrarater and interrater readings. Three examiners located these landmarks in the cone-beam computed tomography images 3 times with readings scheduled at 1-week intervals. Three-dimensional coordinates were determined (x, y, and z coordinates), and the intraclass correlation coefficient was computed to determine intrarater and interrater reliabilities, as well as the mean error difference and confidence intervals for each measurement. Bilateral mental foramina, bilateral infraorbital foramina, anterior nasal spine, incisive canal, and nasion showed the highest precision and accuracy in both intrarater and interrater reliabilities. Subspinale and bilateral lingulae had the lowest precision and accuracy in both intrarater and interrater reliabilities. When choosing the most accurate and precise landmarks for 3-dimensional cephalometric analysis or plane-derived maxillary and mandibular superimpositions, bilateral mental and infraorbital foramina, landmarks in the anterior region of the maxilla, and nasion appeared to be the best options of the analyzed landmarks. Caution is needed when using subspinale and bilateral lingulae because of their higher mean errors in location. Copyright © 2016 American Association of Orthodontists. Published by Elsevier Inc. All rights reserved.

The research of selection model based on LOD in multi-scale display of electronic map

NASA Astrophysics Data System (ADS)

Zhang, Jinming; You, Xiong; Liu, Yingzhen

2008-10-01

This paper proposes a selection model based on LOD to aid the display of electronic map. The ratio of display scale to map scale is regarded as a LOD operator. The categorization rule, classification rule, elementary rule and spatial geometry character rule of LOD operator setting are also concluded.

Comparing conventional and computer-assisted surgery baseplate and screw placement in reverse shoulder arthroplasty.

PubMed

Venne, Gabriel; Rasquinha, Brian J; Pichora, David; Ellis, Randy E; Bicknell, Ryan

2015-07-01

Preoperative planning and intraoperative navigation technologies have each been shown separately to be beneficial for optimizing screw and baseplate positioning in reverse shoulder arthroplasty (RSA) but to date have not been combined. This study describes development of a system for performing computer-assisted RSA glenoid baseplate and screw placement, including preoperative planning, intraoperative navigation, and postoperative evaluation, and compares this system with a conventional approach. We used a custom-designed system allowing computed tomography (CT)-based preoperative planning, intraoperative navigation, and postoperative evaluation. Five orthopedic surgeons defined common preoperative plans on 3-dimensional CT reconstructed cadaveric shoulders. Each surgeon performed 3 computer-assisted and 3 conventional simulated procedures. The 3-dimensional CT reconstructed postoperative units were digitally matched to the preoperative model for evaluation of entry points, end points, and angulations of screws and baseplate. Values were used to find accuracy and precision of the 2 groups with respect to the defined placement. Statistical analysis was performed by t tests (α = .05). Comparison of the groups revealed no difference in accuracy or precision of screws or baseplate entry points (P > .05). Accuracy and precision were improved with use of navigation for end points and angulations of 3 screws (P < .05). Accuracy of the inferior screw showed a trend of improvement with navigation (P > .05). Navigated baseplate end point precision was improved (P < .05), with a trend toward improved accuracy (P > .05). We conclude that CT-based preoperative planning and intraoperative navigation allow improved accuracy and precision for screw placement and precision for baseplate positioning with respect to a predefined placement compared with conventional techniques in RSA. Copyright © 2015 Journal of Shoulder and Elbow Surgery Board of Trustees. Published by Elsevier Inc. All rights reserved.

Simultaneous Determination of Eight Bioactive Compounds in Dianthus superbus by High-performance Liquid Chromatography

PubMed Central

Yun, Bo-Ra; Yang, Hye Jin; Weon, Jin Bae; Lee, Jiwoo; Eom, Min Rye; Ma, Choong Je

2016-01-01

Background: Dianthus superbus, one of traditional herbal medicine, is widely used to treat urethritis, carbuncles and carcinoma. Objective: A simultaneous determination method was established for controlling the quality of D. superbus using the eight compounds, (E)-methyl-4-hydroxy-4-(8a-methyl-3-oxodecahydronaphthalen-4a-yl) (1), diosmetin-7-O(2'',6''-di-O-α-L-rhamnopyranosyl)-β-D-glucopyranoside (2), vanillic acid (3), 4-hydroxyphenyl acetic acid (4), 4-methoxyphenyl acetic acid (5), (E)-4-methoxycinnamic acid (6), 3-methoxy-4-hydroxyphenylethanol (7), and methyl hydroferulate (8) isolated from D. superbus. Materials and Methods: This analysis method was developed using high performance liquid chromatography coupled with diode array detector with a Shishedo C18 column at a column temperature of 3°C. The mobile phase was composed of 0.1% trifluoroacetic acid in water and acetonitrile. The flow rate was 1 ml/min and detection wavelength was set at 205 nm and 280 nm. Validation was performed in order to demonstrate selectivity, accuracy and precision of the method. Results: The calibration curves showed good linearity (R2 > 0.99). The limits of detection and limits of quantification were within the ranges 0.0159–0.6205 μg/ml and 0.3210–1.8802 μg/ml, respectively. Moreover, the relative standard deviations of intra- and inter-day precision were both <2.98%. The overall recoveries were in the range of 96.23–109.87%. Quantitative analysis of eight compounds in 12 D. superbus samples (D-1–D-12) from various regions were analyzed and compared by developed method. Conclusion: As a result, this established method was accurate and sensitive for the quality evaluation of eight compounds isolated from D. superbus and may provide a new basis for quality control of D. superbus. SUMMARY A simultaneous determination method of eight compounds in Dianthus superbus was established by high performance liquid chromatography-diode array detectorDeveloped analysis method is validated with linearity, precious and accuracyThe newly established method was successfully evaluated contents of eight compounds in 12 D. superbus samples (D.1.D.12) from various regions and compared. Abbreviations used: HPLC: High performance liquid chromatography, LOD: Limits of detection, LOQ: Limits of quantification, RSD: Relative standard deviation. PMID:27279718

Simultaneous Determination of Eight Bioactive Compounds in Dianthus superbus by High-performance Liquid Chromatography.

PubMed

Yun, Bo-Ra; Yang, Hye Jin; Weon, Jin Bae; Lee, Jiwoo; Eom, Min Rye; Ma, Choong Je

2016-05-01

Dianthus superbus, one of traditional herbal medicine, is widely used to treat urethritis, carbuncles and carcinoma. A simultaneous determination method was established for controlling the quality of D. superbus using the eight compounds, (E)-methyl-4-hydroxy-4-(8a-methyl-3-oxodecahydronaphthalen-4a-yl) (1), diosmetin-7-O(2'',6''-di-O-α-L-rhamnopyranosyl)-β-D-glucopyranoside (2), vanillic acid (3), 4-hydroxyphenyl acetic acid (4), 4-methoxyphenyl acetic acid (5), (E)-4-methoxycinnamic acid (6), 3-methoxy-4-hydroxyphenylethanol (7), and methyl hydroferulate (8) isolated from D. superbus. This analysis method was developed using high performance liquid chromatography coupled with diode array detector with a Shishedo C18 column at a column temperature of 3°C. The mobile phase was composed of 0.1% trifluoroacetic acid in water and acetonitrile. The flow rate was 1 ml/min and detection wavelength was set at 205 nm and 280 nm. Validation was performed in order to demonstrate selectivity, accuracy and precision of the method. The calibration curves showed good linearity (R (2) > 0.99). The limits of detection and limits of quantification were within the ranges 0.0159-0.6205 μg/ml and 0.3210-1.8802 μg/ml, respectively. Moreover, the relative standard deviations of intra- and inter-day precision were both <2.98%. The overall recoveries were in the range of 96.23-109.87%. Quantitative analysis of eight compounds in 12 D. superbus samples (D-1-D-12) from various regions were analyzed and compared by developed method. As a result, this established method was accurate and sensitive for the quality evaluation of eight compounds isolated from D. superbus and may provide a new basis for quality control of D. superbus. A simultaneous determination method of eight compounds in Dianthus superbus was established by high performance liquid chromatography-diode array detectorDeveloped analysis method is validated with linearity, precious and accuracyThe newly established method was successfully evaluated contents of eight compounds in 12 D. superbus samples (D.1.D.12) from various regions and compared. Abbreviations used: HPLC: High performance liquid chromatography, LOD: Limits of detection, LOQ: Limits of quantification, RSD: Relative standard deviation.

[Pharmacokinetics and relative bioavailability of THC and THC-solid dispersion orally to mice at single dose].

PubMed

Liao, Li; Hua, Hua; Zhao, Jun-Ning; Luo, Heng; Yang, An-Dong

2014-03-01

To establish a fast sensitive, reproducible LC-MS/MS method to study pharmacokinetic properties of THC, and compare relative bioavailability of THC and its solid dispersion in mice. 200 mice were divided randomly into two groups, and administered orally with THC and THC-solid dispersion after fasting (calculate on THC:400 mg x kg(-1)), used HPLC-MS/MS method to determine the THC concentration of each period at the following times: baseline ( predose ), 15, 30, 45 min, 1, 1.5, 2, 3, 4, 6, 24 h after dosing. Calculating the pharmacokinetic parameters according to the C-t curv, and then use the Phoenix WinNonlin software for data analysis. The calibration curves were linear over the range 9.06-972 microg x L(-1) for THC (R2 = 0.999). The limit of detection (LOD) was 0.7 microg x L(-1), respectively. The average extraction recoveries for THC was above 75%, The methodology recoveries were between 79% and 108%. The intra-day and inter-day RSD were less than 13%, the stability test showed that the plasma samples was stable under different conditions (RSD < 15%). The precision, accuracy, recovery and applicability were found to be adequate for pharmacokinetic studies. Pharmacokinetic parameters of THC and THC-solid dispersion orally to mice shows as fllows: T(max), were 60 and 15 min, AUC(0-t) were 44 500.43 and 57 497.81 mg x L(-1) x min, AUC(0-infinity) were 51 226.00 and 68 031.48 mg x L(-1) x min, MRT(0-infinity) were 596.915 6, 661.747 7 min, CL(z)/F were 0.007 809 and 0.005 88 L x min(-1) x kg(-1). Compared with THC, the MRT and t1/2 of the THC-solid dispersion were all slightly extended, the t(max) was significantly reduced, AUC(0-24 h), AUC(0-infinity) and C(max) were all significantly higher, the relative bioavailability of THC-solid dispersion is 1.34 times of THC. The results of the experiment shows that the precision, accuracy, recovery and applicability were found to be adequate for the pharmacokinetic studies. After oral administration to mice, the relative bioavailability of THC-solid dispersion show significant improvement compared to THC.

Validation and comparison of two NGS assays for the detection of EGFR T790M resistance mutation in liquid biopsies of NSCLC patients.

PubMed

Vollbrecht, Claudia; Lehmann, Annika; Lenze, Dido; Hummel, Michael

2018-04-06

Analysis of circulating cell-free DNA (cfDNA) derived from peripheral blood ("liquid biopsy") is an attractive alternative to identify non-small cell lung cancer (NSCLC) patients with the EGFR T790M mutation eligible for 3rd generation tyrosine kinase inhibitor therapy. We evaluated two PCR-based next generation sequencing (NGS) approaches, one including unique molecular identifiers (UMI), with focus on highly sensitive EGFR T790M mutation detection. Therefore, we extracted and sequenced cfDNA from synthetic plasma samples spiked with mutated DNA at decreasing allele frequencies and from 21 diagnostic NSCLC patients. Data evaluation was performed to determine the limit of detection (LoD), accuracy, specificity and sensitivity of both assays. Considering all tested reference dilutions and mutations the UMI assay performed best in terms of LoD (1% vs. 5%), sensitivity (95.8% vs. 81.3%), specificity (100% vs. 93.8%) and accuracy (96.9% vs. 84.4%). Comparing mutation status of diagnostic samples with both assays showed 81.3% concordance with primary mutation verifiable in 52% of cases. EGFR T790M was detected concordantly in 6/7 patients with allele frequencies from 0.1% to 27%. In one patient, the T790M mutation was exclusively detectable with the UMI assay. Our data demonstrate that both assays are applicable as multi-biomarker NGS tools enabling the simultaneous detection of primary EGFR driver and resistance mutations. However, for mutations with low allelic frequencies the use of NGS panels with UMI facilitates a more sensitive and reliable detection.

Validation and comparison of two NGS assays for the detection of EGFR T790M resistance mutation in liquid biopsies of NSCLC patients

PubMed Central

Vollbrecht, Claudia; Lehmann, Annika; Lenze, Dido; Hummel, Michael

2018-01-01

Analysis of circulating cell-free DNA (cfDNA) derived from peripheral blood (“liquid biopsy”) is an attractive alternative to identify non-small cell lung cancer (NSCLC) patients with the EGFR T790M mutation eligible for 3rd generation tyrosine kinase inhibitor therapy. We evaluated two PCR-based next generation sequencing (NGS) approaches, one including unique molecular identifiers (UMI), with focus on highly sensitive EGFR T790M mutation detection. Therefore, we extracted and sequenced cfDNA from synthetic plasma samples spiked with mutated DNA at decreasing allele frequencies and from 21 diagnostic NSCLC patients. Data evaluation was performed to determine the limit of detection (LoD), accuracy, specificity and sensitivity of both assays. Considering all tested reference dilutions and mutations the UMI assay performed best in terms of LoD (1% vs. 5%), sensitivity (95.8% vs. 81.3%), specificity (100% vs. 93.8%) and accuracy (96.9% vs. 84.4%). Comparing mutation status of diagnostic samples with both assays showed 81.3% concordance with primary mutation verifiable in 52% of cases. EGFR T790M was detected concordantly in 6/7 patients with allele frequencies from 0.1% to 27%. In one patient, the T790M mutation was exclusively detectable with the UMI assay. Our data demonstrate that both assays are applicable as multi-biomarker NGS tools enabling the simultaneous detection of primary EGFR driver and resistance mutations. However, for mutations with low allelic frequencies the use of NGS panels with UMI facilitates a more sensitive and reliable detection. PMID:29719623

Accuracy and Measurement Error of the Medial Clear Space of the Ankle.

PubMed

Metitiri, Ogheneochuko; Ghorbanhoseini, Mohammad; Zurakowski, David; Hochman, Mary G; Nazarian, Ara; Kwon, John Y

2017-04-01

Measurement of the medial clear space (MCS) is commonly used to assess deltoid ligament competency and mortise stability when managing ankle fractures. Lacking knowledge of the true anatomic width measured, previous studies have been unable to measure accuracy of measurement. The purpose of this study was to determine MCS measurement error and accuracy and any influencing factors. Using 3 normal transtibial ankle cadaver specimens, deltoid and syndesmotic ligaments were transected and the mortise widened and affixed at a width of 6 mm (specimen 1) and 4 mm (specimen 2). The mortise was left intact in specimen 3. Radiographs were obtained of each cadaver at varying degrees of rotation. Radiographs were randomized, and providers measured the MCS using a standardized technique. Lack of accuracy as well as lack of precision in measurement of the medial clear space compared to a known anatomic value was present for all 3 specimens tested. There were no significant differences in mean delta with regard to level of training for specimens 1 and 2; however, with specimen 3, staff physicians showed increased measurement accuracy compared with trainees. Accuracy and precision of MCS measurements are poor. Provider experience did not appear to influence accuracy and precision of measurements for the displaced mortise. This high degree of measurement error and lack of precision should be considered when deciding treatment options based on MCS measurements.

Variation of Static-PPP Positioning Accuracy Using GPS-Single Frequency Observations (Aswan, Egypt)

NASA Astrophysics Data System (ADS)

Farah, Ashraf

2017-06-01

Precise Point Positioning (PPP) is a technique used for position computation with a high accuracy using only one GNSS receiver. It depends on highly accurate satellite position and clock data rather than broadcast ephemeries. PPP precision varies based on positioning technique (static or kinematic), observations type (single or dual frequency) and the duration of collected observations. PPP-(dual frequency receivers) offers comparable accuracy to differential GPS. PPP-single frequency receivers has many applications such as infrastructure, hydrography and precision agriculture. PPP using low cost GPS single-frequency receivers is an area of great interest for millions of users in developing countries such as Egypt. This research presents a study for the variability of single frequency static GPS-PPP precision based on different observation durations.

Chimeric recombinant antibody fragments in cardiac troponin I immunoassay.

PubMed

Hyytiä, Heidi; Heikkilä, Taina; Brockmann, Eeva-Christine; Kekki, Henna; Hedberg, Pirjo; Puolakanaho, Tarja; Lövgren, Timo; Pettersson, Kim

2015-03-01

To introduce a novel nanoparticle-based immunoassay for cardiac troponin I (cTnI) utilizing chimeric antibody fragments and to demonstrate that removal of antibody Fc-part and antibody chimerization decrease matrix related interferences. A sandwich-type immunoassay for cTnI based on recombinant chimeric (mouse variable/human constant) antigen binding (cFab) antibodies and intrinsically fluorescent nanoparticles was developed. To test whether using chimeric antibody fragments helps to avoid matrix related interferences, samples (n=39) with known amounts of triglycerides, bilirubin, rheumatoid factor (RF) or human anti-mouse antibodies (HAMAs) were measured with the novel assay, along with a previously published nanoparticle-based research assay with the same antibody epitopes. The limit of detection (LoD) was 3.30ng/L. Within-laboratory precision for 29ng/L and 2819ng/L cTnI were 13.7% and 15.9%, respectively. Regression analysis with Siemens ADVIA Centaur® yielded a slope (95% confidence intervals) of 0.18 (0.17-1.19) and a y-intercept of 1.94 (-1.28-3.91) ng/L. When compared to a previously published nanoparticle-based assay, the novel assay showed substantially reduced interference in the tested interference prone samples, 15.4 vs. 51.3%. A rheumatoid factor containing sample was decreased from 241ng/L to

Molecularly imprinted polymers based stir bar sorptive extraction for determination of cefaclor and cefalexin in environmental water.

PubMed

Peng, Jun; Liu, Donghao; Shi, Tian; Tian, Huairu; Hui, Xuanhong; He, Hua

2017-07-01

Although stir bar sportive extraction was thought to be a highly efficiency and simple pretreatment approach, its wide application was limited by low selectivity, short service life, and relatively high cost. In order to improve the performance of the stir bar, molecular imprinted polymers and magnetic carbon nanotubes were combined in the present study. In addition, two monomers were utilized to intensify the selectivity of molecularly imprinted polymers. Fourier transform infrared spectroscopy, scanning electron microscopy, and selectivity experiments showed that the molecularly imprinted polymeric stir bar was successfully prepared. Then micro-extraction based on the obtained stir bar was coupled with HPLC for determination of trace cefaclor and cefalexin in environmental water. This approach had the advantages of stir bar sportive extraction, high selectivity of molecular imprinted polymers, and high sorption efficiency of carbon nanotubes. To utilize this pretreatment approach, pH, extraction time, stirring speed, elution solvent, and elution time were optimized. The LOD and LOQ of cefaclor were found to be 3.5 ng · mL -1 and 12.0 ng · mL -1 , respectively; the LOD and LOQ of cefalexin were found to be 3.0 ng · mL -1 and 10.0 ng · mL -1 , respectively. The recoveries of cefaclor and cefalexin were 86.5 ~ 98.6%. The within-run precision and between-run precision were acceptable (relative standard deviation <7%). Even when utilized in more than 14 cycles, the performance of the stir bar did not decrease dramatically. This demonstrated that the molecularly imprinted polymeric stir bar based micro-extraction was a convenient, efficient, low-cost, and a specific method for enrichment of cefaclor and cefalexin in environmental samples.

Clinical evaluation of Roche COBAS® AmpliPrep/COBAS® TaqMan® CMV Test using non-plasma samples.

PubMed

Hildenbrand, Cynthia; Wedekind, Laura; Li, Ge; vonRentzell, Jeanne E; Shah, Krunal; Rooney, Paul; Harrington, Amanda T; Zhao, Richard Y

2018-05-24

Cytomegalovirus (CMV) infection is a leading cause of loss of hearing, vision, and mental retardation in congenitally infected children. It is also associated with complications of organ-transplant and opportunistic HIV co-infection. The Roche COBAS ® AmpliPrep/COBAS ® TaqMan ® CMV Test is a FDA-approved test that measures CMV DNA viral load in plasma for the diagnosis and management of patients at risk for CMV-associated diseases. Besides plasma, CMV is often found in bronchoalveolar lavage (BAL), cerebrospinal fluid (CSF) and urine. Thus, monitoring of CMV for critical care of patients in these non-plasma samples becomes necessary. The objective of this study was to conduct an analytic and clinical feasibility study of the Roche CMV Test in BAL, CSF, and urine. The lower limit of detection (LOD), analytic measurement range (AMR), assay sensitivity, specificity, and precision were determined. Results of this study showed the LODs were 50, 100 and 300 IU/mL for BAL, CSF, or urine, respectively. The AMRs were from log 10 2.48 to log 10 5.48. The assay specificity was 94.4% for BAL, and 100% for CSF and urine. The assay precision was all within the acceptable range. The performance of Roche test was further compared with two comparators including the RealTime CMV Assay (Abbott Molecular) and a CMV Quantitative PCR Test (Vela Diagnostics). There was a general positive correlation between the Roche method and the Abbott or the Vela method. Overall, this study suggests the Roche CMV Test is suitable for the quantification of CMV viral load DNA in the described non-plasma samples. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Evaluation and comparison of Abbott Jaffe and enzymatic creatinine methods: Could the old method meet the new requirements?

PubMed

Küme, Tuncay; Sağlam, Barıs; Ergon, Cem; Sisman, Ali Rıza

2018-01-01

The aim of this study is to evaluate and compare the analytical performance characteristics of the two creatinine methods based on the Jaffe and enzymatic methods. Two original creatinine methods, Jaffe and enzymatic, were evaluated on Architect c16000 automated analyzer via limit of detection (LOD) and limit of quantitation (LOQ), linearity, intra-assay and inter-assay precision, and comparability in serum and urine samples. The method comparison and bias estimation using patient samples according to CLSI guideline were performed on 230 serum and 141 urine samples by analyzing on the same auto-analyzer. The LODs were determined as 0.1 mg/dL for both serum methods and as 0.25 and 0.07 mg/dL for the Jaffe and the enzymatic urine method respectively. The LOQs were similar with 0.05 mg/dL value for both serum methods, and enzymatic urine method had a lower LOQ than Jaffe urine method, values at 0.5 and 2 mg/dL respectively. Both methods were linear up to 65 mg/dL for serum and 260 mg/dL for urine. The intra-assay and inter-assay precision data were under desirable levels in both methods. The higher correlations were determined between two methods in serum and urine (r=.9994, r=.9998 respectively). On the other hand, Jaffe method gave the higher creatinine results than enzymatic method, especially at the low concentrations in both serum and urine. Both Jaffe and enzymatic methods were found to meet the analytical performance requirements in routine use. However, enzymatic method was found to have better performance in low creatinine levels. © 2017 Wiley Periodicals, Inc.

Complete automation of solid-phase extraction with subsequent liquid chromatography-tandem mass spectrometry for the quantification of benzoylecgonine, m-hydroxybenzoylecgonine, p-hydroxybenzoylecgonine, and norbenzoylecgonine in urine--application to a high-throughput urine analysis laboratory.

PubMed

Robandt, Paul P; Reda, Louis J; Klette, Kevin L

2008-10-01

A fully automated system utilizing a liquid handler and an online solid-phase extraction (SPE) device coupled with liquid chromatography-tandem mass spectrometry (LC-MS-MS) was designed to process, detect, and quantify benzoylecgonine (BZE), meta-hydroxybenzoylecgonine (m-OH BZE), para-hydroxybenzoylecgonine (p-OH BZE), and norbenzoylecgonine (nor-BZE) metabolites in human urine. The method was linear for BZE, m-OH BZE, and p-OH BZE from 1.2 to 10,000 ng/mL with limits of detection (LOD) and quantification (LOQ) of 1.2 ng/mL. Nor-BZE was linear from 5 to 10,000 ng/mL with an LOD and LOQ of 1.2 and 5 ng/mL, respectively. The intrarun precision measured as the coefficient of variation of 10 replicates of a 100 ng/mL control was less than 2.6%, and the interrun precision for 5 replicates of the same control across 8 batches was less than 4.8% for all analytes. No assay interference was noted from controls containing cocaine, cocaethylene, and ecgonine methyl ester. Excellent data concordance (R2 > 0.994) was found for direct comparison of the automated SPE-LC-MS-MS procedure and an existing gas chromatography-MS procedure using 94 human urine samples previously determined to be positive for BZE. The automated specimen handling and SPE procedure, when compared to the traditional extraction schema, eliminates the human factors of specimen handling, processing, extraction, and derivatization, thereby reducing labor costs and rework resulting from batch handling issues, and may reduce the number of fume hoods required in the laboratory.

A simple and rapid chromatographic method to determine unauthorized basic colorants (rhodamine B, auramine O, and pararosaniline) in processed foods.

PubMed

Tatebe, Chiye; Zhong, Xining; Ohtsuki, Takashi; Kubota, Hiroki; Sato, Kyoko; Akiyama, Hiroshi

2014-09-01

A simple and rapid high-performance liquid chromatography (HPLC) method to determine basic colorants such as pararosaniline (PA), auramine O (AO), and rhodamine B (RB) in various processed foods was developed. Linearity of the calibration curves ranged from 0.05 to 50 μg/mL for PA and 0.05-100 μg/mL for AO and RB. The detection and quantification limits (LOD and LOQ) of the basic colorants, which were evaluated as signal-to-noise ratios of 3 for LOD and 10 for LOQ, ranged from 0.0125 to 0.05 and 0.025 to 0.125 μg/g, respectively. The recoveries and relative standard deviations of three basic colorants in six processed foods, namely, chili sauce, curry paste, gochujang (hot pepper paste), tandoori chicken (roasted chicken prepared with yogurt and spices), powder soup, and shrimp powder ranged from 70.2% to 102.8% and 0.8% to 8.0%, respectively. The intraday precision of the recovery test ranged from 1.7% to 4.5%, whereas the interday precision ranged from 3.7% to 7.7%. The reported method has been successfully applied to basic colorant determination in various processed foods such as fat-based food matrices (curry paste and tandoori chicken), chili products (gochujang and chili sauce), and protein-based products (shrimp powder and powder soup). Thin layer chromatography and liquid chromatography/mass spectrometry methods for the determination of basic colorants in processed foods were also developed for rapid analysis and identification, respectively. These methods are very useful for monitoring unauthorized basic colorants in inspection centers or quarantine laboratories in many countries.

Development and validation of a micellar electrokinetic chromatography method for quantitative determination of butenolides in Piper malacophyllum (C. Presl) C. DC.

PubMed

de Oliveira, Alberto; Silva, Claudinei A; Silva, Adalberto M; Tavares, Marina F M; Kato, Massuo J

2010-01-01

A large number of natural and synthetic compounds having butenolides as a core unit have been described and many of them display a wide range of biological activities. Butenolides from P. malacophyllum have presented potential antifungal activities but no specific, fast, and precise method has been developed for their determination. To develop a methodology based on micellar electrokinetic chromatography to determine butenolides in Piper species. The extracts were analysed in an uncoated fused-silica capillaries and for the micellar system 20 mmol/L SDS, 20% (v/v) acetonitrile (ACN) and 10 mmol/L STB aqueous buffer at pH 9.2 were used. The method was validated for precision, linearity, limit of detection (LOD) and limit of quantitation (LOQ) and the standard deviations were determined from the standard errors estimated by the regression line. A micellar electrokinetic chromatography (MEKC) method for determination of butenolides in extracts gave full resolution for 1 and 2. The analytical curve in the range 10.0-50.0 µg/mL (r(2) = 0.999) provided LOD and LOQ for 1 and 2 of 2.1/6.3 and 1.1/3.5 µg/mL, respectively. The RSD for migration times were 0.12 and 1.0% for peak area ratios with 100.0 ± 1.4% of recovery. A novel high-performance MEKC method developed for the analysis of butenolides 1 and 2 in leaf extracts of P. malacophyllum allowed their quantitative determined within an analysis time shorter than 5 min and the results indicated CE to be a feasible analytical technique for the quantitative determination of butenolides in Piper extracts. Copyright © 2010 John Wiley & Sons, Ltd.

Development of a validated HPLC method for the simultaneous determination of flavonoids in Cuscuta chinensis Lam. by ultra-violet detection

PubMed Central

2012-01-01

Background Cuscuta species known as dodder, have been used in traditional medicine of eastern and southern Asian countries as liver and kidney tonic. Flavonoids are considered as the main biologically active constituents in Cuscuta plants especially in C. chinensis Lam. Objective In the present study, a fast, simple and reliable method for the simultaneous determination and quantization of C. chinensis flavonols including hyperoside, rutin, isorhamnetin and kaempferol has been developed. Materials and methods The chromatographic separation was carried out on a reversed phase ACE 5 C18 with eluting at a flow rate of 1 ml/min using a gradient with O-phosphoric acid 0.25% : acetonitrile for 42 min. UV spectra were collected across the range of 200–900 nm, extracting 360 nm for the chromatograms. The method was validated according to linearity, selectivity, precision, recovery, LOD and LOQ. Results The method was selective for determination of rutin, hyperoside, isorhamnetin and kampferol. The calibration graphs of flavonols were linear with r2 > 0.999. RSDs% of intra- and inter-day precisions were found 1.3&3.4 for rutin, 1.5&2.8 for hyperoside, 1.3&3.3 for isorhamnetin and 1.7 & 2.9 for kaempferol which were satisfactory. LODs and LOQs were calculated as 1.73 & 8.19 for rutin, 0.09 & 4.19 for hyperoside, 2.09 & 6.3 for isorhamnetin and 0.18 & 0.56 for kaempferol. The recovery averages of above-mentioned flavonols were 90.3%, 97.4%, 98.7% and 90.0%, respectively. Conclusion The simplicity of the method makes it highly valuable for quality control of C. chinensis according to quantization of flavonols. PMID:23352257

Spectropolarimetry with PEPSI at the LBT: accuracy vs. precision in magnetic field measurements

NASA Astrophysics Data System (ADS)

Ilyin, Ilya; Strassmeier, Klaus G.; Woche, Manfred; Hofmann, Axel

2009-04-01

We present the design of the new PEPSI spectropolarimeter to be installed at the Large Binocular Telescope (LBT) in Arizona to measure the full set of Stokes parameters in spectral lines and outline its precision and the accuracy limiting factors.

Bulk-modified modified screen-printing carbon electrodes with both lactate oxidase (LOD) and horseradish peroxide (HRP) for the determination of L-lactate in flow injection analysis mode.

PubMed

Ghamouss, Fouad; Ledru, Sophie; Ruillé, Nadine; Lantier, Françoise; Boujtita, Mohammed

2006-06-16

A screen-printed carbon electrode modified with both HRP and LOD (SPCE-HRP/LOD) has been developed for the determination of L-lactate concentration in real samples. The resulting SPCE-HRP/LOD was prepared in a one-step procedure, and was then optimised as an amperometric biosensor operating at [0, -100]mV versus Ag/AgCl for L-lactate determination in flow injection mode. A significant improvement in the reproducibility (coefficient variation of about 10%) of the preparation of the biosensors was obtained when graphite powder was modified with LOD in the presence of HRP previously oxidised by periodate ion (IO4-). Optimisation studies were performed by examining the effects of LOD loading, periodation step and rate of the binder on analytical performances of SPCE-HRP/LOD. The sensitivity of the optimised SPCE-HRP/LOD to L-lactate was 0.84 nAL micromol(-1) in a detection range between 10 and 180 microMol. The possibility of using the developed biosensor to determine L-lactate concentrations in various dairy products was also evaluated.

Superior accuracy of model-based radiostereometric analysis for measurement of polyethylene wear

PubMed Central

Stilling, M.; Kold, S.; de Raedt, S.; Andersen, N. T.; Rahbek, O.; Søballe, K.

2012-01-01

Objectives The accuracy and precision of two new methods of model-based radiostereometric analysis (RSA) were hypothesised to be superior to a plain radiograph method in the assessment of polyethylene (PE) wear. Methods A phantom device was constructed to simulate three-dimensional (3D) PE wear. Images were obtained consecutively for each simulated wear position for each modality. Three commercially available packages were evaluated: model-based RSA using laser-scanned cup models (MB-RSA), model-based RSA using computer-generated elementary geometrical shape models (EGS-RSA), and PolyWare. Precision (95% repeatability limits) and accuracy (Root Mean Square Errors) for two-dimensional (2D) and 3D wear measurements were assessed. Results The precision for 2D wear measures was 0.078 mm, 0.102 mm, and 0.076 mm for EGS-RSA, MB-RSA, and PolyWare, respectively. For the 3D wear measures the precision was 0.185 mm, 0.189 mm, and 0.244 mm for EGS-RSA, MB-RSA, and PolyWare respectively. Repeatability was similar for all methods within the same dimension, when compared between 2D and 3D (all p > 0.28). For the 2D RSA methods, accuracy was below 0.055 mm and at least 0.335 mm for PolyWare. For 3D measurements, accuracy was 0.1 mm, 0.2 mm, and 0.3 mm for EGS-RSA, MB-RSA and PolyWare respectively. PolyWare was less accurate compared with RSA methods (p = 0.036). No difference was observed between the RSA methods (p = 0.10). Conclusions For all methods, precision and accuracy were better in 2D, with RSA methods being superior in accuracy. Although less accurate and precise, 3D RSA defines the clinically relevant wear pattern (multidirectional). PolyWare is a good and low-cost alternative to RSA, despite being less accurate and requiring a larger sample size. PMID:23610688

Evaluation and attribution of OCO-2 XCO2 uncertainties

NASA Astrophysics Data System (ADS)

Worden, John R.; Doran, Gary; Kulawik, Susan; Eldering, Annmarie; Crisp, David; Frankenberg, Christian; O'Dell, Chris; Bowman, Kevin

2017-07-01

Evaluating and attributing uncertainties in total column atmospheric CO2 measurements (XCO2) from the OCO-2 instrument is critical for testing hypotheses related to the underlying processes controlling XCO2 and for developing quality flags needed to choose those measurements that are usable for carbon cycle science.Here we test the reported uncertainties of version 7 OCO-2 XCO2 measurements by examining variations of the XCO2 measurements and their calculated uncertainties within small regions (˜ 100 km × 10.5 km) in which natural CO2 variability is expected to be small relative to variations imparted by noise or interferences. Over 39 000 of these small neighborhoods comprised of approximately 190 observations per neighborhood are used for this analysis. We find that a typical ocean measurement has a precision and accuracy of 0.35 and 0.24 ppm respectively for calculated precisions larger than ˜ 0.25 ppm. These values are approximately consistent with the calculated errors of 0.33 and 0.14 ppm for the noise and interference error, assuming that the accuracy is bounded by the calculated interference error. The actual precision for ocean data becomes worse as the signal-to-noise increases or the calculated precision decreases below 0.25 ppm for reasons that are not well understood. A typical land measurement, both nadir and glint, is found to have a precision and accuracy of approximately 0.75 and 0.65 ppm respectively as compared to the calculated precision and accuracy of approximately 0.36 and 0.2 ppm. The differences in accuracy between ocean and land suggests that the accuracy of XCO2 data is likely related to interferences such as aerosols or surface albedo as they vary less over ocean than land. The accuracy as derived here is also likely a lower bound as it does not account for possible systematic biases between the regions used in this analysis.

Accuracy and precision of 3 intraoral scanners and accuracy of conventional impressions: A novel in vivo analysis method.

PubMed

Nedelcu, R; Olsson, P; Nyström, I; Rydén, J; Thor, A

2018-02-01

To evaluate a novel methodology using industrial scanners as a reference, and assess in vivo accuracy of 3 intraoral scanners (IOS) and conventional impressions. Further, to evaluate IOS precision in vivo. Four reference-bodies were bonded to the buccal surfaces of upper premolars and incisors in five subjects. After three reference-scans, ATOS Core 80 (ATOS), subjects were scanned three times with three IOS systems: 3M True Definition (3M), CEREC Omnicam (OMNI) and Trios 3 (TRIOS). One conventional impression (IMPR) was taken, 3M Impregum Penta Soft, and poured models were digitized with laboratory scanner 3shape D1000 (D1000). Best-fit alignment of reference-bodies and 3D Compare Analysis was performed. Precision of ATOS and D1000 was assessed for quantitative evaluation and comparison. Accuracy of IOS and IMPR were analyzed using ATOS as reference. Precision of IOS was evaluated through intra-system comparison. Precision of ATOS reference scanner (mean 0.6 μm) and D1000 (mean 0.5 μm) was high. Pairwise multiple comparisons of reference-bodies located in different tooth positions displayed a statistically significant difference of accuracy between two scanner-groups: 3M and TRIOS, over OMNI (p value range 0.0001 to 0.0006). IMPR did not show any statistically significant difference to IOS. However, deviations of IOS and IMPR were within a similar magnitude. No statistical difference was found for IOS precision. The methodology can be used for assessing accuracy of IOS and IMPR in vivo in up to five units bilaterally from midline. 3M and TRIOS had a higher accuracy than OMNI. IMPR overlapped both groups. Intraoral scanners can be used as a replacement for conventional impressions when restoring up to ten units without extended edentulous spans. Copyright © 2017 The Authors. Published by Elsevier Ltd.. All rights reserved.

Lods, wrods, and mods: the interpretation of lod scores calculated under different models.

PubMed

Hodge, S E; Elston, R C

1994-01-01

In this paper we examine the relationships among classical lod scores, "wrod" scores (lod scores calculated under the wrong genetic model), and "mod" scores (lod scores maximized over genetic model parameters). We compare the behavior of these scores when the state of nature is linkage to their behavior when the state of nature is no linkage. We describe sufficient conditions for mod scores to be valid and discuss their use to determine the correct genetic model. We show that lod scores represent a likelihood-ratio test for independence. We explain the "ascertainment-assumption-free" aspect of using mod scores to determine mode of inheritance and we set this aspect into a well-established statistical framework. Finally, we summarize practical guidelines for the use of mod scores.

Number-Density Measurements of CO2 in Real Time with an Optical Frequency Comb for High Accuracy and Precision

NASA Astrophysics Data System (ADS)

Scholten, Sarah K.; Perrella, Christopher; Anstie, James D.; White, Richard T.; Al-Ashwal, Waddah; Hébert, Nicolas Bourbeau; Genest, Jérôme; Luiten, Andre N.

2018-05-01

Real-time and accurate measurements of gas properties are highly desirable for numerous real-world applications. Here, we use an optical-frequency comb to demonstrate absolute number-density and temperature measurements of a sample gas with state-of-the-art precision and accuracy. The technique is demonstrated by measuring the number density of 12C16O2 with an accuracy of better than 1% and a precision of 0.04% in a measurement and analysis cycle of less than 1 s. This technique is transferable to numerous molecular species, thus offering an avenue for near-universal gas concentration measurements.

Simultaneous Determination of Multiple Ginsenosides in Panax ginseng Herbal Medicines with One Single Reference Standard.

PubMed

Wu, Chunwei; Guan, Qingxiao; Wang, Shumei; Rong, Yueying

2017-01-01

Root of Panax ginseng C. A. Mey (Renseng in Chinese) is a famous Traditional Chinese Medicine. Ginsenosides are the major bioactive components. However, the shortage and high cost of some ginsenoside reference standards make it is difficult for quality control of P. ginseng . A method, single standard for determination of multicomponents (SSDMC), was developed for the simultaneous determination of nine ginsenosides in P. ginseng (ginsenoside Rg 1 , Re, Rf, Rg 2 , Rb 1 , Rc, Rb 2 , Rb 3 , Rd). The analytes were separated on Inertsil ODS-3 C18 (250 mm × 4.6 mm, 5 μm) with gradient elution of acetonitrile and water. The flow rate was 1 mL/min and detection wavelength was set at 203 nm. The feasibility and accuracy of SSDMC were checked by the external standard method, and various high-performance liquid chromatographic (HPLC) instruments and chromatographic conditions were investigated to verify its applicability. Using ginsenoside Rg 1 as the internal reference substance, the contents of other eight ginsenosides were calculated according to conversion factors (F) by HPLC. The method was validated with linearity ( r 2 ≥ 0.9990), precision (relative standard deviation [RSD] ≤2.9%), accuracy (97.5%-100.8%, RSD ≤ 1.6%), repeatability, and stability. There was no significant difference between the SSDMC method and the external standard method. New SSDMC method could be considered as an ideal mean to analyze the components for which reference standards are not readily available. A method, single standard for determination of multicomponents (SSDMC), was established by high-performance liquid chromatography for the simultaneous determination of nine ginsenosides in Panax ginseng (ginsenoside Rg1, Re, Rf, Rg2, Rb1, Rc, Rb2, Rb3, Rd)Various chromatographic conditions were investigated to verify applicability of FsThe feasibility and accuracy of SSDMC were checked by the external standard method. Abbreviations used: DRT: Different value of retention time; F: Conversion factor; HPLC: High-performance Liquid Chromatography; LOD: Limit of detection; LOQ: Limit of quantitation; PD: Percent difference; PPD: 20(S)-protopanaxadiol; PPT: 20(S)-protopanaxatriol; RSD: Relative standard deviation; SSDMC: Single Standard for Determination of Multicomponents; TCM: Traditional Chinese Medicine.

Accuracy and precision of occlusal contacts of stereolithographic casts mounted by digital interocclusal registrations.

PubMed

Krahenbuhl, Jason T; Cho, Seok-Hwan; Irelan, Jon; Bansal, Naveen K

2016-08-01

Little peer-reviewed information is available regarding the accuracy and precision of the occlusal contact reproduction of digitally mounted stereolithographic casts. The purpose of this in vitro study was to evaluate the accuracy and precision of occlusal contacts among stereolithographic casts mounted by digital occlusal registrations. Four complete anatomic dentoforms were arbitrarily mounted on a semi-adjustable articulator in maximal intercuspal position and served as the 4 different simulated patients (SP). A total of 60 digital impressions and digital interocclusal registrations were made with a digital intraoral scanner to fabricate 15 sets of mounted stereolithographic (SLA) definitive casts for each dentoform. After receiving a total of 60 SLA casts, polyvinyl siloxane (PVS) interocclusal records were made for each set. The occlusal contacts for each set of SLA casts were measured by recording the amount of light transmitted through the interocclusal records. To evaluate the accuracy between the SP and their respective SLA casts, the areas of actual contact (AC) and near contact (NC) were calculated. For precision analysis, the coefficient of variation (CoV) was used. The data was analyzed with t tests for accuracy and the McKay and Vangel test for precision (α=.05). The accuracy analysis showed a statistically significant difference between the SP and the SLA cast of each dentoform (P<.05). For the AC in all dentoforms, a significant increase was found in the areas of actual contact of SLA casts compared with the contacts present in the SP (P<.05). Conversely, for the NC in all dentoforms, a significant decrease was found in the occlusal contact areas of the SLA casts compared with the contacts in the SP (P<.05). The precision analysis demonstrated the different CoV values between AC (5.8 to 8.8%) and NC (21.4 to 44.6%) of digitally mounted SLA casts, indicating that the overall precision of the SLA cast was low. For the accuracy evaluation, statistically significant differences were found between the occlusal contacts of all digitally mounted SLA casts groups, with an increase in AC values and a decrease in NC values. For the precision assessment, the CoV values of the AC and NC showed the digitally articulated cast's inability to reproduce the uniform occlusal contacts. Copyright © 2016 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

IEEE-1588(Trademark) Standard for a Precision Clock Synchronization Protocol for Networked Measurement and Control Systems

DTIC Science & Technology

2002-12-01

34th Annual Precise Time and Time Interval (PTTI) Meeting 243 IEEE-1588™ STANDARD FOR A PRECISION CLOCK SYNCHRONIZATION PROTOCOL FOR... synchronization . 2. Cyclic-systems. In cyclic-systems, timing is periodic and is usually defined by the characteristics of a cyclic network or bus...incommensurate, timing schedules for each device are easily implemented. In addition, synchronization accuracy depends on the accuracy of the common

Distribution in microbial genomes of genes similar to lodA and goxA which encode a novel family of quinoproteins with amino acid oxidase activity.

PubMed

Campillo-Brocal, Jonatan C; Chacón-Verdú, María Dolores; Lucas-Elío, Patricia; Sánchez-Amat, Antonio

2015-03-24

L-Amino acid oxidases (LAOs) have been generally described as flavoproteins that oxidize amino acids releasing the corresponding ketoacid, ammonium and hydrogen peroxide. The generation of hydrogen peroxide gives to these enzymes antimicrobial characteristics. They are involved in processes such as biofilm development and microbial competition. LAOs are of great biotechnological interest in different applications such as the design of biosensors, biotransformations and biomedicine. The marine bacterium Marinomonas mediterranea synthesizes LodA, the first known LAO that contains a quinone cofactor. LodA is encoded in an operon that contains a second gene coding for LodB, a protein required for the post-translational modification generating the cofactor. Recently, GoxA, a quinoprotein with sequence similarity to LodA but with a different enzymatic activity (glycine oxidase instead of lysine-ε-oxidase) has been described. The aim of this work has been to study the distribution of genes similar to lodA and/or goxA in sequenced microbial genomes and to get insight into the evolution of this novel family of proteins through phylogenetic analysis. Genes encoding LodA-like proteins have been detected in several bacterial classes. However, they are absent in Archaea and detected only in a small group of fungi of the class Agaromycetes. The vast majority of the genes detected are in a genome region with a nearby lodB-like gene suggesting a specific interaction between both partner proteins. Sequence alignment of the LodA-like proteins allowed the detection of several conserved residues. All of them showed a Cys and a Trp that aligned with the residues that are forming part of the cysteine tryptophilquinone (CTQ) cofactor in LodA. Phylogenetic analysis revealed that LodA-like proteins can be clustered in different groups. Interestingly, LodA and GoxA are in different groups, indicating that those groups are related to the enzymatic activity of the proteins detected. Genome mining has revealed for the first time the broad distribution of LodA-like proteins containing a CTQ cofactor in many different microbial groups. This study provides a platform to explore the potentially novel enzymatic activities of the proteins detected, the mechanisms of post-translational modifications involved in their synthesis, as well as their biological relevance.

Presentation Accuracy of the Web Revisited: Animation Methods in the HTML5 Era

PubMed Central

Garaizar, Pablo; Vadillo, Miguel A.; López-de-Ipiña, Diego

2014-01-01

Using the Web to run behavioural and social experiments quickly and efficiently has become increasingly popular in recent years, but there is some controversy about the suitability of using the Web for these objectives. Several studies have analysed the accuracy and precision of different web technologies in order to determine their limitations. This paper updates the extant evidence about presentation accuracy and precision of the Web and extends the study of the accuracy and precision in the presentation of multimedia stimuli to HTML5-based solutions, which were previously untested. The accuracy and precision in the presentation of visual content in classic web technologies is acceptable for use in online experiments, although some results suggest that these technologies should be used with caution in certain circumstances. Declarative animations based on CSS are the best alternative when animation intervals are above 50 milliseconds. The performance of procedural web technologies based on the HTML5 standard is similar to that of previous web technologies. These technologies are being progressively adopted by the scientific community and have promising futures, which makes their use advisable to utilizing more obsolete technologies. PMID:25302791

Optimal Parameters to Determine the Apparent Diffusion Coefficient in Diffusion Weighted Imaging via Simulation

NASA Astrophysics Data System (ADS)

Perera, Dimuthu

Diffusion weighted (DW) Imaging is a non-invasive MR technique that provides information about the tissue microstructure using the diffusion of water molecules. The diffusion is generally characterized by the apparent diffusion coefficient (ADC) parametric map. The purpose of this study is to investigate in silico how the calculation of ADC is affected by image SNR, b-values, and the true tissue ADC. Also, to provide optimal parameter combination depending on the percentage accuracy and precision for prostate peripheral region cancer application. Moreover, to suggest parameter choices for any type of tissue, while providing the expected accuracy and precision. In this research DW images were generated assuming a mono-exponential signal model at two different b-values and for known true ADC values. Rician noise of different levels was added to the DWI images to adjust the image SNR. Using the two DWI images, ADC was calculated using a mono-exponential model for each set of b-values, SNR, and true ADC. 40,000 ADC data were collected for each parameter setting to determine the mean and the standard-deviation of the calculated ADC, as well as the percentage accuracy and precision with respect to the true ADC. The accuracy was calculated using the difference between known and calculated ADC. The precision was calculated using the standard-deviation of calculated ADC. The optimal parameters for a specific study was determined when both the percentage accuracy and precision were minimized. In our study, we simulated two true ADCs (ADC 0.00102 for tumor and 0.00180 mm2/s for normal prostate peripheral region tissue). Image SNR was varied from 2 to 100 and b-values were varied from 0 to 2000s/mm2. The results show that the percentage accuracy and percentage precision were minimized with image SNR. To increase SNR, 10 signal-averagings (NEX) were used considering the limitation in total scan time. The optimal NEX combination for tumor and normal tissue for prostate peripheral region was 1: 9. Also, the minimum percentage accuracy and percentage precision were obtained when low b-value is 0 and high b-value is 800 mm2/s for normal tissue and 1400 mm2/s for tumor tissue. Results also showed that for tissues with 1 x 10-3 < ADC < 2.1 x 10-3 mm 2/s the parameter combination at SNR = 20, b-value pair 0, 800 mm 2/s with NEX = 1:9 can calculate ADC with a percentage accuracy of less than 2% and percentage precision of 6-8%. Also, for tissues with 0.6 x 10-3 < ADC < 1.25 x 10-3 mm2 /s the parameter combination at SNR = 20, b-value pair 0, 1400 mm 2/s with NEX =1:9 can calculate ADC with a percentage accuracy of less than 2% and percentage precision of 6-8%.

Is digital photography an accurate and precise method for measuring range of motion of the hip and knee?

PubMed

Russo, Russell R; Burn, Matthew B; Ismaily, Sabir K; Gerrie, Brayden J; Han, Shuyang; Alexander, Jerry; Lenherr, Christopher; Noble, Philip C; Harris, Joshua D; McCulloch, Patrick C

2017-09-07

Accurate measurements of knee and hip motion are required for management of musculoskeletal pathology. The purpose of this investigation was to compare three techniques for measuring motion at the hip and knee. The authors hypothesized that digital photography would be equivalent in accuracy and show higher precision compared to the other two techniques. Using infrared motion capture analysis as the reference standard, hip flexion/abduction/internal rotation/external rotation and knee flexion/extension were measured using visual estimation, goniometry, and photography on 10 fresh frozen cadavers. These measurements were performed by three physical therapists and three orthopaedic surgeons. Accuracy was defined by the difference from the reference standard, while precision was defined by the proportion of measurements within either 5° or 10°. Analysis of variance (ANOVA), t-tests, and chi-squared tests were used. Although two statistically significant differences were found in measurement accuracy between the three techniques, neither of these differences met clinical significance (difference of 1.4° for hip abduction and 1.7° for the knee extension). Precision of measurements was significantly higher for digital photography than: (i) visual estimation for hip abduction and knee extension, and (ii) goniometry for knee extension only. There was no clinically significant difference in measurement accuracy between the three techniques for hip and knee motion. Digital photography only showed higher precision for two joint motions (hip abduction and knee extension). Overall digital photography shows equivalent accuracy and near-equivalent precision to visual estimation and goniometry.

Fast-PPP assessment in European and equatorial region near the solar cycle maximum

NASA Astrophysics Data System (ADS)

Rovira-Garcia, Adria; Juan, José Miguel; Sanz, Jaume

2014-05-01

The Fast Precise Point Positioning (Fast-PPP) is a technique to provide quick high-accuracy navigation with ambiguity fixing capability, thanks to an accurate modelling of the ionosphere. Indeed, once the availability of real-time precise satellite orbits and clocks is granted to users, the next challenge is the accuracy of real-time ionospheric corrections. Several steps had been taken by gAGE/UPC to develop such global system for precise navigation. First Wide-Area Real-Time Kinematics (WARTK) feasibility studies enabled precise relative continental navigation using a few tens of reference stations. Later multi-frequency and multi-constellation assessments in different ionospheric scenarios, including maximum solar-cycle conditions, were focussed on user-domain performance. Recently, a mature evolution of the technique consists on a dual service scheme; a global Precise Point Positioning (PPP) service, together with a continental enhancement to shorten convergence. A end to end performance assessment of the Fast-PPP technique is presented in this work, focussed in Europe and in the equatorial region of South East Asia (SEA), both near the solar cycle maximum. The accuracy of the Central Processing Facility (CPF) real-time precise satellite orbits and clocks is respectively, 4 centimetres and 0.2 nanoseconds, in line with the accuracy of the International GNSS Service (IGS) analysis centres. This global PPP service is enhanced by the Fast-PPP by adding the capability of global undifferenced ambiguity fixing thanks to the fractional part of the ambiguities determination. The core of the Fast-PPP is the capability to compute real-time ionospheric determinations with accuracies at the level or better than 1 Total Electron Content Unit (TECU), improving the widely-accepted Global Ionospheric Maps (GIM), with declared accuracies of 2-8 TECU. This large improvement in the modelling accuracy is achieved thanks to a two-layer description of the ionosphere combined with the carrier-phase ambiguity fixing performed in the Fast-PPP CPF. The Fast-PPP user domain positioning takes benefit of such precise ionospheric modelling. Convergence time of dual-frequency classic PPP solutions is reduced from the best part of an hour to 5-10 minutes not only in European mid-latitudes but also in the much more challenging equatorial region. The improvement of ionospheric modelling is directly translated into the accuracy of single-frequency mass-market users, achieving 2-3 decimetres of error after any cold start. Since all Fast-PPP corrections are broadcast together with their confidence level (sigma), such high-accuracy navigation is protected with safety integrity bounds.

The Plus or Minus Game--Teaching Estimation, Precision, and Accuracy

ERIC Educational Resources Information Center

Forringer, Edward R.; Forringer, Richard S.; Forringer, Daniel S.

2016-01-01

A quick survey of physics textbooks shows that many (Knight, Young, and Serway for example) cover estimation, significant digits, precision versus accuracy, and uncertainty in the first chapter. Estimation "Fermi" questions are so useful that there has been a column dedicated to them in "TPT" (Larry Weinstein's "Fermi…

Are LOD and LOQ Reliable Parameters for Sensitivity Evaluation of Spectroscopic Methods?

PubMed

Ershadi, Saba; Shayanfar, Ali

2018-03-22

The limit of detection (LOD) and the limit of quantification (LOQ) are common parameters to assess the sensitivity of analytical methods. In this study, the LOD and LOQ of previously reported terbium sensitized analysis methods were calculated by different methods, and the results were compared with sensitivity parameters [lower limit of quantification (LLOQ)] of U.S. Food and Drug Administration guidelines. The details of the calibration curve and standard deviation of blank samples of three different terbium-sensitized luminescence methods for the quantification of mycophenolic acid, enrofloxacin, and silibinin were used for the calculation of LOD and LOQ. A comparison of LOD and LOQ values calculated by various methods and LLOQ shows a considerable difference. The significant difference of the calculated LOD and LOQ with various methods and LLOQ should be considered in the sensitivity evaluation of spectroscopic methods.

The score statistic of the LD-lod analysis: detecting linkage adaptive to linkage disequilibrium.

PubMed

Huang, J; Jiang, Y

2001-01-01

We study the properties of a modified lod score method for testing linkage that incorporates linkage disequilibrium (LD-lod). By examination of its score statistic, we show that the LD-lod score method adaptively combines two sources of information: (a) the IBD sharing score which is informative for linkage regardless of the existence of LD and (b) the contrast between allele-specific IBD sharing scores which is informative for linkage only in the presence of LD. We also consider the connection between the LD-lod score method and the transmission-disequilibrium test (TDT) for triad data and the mean test for affected sib pair (ASP) data. We show that, for triad data, the recessive LD-lod test is asymptotically equivalent to the TDT; and for ASP data, it is an adaptive combination of the TDT and the ASP mean test. We demonstrate that the LD-lod score method has relatively good statistical efficiency in comparison with the ASP mean test and the TDT for a broad range of LD and the genetic models considered in this report. Therefore, the LD-lod score method is an interesting approach for detecting linkage when the extent of LD is unknown, such as in a genome-wide screen with a dense set of genetic markers. Copyright 2001 S. Karger AG, Basel

Basic investigation of dual-energy x-ray absorptiometry for bone densitometry using computed radiography

NASA Astrophysics Data System (ADS)

Shimura, Kazuo; Nakajima, Nobuyoshi; Tanaka, Hiroshi; Ishida, Masamitsu; Kato, Hisatoyo

1993-09-01

Dual-energy X-ray absorptiometry (DXA) is one of the bone densitometry techniques to diagnose osteoporosis, and has been gradually getting popular due to its high degree of precision. However, DXA involves a time-consuming examination because of its pencil-beam scan, and the equipment is expensive. In this study, we examined a new bone densitometry technique (CR-DXA) utilizing an X-ray imaging system and Computed Radiography (CR) used for medical X-ray image diagnosis. High level of measurement precision and accuracy could be achieved by X-ray rube voltage/filter optimization and various nonuniformity corrections based on simulation and experiment. The phantom study using a bone mineral block showed precision of 0.83% c.v. (coefficient of variation), and accuracy of 0.01 g/cm2, suggesting that a practically equivalent degree of measurement precision and accuracy to that of the DXA approach is achieved. CR-DXA is considered to provide bone mineral densitometry to facilitate simple, quick and precise bone mineral density measurement.

Influence of Waveform Characteristics on LiDAR Ranging Accuracy and Precision

PubMed Central

Yang, Bingwei; Xie, Xinhao; Li, Duan

2018-01-01

Time of flight (TOF) based light detection and ranging (LiDAR) is a technology for calculating distance between start/stop signals of time of flight. In lab-built LiDAR, two ranging systems for measuring flying time between start/stop signals include time-to-digital converter (TDC) that counts time between trigger signals and analog-to-digital converter (ADC) that processes the sampled start/stop pulses waveform for time estimation. We study the influence of waveform characteristics on range accuracy and precision of two kinds of ranging system. Comparing waveform based ranging (WR) with analog discrete return system based ranging (AR), a peak detection method (WR-PK) shows the best ranging performance because of less execution time, high ranging accuracy, and stable precision. Based on a novel statistic mathematical method maximal information coefficient (MIC), WR-PK precision has a high linear relationship with the received pulse width standard deviation. Thus keeping the received pulse width of measuring a constant distance as stable as possible can improve ranging precision. PMID:29642639

One-step liquid-liquid extraction of cocaine from urine samples for gas chromatographic analysis.

PubMed

Farina, Marcelo; Yonamine, Maurício; Silva, Ovandir A

2002-07-17

An improved technique for cocaine extraction from urine samples for gas chromatographic (GC) analysis is described. Employing a simple liquid-liquid extraction (LLE) of cocaine with a mixture of ethyl ether:isopropanol (9:1) the method presents a mean recovery of 74.49%. Limit of detection (LOD) and limit of quantification (LOQ) were 5 and 20 ng/ml, respectively. The method is highly precise (coefficient of variation (CV) <8%) and linear from 20 to 2000 ng/ml. It can he applied to detect the presence of cocaine in urine as a marker of its recent use in drug abuse treatment protocols.

13 Years of TOPEX/POSEIDON Precision Orbit Determination and the 10-fold Improvement in Expected Orbit Accuracy

NASA Technical Reports Server (NTRS)

Lemoine, F. G.; Zelensky, N. P.; Luthcke, S. B.; Rowlands, D. D.; Beckley, B. D.; Klosko, S. M.

2006-01-01

Launched in the summer of 1992, TOPEX/POSEIDON (T/P) was a joint mission between NASA and the Centre National d Etudes Spatiales (CNES), the French Space Agency, to make precise radar altimeter measurements of the ocean surface. After the remarkably successful 13-years of mapping the ocean surface T/P lost its ability to maneuver and was de-commissioned January 2006. T/P revolutionized the study of the Earth s oceans by vastly exceeding pre-launch estimates of surface height accuracy recoverable from radar altimeter measurements. The precision orbit lies at the heart of the altimeter measurement providing the reference frame from which the radar altimeter measurements are made. The expected quality of orbit knowledge had limited the measurement accuracy expectations of past altimeter missions, and still remains a major component in the error budget of all altimeter missions. This paper describes critical improvements made to the T/P orbit time series over the 13-years of precise orbit determination (POD) provided by the GSFC Space Geodesy Laboratory. The POD improvements from the pre-launch T/P expectation of radial orbit accuracy and Mission requirement of 13-cm to an expected accuracy of about 1.5-cm with today s latest orbits will be discussed. The latest orbits with 1.5 cm RMS radial accuracy represent a significant improvement to the 2.0-cm accuracy orbits currently available on the T/P Geophysical Data Record (GDR) altimeter product.

System and method for high precision isotope ratio destructive analysis

DOEpatents

Bushaw, Bruce A; Anheier, Norman C; Phillips, Jon R

2013-07-02

A system and process are disclosed that provide high accuracy and high precision destructive analysis measurements for isotope ratio determination of relative isotope abundance distributions in liquids, solids, and particulate samples. The invention utilizes a collinear probe beam to interrogate a laser ablated plume. This invention provides enhanced single-shot detection sensitivity approaching the femtogram range, and isotope ratios that can be determined at approximately 1% or better precision and accuracy (relative standard deviation).

Nance-Horan syndrome: localization within the region Xp21.1-Xp22.3 by linkage analysis.

PubMed

Stambolian, D; Lewis, R A; Buetow, K; Bond, A; Nussbaum, R

1990-07-01

Nance-Horan Syndrome (NHS) or X-linked cataract-dental syndrome (MIM 302350) is a disease of unknown pathogenesis characterized by congenital cataracts and dental anomalies. We performed linkage analysis in three kindreds with NHS by using six RFLP markers between Xp11.3 and Xp22.3. Close linkage was found between NHS and polymorphic loci DXS43 (theta = 0 with lod score 2.89), DXS41 (theta = 0 with lod score 3.44), and DXS67 (theta = 0 with lod score 2.74), defined by probes pD2, p99-6, and pB24, respectively. Recombinations were found with the marker loci DXS84 (theta = .04 with lod score 4.13), DXS143 (theta = .06 with lod score 3.11) and DXS7 (theta = .09 with lod score 1.68). Multipoint linkage analysis determined the NHS locus to be linked completely to DXS41 (lod score = 7.07). Our linkage results, combined with analysis of Xp interstitial deletions, suggest that the NHS locus is located within or close to the Xp22.1-Xp22.2 region.

Nance-Horan syndrome: localization within the region Xp21.1-Xp22.3 by linkage analysis.

PubMed Central

Stambolian, D; Lewis, R A; Buetow, K; Bond, A; Nussbaum, R

1990-01-01

Nance-Horan Syndrome (NHS) or X-linked cataract-dental syndrome (MIM 302350) is a disease of unknown pathogenesis characterized by congenital cataracts and dental anomalies. We performed linkage analysis in three kindreds with NHS by using six RFLP markers between Xp11.3 and Xp22.3. Close linkage was found between NHS and polymorphic loci DXS43 (theta = 0 with lod score 2.89), DXS41 (theta = 0 with lod score 3.44), and DXS67 (theta = 0 with lod score 2.74), defined by probes pD2, p99-6, and pB24, respectively. Recombinations were found with the marker loci DXS84 (theta = .04 with lod score 4.13), DXS143 (theta = .06 with lod score 3.11) and DXS7 (theta = .09 with lod score 1.68). Multipoint linkage analysis determined the NHS locus to be linked completely to DXS41 (lod score = 7.07). Our linkage results, combined with analysis of Xp interstitial deletions, suggest that the NHS locus is located within or close to the Xp22.1-Xp22.2 region. PMID:1971992

Percentiles of the null distribution of 2 maximum lod score tests.

PubMed

Ulgen, Ayse; Yoo, Yun Joo; Gordon, Derek; Finch, Stephen J; Mendell, Nancy R

2004-01-01

We here consider the null distribution of the maximum lod score (LOD-M) obtained upon maximizing over transmission model parameters (penetrance values, dominance, and allele frequency) as well as the recombination fraction. Also considered is the lod score maximized over a fixed choice of genetic model parameters and recombination-fraction values set prior to the analysis (MMLS) as proposed by Hodge et al. The objective is to fit parametric distributions to MMLS and LOD-M. Our results are based on 3,600 simulations of samples of n = 100 nuclear families ascertained for having one affected member and at least one other sibling available for linkage analysis. Each null distribution is approximately a mixture p(2)(0) + (1 - p)(2)(v). The values of MMLS appear to fit the mixture 0.20(2)(0) + 0.80chi(2)(1.6). The mixture distribution 0.13(2)(0) + 0.87chi(2)(2.8). appears to describe the null distribution of LOD-M. From these results we derive a simple method for obtaining critical values of LOD-M and MMLS. Copyright 2004 S. Karger AG, Basel

Geodynamo Modeling of Core-Mantle Interactions

NASA Technical Reports Server (NTRS)

Kuang, Wei-Jia; Chao, Benjamin F.; Smith, David E. (Technical Monitor)

2001-01-01

Angular momentum exchange between the Earth's mantle and core influences the Earth's rotation on time scales of decades and longer, in particular in the length of day (LOD) which have been measured with progressively increasing accuracy for the last two centuries. There are four possible coupling mechanisms for transferring the axial angular momentum across the core-mantle boundary (CMB): viscous, magnetic, topography, and gravitational torques. Here we use our scalable, modularized, fully dynamic geodynamo model for the core to assess the importance of these torques. This numerical model, as an extension of the Kuang-Bloxham model that has successfully simulated the generation of the Earth's magnetic field, is used to obtain numerical results in various physical conditions in terms of specific parameterization consistent with the dynamical processes in the fluid outer core. The results show that depending on the electrical conductivity of the lower mantle and the amplitude of the boundary topography at CMB, both magnetic and topographic couplings can contribute significantly to the angular momentum exchange. This implies that the core-mantle interactions are far more complex than has been assumed and that there is unlikely a single dominant coupling mechanism for the observed decadal LOD variation.

Determination of volatile compounds in wine by gas chromatography-flame ionization detection: comparison between the U.S. Environmental Protection Agency 3sigma approach and Hubaux-Vos calculation of detection limits using ordinary and bivariate least squares.

PubMed

Caruso, Rosario; Scordino, Monica; Traulo, Pasqualino; Gagliano, Giacomo

2012-01-01

A capillary GC-flame ionization detection (FID) method to determine volatile compounds (ethyl acetate, 1,1-diethoxyethane, methyl alcohol, 1-propanol, 2-methyl-1-propanol, 2-methyl-1-butanol, 3-methyl-1-butanol, 1-butanol, and 2-butanol) in wine was investigated in terms of calculation of detection limits and calibration method. The main objectives were: (1) calculation of regression coefficient parameters by ordinary least-squares (OLS) and bivariate least-squares (BLS) regression models, taking into account errors in both axes; (2) estimation of linear dynamic range (LDR) according to International Conference on Harmonization recommendations; (3) performance evaluation of a method by using three different internal standards (ISs) such as acetonitrile, acetone, and 1-pentanol; (4) evaluation of LODs according to the U.S. Environmental Protection Agency (EPA) 3sigma approach and the Hubaux-Vos (H-V) method; (5) application of H-V theory to a gas chromatographic analytical method and to a food matrix; and (6) accuracy assessment of the method relative to methyl alcohol content through a Unione Italiana Vini (UIV) interlaboratory proficiency test. Calibration curves calculated via BLS and OLS show similar slopes, while intercepts are closer to zero in the first case, independent of the chosen IS. The studied ISs show a substantially equivalent behavior, even though the IS closer to the analyte retention time seems to be more appropriate in terms of LDR and LOD. Results indicate an underestimation of LODs using the EPA 3sigma approach instead of the more realistic H-V method, both with OLS and BLS regression models. Methanol contents compared with UIV average values indicate recovery between 90 and 110%.

Ultra-HPLC method for quality and adulterant assessment of steviol glycosides sweeteners - Stevia rebaudiana and stevia products.

PubMed

Wang, Yan-Hong; Avula, Bharathi; Tang, Wenzhao; Wang, Mei; Elsohly, Mahmoud A; Khan, Ikhlas A

2015-01-01

Stevia products are advertised as a zero-calorie sweetener. Glucose should not be an intrinsic component of this product, but it has been identified from some of stevia products in a preliminary study. An UHPLC-UV method was developed for the quantitative determination of glucose from stevia products. After stevia products reacted with 1-phenyl-3-methyl-5-pyrazolone (PMP), PMP derivatives were analysed and glucose was found in seven out of 35 products in the range 0.3-91.5% (w/w). Two products, SPR-12 and SPR-27, showed remarkable amounts of glucose at 61.6% and 91.5%, respectively. In addition, an UHPLC-UV-evaporative light-scattering detector (ELSD) method was developed for the quantitative determination of rebaudioside A, stevioside, rebaudioside D, dulcoside A and steviolbioside from Stevia rebaudiana and related products. In a 12 min run, five steviol glycosides were baseline-separated. ELSD and ultraviolet (UV) detections showed comparable results. The LC methods were validated for linearity, repeatability, accuracy, limits of detection (LOD) and limits of quantification (LOQ). For steviol glycosides, the LODs and LOQs were found to be less than 10 and 30 μg ml(-1), respectively. The RSD for intra- and inter-day analyses was less than 2.5%, and the recovery was 90-94%. For PMP derivative of glucose, the LOD and LOQ were 0.01 and 0.05 μg ml(-1), respectively. Repeatability (RSD) was less than 2.6%; recovery was 98.6-101.7%. The methods are useful for the identification, quality assurance, and adulterant assessment of S. rebaudiana and steviol glycosides sweeteners (stevia products).

Detection of the significant geomagnetic field signals in the interannual variations of Length-of-Day using wavelet method

NASA Astrophysics Data System (ADS)

Liu, Genyou; Duan, Pengshuo; Hao, Xiaoguang; Hu, Xiaogang

2015-04-01

The previous studies indicated that the most of the interannual variations in Length-Of-Day (LOD) could be explained by the joint effects of ENSO (EI Nino-Southern Oscillations) and QBO (Quasi-Biennial Oscillation) phenomenon in the atmosphere. Due to the limit of the used methods, those results cannot give the 'time-frequency' coherence spectrum between ENSO and LOD, and cannot indicate in which specific periods the weak coherence occurred and difficult to give the reliable reason. This paper uses Daubechies wavelet with 10 order vanishing moment to analyze the LOD monthly time series from 1962 to 2011. Based on cross-wavelet and wavelet coherence methods, the analysis of the time-frequency correlations between ENSO and LOD series (1962-2011) on the 1.3~10.7 year scales is given. We have extracted and reconstructed the LOD signals on 1.3~10.7year scales. The result shows that there is obvious weak coherence on both biennial and 5~8 year scales after 1982 relative to before 1982. According to the previous works, the biennial weak coherence is due to QBO, but the weak coherence on 5~8 year scales cannot be interpreted by the effects of ENSO and QBO. In this study, the Geomagnetic field signals (can be characterized as Aa index) are introduced, we have further extracted and reconstructed the LOD, ENSO and Aa signals in 5-8.0 year band using wavelet packet analysis. Through analyzing the standardized series of the three signals, we found a linear time-frequency formula among the original observation series: LOD(t,f) =αENSO(t,f) +βAa(t,f). This study indicates that the LOD signals on 5.3~8.0 year scales can be expressed in term of linear combination of ENSO and Aa signals. Especially after 1982, the contributions of ENSO and Aa to LOD respectively reach about 0.95ms and 1.0ms.The results also imply that there is an obvious Geomagnetic field signal in interannual variations of LOD. Furthermore, after considering the geomagnetic field signal correction, the Pearson correlation coefficient between LOD and ENSO will increase from 0.51 to 0.98. Consequently, we can conclude that the weak coherence after 1982 on 5.3-8.0 year scales between LOD and ENSO is mainly due to the disturbance of Aa signal, and the observed LOD series is the result of the interaction between ENSO and geomagnetic field signals.

40 CFR 98.154 - Monitoring and QA/QC requirements.

Code of Federal Regulations, 2011 CFR

2011-07-01

... equipment and methods (e.g., gas chromatography) with an accuracy and precision of 5 percent or better at... equipment and methods (e.g., gas chromatography) with an accuracy and precision of 5 percent or better at... (CONTINUED) MANDATORY GREENHOUSE GAS REPORTING HCFC-22 Production and HFC-23 Destruction § 98.154 Monitoring...

Making and Measuring a Model of a Salt Marsh

ERIC Educational Resources Information Center

Fogleman, Tara; Curran, Mary Carla

2007-01-01

Students are often confused by the difference between the terms "accuracy" and "precision." In the following activities, students explore the definitions of accuracy and precision while learning about salt march ecology and the methods used by scientists to assess salt marsh health. The activities also address the concept that the ocean supports a…

Exploiting the chaotic behaviour of atmospheric models with reconfigurable architectures

NASA Astrophysics Data System (ADS)

Russell, Francis P.; Düben, Peter D.; Niu, Xinyu; Luk, Wayne; Palmer, T. N.

2017-12-01

Reconfigurable architectures are becoming mainstream: Amazon, Microsoft and IBM are supporting such architectures in their data centres. The computationally intensive nature of atmospheric modelling is an attractive target for hardware acceleration using reconfigurable computing. Performance of hardware designs can be improved through the use of reduced-precision arithmetic, but maintaining appropriate accuracy is essential. We explore reduced-precision optimisation for simulating chaotic systems, targeting atmospheric modelling, in which even minor changes in arithmetic behaviour will cause simulations to diverge quickly. The possibility of equally valid simulations having differing outcomes means that standard techniques for comparing numerical accuracy are inappropriate. We use the Hellinger distance to compare statistical behaviour between reduced-precision CPU implementations to guide reconfigurable designs of a chaotic system, then analyse accuracy, performance and power efficiency of the resulting implementations. Our results show that with only a limited loss in accuracy corresponding to less than 10% uncertainty in input parameters, the throughput and energy efficiency of a single-precision chaotic system implemented on a Xilinx Virtex-6 SX475T Field Programmable Gate Array (FPGA) can be more than doubled.

Improved geophysical excitation of length-of-day constrained by Earth orientation parameters and satellite gravimetry products

NASA Astrophysics Data System (ADS)

Yu, Nan; Li, Jiancheng; Ray, Jim; Chen, Wei

2018-05-01

At time scales shorter than about two years, non-tidal LOD variations are mainly excited by angular momentum exchanges between the atmospheric, oceanic, and continental hydrological fluid envelopes and the underlying solid Earth. But, neither agreement among different geophysical models for the fluid dynamics nor consistency with geodetic observations of LOD has reached satisfactory levels. This is mainly ascribed to significant discrepancies and uncertainties in the theories and assumptions adopted by different modeling groups, in their numerical methods, and in the accuracy and coverage of global input data fields. Based on careful comparisons with more accurate geodetic measurements and satellite gravimetry products (from satellite laser ranging, SLR), observed length-of day (LOD) and C20 geopotential time series can provide strong constraints to evaluate or form combined geophysical models. In this study, wavelet decomposition is used to extract several narrow-band components to compare in addition to considering the total signals. We then make refinements to the least difference combination (LDC) method proposed by Chen et al. (2013b) to form multi-model geophysical excitations. Two combination variants, called the weighted mean combination (WMC2 and WMC4), are also evaluated. All the multi-model methods attempt to extract the best-modeled frequency components from each geophysical model by relying on geodetic excitation and the C20 series as references. The comparative performances of the three combinations LDC, WMC2 and WMC4 and the original single models are determined. We find that (1) the Estimating the Circulation and Climate of the Ocean (ECCO) and Max-Planck-Institute for Meteorology Ocean Model (MPIOM) give a more reliable view of the ocean redistributions than the Ocean Model for Circulation and Tides (OMCT) used by European Centre for Medium-Range Weather Forecasts (ECMWF), especially for the annual component; (2) C20 series from SLR can provide a rigorous constraint for the total matter excitation of the geophysical fluids, especially for broadband parts; (3) the Sea-Level Angular Momentum functions (SLAM) term, correcting for sea level effects (global mass balance) put forward by the Earth System Modelling group at GFZ German Research Centre for Geosciences (ESMGFZ), can significantly improve the Hydrospheric Effective Angular Momentum functions (HAM) matter terms; (4) the LDC/WMC combinations are much better than the original individual geophysical model excitations, reducing the magnitude of unexplained LOD excitations to roughly the 10 μs level; (5) the level of residual LOD variations after removing models or model combinations is remarkably invariant with respect to LOD periods between ˜2 months and ˜3 years, being 12 to 14 μs for the best original models and 7 to 12 μs for our combinations; (6) while differences between the IERS 14C04 and the JPL SPACE2015 geodetic LOD time series are not negligible, errors in both series are still not large compared to the geophysical models (for periods >2 months) so the impact on excitation studies is minimal except at semi-annual periods and usually 14C04 compares better with excitation models. The improved geophysical models are recommended to replace the original ones as they present overwhelming advantages.

Development of an Ultrasonication-Assisted Extraction Based HPLC With a Fluorescence Method for Sensitive Determination of Aflatoxins in Highly Acidic Hibiscus sabdariffa

PubMed Central

Liu, Xiaofei; Ying, Guangyao; Sun, Chaonan; Yang, Meihua; Zhang, Lei; Zhang, Shanshan; Xing, Xiaoyan; Li, Qian; Kong, Weijun

2018-01-01

The high acidity and complex components of Hibiscus sabdariffa have provided major challenges for sensitive determination of trace aflatoxins. In this study, sample pretreatment of H. sabdariffa was systematically developed for sensitive high performance liquid chromatography-fluorescence detection (HPLC-FLD) after ultrasonication-assisted extraction, immunoaffinity column (IAC) clean-up and on-line post-column photochemical derivatization (PCD). Aflatoxins B1, B2, G1, G2 were extracted from samples by using methanol/water (70:30, v/v) with the addition of NaCl. The solutions were diluted 1:8 with 0.1 M phosphate buffer (pH 8.0) to negate the issues of high acidity and matrix interferences. The established method was validated with satisfactory linearity (R > 0.999), sensitivity (limits of detection (LODs) and limits of quantitation (LOQs) of 0.15–0.65 and 0.53–2.18 μg/kg, respectively), precision (RSD <11%), stability (RSD of 0.2–3.6%), and accuracy (recovery rates of 86.0–102.3%), which all met the stipulated analytical requirements. Analysis of 28 H. sabdariffa samples indicated that one sample incubated with Aspergillus flavus was positive with aflatoxin B1 (AFB1) at 3.11 μg/kg. The strategy developed in this study also has the potential to reliably extract and sensitively detect more mycotoxins in other complex acidic matrices, such as traditional Chinese medicines, foodstuffs, etc. PMID:29681848

A simple, sensitive and rapid isocratic reversed-phase high-performance liquid chromatography method for determination and stability study of curcumin in pharmaceutical samples

PubMed Central

Amanolahi, Farjad; Mohammadi, Ali; Kazemi Oskuee, Reza; Nassirli, Hooriyeh; Malaekeh-Nikouei, Bizhan

2017-01-01

Objective: This study was designed to develop and validate a new reversed-phase high-performance liquid chromatography (RP-HPLC) method based on Q2 (R1) International Conference on Harmonization (ICH) guideline for determination of curcumin in pharmaceutical samples. Materials and Methods: The HPLC instrument method was optimized with isocratic elution with acetonitrile: ammonium acetate (45:55, v/v, pH 3.5), C18 column (150 mm×4.6 mm×5 µm particle size) and a flow rate of 1 ml/min in ambient condition and total retention time of 17 min. The volume of injection was set at 20 µl and detection was recorded at 425 nm. The robustness of the method was examined by changing the mobile phase composition, mobile phase pH, and flow rate. Results: The method was validated with respect to precision, accuracy and linearity in a concentration range of 2-100 µg/ml. The limit of detection (LOD) and limit of quantification (LOQ) were 0.25 and 0.5 µg/ml, respectively. The percentage of recovery was 98.9 to 100.5 with relative standard deviation (RSD) < 0.638%. Conclusion: The method was found to be simple, sensitive and rapid for determination of curcumin in pharmaceutical samples and had enough sensitivity to detect degradation product of curcumin produced under photolysis and hydrolysis stress condition. PMID:29062806

Quantification of melamine in drinking water and wastewater by micellar liquid chromatography.

PubMed

Beltrán-Martinavarro, Beatriz; Peris-Vicente, Juan; Rambla-Alegre, Maria; Marco-Peiró, Sergio; Esteve-Romero, Josep; Carda-Broch, Samuel

2013-01-01

Because of the large potential health impact caused by deliberate contamination with the synthetic chemical melamine of different products for human and animal consumption, the World Health Organization and the Food and Agriculture Organization of the United Nations provided a range of recommendations in order to facilitate obtaining needed data, among which was the determination of the background levels of melamine in drinking water and wastewater (December 4, 2008). A chromatographic procedure using a C18 column, a micellar mobile phase consisting of sodium dodecyl sulfate (0.1 M), and 1-propanol (7.5%) buffered at pH 3, and detection by absorbance at 210 nm is reported in this paper for the quantification of melamine in drinking water and wastewater. Samples were filtered and directly injected into the chromatographic system, thus avoiding an extraction procedure. The optimal mobile phase composition was obtained by a chemometrics approach that considered the retention factor, efficiency, and peak shape. Melamine was eluted in about 6.2 min without interferences. Validation was performed following U.S. Food and Drug Administration guidelines. The analytical parameters studied were linearity (0.03-5 microg/mL, R2 = 0.998), LOD (13 nglmL), intraday and interday accuracy (between 4.1 and 12.2%), intraday and interday precision (less than 14.8%), and robustness (RSD < 5.1% for retention time and <9.0% for area). The proposed methodology was successfully applied for analysis of local wastewater and drinking water, in which no melamine was found.

New Sensitive Kinetic Spectrophotometric Methods for Determination of Omeprazole in Dosage Forms

PubMed Central

Mahmoud, Ashraf M.

2009-01-01

New rapid, sensitive, and accurate kinetic spectrophotometric methods were developed, for the first time, to determine omeprazole (OMZ) in its dosage forms. The methods were based on the formation of charge-transfer complexes with both iodine and 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ). The variables that affected the reactions were carefully studied and optimized. The formed complexes and the site of interaction were examined by UV/VIS, IR, and 1H-NMR techniques, and computational molecular modeling. Under optimum conditions, the stoichiometry of the reactions between OMZ and the acceptors was found to be 1 : 1. The order of the reactions and the specific rate constants were determined. The thermodynamics of the complexes were computed and the mechanism of the reactions was postulated. The initial rate and fixed time methods were utilized for the determination of OMZ concentrations. The linear ranges for the proposed methods were 0.10–3.00 and 0.50–25.00 μg mL−1 with the lowest LOD of 0.03 and 0.14 μg mL−1 for iodine and DDQ, respectively. Analytical performance of the methods was statistically validated; RSD was <1.25% for the precision and <1.95% for the accuracy. The proposed methods were successfully applied to the analysis of OMZ in its dosage forms; the recovery was 98.91–100.32% ± 0.94–1.84, and was found to be comparable with that of reference method. PMID:20140076

Development of an Ultrasonication-Assisted Extraction Based HPLC With a Fluorescence Method for Sensitive Determination of Aflatoxins in Highly Acidic Hibiscus sabdariffa.

PubMed

Liu, Xiaofei; Ying, Guangyao; Sun, Chaonan; Yang, Meihua; Zhang, Lei; Zhang, Shanshan; Xing, Xiaoyan; Li, Qian; Kong, Weijun

2018-01-01

The high acidity and complex components of Hibiscus sabdariffa have provided major challenges for sensitive determination of trace aflatoxins. In this study, sample pretreatment of H. sabdariffa was systematically developed for sensitive high performance liquid chromatography-fluorescence detection (HPLC-FLD) after ultrasonication-assisted extraction, immunoaffinity column (IAC) clean-up and on-line post-column photochemical derivatization (PCD). Aflatoxins B 1 , B 2 , G 1 , G 2 were extracted from samples by using methanol/water (70:30, v/v ) with the addition of NaCl. The solutions were diluted 1:8 with 0.1 M phosphate buffer (pH 8.0) to negate the issues of high acidity and matrix interferences. The established method was validated with satisfactory linearity ( R > 0.999), sensitivity (limits of detection (LODs) and limits of quantitation (LOQs) of 0.15-0.65 and 0.53-2.18 μg/kg, respectively), precision (RSD <11%), stability (RSD of 0.2-3.6%), and accuracy (recovery rates of 86.0-102.3%), which all met the stipulated analytical requirements. Analysis of 28 H. sabdariffa samples indicated that one sample incubated with Aspergillus flavus was positive with aflatoxin B 1 (AFB 1 ) at 3.11 μg/kg. The strategy developed in this study also has the potential to reliably extract and sensitively detect more mycotoxins in other complex acidic matrices, such as traditional Chinese medicines, foodstuffs, etc.

Evaluation of boldenone formation and related steroids transformations in veal faeces by liquid chromatography/tandem mass spectrometry.

PubMed

Arioli, Francesco; Gavinelli, Matteo P; Fracchiolla, Maria L; Casati, Alessio; Fidani, Marco; Ferrer, Emilia; Pompa, Giuseppe

2008-01-01

It is established that bovine urine can result positive for boldenone and androstadienedione in consequence of faecal contamination. The simple transfer of steroids to urine is one minor aspect of faecal contamination. A high de novo production of steroids in faeces after deposition and in faeces-contaminated urine is almost certainly due to microbial activity, although the precursor compounds and transformations leading to the presence of these illegal steroids are unclear. We developed a simple in vitro method - incubation of faecal matter suspended in 0.9% saline - to induce steroid transformations in faeces, and analyzed the products by liquid chromatography/tandem mass spectrometry, without the need for prior extraction. Norethandrolone was the internal standard. The linearity (R(2): 0.987-0.999), sensitivity (LODs: 0.3 to 1.0 ng/mL; LOQs: 1.0 to 3.0 ng/mL), precision (intra-day CVs: 2.6-8.2; inter-day CVs: 4.5-11.5) and accuracy (percentage recovery: 89-120%) were calculated for the studied steroids. Androstenedione, androstadienedione, alpha- and beta-boldenone, testosterone and epitestosterone transformations were investigated. Mutual interconversion of steroids was observed, although 17beta-hydroxy steroids had low stability compared with 17alpha-hydroxy and 17-keto steroids. The results suggest that this simple in vitro system may be an effective way of studying hormone transformations in faeces and, after analogue studies, in faeces-contaminated urine. Copyright (c) 2007 John Wiley & Sons, Ltd.

HPTLC method for the simultaneous determination of four indole alkaloids in Rauwolfia tetraphylla: a study of organic/green solvent and continuous/pulse sonication.

PubMed

Gupta, Shikha; Shanker, Karuna; Srivastava, Santosh K

2012-07-01

A new validated high-performance thin-layer chromatographic (HPTLC) method has been developed for the simultaneous quantitation of four antipsychotic indole alkaloids (IAs), reserpiline (RP, 1), α-yohimbine (YH, 2), isoreserpiline (IRP, 3) and 10-methoxy tetrahydroalstonine (MTHA, 4) as markers in the leaves of Rauwolfia tetraphylla. Extraction efficiency of the targeted IAs from the leaf matrix with organic and ecofriendly (green) solvents using percolation, ultrasonication and microwave techniques were studied. Non-ionic surfactants, viz. Triton X-100, Triton X-114 and Genapol X-80 were used for extraction and no back-extraction or liquid chromatographic steps were used to remove the targeted IAs from the surfactant-rich extractant phase. The optimized cloud point extraction was found a potentially useful methodology for the preconcentration of the targeted IAs. The separation was achieved on silica gel 60F(254) HPTLC plates using hexane-ethylacetate-methanol (5:4:1, v/v/v) as mobile phase. The quantitation of IAs (1-4) was carried out using the densitometric reflection/absorption mode at 520 nm after post chromatographic derivatization using Dragendorff's reagent. The method was validated for peak purity, precision, accuracy, robustness, limit of detection (LOD) and quantitation (LOQ). Method specificity was confirmed using retention factor (R(f)) and visible spectral (post chromatographic scan) correlation of marker compounds in the samples and standard tracks. Copyright © 2012 Elsevier B.V. All rights reserved.

A Validated Stability-Indicating RP-UPLC Method for Simultaneous Determination of Desloratadine and Sodium Benzoate in Oral Liquid Pharmaceutical Formulations.

PubMed

Kumar, Navneet; Sangeetha, Dhanaraj; Reddy, Pingili Sunil; Prakash, Lakkireddy

2012-01-01

A novel, sensitive and selective stability-indicating gradient reverse phase ultra performance liquid chromatographic method was developed and validated for the quantitative determination of desloratadine and sodium benzoate in pharmaceutical oral liquid formulation. The chromatographic separation was achieved on Acquity BEH C8 (100 mm × 2.1 mm) 1.7 μm column by using mobile phase containing a gradient mixture of solvent A (0.05 M KH(2)PO(4) and 0.07 M triethylamine, pH 3.0) and B (50:25:25 v/v/v mixture of acetonitrile, methanol and water) at flow rate of 0.4 mL/min. Column temperature was maintained at 40°C and detection was carried out at a wavelength of 272 nm. The described method shows excellent linearity over a range of 0.254 μg/mL to 76.194 μg/mL for desloratadine and 1.006 μg/mL to 301.67 μg/mL for sodium benzoate. The correlation coefficient for desloratadine and sodium benzoate was more than 0.999. To establish stability-indicating capability of the method, drug product was subjected to the stress conditions of acid, base, oxidative, hydrolytic, thermal and photolytic degradation. The degradation products were well resolved from desloratadine and sodium benzoate. The developed method was validated as per international ICH guidelines with respect to specificity, linearity, LOD, LOQ, accuracy, precision and robustness.

Validated semiquantitative/quantitative screening of 51 drugs in whole blood as silylated derivatives by gas chromatography-selected ion monitoring mass spectrometry and gas chromatography electron capture detection.

PubMed

Gunnar, Teemu; Mykkänen, Sirpa; Ariniemi, Kari; Lillsunde, Pirjo

2004-07-05

A comprehensively validated procedure is presented for simultaneous semiquantitative/quantitative screening of 51 drugs of abuse or drugs potentially hazardous for traffic safety in serum, plasma or whole blood. Benzodiazepines (12), cannabinoids (3), opioids (8), cocaine, antidepressants (13), antipsychotics (5) and antiepileptics (2) as well as zolpidem, zaleplon, zopiclone, meprobamate, carisoprodol, tizanidine and orphenadrine and internal standard flurazepam, were isolated by high-yield liquid-liquid extraction (LLE). The dried extracts were derivatized by two-step silylation and analyzed by the combination of two different gas chromatographic (GC) separations with both electron capture detection (ECD) and mass spectrometry (MS) operating in a selected ion-monitoring (SIM) mode. Quantitative or semiquantitative results were obtained for each substance based on four-point calibration. In the validation tests, accuracy, reproducibility, linearity, limit of detection (LOD) and limit of quantitation (LOQ), selectivity, as well as extraction efficiency and stability of standard stock solutions were tested, and derivatization was optimized in detail. Intra- and inter-day precisions were within 2.5-21.8 and 6.0-22.5%, and square of correlation coefficients of linearity ranged from 0.9896 to 0.9999. The limit of quantitation (LOQ) varied from 2 to 2000 ng/ml due to a variety of the relevant concentrations of the analyzed substances in blood. The method is feasible for highly sensitive, reliable and possibly routinely performed clinical and forensic toxicological analyses.

Solution-based calibration strategy for laser ablation-inductively coupled plasma-mass spectrometry using desolvating nebulizer system

NASA Astrophysics Data System (ADS)

Zhang, Guoxia; Li, Qing; Zhu, Yan; Wang, Zheng

2018-07-01

An additional quantification strategy using a desolvating nebulizer system (DNS) for solution-based calibration was developed. For quantitative analysis, laser ablation (LA) and DNS-generated aerosols were coupled using a "Y" connector and introduced into the inductively coupled plasma (ICP). These aerosols were also observed by scanning electron microscopy following collection on a silicon chip. Internal standards (108Ag, 64Cu, 89Y) were used to correct for the different aerosol transport efficiencies between the DNS and LA. The correlation coefficients of the calibration curves for all elements ranged from 0.9986 to 0.9999. Standard reference materials (NIST 610-616 and GBW08407-08411) were used to demonstrate the accuracy and precision of the method. The results were in good agreement with certified values, and the relative standard deviation (RSD) of most elements was <3%. The limits of detection (LODs) for 50Cr, 55Mn, 59Co, 60Ni, 66Zn, 89Y, 110Cd, 139La, 140Ce, 146Nd, 147Sm, 157Gd, 163Dy, 166Er, and 208Pb were 23, 3, 3, 19, 31, 4, 12, 0.4, 0.9, 0.1, 0.2, 2, 0.3, 0.4, and 21 ng/g, respectively, which were significantly better than those obtained by other methods. Further, this approach was applied for the analysis of multiple elements in biological tissues, and the results were in good agreement with those obtained using solution-based inductively coupled plasma-mass spectrometry (ICP-MS).

Qualitative and quantitative analysis of nine major compounds in the Bozhougyiqi-Tang using a high-performance liquid chromatography coupled with a diode array detector and electrospray ionization mass spectrometer

PubMed Central

Weon, Jin Bae; Ma, Jin Yeul; Yang, Hye Jin; Lee, Bohyoung; Yun, Bo-Ra; Ma, Choong Je

2013-01-01

Background: Bozhougyiqi-Tang (BZYQT) is of traditional herbal medicine used for enhancement of digestive capacity. Objective: An accurate and reliable simultaneous determination using a HPLC-DAD and ESI-MS was developed and validated for the qualitative and quantitative analysis of 9 major compounds, ferulic acid (1), naringin (2), hesperidin (3), decursinol (4), glycyrrhizin (5), saikosaponin A (6), 6-gingerol (7), ginsenoside Rg3 (8), decursin (9), in traditional herbal medicine ‘Bozhougyiqi-Tang.’ Materials and Methods: The chromatographic separation of 9 compounds was performed on a SHISEIDO C18 column (250 mm × 4.6 mm i.d., S-5 μm) using gradient elution with 0.1% trifluoroacetic acid and acetonitrile at a flow rate of 1.0 ml/min. The 9 compounds were identified based on peak retention time and UV spectrum and MS data of these compounds. Results: This developed method showed good linearity (R2 > 0.999). The LOD and LOQ of the major compounds were less than 0.09 and 0.28 μg/ml, respectively. The intra - day and inter - day RSD values were within 2.06% and 1.64%, respectively. The mean recoveries were from 92.10% to 108.56% with less than 1.88%. The results indicated that established method had good precision and accuracy. Conclusion: The new method was successfully applied to the simultaneous analysis of 9 compounds in Bozhougyiqi-Tangs samples. PMID:23930013

HPLC-ELSD Quantification and Centrifugal Partition Chromatography Isolation of 8-O-Acetylharpagide from Oxera coronata (Lamiaceae).

PubMed

Remeur, Camille; Le Borgne, Erell; Gauthier, Léa; Grougnet, Raphaël; Deguin, Brigitte; Poullain, Cyril; Litaudon, Marc

2017-05-01

Iridoid glycosides possess highly functionalised monoterpenoid aglycon with several contiguous stereocentres. For the most common, they are often present in quantities reaching several percentage of the fresh plant weight, and thus they may be regarded as starting material for the synthesis of a number of new chiral and bioactive molecules. To quantify and to isolate 8-O-acetylharpagide (AH) from several extracts of Oxera coronata R.P.J. de Kok, a Lamiaceae species endemic to New Caledonia, using HPLC-ELSD (evaporative light scattering detector) and centrifugal partition chromatography (CPC). Oxera coronata produces high amounts of AH in leaves, twigs and fruits. Water and methanol extracts of these plant parts were prepared. The content of AH in each extract was quantified by HPLC-ELSD, using acetonitrile-water (+0.1% formic acid) gradient elution. The HPLC method was validated for precision, linearity, limit of detection (LOD), limit of quantification (LOQ) and accuracy. A ternary solvent system ethyl acetate/n-propanol/water (3:2:5, v/v/v) was selected and applied to recover the target compound using Spot CPC from the leaves aqueous extract. HPLC-ELSD analysis followed by CPC purification led to the efficient isolation of AH from O. coronata leaves aqueous extract. HPLC-ELSD has proven to be a well-adapted detection and quantification method for iridoid glycosides, while CPC confirmed to be an efficient technique for the isolation of polar compounds. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Natural deep eutectic solvents as eco-friendly and sustainable dilution medium for the determination of residual organic solvents in pharmaceuticals with static headspace-gas chromatography.

PubMed

Wang, Meilian; Fang, Sheng; Liang, Xianrui

2018-06-04

Reported here is a simple and rapid static headspace gas chromatography (SHS-GC) method for the determination of trace solvents including ethanol, isopropanol, n-butanol, 1,4-dioxane, tetrahydrofuran, acetonitrile, methanol and acetone which commonly used in drug production process. Natural deep eutectic solvents (NADESs) are firstly used as the matrix medium for this method, which provided high sensitivity for residual solvents detection. With the optimized method, validation experiments were performed and the data showed excellent linearity for all the solvents (R 2 ≥ 0.999, n = 7). The limits of detection (LOD) for ethanol, isopropanol, n-butanol, 1,4-dioxane, tetrahydrofuran, acetonitrile, methanol and acetone are 0.09, 0.08, 0.07, 0.11, 0.06, 0.10, 0.12 and 0.08 μg g -1 , respectively. Accuracy was checked by a recovery experiment at three different levels, and the recoveries of the tested solvents were ranged from 94.3% to 105.4%. The relative standard deviation (RSD) of each solvent for intra- and inter-day precision is in the range of 0.85 to 3.65 and 1.51 to 4.53, respectively. The developed approach can be readily used for determination of the residual solvents in six active pharmaceutical ingredients including pramipexole dihydrochloride, rivaroxaban, lisinopril, ramipril, imatinib mesylate and sitagliptin. Copyright © 2018 Elsevier B.V. All rights reserved.

A Rapid LC-HRMS Method for the Determination of Domoic Acid in Urine Using a Self-Assembly Pipette Tip Solid-Phase Extraction

PubMed Central

Zhang, Yiping; Chen, Dawei; Hong, Zhuan

2015-01-01

In this study, we developed a self-assembly pipette tip solid-phase extraction (PTSPE) method using a high molecular weight polymer material (PAX) as the adsorbent for the determination of domoic acid (DA) in human urine samples by liquid chromatography high-resolution mass spectrometry (LC-HRMS) analysis. The PTSPE cartridge, assembled by packing 9.1 mg of PAX as sorbent into a 200 μL pipette tip, showed high adsorption capacity for DA owing to the strong cationic properties of PAX. Compared with conventional SPE, the PTSPE is simple and fast, and shows some advantages in the aspects of less solvent consumption, low cost, the absence of the evaporation step, and short time requirement. All the parameters influencing the extraction efficiency such as pH, the amount of sorbent, the number of aspirating/dispensing cycles, and the type and volume of eluent in PTSPE were carefully investigated and optimized. Under the optimized conditions, the limit of detection (LOD) and limit of quantification (LOQ) values of DA were 0.12 μg/L and 0.37 μg/L respectively. The extraction recoveries of DA from the urine samples spiked at four different concentrations were in a range from 88.4% to 102.5%. The intra- and inter-day precisions varied from 2.1% to 7.6% and from 2.6% to 12.7%, respectively. The accuracy ranged from −1.9% to −7.4%. PMID:26729165

A rapid and highly sensitive UPLC-MS/MS method using pre-column derivatization with 2-picolylamine for intravenous and percutaneous pharmacokinetics of valproic acid in rats.

PubMed

Joo, Kyung-Mi; Choi, Dalwoong; Park, Yang-Hui; Yi, Chang-Geun; Jeong, Hye-Jin; Cho, Jun-Cheol; Lim, Kyung-Min

2013-11-01

A rapid, highly sensitive and specific ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) for the detection of valproic acid (VPA) in rat plasma following the topical application was developed and validated. This method was carried out with pre-column derivatization using 2-picolylamine (PA) which reacts with the carboxylic acid group of VPA. The derivatization was completed in 10min and the resulting PA-VPA derivative enabled the sensitive detection of VPA in selected reaction monitoring (SRM) mode. Sample preparation was done with simple liquid-liquid extraction and chromatographic separation was achieved within 5min on a C18 column using a gradient elution with the mobile phase of 2mM ammonium formate containing 0.1% formic acid and methanol. The standard curves were linear over the concentration range of 0.07-200μg/mL with a correlation coefficient higher than 0.99. The limit of detection (LOD) and the lower limit of quantification (LLOQ) was 0.03 and 0.07μg/mL, respectively with 100μL of plasma sample. The intra- and inter-day precisions were measured to be below 10.7% and accuracies were within the range of 94.1-115.9%. The validated method was successfully applied to the pharmacokinetics of VPA in the rat following topical and intravenous applications. Copyright © 2013 Elsevier B.V. All rights reserved.

Rapid liquid chromatography-tandem mass spectrometry analysis of 4-hydroxynonenal for the assessment of oxidative degradation and safety of vegetable oils.

PubMed

Gabbanini, Simone; Matera, Riccardo; Valvassori, Alice; Valgimigli, Luca

2015-04-15

A novel method for the UHPLC-MS/MS analysis of (E)-4-hydroxynonenal (4-HNE) is described. The method is based on derivatization of 4-HNE with pentafluorophenylhydrazine (1) or 4-trifluoromethylphenylhydrazine (2) in acetonitrile in the presence of trifluoroacetic acid as catalyst at room temperature and allows complete analysis of one sample of vegetable oil in only 21 min, including sample preparation and chromatography. The method involving hydrazine 1, implemented in an ion trap instrument with analysis of the transition m/z 337→154 showed LOD=10.9 nM, average accuracy of 101% and precision ranging 2.5-4.0% RSD intra-day (2.7-4.1% RSD inter-day), with 4-HNE standard solutions. Average recovery from lipid matrices was 96.3% from vaseline oil, 91.3% from sweet almond oil and 105.3% from olive oil. The method was tested on the assessment of safety and oxidative degradation of seven samples of dietary oil (soybean, mixed seeds, corn, peanut, sunflower, olive) and six cosmetic-grade oils (avocado, blackcurrant, apricot kernel, echium, sesame, wheat germ) and effectively detected increased 4-HNE levels in response to chemical (Fenton reaction), photochemical, or thermal stress and aging, aimed at mimicking typical oxidation associated with storage or industrial processing. The method is a convenient, cost-effective and reliable tool to assess quality and safety of vegetable oils. Copyright © 2015 Elsevier B.V. All rights reserved.

Development of QuEChERS-based extraction and liquid chromatography-tandem mass spectrometry method for quantifying flumethasone residues in beef muscle.

PubMed

Park, Ki Hun; Choi, Jeong-Heui; Abd El-Aty, A M; Cho, Soon-Kil; Park, Jong-Hyouk; Kwon, Ki Sung; Park, Hee Ra; Kim, Hyung Soo; Shin, Ho-Chul; Kim, Mi Ra; Shim, Jae-Han

2012-12-01

A rapid, specific, and sensitive method based on liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM) was developed and validated to quantify flumethasone residues in beef muscle. Methods were compared between the original as well as the EN quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based extraction. Good linearity was achieved at concentration levels of 5-30 μg/kg. Estimated recovery rates at spiking levels of 5 and 10 μg/kg ranged from 72.1 to 84.6%, with relative standard deviations (RSDs)<7%. The results of the inter-day study, which was performed by fortifying beef muscle samples (n=18) on 3 separate days, showed an accuracy of 93.4-94.4%. The precision (expressed as relative standard deviation values) for the inter-day variation at two levels of fortification (10 and 20 μg/kg) was 1.9-5.2%. The limit of detection (LOD) and limit of quantitation (LOQ) were 1.7 and 5 μg/kg, at signal-to-noise ratios (S/Ns) of 3 and 10, respectively. The method was successfully applied to analyze real samples obtained from large markets throughout the Korean Peninsula. The method proved to be sensitive and reliable and, thus, rendered an appropriate means for residue analysis studies. Copyright © 2012 Elsevier Ltd. All rights reserved.

Concentrations of nandrolone metabolites in urine after the therapeutic administration of an ophthalmic solution.

PubMed

Avois, Lidia; Mangin, Patrice; Saugy, Martial

2007-05-09

Nandrolone, an anabolic steroid, is used for the treatment of several diseases and is available in various pharmaceutical formulations. The most widely used pharmaceutical formulation is Deca-Durabolin, but other products, such as Keratyl eye drops solution, are also currently administered. Nandrolone is one of the most abused anabolic steroid in sports. Analyses for this anabolic steroid according to the World Anti-Doping Agency (WADA) protocol are based on the identification of the nandrolone two main urinary metabolites which, in humans, are glucuronides of 19-norandrosterone and 19-noretiocholanolone. A positive cut off limit of 2 ng/mL has been set by the anti-doping code for the first metabolite, 19-norandrosterone. In this preliminary study, an eye drops solution (Keratyl) containing a therapeutic dose of a nandrolone sodium sulphate was administered to several male volunteers during 3 days and urines were collected during 3 weeks. Surprisingly, contrary to all expectations, the urinary concentrations measured in urines reached 450 ng/mL and 70 ng/mL for norandrosterone and noretiocholanolone, respectively. Moreover, concentration levels near to 2 ng/mL were found, more than 2 weeks after the last administration, depending on individual metabolism. Inter-variability as well as intra-variability of nandrolone excretion kinetic, regarding this particular administration mode, were also evaluated. Quantification of nandrolone metabolites was performed by GC-MS. The method was previously validated in terms of specificity, precision, linearity, LOD, LOQ, robustness, accuracy and the expanded uncertainty was also evaluated.

Determination of ketamine and its major metabolite, norketamine, in urine and plasma samples using microextraction by packed sorbent and gas chromatography-tandem mass spectrometry.

PubMed

Moreno, Ivo; Barroso, Mário; Martinho, Ana; Cruz, Angelines; Gallardo, Eugenia

2015-11-01

Ketamine is a club drug widely abused for its hallucinogenic effects, being also used as a "date-rape" drug in recent years. We have developed an analytical method using gas chromatography-tandem mass spectrometry (GC-MS/MS) for the identification and quantification of ketamine and its major metabolite in urine and plasma. No derivatization step is needed to accomplish analysis. The compounds were extracted from 0.25mL of sample using microextraction by packed sorbent on mixed mode (M1) cartridges. Calibration curves were linear in the range of 10-250ng/mL for urine and 10-500ng/mL for plasma, with determination coefficients higher than 0.99. The limit of detection (LOD) was 5ng/mL for both compounds in both specimens. Recoveries ranged from 63 to 101%, while precision and accuracy were below 14% and 15%, respectively. These low limits of detection and the quite high recoveries obtained, in very low sample amounts, allow detecting small quantities of the compounds, making this procedure suitable for those laboratories performing routine analysis in the field of forensic toxicology. Compared with existing methods, the herein described procedure is fast, since no derivatization step is required, and cost effective for the quantification of ketamine and norketamine in biological specimens by gas chromatography. Copyright © 2015 Elsevier B.V. All rights reserved.

Application of 3-methylbenzothiazolin-2-one hydrazone for the quantitative spectrophotometric determination of oxcarbazepine in pharmaceuticals with cerium(IV) and periodate

NASA Astrophysics Data System (ADS)

Rajendraprasad, N.; Basavaiah, K.; Vinay, K. B.

2012-09-01

Two simple, sensitive, selective, accurate, and cost-effective spectrophotometric methods are described for the assay of oxcarbazepine (OXC) in bulk drug and in tablets. The methods are based on an oxidative coupling reaction involving OXC, 3-methylbenzothiazolin-2-one hydrazone (MBTH), and cerium(IV) sulfate at pH 4.28 ± 0.07 (method A) or sodium periodate at pH > 4.0 (method B) to form an orange colored product with an absorption maximum at 450 nm. Under optimized experimental conditions, the calibration graphs are linear over the ranges of 4-80 and 2-32 μg/ml for methods A and B, respectively, with correlation coefficient (r) values of 0.9984 and 0.9976. The apparent molar absorptivity values are 3.13ṡ103 and 9.13ṡ103 l/molṡcm for methods A and B, respectively. The other optical characteristics such as Sandell's sensitivity, limits of detection (LOD) and quantification (LOQ) values are also reported. The accuracy and precision of the methods were evaluated based on intra-day and inter-day variations. The proposed methods were successfully applied to the determination of OXC in tablets: the results were comparable with the published data obtained using the reference method. The reaction stoichiometry of OXC with MBTH (1:1 in method A and 1:2 in method B) was also evaluated using the limiting logarithmic method, and a possible reaction pathway is presented for the both methods.

Highly Sensitive and Validated Spectrophotometric Technique for the Assay of Some Antidepressant Drugs

NASA Astrophysics Data System (ADS)

Deepakumari, H. N.; Prashanth, M. K.; Kumar, B. C. Vasantha; Revanasiddappa, H. D.

2015-01-01

The present paper describes a simple, rapid, reproducible, and highly sensitive spectrophotometric method for the determination of the tricyclic antidepressant drugs: amitriptyline hydrochloride (AMT), imipramine hydrochloride (IMH), clomipramine hydrochloride (CPH) and desipramine hydrochloride (DPH) in pure and in pharmaceutical preparations. The method is based on the bromination of the above drugs with known excess of bromine. The unreacted bromine is determined based on its ability to bleach the dye methyl red quantitatively at 520 nm. Regression analysis of Beer-Lambert plots showed a good correlation in the concentration range 0.0-2.5, 0-1.4, 0-1.4, and 0-1.0 μg/ml for AMT, IMH, CPH, and DPH, respectively. The molar absorptivity values were found to be 0.65 × 105, 1.41 × 105, 1.93 × 105, and 2.96 × 105l/mol/cm, with the corresponding Sandell's sensitivity values were 0.0048, 0.0022, 0.0018, and 0.0010 μg/cm2 for AMT, IMH, CPH, and DPH, respectively. The limits of detection (LOD) and quantification (LOQ) are also reported for the developed method. Intra- and inter-day accuracy and precision was established according to the current ICH guidelines. Application of the procedure to the analysis of various pharmaceutical preparations gave reproducible and accurate results. Further, the validity of the proposed method was confirmed by applying the standard addition technique, and the results obtained are in good agreement with those obtained by the official method.

Development and validation of a stability-indicating size-indicating size-exclusion LC method for the determination of rhIFN-alpha2a in pharmaceutical formulations.

PubMed

Zimmermann, Estevan Sonego; da Silva, Lucélia Magalhães; Calegari, Guilherme Zanini; Stamm, Fernanda Pavani; Souto, Ricardo Bizogne; Dalmora, Sérgio Luiz

2013-01-01

A size-exclusion LC method was validated for the determination of interferon-a2a (rhlFN-alpha2a) in pharmaceutical formulations without interference from human serum albumin. Chromatographic separation was performed on a BioSep-SEC-S 2000 column (300 x 7.8 mm id). The mobile phase consisted of 0.001 M monobasic potassium phosphate, 0.008 M sodium phosphate dibasic; 0.2 M sodium chloride buffer, pH 7.4, run at a gradient flow rate and using photodiode array detection at 214 nm, was used. Chromatographic separation was achieved with a retention time of 17.2 min, and the analysis was linear over the concentration range of 1.98 to 198 microg/mL (r2 = 0.9996). The accuracy was 101.39%, with bias lower than 1.67%. The LOD and LOQ were 0.87 and 1.98 microg/mL, respectively. Moreover, method validation demonstrated acceptable results for precision and robustness. The method was applied to the assessment of rhlFN-alpha2a and related proteins in biopharmaceutical dosage forms, and the content/potencies were correlated to those given by a validated RP-LC method and an in vitro bioassay. It was concluded that use of the methods in conjunction allows a great improvement in monitoring stability and QC, thereby ensuring the therapeutic efficacy of the biotechnology-derived medicine.

Novel liquid chromatography method based on linear weighted regression for the fast determination of isoprostane isomers in plasma samples using sensitive tandem mass spectrometry detection.

PubMed

Aszyk, Justyna; Kot, Jacek; Tkachenko, Yurii; Woźniak, Michał; Bogucka-Kocka, Anna; Kot-Wasik, Agata

2017-04-15

A simple, fast, sensitive and accurate methodology based on a LLE followed by liquid chromatography-tandem mass spectrometry for simultaneous determination of four regioisomers (8-iso prostaglandin F 2α , 8-iso-15(R)-prostaglandin F 2α , 11β-prostaglandin F 2α , 15(R)-prostaglandin F 2α ) in routine analysis of human plasma samples was developed. Isoprostanes are stable products of arachidonic acid peroxidation and are regarded as the most reliable markers of oxidative stress in vivo. Validation of method was performed by evaluation of the key analytical parameters such as: matrix effect, analytical curve, trueness, precision, limits of detection and limits of quantification. As a homoscedasticity was not met for analytical data, weighted linear regression was applied in order to improve the accuracy at the lower end points of calibration curve. The detection limits (LODs) ranged from 1.0 to 2.1pg/mL. For plasma samples spiked with the isoprostanes at the level of 50pg/mL, intra-and interday repeatability ranged from 2.1 to 3.5% and 0.1 to 5.1%, respectively. The applicability of the proposed approach has been verified by monitoring of isoprostane isomers level in plasma samples collected from young patients (n=8) subjected to hyperbaric hyperoxia (100% oxygen at 280kPa(a) for 30min) in a multiplace hyperbaric chamber. Copyright © 2017 Elsevier B.V. All rights reserved.

Development and validation of a high performance liquid chromatographic method for the separation of exo and endo isomers of granatamine (9-methyl-9-azabicyclo[3.3.1]nonan-3-amine); a key intermediate of granisetron.

PubMed

Krishna, S Radha; Babu, P Suresh; Rao, B M; Rao, N Someswara

2009-12-01

A simple and accurate high-performance liquid chromatographic method was developed for the determination of exo-9-methyl-9-azabicyclo[3.3.1]nonan-3-amine in endo-9-methyl-9-azabicyclo[3.3.1]nonan-3-amine, commercially known as grantamine and used as a key intermediate in the preparation of granisetron bulk drug. Chromatographic separation of the exo and endo isomers of 9-methyl-9-azabicyclo[3.3.1]nonan-3-amine was achieved on an Inertsil C8 column using a mobile phase containing 0.3% trifluoroacetic acid. The resolution between the two isomers was found to be more than 4. The limit of detection (LOD) and limit of quantification (LOQ) of exo isomer were 0.8 and 2.5 microg x mL(-1) respectively, for a 10 microL injection volume. The percentage recovery of exo-isomer ranged from 99 to 102% w/w in the endo-9-methyl-9-azabicyclo[3.3.1]nonan-3-amine sample. The test solution and mobile phase were observed to be stable up to 48 h after preparation. The validated method yielded good results for precision, linearity, accuracy, robustness and ruggedness. The proposed method was found to be suitable and accurate for the quantitative determination of exo-isomer in bulk samples of endo-9-methyl-9-azabicyclo[3.3.1]nonan-3-amine.

Multiplexed detection of tumor markers with multicolor quantum dots based on fluorescence polarization immunoassay.

PubMed

Tian, Jianniao; Zhou, Liujin; Zhao, Yanchun; Wang, Yuan; Peng, Yan; Zhao, Shulin

2012-04-15

A multicolor quantum dot (QD)-based nanosensor for multiplex detection of two tumor markers in a homogeneous format based on fluorescence polarization immunoassay was proposed. QDs520 and QDs620 were labeled alpha-fetoprotein(α-AFP) and carcinoembryonic antigen (CEA), respectively. After separated and purified by ultrafiltration, they were used in fluorescence polarization immunoassay for the simultaneous detection of human serum alpha-fetoprotein and carcinoembryonic antigen. Under the optimal conditions, the multi-analyte immunosensor had a wide linear range (from 0.5 ng mL(-1) to 500 ng mL(-1)) for both two tumor markers and good correlation (0.996 for α-AFP and 0.993 for CEA). The detection limits (LOD) were 0.36 ng mL(-1) for CEA and 0.28 ng mL(-1) for α-AFP (S/N=3). The carcinoembryonic antigen and fetoprotein in clinical serum samples were simultaneously detected. The results from 28 serum samples had a good agreement with enzyme-linked immunosorbent assay (ELISA). The relative standard deviation and the recovery suggested that the precision and the accuracy of this analytical method were satisfactory. This strategy with high sensitivity, good specificity, easy procedures and short analysis time shows great promise for clinical diagnoses and basic discovery. The application of QDs with longer fluorescence lifetime and small fluorescence polarization can be used for the determination of high molecular-weight substances which cannot be analyzed using dye fluorescence polarization immunoassay. Copyright © 2012 Elsevier B.V. All rights reserved.

Relationships Between the Performance of Time/Frequency Standards and Navigation/Communication Systems

NASA Technical Reports Server (NTRS)

Hellwig, H.; Stein, S. R.; Walls, F. L.; Kahan, A.

1978-01-01

The relationship between system performance and clock or oscillator performance is discussed. Tradeoffs discussed include: short term stability versus bandwidth requirements; frequency accuracy versus signal acquisition time; flicker of frequency and drift versus resynchronization time; frequency precision versus communications traffic volume; spectral purity versus bit error rate, and frequency standard stability versus frequency selection and adjustability. The benefits and tradeoffs of using precise frequency and time signals are various levels of precision and accuracy are emphasized.

An Application to the Prediction of LOD Change Based on General Regression Neural Network

NASA Astrophysics Data System (ADS)

Zhang, X. H.; Wang, Q. J.; Zhu, J. J.; Zhang, H.

2011-07-01

Traditional prediction of the LOD (length of day) change was based on linear models, such as the least square model and the autoregressive technique, etc. Due to the complex non-linear features of the LOD variation, the performances of the linear model predictors are not fully satisfactory. This paper applies a non-linear neural network - general regression neural network (GRNN) model to forecast the LOD change, and the results are analyzed and compared with those obtained with the back propagation neural network and other models. The comparison shows that the performance of the GRNN model in the prediction of the LOD change is efficient and feasible.

Commissioning Procedures for Mechanical Precision and Accuracy in a Dedicated LINAC

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ballesteros-Zebadua, P.; Larrga-Gutierrez, J. M.; Garcia-Garduno, O. A.

2008-08-11

Mechanical precision measurements are fundamental procedures for the commissioning of a dedicated LINAC. At our Radioneurosurgery Unit, these procedures can be suitable as quality assurance routines that allow the verification of the equipment geometrical accuracy and precision. In this work mechanical tests were performed for gantry and table rotation, obtaining mean associated uncertainties of 0.3 mm and 0.71 mm, respectively. Using an anthropomorphic phantom and a series of localized surface markers, isocenter accuracy showed to be smaller than 0.86 mm for radiosurgery procedures and 0.95 mm for fractionated treatments with mask. All uncertainties were below tolerances. The highest contribution tomore » mechanical variations is due to table rotation, so it is important to correct variations using a localization frame with printed overlays. Mechanical precision knowledge would allow to consider the statistical errors in the treatment planning volume margins.« less

Comprehensive Numerical Analysis of Finite Difference Time Domain Methods for Improving Optical Waveguide Sensor Accuracy

PubMed Central

Samak, M. Mosleh E. Abu; Bakar, A. Ashrif A.; Kashif, Muhammad; Zan, Mohd Saiful Dzulkifly

2016-01-01

This paper discusses numerical analysis methods for different geometrical features that have limited interval values for typically used sensor wavelengths. Compared with existing Finite Difference Time Domain (FDTD) methods, the alternating direction implicit (ADI)-FDTD method reduces the number of sub-steps by a factor of two to three, which represents a 33% time savings in each single run. The local one-dimensional (LOD)-FDTD method has similar numerical equation properties, which should be calculated as in the previous method. Generally, a small number of arithmetic processes, which result in a shorter simulation time, are desired. The alternating direction implicit technique can be considered a significant step forward for improving the efficiency of unconditionally stable FDTD schemes. This comparative study shows that the local one-dimensional method had minimum relative error ranges of less than 40% for analytical frequencies above 42.85 GHz, and the same accuracy was generated by both methods.

Comparative analysis of EPA and DHA in fish oil nutritional capsules by GC-MS.

PubMed

Yi, Tao; Li, Shuk-Man; Fan, Jia-Yi; Fan, Lan-Lan; Zhang, Zhi-Feng; Luo, Pei; Zhang, Xiao-Jun; Wang, Jian-Gang; Zhu, Lin; Zhao, Zhong-Zhen; Chen, Hu-Biao

2014-12-13

Fish oil is a popular nutritional product consumed in Hong Kong. Eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) are the two main bioactive components responsible for the health benefits of fish oil. Market survey in Hong Kong demonstrated that various fish oil capsules with different origins and prices are sold simultaneously. However, these capsules are labelled with same ingredient levels, namely EPA 180 mg/g and DHA 120 mg/g. This situation makes the consumers very confused. To evaluate the quality of various fish oil capsules, a comparative analysis of the contents of EPA and DHA in fish oil is crucial. A gas chromatography-mass spectrometry (GC-MS) method was developed for identification and determination of EPA and DHA in fish oil capsules. A comprehensive validation of the developed method was conducted. Ten batches of fish oil capsules samples purchased from drugstores of Hong Kong were analyzed by using the developed method. The present method presented good sensitivity, precision and accuracy. The limits of detection (LOD) for EPA and DHA were 0.08 ng and 0.21 ng, respectively. The relative standard deviation (RSD) values of EPA and DHA for repeatability tests were both less than 1.05%; and the recovery for accuracy test of EPA and DHA were 100.50% and 103.83%, respectively. In ten fish oil samples, the contents of EPA ranged from 39.52 mg/g to 509.16 mg/g, and the contents of DHA ranged from 35.14 mg/g to 645.70 mg/g. The present method is suitable for the quantitative analysis of EPA and DHA in fish oil capsules. There is a significant variation in the contents of the quantified components in fish oil samples, and there is not a linear relationship between price and contents of EPA and DHA. Strict supervision of the labelling of the fish oil capsules is urgently needed.

Sensitive determination of sulfonamides in environmental water by capillary electrophoresis coupled with both silvering detection window and in-capillary optical fiber light-emitting diode-induced fluorescence detector.

PubMed

Ji, Hongyun; Wu, Yu; Duan, Zhijuan; Yang, Feng; Yuan, Hongyan; Xiao, Dan

2017-02-01

A new detector, silvering detection window and in-capillary optical fiber light-emitting diode-induced fluorescence detector (SDW-ICOF-LED-IFD), is introduced for capillary electrophoresis (CE). The strategy of the work was that half surface of the detection window was coated with silver mirror, which could reflect the undetected fluorescence to the photomultiplier tube to be detected, consequently enhancing the detection sensitivity. Sulfonamides (SAs) are important antibiotics that achieved great applications in many fields. However, they pose a serious threat on the environment and human health when they enter into the environment. The SDW-ICOF-LED-IFD-CE system was used to determine fluorescein isothiocyanate (FITC)-labeled sulfadoxine (SDM), sulfaguanidine (SGD) and sulfamonomethoxine sodium (SMM-Na) in environmental water. The detection results obtained by the SDW-ICOF-LED-IFD-CE system were compared to those acquired by the CE with in-capillary optical fiber light-emitting diode-induced fluorescence detection (ICOF-LED-IFD-CE). The limits of detection (LODs) of SDW-ICOF-LED-IFD-CE and ICOF-LED-IFD-CE were 1.0-2.0 nM and 2.5-7.7 nM (S/N = 3), respectively. The intraday (n = 6) and interday (n = 6) precision of migration time and corresponding peak area for both types of CE were all less than 0.86% and 3.68%, respectively. The accuracy of the proposed method was judged by employing standard addition method, and recoveries obtained were in the range of 92.5-102.9%. The results indicated that the sensitivity of the SDW-ICOF-LED-IFD-CE system was improved, and that its reproducibility and accuracy were satisfactory. It was successfully applied to analyze SAs in environmental water. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development and validation of a selective, sensitive and stability indicating UPLC-MS/MS method for rapid, simultaneous determination of six process related impurities in darunavir drug substance.

PubMed

A, Vijaya Bhaskar Reddy; Yusop, Zulkifli; Jaafar, Jafariah; Aris, Azmi B; Majid, Zaiton A; Umar, Khalid; Talib, Juhaizah

2016-09-05

In this study a sensitive and selective gradient reverse phase UPLC-MS/MS method was developed for the simultaneous determination of six process related impurities viz., Imp-I, Imp-II, Imp-III, Imp-IV, Imp-V and Imp-VI in darunavir. The chromatographic separation was performed on Acquity UPLC BEH C18 (50 mm×2.1mm, 1.7μm) column using gradient elution of acetonitrile-methanol (80:20, v/v) and 5.0mM ammonium acetate containing 0.01% formic acid at a flow rate of 0.4mL/min. Both negative and positive electrospray ionization (ESI) modes were operated simultaneously using multiple reaction monitoring (MRM) for the quantification of all six impurities in darunavir. The developed method was fully validated following ICH guidelines with respect to specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, precision, robustness and sample solution stability. The method was able to quantitate Imp-I, Imp-IV, Imp-V at 0.3ppm and Imp-II, Imp-III, and Imp-VI at 0.2ppm with respect to 5.0mg/mL of darunavir. The calibration curves showed good linearity over the concentration range of LOQ to 250% for all six impurities. The correlation coefficient obtained was >0.9989 in all the cases. The accuracy of the method lies between 89.90% and 104.60% for all six impurities. Finally, the method has been successfully applied for three formulation batches of darunavir to determine the above mentioned impurities, however no impurity was found beyond the LOQ. This method is a good quality control tool for the trace level quantification of six process related impurities in darunavir during its synthesis. Copyright © 2016 Elsevier B.V. All rights reserved.

Accuracy assessment of the Precise Point Positioning method applied for surveys and tracking moving objects in GIS environment

NASA Astrophysics Data System (ADS)

Ilieva, Tamara; Gekov, Svetoslav

2017-04-01

The Precise Point Positioning (PPP) method gives the users the opportunity to determine point locations using a single GNSS receiver. The accuracy of the determined by PPP point locations is better in comparison to the standard point positioning, due to the precise satellite orbit and clock corrections that are developed and maintained by the International GNSS Service (IGS). The aim of our current research is the accuracy assessment of the PPP method applied for surveys and tracking moving objects in GIS environment. The PPP data is collected by using preliminary developed by us software application that allows different sets of attribute data for the measurements and their accuracy to be used. The results from the PPP measurements are directly compared within the geospatial database to different other sets of terrestrial data - measurements obtained by total stations, real time kinematic and static GNSS.

Precision time distribution within a deep space communications complex

NASA Technical Reports Server (NTRS)

Curtright, J. B.

1972-01-01

The Precision Time Distribution System (PTDS) at the Golstone Deep Space Communications Complex is a practical application of existing technology to the solution of a local problem. The problem was to synchronize four station timing systems to a master source with a relative accuracy consistently and significantly better than 10 microseconds. The solution involved combining a precision timing source, an automatic error detection assembly and a microwave distribution network into an operational system. Upon activation of the completed PTDS two years ago, synchronization accuracy at Goldstone (two station relative) was improved by an order of magnitude. It is felt that the validation of the PTDS mechanization is now completed. Other facilities which have site dispersion and synchronization accuracy requirements similar to Goldstone may find the PTDS mechanization useful in solving their problem. At present, the two station relative synchronization accuracy at Goldstone is better than one microsecond.

Accuracy enhancement of a multivariate calibration for lead determination in soils by laser induced breakdown spectroscopy

NASA Astrophysics Data System (ADS)

Zaytsev, Sergey M.; Krylov, Ivan N.; Popov, Andrey M.; Zorov, Nikita B.; Labutin, Timur A.

2018-02-01

We have investigated matrix effects and spectral interferences on example of lead determination in different types of soils by laser induced breakdown spectroscopy (LIBS). Comparison between analytical performances of univariate and multivariate calibrations with the use of different laser wavelength for ablation (532, 355 and 266 nm) have been reported. A set of 17 soil samples (Ca-rich, Fe-rich, lean soils etc., 8.5-280 ppm of Pb) was involved into construction of the calibration models. Spectral interferences from main components (Ca, Fe, Ti, Mg) and trace components (Mn, Nb, Zr) were estimated by spectra modeling, and they were a reason for significant differences between the univariate calibration models obtained for a three different soil types (black, red, gray) separately. Implementation of 3rd harmonic of Nd:YAG laser in combination with multivariate calibration model based on PCR with 3 principal components provided the best analytical results: the RMSEC has been lowered down to 8 ppm. The sufficient improvement of the relative uncertainty (up to 5-10%) in comparison with univariate calibration was observed at the Pb concentration level > 50 ppm, while the problem of accuracy still remains for some samples with Pb concentration at the 20 ppm level. We have also discussed a few possible ways to estimate LOD without a blank sample. The most rigorous criterion has resulted in LOD of Pb in soils being 13 ppm. Finally, a good agreement between the values of lead content predicted by LIBS (46 ± 5 ppm) and XRF (42.1 ± 3.3 ppm) in the unknown soil sample from Lomonosov Moscow State University area was demonstrated.

Optimetrics for Precise Navigation

NASA Technical Reports Server (NTRS)

Yang, Guangning; Heckler, Gregory; Gramling, Cheryl

2017-01-01

Optimetrics for Precise Navigation will be implemented on existing optical communication links. The ranging and Doppler measurements are conducted over communication data frame and clock. The measurement accuracy is two orders of magnitude better than TDRSS. It also has other advantages of: The high optical carrier frequency enables: (1) Immunity from ionosphere and interplanetary Plasma noise floor, which is a performance limitation for RF tracking; and (2) High antenna gain reduces terminal size and volume, enables high precision tracking in Cubesat, and in deep space smallsat. High Optical Pointing Precision provides: (a) spacecraft orientation, (b) Minimal additional hardware to implement Precise Optimetrics over optical comm link; and (c) Continuous optical carrier phase measurement will enable the system presented here to accept future optical frequency standard with much higher clock accuracy.

Accuracy Assessment of Professional Grade Unmanned Systems for High Precision Airborne Mapping

NASA Astrophysics Data System (ADS)

Mostafa, M. M. R.

2017-08-01

Recently, sophisticated multi-sensor systems have been implemented on-board modern Unmanned Aerial Systems. This allows for producing a variety of mapping products for different mapping applications. The resulting accuracies match the traditional well engineered manned systems. This paper presents the results of a geometric accuracy assessment project for unmanned systems equipped with multi-sensor systems for direct georeferencing purposes. There are a number of parameters that either individually or collectively affect the quality and accuracy of a final airborne mapping product. This paper focuses on identifying and explaining these parameters and their mutual interaction and correlation. Accuracy Assessment of the final ground object positioning accuracy is presented through real-world 8 flight missions that were flown in Quebec, Canada. The achievable precision of map production is addressed in some detail.

[LC-MS/MS analysis of determination of strychnine and brucine in formaldehyde fixed tissue].

PubMed

Zhan, Lan-fen; Liu, Ming-dong; Yan, You-yi; Ye, Yi; Wang, Wei; Wang, Zhi-hui; Zhao, Jun-hong; Liao, Lin-chuan

2012-10-01

To establish a method for determination of strychnine and brucine in formaldehyde fixed tissue by LC-MS/MS analysis. The samples were pretreated with solid phase extraction using SCX cartridges and separated on SB-C18 column with mobile phase 0.1% formic acid : 0.1% formic acid-acetonitrile (75:25). Electrospray ionization (ESI) source was utilized and operated in positive ion mode. Multiple reactions monitoring (MRM) mode was applied. External standard method was applied for quantitation. The chromatographic separation of strychnine and brucine in formaldehyde fixed nephritic and hepatic tissues resulted successfully. The standard curve was linear in the range of 0.002-2.0 microg/g for strychnine and brucine in formaldehyde fixed tissues, and the correlation coefficient was more than 0.996. The limits of detection (LOD) of strychnine and brucine in nephritic tissues were 0.06ng/g and 0.03 ng/g, respectively. The LOD of both chemicals were 0.3 ng/g in hepatic tissues. The extraction recovery rate was more than 74.5%. The precision of intra-day and inter-day were both less than 8.2%. Strychnine and brucine can be sensitive to be determined in formaldehyde fixed tissue by LC-MS/MS analysis. It can be applied in the forensic toxicological analysis.

Familial isolated hyperparathyroidism is linked to a 1.7 Mb region on chromosome 2p13.3–14

PubMed Central

Warner, J; Nyholt, D R; Busfield, F; Epstein, M; Burgess, J; Stranks, S; Hill, P; Perry‐Keene, D; Learoyd, D; Robinson, B; Teh, B T; Prins, J B; Cardinal, J W

2006-01-01

Bachground Familial isolated hyperparathyroidism (FIHP) is an autosomal dominantly inherited form of primary hyperparathyroidism. Although comprising only about 1% of cases of primary hyperparathyroidism, identification and functional analysis of a causative gene for FIHP is likely to advance our understanding of parathyroid physiology and pathophysiology. Methods A genome‐wide screen of DNA from seven pedigrees with FIHP was undertaken in order to identify a region of genetic linkage with the disorder. Results Multipoint linkage analysis identified a region of suggestive linkage (LOD score 2.68) on chromosome 2. Fine mapping with the addition of three other families revealed significant linkage adjacent to D2S2368 (maximum multipoint LOD score 3.43). Recombination events defined a 1.7 Mb region of linkage between D2S2368 and D2S358 in nine pedigrees. Sequencing of the two most likely candidate genes in this region, however, did not identify a gene for FIHP. Conclusions We conclude that a causative gene for FIHP lies within this interval on chromosome 2. This is a major step towards eventual precise identification of a gene for FIHP, likely to be a key component in the genetic regulation of calcium homeostasis. PMID:16525030

Self-Referenced Smartphone-Based Nanoplasmonic Imaging Platform for Colorimetric Biochemical Sensing.

PubMed

Wang, Xinhao; Chang, Te-Wei; Lin, Guohong; Gartia, Manas Ranjan; Liu, Gang Logan

2017-01-03

Colorimetric sensors usually suffer due to errors from variation in light source intensity, the type of light source, the Bayer filter algorithm, and the sensitivity of the camera to incoming light. Here, we demonstrate a self-referenced portable smartphone-based plasmonic sensing platform integrated with an internal reference sample along with an image processing method to perform colorimetric sensing. Two sensing principles based on unique nanoplasmonics enabled phenomena from a nanostructured plasmonic sensor, named as nanoLCA (nano Lycurgus cup array), were demonstrated here for colorimetric biochemical sensing: liquid refractive index sensing and optical absorbance enhancement sensing. Refractive indices of colorless liquids were measured by simple smartphone imaging and color analysis. Optical absorbance enhancement in the colorimetric biochemical assay was achieved by matching the plasmon resonance wavelength with the chromophore's absorbance peak wavelength. Such a sensing mechanism improved the limit of detection (LoD) by 100 times in a microplate reader format. Compared with a traditional colorimetric assay such as urine testing strips, a smartphone plasmon enhanced colorimetric sensing system provided 30 times improvement in the LoD. The platform was applied for simulated urine testing to precisely identify the samples with higher protein concentration, which showed potential point-of-care and early detection of kidney disease with the smartphone plasmonic resonance sensing system.

A simple method to produce 2D and 3D microfluidic paper-based analytical devices for clinical analysis.

PubMed

de Oliveira, Ricardo A G; Camargo, Fiamma; Pesquero, Naira C; Faria, Ronaldo Censi

2017-03-08

This paper describes the fabrication of 2D and 3D microfluidic paper-based analytical devices (μPADs) for monitoring glucose, total protein, and nitrite in blood serum and artificial urine. A new method of cutting and sealing filter paper to construct μPADs was demonstrated. Using an inexpensive home cutter printer soft cellulose-based filter paper was easily and precisely cut to produce pattern hydrophilic microchannels. 2D and 3D μPADs were designed with three detection zones each for the colorimetric detection of the analytes. A small volume of samples was added to the μPADs, which was photographed after 15 min using a digital camera. Both μPADs presented an excellent analytical performance for all analytes. The 2D device was applied in artificial urine samples and reached limits of detection (LODs) of 0.54 mM, 5.19 μM, and 2.34 μM for glucose, protein, and nitrite, respectively. The corresponding LODs of the 3D device applied for detecting the same analytes in artificial blood serum were 0.44 mM, 1.26 μM, and 4.35 μM. Copyright © 2017 Elsevier B.V. All rights reserved.

Sex-specific quantitative trait loci contribute to normal variation in bone structure at the proximal femur in men

PubMed Central

Peacock, Munro; Koller, Daniel L.; Lai, Dongbing; Hui, Siu; Foroud, Tatiana; Econs, Michael J.

2006-01-01

Bone structure is an important determinant of osteoporotic fracture. In women bone structure is highly heritable and several quantitative trait loci (QTL) have been reported. There are few comparable data in men. This study in men aimed at establishing the heritability of bone structure at the proximal femur, identifying QTL contributing to normal variation in bone structure, and determining which QTL might be sex-specific. Bone structure at the proximal femur was measured in 205 pairs of brothers age 18–61. Heritability was calculated and linkage analysis performed on phenotypes at the proximal femur. Heritability estimates ranged from 0.99 to 0.39. A genome wide scan identified suggestive QTL (LOD>2.2) for femoral shaft width on chromosome 14q (LOD=2.69 at position 99cM), calcar femorale at chromosome 2p (LOD= 3.97 at position 194cM) and at the X chromosome (LOD= 3.01 at position 77cM), femoral neck width on chromosome 5p (LOD=2.28 at position 0 cM), femoral head width on chromosome 11q (LOD=2.30 at position 131 cM) and 15q (LOD=3.11 at position 90 cM), and pelvic axis length on chromosome 4q (LOD= 4.16 at 99cM) and 17q (LOD=2.80 at position 112 cM). Comparison with published data in 437 pairs of premenopausal sisters from the same geographical region suggested that 3 of the 7 autosomal QTL were male-specific. This study demonstrates that bone structure at the proximal femur in healthy men is highly heritable. The occurrence of sex-specific genes in humans for bone structure has important implications for the pathogenesis and treatment of osteoporosis. PMID:16046210

LODVIEW: a computer program for the graphical evaluation of lod score results in exclusion mapping of human disease genes.

PubMed

Hildebrandt, F; Pohlmann, A; Omran, H

1993-12-01

For linkage analysis projects aimed at mapping hereditary disease genes in humans, hundreds of highly polymorphic microsatellite markers which can be typed by PCR (PCR markers) have become available. With this technical improvement, the availability of a technique allowing for transparency in the handling of rapidly generated lod score data is becoming important. We present a computer program LODVIEW for the graphical representation of lod score data. It is designed for the input of lod score data generated with the LINKAGE package or similar programs. LODVIEW consists of 24 preformatted files, one for each chromosome. Each file contains a table for the input of lod score data and a file for the graphical representation of the data, which will show automatically any entry that is made in the respective input table. The program provides the user with published PCR marker information pre-entered into a table and graph at the correct positions corresponding to the genetic distances between markers. The graphical display of LODVIEW allows for the rapid evaluation of lod score results calculated from PCR markers on each chromosome. The following information can be obtained from the graphical display at one glance: (i) Regions of exclusion (Z(theta) < -2) and nonexclusion, (ii) markers with positive lod scores, (iii) the distribution of positive and negative lod scores among the families examined (indication of genetic heterogeneity), (iv) multipoint lod scores, and (v) the availability of PCR markers in regions of interest. The program is continually updated for novel PCR marker information from the literature. The program will help to efficiently monitor and direct the progress of exclusion mapping projects.

Systematic effects in LOD from SLR observations

NASA Astrophysics Data System (ADS)

Bloßfeld, Mathis; Gerstl, Michael; Hugentobler, Urs; Angermann, Detlef; Müller, Horst

2014-09-01

Beside the estimation of station coordinates and the Earth’s gravity field, laser ranging observations to near-Earth satellites can be used to determine the rotation of the Earth. One parameter of this rotation is ΔLOD (excess Length Of Day) which describes the excess revolution time of the Earth w.r.t. 86,400 s. Due to correlations among the different parameter groups, it is difficult to obtain reliable estimates for all parameters. In the official ΔLOD products of the International Earth Rotation and Reference Systems Service (IERS), the ΔLOD information determined from laser ranging observations is excluded from the processing. In this paper, we study the existing correlations between ΔLOD, the orbital node Ω, the even zonal gravity field coefficients, cross-track empirical accelerations and relativistic accelerations caused by the Lense-Thirring and deSitter effect in detail using first order Gaussian perturbation equations. We found discrepancies due to different a priories by using different gravity field models of up to 1.0 ms for polar orbits at an altitude of 500 km and up to 40.0 ms, if the gravity field coefficients are estimated using only observations to LAGEOS 1. If observations to LAGEOS 2 are included, reliable ΔLOD estimates can be achieved. Nevertheless, an impact of the a priori gravity field even on the multi-satellite ΔLOD estimates can be clearly identified. Furthermore, we investigate the effect of empirical cross-track accelerations and the effect of relativistic accelerations of near-Earth satellites on ΔLOD. A total effect of 0.0088 ms is caused by not modeled Lense-Thirring and deSitter terms. The partial derivatives of these accelerations w.r.t. the position and velocity of the satellite cause very small variations (0.1 μs) on ΔLOD.

Statins Reduces the Risk of Dementia in Patients with Late-Onset Depression: A Retrospective Cohort Study.

PubMed

Yang, Ya-Hsu; Teng, Hao-Wei; Lai, Yen-Ting; Li, Szu-Yuan; Lin, Chih-Ching; Yang, Albert C; Chan, Hsiang-Lin; Hsieh, Yi-Hsuan; Lin, Chiao-Fan; Hsu, Fu-Ying; Liu, Chih-Kuang; Liu, Wen-Sheng

2015-01-01

Patients with late-onset depression (LOD) have been reported to run a higher risk of subsequent dementia. The present study was conducted to assess whether statins can reduce the risk of dementia in these patients. We used the data from National Health Insurance of Taiwan during 1996-2009. Standardized Incidence Ratios (SIRs) were calculated for LOD and subsequent dementia. The criteria for LOD diagnoses included age ≥65 years, diagnosis of depression after 65 years of age, at least three service claims, and treatment with antidepressants. The time-dependent Cox proportional hazards model was applied for multivariate analyses. Propensity scores with the one-to-one nearest-neighbor matching model were used to select matching patients for validation studies. Kaplan-Meier curve estimate was used to measure the group of patients with dementia living after diagnosis of LOD. Totally 45,973 patients aged ≥65 years were enrolled. The prevalence of LOD was 12.9% (5,952/45,973). Patients with LOD showed to have a higher incidence of subsequent dementia compared with those without LOD (Odds Ratio: 2.785; 95% CI 2.619-2.958). Among patients with LOD, lipid lowering agent (LLA) users (for at least 3 months) had lower incidence of subsequent dementia than non-users (Hazard Ratio = 0.781, 95% CI 0.685-0.891). Nevertheless, only statins users showed to have reduced risk of dementia (Hazard Ratio = 0.674, 95% CI 0.547-0.832) while other LLAs did not, which was further validated by Kaplan-Meier estimates after we used the propensity scores with the one-to-one nearest-neighbor matching model to control the confounding factors. Statins may reduce the risk of subsequent dementia in patients with LOD.

Complete genomic screen in Parkinson disease: evidence for multiple genes.

PubMed

Scott, W K; Nance, M A; Watts, R L; Hubble, J P; Koller, W C; Lyons, K; Pahwa, R; Stern, M B; Colcher, A; Hiner, B C; Jankovic, J; Ondo, W G; Allen, F H; Goetz, C G; Small, G W; Masterman, D; Mastaglia, F; Laing, N G; Stajich, J M; Slotterbeck, B; Booze, M W; Ribble, R C; Rampersaud, E; West, S G; Gibson, R A; Middleton, L T; Roses, A D; Haines, J L; Scott, B L; Vance, J M; Pericak-Vance, M A

2001-11-14

The relative contribution of genes vs environment in idiopathic Parkinson disease (PD) is controversial. Although genetic studies have identified 2 genes in which mutations cause rare single-gene variants of PD and observational studies have suggested a genetic component, twin studies have suggested that little genetic contribution exists in the common forms of PD. To identify genetic risk factors for idiopathic PD. Genetic linkage study conducted 1995-2000 in which a complete genomic screen (n = 344 markers) was performed in 174 families with multiple individuals diagnosed as having idiopathic PD, identified through probands in 13 clinic populations in the continental United States and Australia. A total of 870 family members were studied: 378 diagnosed as having PD, 379 unaffected by PD, and 113 with unclear status. Logarithm of odds (lod) scores generated from parametric and nonparametric genetic linkage analysis. Two-point parametric maximum parametric lod score (MLOD) and multipoint nonparametric lod score (LOD) linkage analysis detected significant evidence for linkage to 5 distinct chromosomal regions: chromosome 6 in the parkin gene (MLOD = 5.07; LOD = 5.47) in families with at least 1 individual with PD onset at younger than 40 years, chromosomes 17q (MLOD = 2.28; LOD = 2.62), 8p (MLOD = 2.01; LOD = 2.22), and 5q (MLOD = 2.39; LOD = 1.50) overall and in families with late-onset PD, and chromosome 9q (MLOD = 1.52; LOD = 2.59) in families with both levodopa-responsive and levodopa-nonresponsive patients. Our data suggest that the parkin gene is important in early-onset PD and that multiple genetic factors may be important in the development of idiopathic late-onset PD.

Looking Beyond Where Children Die: Determinants and Effects of Planning a Child’s Location of Death

PubMed Central

Dussel, Veronica; Kreicbergs, Ulrika; Hilden, Joanne M.; Watterson, Jan; Moore, Caron; Turner, Brian G.; Weeks, Jane C.; Wolfe, Joanne

2009-01-01

While dying at home may be the choice of many, where people die may be less important than argued. We examined factors associated with parental planning of a child’s location of death (LOD) and its effects on patterns of care and parent’s experience. In a cross-sectional study of 140 parents who lost a child to cancer at one of two tertiary level U.S. pediatric hospitals, 88 (63%) planned the child’s LOD and 97% accomplished their plan. After adjusting for disease and family characteristics, families whose primary oncologist clearly explained treatment options during the child’s end of life (EOL) and who had home care involved were more likely to plan LOD. Planning LOD was associated with more home deaths (72% versus 8% among those who did not plan, P<0.001) and fewer hospital admissions (54% versus 98%, P<0.001). Parents who planned were more likely to feel very prepared for the child’s EOL (33% versus 12%, P=0.007) and very comfortable with LOD (84% versus 40%, P<0.001), and less likely to have preferred a different LOD (2% versus 46%, P<0.001). Among the 73 non-home deaths, planning was associated with more deaths occurring in the ward than in the intensive care unit or other hospital (92% versus 33%, P<0.001), and fewer children being intubated (21% versus 48%, P=0.029). Comprehensive physician communication and home care involvement increase the likelihood of planning a child’s LOD. Opportunity to plan LOD is associated with outcomes consistent with high quality palliative care, even among non-home deaths, and thus may represent a more relevant outcome than actual LOD. PMID:18538973

40 CFR Appendix D to Part 136 - Precision and Recovery Statements for Methods for Measuring Metals

Code of Federal Regulations, 2011 CFR

2011-07-01

... Accuracy Section with the following: Precision and Accuracy An interlaboratory study on metal analyses by... details are found in “USEPA Method Study 7, Analyses for Trace Methods in water by Atomic Absorption... study on metal analyses by this method was conducted by the Quality Assurance Branch (QAB) of the...

Obtaining identical results with double precision global accuracy on different numbers of processors in parallel particle Monte Carlo simulations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cleveland, Mathew A., E-mail: cleveland7@llnl.gov; Brunner, Thomas A.; Gentile, Nicholas A.

2013-10-15

We describe and compare different approaches for achieving numerical reproducibility in photon Monte Carlo simulations. Reproducibility is desirable for code verification, testing, and debugging. Parallelism creates a unique problem for achieving reproducibility in Monte Carlo simulations because it changes the order in which values are summed. This is a numerical problem because double precision arithmetic is not associative. Parallel Monte Carlo, both domain replicated and decomposed simulations, will run their particles in a different order during different runs of the same simulation because the non-reproducibility of communication between processors. In addition, runs of the same simulation using different domain decompositionsmore » will also result in particles being simulated in a different order. In [1], a way of eliminating non-associative accumulations using integer tallies was described. This approach successfully achieves reproducibility at the cost of lost accuracy by rounding double precision numbers to fewer significant digits. This integer approach, and other extended and reduced precision reproducibility techniques, are described and compared in this work. Increased precision alone is not enough to ensure reproducibility of photon Monte Carlo simulations. Non-arbitrary precision approaches require a varying degree of rounding to achieve reproducibility. For the problems investigated in this work double precision global accuracy was achievable by using 100 bits of precision or greater on all unordered sums which where subsequently rounded to double precision at the end of every time-step.« less

Application of General Regression Neural Network to the Prediction of LOD Change

NASA Astrophysics Data System (ADS)

Zhang, Xiao-Hong; Wang, Qi-Jie; Zhu, Jian-Jun; Zhang, Hao

2012-01-01

Traditional methods for predicting the change in length of day (LOD change) are mainly based on some linear models, such as the least square model and autoregression model, etc. However, the LOD change comprises complicated non-linear factors and the prediction effect of the linear models is always not so ideal. Thus, a kind of non-linear neural network — general regression neural network (GRNN) model is tried to make the prediction of the LOD change and the result is compared with the predicted results obtained by taking advantage of the BP (back propagation) neural network model and other models. The comparison result shows that the application of the GRNN to the prediction of the LOD change is highly effective and feasible.

Accuracy and precision of four value-added blood glucose meters: the Abbott Optium, the DDI Prodigy, the HDI True Track, and the HypoGuard Assure Pro.

PubMed

Sheffield, Catherine A; Kane, Michael P; Bakst, Gary; Busch, Robert S; Abelseth, Jill M; Hamilton, Robert A

2009-09-01

This study compared the accuracy and precision of four value-added glucose meters. Finger stick glucose measurements in diabetes patients were performed using the Abbott Diabetes Care (Alameda, CA) Optium, Diagnostic Devices, Inc. (Miami, FL) DDI Prodigy, Home Diagnostics, Inc. (Fort Lauderdale, FL) HDI True Track Smart System, and Arkray, USA (Minneapolis, MN) HypoGuard Assure Pro. Finger glucose measurements were compared with laboratory reference results. Accuracy was assessed by a Clarke error grid analysis (EGA), a Parkes EGA, and within 5%, 10%, 15%, and 20% of the laboratory value criteria (chi2 analysis). Meter precision was determined by calculating absolute mean differences in glucose values between duplicate samples (Kruskal-Wallis test). Finger sticks were obtained from 125 diabetes patients, of which 90.4% were Caucasian, 51.2% were female, 83.2% had type 2 diabetes, and average age of 59 years (SD 14 years). Mean venipuncture blood glucose was 151 mg/dL (SD +/-65 mg/dL; range, 58-474 mg/dL). Clinical accuracy by Clarke EGA was demonstrated in 94% of Optium, 82% of Prodigy, 61% of True Track, and 77% of the Assure Pro samples (P < 0.05 for Optium and True Track compared to all others). By Parkes EGA, the True Track was significantly less accurate than the other meters. Within 5% accuracy was achieved in 34%, 24%, 29%, and 13%, respectively (P < 0.05 for Optium, Prodigy, and Assure Pro compared to True Track). Within 10% accuracy was significantly greater for the Optium, Prodigy, and Assure Pro compared to True Track. Significantly more Optium results demonstrated within 15% and 20% accuracy compared to the other meter systems. The HDI True Track was significantly less precise than the other meter systems. The Abbott Optium was significantly more accurate than the other meter systems, whereas the HDI True Track was significantly less accurate and less precise compared to the other meter systems.

Laparoscopic ovarian drilling for clomiphene-resistant polycystic ovary syndrome.

PubMed

Flyckt, Rebecca L; Goldberg, Jeffrey M

2011-03-01

Laparoscopic ovarian drilling (LOD) is an alternative to ovulation induction with gonadotropins for polycystic ovarian syndrome (PCOS) patients unresponsive to clomiphene. It is quick and easy to perform, although the number of punctures and energy doses has not been standardized. The mechanism of LOD is unclear, but it is likely mediated by a reduction in intraovarian androgen production. Serum luteinizing hormone and testosterone levels are rapidly normalized, and these changes are sustained over long-term follow-up. Studies have shown that ovulation and pregnancy rates are comparable between ovulation induction with gonadotropins and LOD, but LOD avoids the risks of multiple pregnancy and ovarian hyperstimulation syndrome. LOD is also more cost effective and better tolerated than gonadotropin therapy. Concerns regarding clinically significant adhesion formation and premature ovarian failure are not supported by the available data. Transvaginal hydrolaparoscopy and ultrasound guidance are less invasive techniques for performing ovarian drilling and may encourage LOD earlier in the course of treatment for PCOS. © Thieme Medical Publishers.

The lod score method.

PubMed

Rice, J P; Saccone, N L; Corbett, J

2001-01-01

The lod score method originated in a seminal article by Newton Morton in 1955. The method is broadly concerned with issues of power and the posterior probability of linkage, ensuring that a reported linkage has a high probability of being a true linkage. In addition, the method is sequential, so that pedigrees or lod curves may be combined from published reports to pool data for analysis. This approach has been remarkably successful for 50 years in identifying disease genes for Mendelian disorders. After discussing these issues, we consider the situation for complex disorders, where the maximum lod score (MLS) statistic shares some of the advantages of the traditional lod score approach but is limited by unknown power and the lack of sharing of the primary data needed to optimally combine analytic results. We may still learn from the lod score method as we explore new methods in molecular biology and genetic analysis to utilize the complete human DNA sequence and the cataloging of all human genes.

Major to ultra trace element bulk rock analysis of nanoparticulate pressed powder pellets by LA-ICP-MS

NASA Astrophysics Data System (ADS)

Peters, Daniel; Pettke, Thomas

2016-04-01

An efficient, clean procedure for bulk rock major to trace element analysis by 193 nm Excimer LA-ICP-MS analysis of nanoparticulate pressed powder pellets (PPPs) employing a binder is presented. Sample powders are milled in water suspension in a planetary ball mill, reducing average grain size by about one order of magnitude compared to common dry milling protocols. Microcrystalline cellulose (MCC) is employed as a binder, improving the mechanical strength of the PPP and the ablation behaviour, because MCC absorbs 193 nm laser light well. Use of MCC binder allows for producing cohesive pellets of materials that cannot be pelletized in their pure forms, such as quartz powder. Rigorous blank quantification was performed on synthetic quartz treated like rock samples, demonstrating that procedural blanks are irrelevant except for a few elements at the 10 ng g-1 concentration level. The LA-ICP-MS PPP analytical procedure was optimised and evaluated using six different SRM powders (JP-1, UB-N, BCR-2, GSP-2, OKUM, and MUH-1). Calibration based on external standardization using SRM 610, SRM 612, BCR-2G, and GSD-1G glasses allows for evaluation of possible matrix effects during LA-ICP-MS analysis. The data accuracy of the PPP LA-ICP-MS analytical procedure compares well to that achieved for liquid ICP-MS and LA-ICP-MS glass analysis, except for element concentrations below ˜30 ng g-1, where liquid ICP-MS offers more precise data and in part lower limits of detection. Uncertainties on the external reproducibility of LA-ICP-MS PPP element concentrations are of the order of 0.5 to 2 % (1σ standard deviation) for concentrations exceeding ˜1 μg g-1. For lower element concentrations these uncertainties increase to 5-10% or higher when analyte-depending limits of detection (LOD) are approached, and LODs do not significantly differ from glass analysis. Sample homogeneity is demonstrated by the high analytical precision, except for very few elements where grain size effects can rarely still be resolved analytically. Matrix effects are demonstrated for PPP analysis of diverse rock compositions and basalt glass analysis when externally calibrated based on SRM 610 and SRM 612 glasses; employing basalt glass GSD-1G or BCR-2G for external standardisation basically eliminates these problems. Perhaps the most prominent progress of the LA-ICP-MS PPP analytical procedure presented here is the fact that trace elements not commonly analysed, i.e. new, unconventional geochemical tracers, can be measured straightforwardly, including volatile elements, the flux elements Li and B, the chalcophile elements As, Sb, Tl, Bi, and elements that alloy with metal containers employed in conventional glass production approaches. The method presented here thus overcomes many common problems and limitations in analytical geochemistry and is shown to be an efficient alternative for bulk rock trace elements analysis.

Randomized controlled trial comparing laparoscopic ovarian diathermy with clomiphene citrate as a first-line method of ovulation induction in women with polycystic ovary syndrome.

PubMed

Amer, S A; Li, T C; Metwally, M; Emarh, M; Ledger, W L

2009-01-01

Laparoscopic ovarian diathermy (LOD) is currently accepted as a successful second-line treatment for ovulation induction (OI) in clomiphene citrate (CC)-resistant women with polycystic ovary syndrome (PCOS). The aim of this study was to test the hypothesis that LOD may be superior to CC as a first-line treatment. The study included 72 anovulatory women with PCOS who were randomized to LOD (n = 36) or CC (n = 36). Women who remained anovulatory after LOD were offered CC. Similarly, women receiving CC who failed to ovulate or conceive were offered LOD. Pregnancy rates were compared between the two groups using chi(2) and odds ratio with 95% confidence interval (OR, 95% CI). After randomization, six women conceived before starting treatment and another patient postponed treatment. The remaining 65 women received the treatment (33 underwent LOD and 32 received CC). After the primary treatment, more pregnancies (44%) occurred in women receiving CC than in those undergoing LOD (27%), although the difference did not reach statistical significance [P = 0.13, OR 2.1 (0.7 - 5.8)]. After adding the second treatment, the pregnancy rate was still higher, but to a less extent, in the CC group [63% versus 52%, P = 0.2, OR 1.6 (0.6 - 4.2)]. LOD is not superior to CC as a first-line method of OI in women with PCOS. The trial is registered with ClinicalTrials.gov with an identifier number NCT00220545.

A Method for Assessing the Accuracy of a Photogrammetry System for Precision Deployable Structures

NASA Technical Reports Server (NTRS)

Moore, Ashley

2005-01-01

The measurement techniques used to validate analytical models of large deployable structures are an integral Part of the technology development process and must be precise and accurate. Photogrammetry and videogrammetry are viable, accurate, and unobtrusive methods for measuring such large Structures. Photogrammetry uses Software to determine the three-dimensional position of a target using camera images. Videogrammetry is based on the same principle, except a series of timed images are analyzed. This work addresses the accuracy of a digital photogrammetry system used for measurement of large, deployable space structures at JPL. First, photogrammetry tests are performed on a precision space truss test article, and the images are processed using Photomodeler software. The accuracy of the Photomodeler results is determined through, comparison with measurements of the test article taken by an external testing group using the VSTARS photogrammetry system. These two measurements are then compared with Australis photogrammetry software that simulates a measurement test to predict its accuracy. The software is then used to study how particular factors, such as camera resolution and placement, affect the system accuracy to help design the setup for the videogrammetry system that will offer the highest level of accuracy for measurement of deploying structures.

Is digital photography an accurate and precise method for measuring range of motion of the shoulder and elbow?

PubMed

Russo, Russell R; Burn, Matthew B; Ismaily, Sabir K; Gerrie, Brayden J; Han, Shuyang; Alexander, Jerry; Lenherr, Christopher; Noble, Philip C; Harris, Joshua D; McCulloch, Patrick C

2018-03-01

Accurate measurements of shoulder and elbow motion are required for the management of musculoskeletal pathology. The purpose of this investigation was to compare three techniques for measuring motion. The authors hypothesized that digital photography would be equivalent in accuracy and show higher precision compared to the other two techniques. Using infrared motion capture analysis as the reference standard, shoulder flexion/abduction/internal rotation/external rotation and elbow flexion/extension were measured using visual estimation, goniometry, and digital photography on 10 fresh frozen cadavers. These measurements were performed by three physical therapists and three orthopaedic surgeons. Accuracy was defined by the difference from the reference standard (motion capture analysis), while precision was defined by the proportion of measurements within the authors' definition of clinical significance (10° for all motions except for elbow extension where 5° was used). Analysis of variance (ANOVA), t-tests, and chi-squared tests were used. Although statistically significant differences were found in measurement accuracy between the three techniques, none of these differences met the authors' definition of clinical significance. Precision of the measurements was significantly higher for both digital photography (shoulder abduction [93% vs. 74%, p < 0.001], shoulder internal rotation [97% vs. 83%, p = 0.001], and elbow flexion [93% vs. 65%, p < 0.001]) and goniometry (shoulder abduction [92% vs. 74%, p < 0.001] and shoulder internal rotation [94% vs. 83%, p = 0.008]) than visual estimation. Digital photography was more precise than goniometry for measurements of elbow flexion only [93% vs. 76%, p < 0.001]. There was no clinically significant difference in measurement accuracy between the three techniques for shoulder and elbow motion. Digital photography showed higher measurement precision compared to visual estimation for shoulder abduction, shoulder internal rotation, and elbow flexion. However, digital photography was only more precise than goniometry for measurements of elbow flexion. Overall digital photography shows equivalent accuracy to visual estimation and goniometry, but with higher precision than visual estimation. Copyright © 2017. Published by Elsevier B.V.

A priori evaluation of two-stage cluster sampling for accuracy assessment of large-area land-cover maps

USGS Publications Warehouse

Wickham, J.D.; Stehman, S.V.; Smith, J.H.; Wade, T.G.; Yang, L.

2004-01-01

Two-stage cluster sampling reduces the cost of collecting accuracy assessment reference data by constraining sample elements to fall within a limited number of geographic domains (clusters). However, because classification error is typically positively spatially correlated, within-cluster correlation may reduce the precision of the accuracy estimates. The detailed population information to quantify a priori the effect of within-cluster correlation on precision is typically unavailable. Consequently, a convenient, practical approach to evaluate the likely performance of a two-stage cluster sample is needed. We describe such an a priori evaluation protocol focusing on the spatial distribution of the sample by land-cover class across different cluster sizes and costs of different sampling options, including options not imposing clustering. This protocol also assesses the two-stage design's adequacy for estimating the precision of accuracy estimates for rare land-cover classes. We illustrate the approach using two large-area, regional accuracy assessments from the National Land-Cover Data (NLCD), and describe how the a priorievaluation was used as a decision-making tool when implementing the NLCD design.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Grout, Ray W. S.

Convergence of spectral deferred correction (SDC), where low-order time integration methods are used to construct higher-order methods through iterative refinement, can be accelerated in terms of computational effort by using mixed-precision methods. Using ideas from multi-level SDC (in turn based on FAS multigrid ideas), some of the SDC correction sweeps can use function values computed in reduced precision without adversely impacting the accuracy of the final solution. This is particularly beneficial for the performance of combustion solvers such as S3D [6] which require double precision accuracy but are performance limited by the cost of data motion.

Geometrical accuracy of metallic objects produced with additive or subtractive manufacturing: A comparative in vitro study.

PubMed

Braian, Michael; Jönsson, David; Kevci, Mir; Wennerberg, Ann

2018-07-01

To evaluate the accuracy and precision of objects produced by additive manufacturing systems (AM) for use in dentistry and to compare with subtractive manufacturing systems (SM). Ten specimens of two geometrical objects were produced by five different AM machines and one SM machine. Object A mimics an inlay-shaped object, while object B imitates a four-unit bridge model. All the objects were sorted into different measurement dimensions (x, y, z), linear distances, angles and corner radius. None of the additive manufacturing or subtractive manufacturing groups presented a perfect match to the CAD file with regard to all parameters included in the present study. Considering linear measurements, the precision for subtractive manufacturing group was consistent in all axes for object A, presenting results of <0.050mm. The additive manufacturing groups had consistent precision in the x-axis and y-axis but not in the z-axis. With regard to corner radius measurements, the SM group had the best overall accuracy and precision for both objects A and B when compared to the AM groups. Within the limitations of this in vitro study, the conclusion can be made that subtractive manufacturing presented overall precision on all measurements below 0.050mm. The AM machines also presented fairly good precision, <0.150mm, on all axes except for the z-axis. Knowledge regarding accuracy and precision for different production techniques utilized in dentistry is of great clinical importance. The dental community has moved from casting to milling and additive techniques are now being implemented. Thus all these production techniques need to be tested, compared and validated. Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.

Interactive distributed hardware-accelerated LOD-sprite terrain rendering with stable frame rates

NASA Astrophysics Data System (ADS)

Swan, J. E., II; Arango, Jesus; Nakshatrala, Bala K.

2002-03-01

A stable frame rate is important for interactive rendering systems. Image-based modeling and rendering (IBMR) techniques, which model parts of the scene with image sprites, are a promising technique for interactive systems because they allow the sprite to be manipulated instead of the underlying scene geometry. However, with IBMR techniques a frequent problem is an unstable frame rate, because generating an image sprite (with 3D rendering) is time-consuming relative to manipulating the sprite (with 2D image resampling). This paper describes one solution to this problem, by distributing an IBMR technique into a collection of cooperating threads and executable programs across two computers. The particular IBMR technique distributed here is the LOD-Sprite algorithm. This technique uses a multiple level-of-detail (LOD) scene representation. It first renders a keyframe from a high-LOD representation, and then caches the frame as an image sprite. It renders subsequent spriteframes by texture-mapping the cached image sprite into a lower-LOD representation. We describe a distributed architecture and implementation of LOD-Sprite, in the context of terrain rendering, which takes advantage of graphics hardware. We present timing results which indicate we have achieved a stable frame rate. In addition to LOD-Sprite, our distribution method holds promise for other IBMR techniques.

Accuracy and precision of two indirect methods for estimating canopy fuels

Treesearch

Abran Steele-Feldman; Elizabeth Reinhardt; Russell A. Parsons

2006-01-01

We compared the accuracy and precision of digital hemispherical photography and the LI-COR LAI-2000 plant canopy analyzer as predictors of canopy fuels. We collected data on 12 plots in western Montana under a variety of lighting and sky conditions, and used a variety of processing methods to compute estimates. Repeated measurements from each method displayed...

The Accuracy of Webcams in 2D Motion Analysis: Sources of Error and Their Control

ERIC Educational Resources Information Center

Page, A.; Moreno, R.; Candelas, P.; Belmar, F.

2008-01-01

In this paper, we show the potential of webcams as precision measuring instruments in a physics laboratory. Various sources of error appearing in 2D coordinate measurements using low-cost commercial webcams are discussed, quantifying their impact on accuracy and precision, and simple procedures to control these sources of error are presented.…

Parallelism measurement for base plate of standard artifact with multiple tactile approaches

NASA Astrophysics Data System (ADS)

Ye, Xiuling; Zhao, Yan; Wang, Yiwen; Wang, Zhong; Fu, Luhua; Liu, Changjie

2018-01-01

Nowadays, as workpieces become more precise and more specialized which results in more sophisticated structures and higher accuracy for the artifacts, higher requirements have been put forward for measuring accuracy and measuring methods. As an important method to obtain the size of workpieces, coordinate measuring machine (CMM) has been widely used in many industries. In order to achieve the calibration of a self-developed CMM, it is found that the parallelism of the base plate used for fixing the standard artifact is an important factor which affects the measurement accuracy in the process of studying self-made high-precision standard artifact. And aimed to measure the parallelism of the base plate, by using the existing high-precision CMM, gauge blocks, dial gauge and marble platform with the tactile approach, three methods for parallelism measurement of workpieces are employed, and comparisons are made within the measurement results. The results of experiments show that the final accuracy of all the three methods is able to reach micron level and meets the measurement requirements. Simultaneously, these three approaches are suitable for different measurement conditions which provide a basis for rapid and high-precision measurement under different equipment conditions.

Application of high precision two-way S-band ranging to the navigation of the Galileo Earth encounters

NASA Technical Reports Server (NTRS)

Pollmeier, Vincent M.; Kallemeyn, Pieter H.; Thurman, Sam W.

1993-01-01

The application of high-accuracy S/S-band (2.1 GHz uplink/2.3 GHz downlink) ranging to orbit determination with relatively short data arcs is investigated for the approach phase of each of the Galileo spacecraft's two Earth encounters (8 December 1990 and 8 December 1992). Analysis of S-band ranging data from Galileo indicated that under favorable signal levels, meter-level precision was attainable. It is shown that ranginging data of sufficient accuracy, when acquired from multiple stations, can sense the geocentric angular position of a distant spacecraft. Explicit modeling of ranging bias parameters for each station pass is used to largely remove systematic ground system calibration errors and transmission media effects from the Galileo range measurements, which would otherwise corrupt the angle finding capabilities of the data. The accuracy achieved using the precision range filtering strategy proved markedly better when compared to post-flyby reconstructions than did solutions utilizing a traditional Doppler/range filter strategy. In addition, the navigation accuracy achieved with precision ranging was comparable to that obtained using delta-Differenced One-Way Range, an interferometric measurement of spacecraft angular position relative to a natural radio source, which was also used operationally.

Assay of lovastatin containing dietary supplement by LC-MS/MS under MRM condition.

PubMed

Di Donna, Leonardo; Bartella, Lucia; Napoli, Anna; Sindona, Giovanni; Mazzotti, Fabio

2018-05-16

Monacolin K, the active ingredient present in dietary supplement, is a nutraceutical whose health benefits have been widely documented. A fast approach for the assay of lovastatin in both form, lactone and acid, by mass spectrometry is presented. The quantitative assay is carried out by HPLC-MS/MS using the multiple reaction monitoring (MRM) mode and simvastatin and pravastatin as internal standards. The accuracy values ranged from 97 to 101%; the analytical parameters values of LOQ, LOD, recovery and reproducibility, were calculated analyzing fortified samples, confirming the reliability of the proposed approach. This article is protected by copyright. All rights reserved.

Accuracy evaluation of intraoral optical impressions: A clinical study using a reference appliance.

PubMed

Atieh, Mohammad A; Ritter, André V; Ko, Ching-Chang; Duqum, Ibrahim

2017-09-01

Trueness and precision are used to evaluate the accuracy of intraoral optical impressions. Although the in vivo precision of intraoral optical impressions has been reported, in vivo trueness has not been evaluated because of limitations in the available protocols. The purpose of this clinical study was to compare the accuracy (trueness and precision) of optical and conventional impressions by using a novel study design. Five study participants consented and were enrolled. For each participant, optical and conventional (vinylsiloxanether) impressions of a custom-made intraoral Co-Cr alloy reference appliance fitted to the mandibular arch were obtained by 1 operator. Three-dimensional (3D) digital models were created for stone casts obtained from the conventional impression group and for the reference appliances by using a validated high-accuracy reference scanner. For the optical impression group, 3D digital models were obtained directly from the intraoral scans. The total mean trueness of each impression system was calculated by averaging the mean absolute deviations of the impression replicates from their 3D reference model for each participant, followed by averaging the obtained values across all participants. The total mean precision for each impression system was calculated by averaging the mean absolute deviations between all the impression replicas for each participant (10 pairs), followed by averaging the obtained values across all participants. Data were analyzed using repeated measures ANOVA (α=.05), first to assess whether a systematic difference in trueness or precision of replicate impressions could be found among participants and second to assess whether the mean trueness and precision values differed between the 2 impression systems. Statistically significant differences were found between the 2 impression systems for both mean trueness (P=.010) and mean precision (P=.007). Conventional impressions had higher accuracy with a mean trueness of 17.0 ±6.6 μm and mean precision of 16.9 ±5.8 μm than optical impressions with a mean trueness of 46.2 ±11.4 μm and mean precision of 61.1 ±4.9 μm. Complete arch (first molar-to-first molar) optical impressions were less accurate than conventional impressions but may be adequate for quadrant impressions. Copyright © 2016 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

The null distribution of the heterogeneity lod score does depend on the assumed genetic model for the trait.

PubMed

Huang, J; Vieland, V J

2001-01-01

It is well known that the asymptotic null distribution of the homogeneity lod score (LOD) does not depend on the genetic model specified in the analysis. When appropriately rescaled, the LOD is asymptotically distributed as 0.5 chi(2)(0) + 0.5 chi(2)(1), regardless of the assumed trait model. However, because locus heterogeneity is a common phenomenon, the heterogeneity lod score (HLOD), rather than the LOD itself, is often used in gene mapping studies. We show here that, in contrast with the LOD, the asymptotic null distribution of the HLOD does depend upon the genetic model assumed in the analysis. In affected sib pair (ASP) data, this distribution can be worked out explicitly as (0.5 - c)chi(2)(0) + 0.5chi(2)(1) + cchi(2)(2), where c depends on the assumed trait model. E.g., for a simple dominant model (HLOD/D), c is a function of the disease allele frequency p: for p = 0.01, c = 0.0006; while for p = 0.1, c = 0.059. For a simple recessive model (HLOD/R), c = 0.098 independently of p. This latter (recessive) distribution turns out to be the same as the asymptotic distribution of the MLS statistic under the possible triangle constraint, which is asymptotically equivalent to the HLOD/R. The null distribution of the HLOD/D is close to that of the LOD, because the weight c on the chi(2)(2) component is small. These results mean that the cutoff value for a test of size alpha will tend to be smaller for the HLOD/D than the HLOD/R. For example, the alpha = 0.0001 cutoff (on the lod scale) for the HLOD/D with p = 0.05 is 3.01, while for the LOD it is 3.00, and for the HLOD/R it is 3.27. For general pedigrees, explicit analytical expression of the null HLOD distribution does not appear possible, but it will still depend on the assumed genetic model. Copyright 2001 S. Karger AG, Basel

Three decades after Gjönnaess's laparoscopic ovarian drilling for treatment of PCOS; what do we know? An evidence-based approach.

PubMed

Abu Hashim, Hatem; Al-Inany, Hesham; De Vos, Michel; Tournaye, Herman

2013-08-01

The introduction of laparoscopic ovarian drilling (LOD) by Gjönnaess in 1984 as a substitute for ovarian wedge resection created opportunities for extensive research given its worldwide application for ovulation induction in women with polycystic ovary syndrome (PCOS). To critically evaluate and summarize the current body of literature regarding the role of LOD for the management of PCOS entailing its different preoperative, operative and postoperative aspects. In addition, long-term efficacy, cost-effectiveness, patient preference and health-related quality of life issues will be evaluated together with other available alternatives of ovulation induction treatments. A PubMed search was conducted looking for the different trials, reviews and various guidelines relating to the role of LOD in the management of PCOS. LOD whether unilateral or bilateral is a beneficial second-line treatment in infertile women with clomiphene citrate (CC)-resistant PCOS. It is as effective as gonadotrophin treatment but without the risk of multiple pregnancy or ovarian hyperstimulation and does not require intensive monitoring. Increased responsiveness of the ovary to CC especially in patients who remain anovulatory following LOD is another advantage. Recent evidence suggests that relatively novel oral methods of ovulation induction, e.g. CC plus metformin, CC plus tamoxifen, rosiglitazone plus CC and aromatase inhibitors represent a successful alternative to LOD in CC-resistant PCOS. Meanwhile current evidence does not support LOD as a first-line approach in PCOS-related anovulation or before IVF. LOD is currently recommended as a successful and economical second-line treatment for ovulation induction in women with CC-resistant PCOS.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hoegg, Edward D.; Barinaga, Charles J.; Hager, George J.

ABSTRACT In order to meet a growing need for fieldable mass spectrometer systems for precise elemental and isotopic analyses, the liquid sampling-atmospheric pressure glow discharge (LS-APGD) has a number of very promising characteristics. One key set of attributes that await validation deals with the performance characteristics relative to isotope ratio precision and accuracy. Due to its availability and prior experience with this research team, the initial evaluation of isotope ratio (IR) performance was performed on a Thermo Scientific Exactive Orbitrap instrument. While the mass accuracy and resolution performance for orbitrap analyzers are very well documented, no detailed evaluations of themore » IR performance have been published. Efforts described here involve two variables: the inherent IR precision and accuracy delivered by the LSAPGD microplasma and the inherent IR measurement qualities of orbitrap analyzers. Important to the IR performance, the various operating parameters of the orbitrap sampling interface, HCD dissociation stage, and ion injection/data acquisition have been evaluated. The IR performance for a range of other elements, including natural, depleted, and enriched uranium isotopes was determined. In all cases the precision and accuracy are degraded when measuring low abundance (<0.1% isotope fractions). In the best case, IR precision on the order of 0.1 %RSD can be achieved, with values of 1-3 %RSD observed for low-abundance species. The results suggest that the LSAPGD is a very good candidate for field deployable MS analysis and that the high resolving powers of the orbitrap may be complemented with a here-to-fore unknown capacity to deliver high-precision isotope ratios.« less

75 FR 53730 - Culturally Significant Object Imported for Exhibition Determinations: “The Roman Mosaic from Lod...

Federal Register 2010, 2011, 2012, 2013, 2014

2010-09-01

... DEPARTMENT OF STATE [Public Notice 7145] Culturally Significant Object Imported for Exhibition Determinations: ``The Roman Mosaic from Lod, Israel'' SUMMARY: Notice is hereby given of the following... object to be included in the exhibition ``The Roman Mosaic from Lod, Israel,'' imported from abroad for...

Establishment of National Gravity Base Network of Iran

NASA Astrophysics Data System (ADS)

Hatam Chavari, Y.; Bayer, R.; Hinderer, J.; Ghazavi, K.; Sedighi, M.; Luck, B.; Djamour, Y.; Le Moign, N.; Saadat, R.; Cheraghi, H.

2009-04-01

A gravity base network is supposed to be a set of benchmarks uniformly distributed across the country and the absolute gravity values at the benchmarks are known to the best accessible accuracy. The gravity at the benchmark stations are either measured directly with absolute devices or transferred by gravity difference measurements by gravimeters from known stations. To decrease the accumulation of random measuring errors arising from these transfers, the number of base stations distributed across the country should be as small as possible. This is feasible if the stations are selected near to the national airports long distances apart but faster accessible and measurable by a gravimeter carried in an airplane between the stations. To realize the importance of such a network, various applications of a gravity base network are firstly reviewed. A gravity base network is the required reference frame for establishing 1st , 2nd and 3rd order gravity networks. Such a gravity network is used for the following purposes: a. Mapping of the structure of upper crust in geology maps. The required accuracy for the measured gravity values is about 0.2 to 0.4 mGal. b. Oil and mineral explorations. The required accuracy for the measured gravity values is about 5 µGal. c. Geotechnical studies in mining areas for exploring the underground cavities as well as archeological studies. The required accuracy is about 5 µGal and better. d. Subsurface water resource explorations and mapping crustal layers which absorb it. An accuracy of the same level of previous applications is required here too. e. Studying the tectonics of the Earth's crust. Repeated precise gravity measurements at the gravity network stations can assist us in identifying systematic height changes. The accuracy of the order of 5 µGal and more is required. f. Studying volcanoes and their evolution. Repeated precise gravity measurements at the gravity network stations can provide valuable information on the gradual upward movement of lava. g. Producing precise mean gravity anomaly for precise geoid determination. Replacing precise spirit leveling by the GPS leveling using precise geoid model is one of the forth coming application of the precise geoid. A gravity base network of 28 stations established over Iran. The stations were built mainly at bedrocks. All stations were measured by an FG5 absolute gravimeter, at least 12 hours at each station, to obtain an accuracy of a few micro gals. Several stations were repeated several times during recent years to estimate the gravity changes.

Estimation of suspended-sediment rating curves and mean suspended-sediment loads

USGS Publications Warehouse

Crawford, Charles G.

1991-01-01

A simulation study was done to evaluate: (1) the accuracy and precision of parameter estimates for the bias-corrected, transformed-linear and non-linear models obtained by the method of least squares; (2) the accuracy of mean suspended-sediment loads calculated by the flow-duration, rating-curve method using model parameters obtained by the alternative methods. Parameter estimates obtained by least squares for the bias-corrected, transformed-linear model were considerably more precise than those obtained for the non-linear or weighted non-linear model. The accuracy of parameter estimates obtained for the biascorrected, transformed-linear and weighted non-linear model was similar and was much greater than the accuracy obtained by non-linear least squares. The improved parameter estimates obtained by the biascorrected, transformed-linear or weighted non-linear model yield estimates of mean suspended-sediment load calculated by the flow-duration, rating-curve method that are more accurate and precise than those obtained for the non-linear model.

LOD 1 VS. LOD 2 - Preliminary Investigations Into Differences in Mobile Rendering Performance

NASA Astrophysics Data System (ADS)

Ellul, C.; Altenbuchner, J.

2013-09-01

The increasing availability, size and detail of 3D City Model datasets has led to a challenge when rendering such data on mobile devices. Understanding the limitations to the usability of such models on these devices is particularly important given the broadening range of applications - such as pollution or noise modelling, tourism, planning, solar potential - for which these datasets and resulting visualisations can be utilized. Much 3D City Model data is created by extrusion of 2D topographic datasets, resulting in what is known as Level of Detail (LoD) 1 buildings - with flat roofs. However, in the UK the National Mapping Agency (the Ordnance Survey, OS) is now releasing test datasets to Level of Detail (LoD) 2 - i.e. including roof structures. These datasets are designed to integrate with the LoD 1 datasets provided by the OS, and provide additional detail in particular on larger buildings and in town centres. The availability of such integrated datasets at two different Levels of Detail permits investigation into the impact of the additional roof structures (and hence the display of a more realistic 3D City Model) on rendering performance on a mobile device. This paper describes preliminary work carried out to investigate this issue, for the test area of the city of Sheffield (in the UK Midlands). The data is stored in a 3D spatial database as triangles and then extracted and served as a web-based data stream which is queried by an App developed on the mobile device (using the Android environment, Java and OpenGL for graphics). Initial tests have been carried out on two dataset sizes, for the city centre and a larger area, rendering the data onto a tablet to compare results. Results of 52 seconds for rendering LoD 1 data, and 72 seconds for LoD 1 mixed with LoD 2 data, show that the impact of LoD 2 is significant.

Genome-wide linkage scans for type 2 diabetes mellitus in four ethnically diverse populations-significant evidence for linkage on chromosome 4q in African Americans: the Family Investigation of Nephropathy and Diabetes Research Group.

PubMed

Malhotra, Alka; Igo, Robert P; Thameem, Farook; Kao, W H Linda; Abboud, Hanna E; Adler, Sharon G; Arar, Nedal H; Bowden, Donald W; Duggirala, Ravindranath; Freedman, Barry I; Goddard, Katrina A B; Ipp, Eli; Iyengar, Sudha K; Kimmel, Paul L; Knowler, William C; Kohn, Orly; Leehey, David; Meoni, Lucy A; Nelson, Robert G; Nicholas, Susanne B; Parekh, Rulan S; Rich, Stephen S; Chen, Yii-Der I; Saad, Mohammed F; Scavini, Marina; Schelling, Jeffrey R; Sedor, John R; Shah, Vallabh O; Taylor, Kent D; Thornley-Brown, Denyse; Zager, Philip G; Horvath, Amanda; Hanson, Robert L

2009-11-01

Previous studies have shown that in addition to environmental influences, type 2 diabetes mellitus (T2DM) has a strong genetic component. The goal of the current study is to identify regions of linkage for T2DM in ethnically diverse populations. Phenotypic and genotypic data were obtained from African American (AA; total number of individuals [N] = 1004), American Indian (AI; N = 883), European American (EA; N = 537), and Mexican American (MA; N = 1634) individuals from the Family Investigation of Nephropathy and Diabetes. Non-parametric linkage analysis, using an average of 4404 SNPs, was performed in relative pairs affected with T2DM in each ethnic group. In addition, family-based tests were performed to detect association with T2DM. Statistically significant evidence for linkage was observed on chromosome 4q21.1 (LOD = 3.13; genome-wide p = 0.04) in AA. In addition, a total of 11 regions showed suggestive evidence for linkage (estimated at LOD > 1.71), with the highest LOD scores on chromosomes 12q21.31 (LOD = 2.02) and 22q12.3 (LOD = 2.38) in AA, 2p11.1 (LOD = 2.23) in AI, 6p12.3 (LOD = 2.77) in EA, and 13q21.1 (LOD = . 2.24) in MA. While no region overlapped across all ethnic groups, at least five loci showing LOD > 1.71 have been identified in previously published studies. The results from this study provide evidence for the presence of genes affecting T2DM on chromosomes 4q, 12q, and 22q in AA; 6p in EA; 2p in AI; and 13q in MA. The strong evidence for linkage on chromosome 4q in AA provides important information given the paucity of diabetes genetic studies in this population.

LAI-2000 Accuracy, Precision, and Application to Visual Estimation of Leaf Area Index of Loblolly Pine

Treesearch

Jason A. Gatch; Timothy B. Harrington; James P. Castleberry

2002-01-01

Leaf area index (LAI) is an important parameter of forest stand productivity that has been used to diagnose stand vigor and potential fertilizer response of southern pines. The LAI-2000 was tested for its ability to provide accurate and precise estimates of LAI of loblolly pine (Pinus taeda L.). To test instrument accuracy, regression was used to...

40 CFR 86.110-90 - Exhaust gas sampling system; diesel vehicles.

Code of Federal Regulations, 2010 CFR

2010-07-01

... probe. The sensor shall have an accuracy and precision of ±2 °F (1.1 °C). (14) The dilute exhaust gas... probe. The sensor shall have an accuracy and precision of ±2 °F (1.1 °C). (14) The dilute exhaust gas... 40 Protection of Environment 18 2010-07-01 2010-07-01 false Exhaust gas sampling system; diesel...

40 CFR 86.110-90 - Exhaust gas sampling system; diesel vehicles.

Code of Federal Regulations, 2011 CFR

2011-07-01

... probe. The sensor shall have an accuracy and precision of ±2 °F (1.1 °C). (14) The dilute exhaust gas... probe. The sensor shall have an accuracy and precision of ±2 °F (1.1 °C). (14) The dilute exhaust gas... 40 Protection of Environment 18 2011-07-01 2011-07-01 false Exhaust gas sampling system; diesel...

Effects of lodoxamide (LOD), disodium cromoglycate (DSCG) and N-acetyl-aspartyl-glutamate sodium salt (NAAGA) on ocular active anaphylaxis.

PubMed

Goldschmidt, P; Luyckx, J

1996-04-01

LOD, DSCG and NAAGA eye-drops were evaluated on experimentally-induced ocular active anaphylaxis in guinea pigs. Twelve animals per group were sensitized with egg albumin i.p. and challenged on the surface of the eye 14 days later. Two days before challenge, animals were treated with LOD, DSCG or NAAGA 4 times a day. Permeability indexes were calculated after intracardiac injection of Evans Blue. No effect on ocular active anaphylaxis was found with LOD nor with DSCG. NAAGA was able to significantly reduce blood-eye permeability indexes.

Wavelet analysis of interannual LOD, AAM, and ENSO: 1997-98 El Niño and 1998-99 La Niña signals

NASA Astrophysics Data System (ADS)

Zhou, Y. H.; Zheng, D. W.; Liao, X. H.

2001-05-01

On the basis of the data series of the length of day (LOD), the atmospheric angular momentum (AAM) and the Southern Oscillation Index (SOI) for January 1970-June 1999, the relationship among Interannual LOD, AAM, and the EL Niño/Southern Oscillation (ENSO) is analyzed by the wavelet transform method. The results suggest that they have similar time-varying spectral structures. The signals of 1997-98 El Niño and 1998-99 La Niña events can be detected from the LOD or AAM data.

Magnetic field variation caused by rotational speed change in a magnetohydrodynamic dynamo.

PubMed

Miyagoshi, Takehiro; Hamano, Yozo

2013-09-20

We have performed numerical magnetohydrodynamic dynamo simulations in a spherical shell with rotational speed or length-of-day (LOD) variation, which is motivated by correlations between geomagnetic field and climatic variations with ice and non-ice ages. The results show that LOD variation leads to magnetic field variation whose amplitude is considerably larger than that of LOD variation. The heat flux at the outer sphere and the zonal flow also change. The mechanism of the magnetic field variation due to LOD variation is also found. The keys are changes of dynamo activity and Joule heating.

Evaluation of accuracy and precision of a smartphone based automated parasite egg counting system in comparison to the McMaster and Mini-FLOTAC methods.

PubMed

Scare, J A; Slusarewicz, P; Noel, M L; Wielgus, K M; Nielsen, M K

2017-11-30

Fecal egg counts are emphasized for guiding equine helminth parasite control regimens due to the rise of anthelmintic resistance. This, however, poses further challenges, since egg counting results are prone to issues such as operator dependency, method variability, equipment requirements, and time commitment. The use of image analysis software for performing fecal egg counts is promoted in recent studies to reduce the operator dependency associated with manual counts. In an attempt to remove operator dependency associated with current methods, we developed a diagnostic system that utilizes a smartphone and employs image analysis to generate automated egg counts. The aims of this study were (1) to determine precision of the first smartphone prototype, the modified McMaster and ImageJ; (2) to determine precision, accuracy, sensitivity, and specificity of the second smartphone prototype, the modified McMaster, and Mini-FLOTAC techniques. Repeated counts on fecal samples naturally infected with equine strongyle eggs were performed using each technique to evaluate precision. Triplicate counts on 36 egg count negative samples and 36 samples spiked with strongyle eggs at 5, 50, 500, and 1000 eggs per gram were performed using a second smartphone system prototype, Mini-FLOTAC, and McMaster to determine technique accuracy. Precision across the techniques was evaluated using the coefficient of variation. In regards to the first aim of the study, the McMaster technique performed with significantly less variance than the first smartphone prototype and ImageJ (p<0.0001). The smartphone and ImageJ performed with equal variance. In regards to the second aim of the study, the second smartphone system prototype had significantly better precision than the McMaster (p<0.0001) and Mini-FLOTAC (p<0.0001) methods, and the Mini-FLOTAC was significantly more precise than the McMaster (p=0.0228). Mean accuracies for the Mini-FLOTAC, McMaster, and smartphone system were 64.51%, 21.67%, and 32.53%, respectively. The Mini-FLOTAC was significantly more accurate than the McMaster (p<0.0001) and the smartphone system (p<0.0001), while the smartphone and McMaster counts did not have statistically different accuracies. Overall, the smartphone system compared favorably to manual methods with regards to precision, and reasonably with regards to accuracy. With further refinement, this system could become useful in veterinary practice. Copyright © 2017 Elsevier B.V. All rights reserved.

Quantitative determination of total cesium in highly active liquid waste by using liquid electrode plasma optical emission spectrometry.

PubMed

Do, Van-Khoai; Yamamoto, Masahiko; Taguchi, Shigeo; Takamura, Yuzuru; Surugaya, Naoki; Kuno, Takehiko

2018-06-01

A sensitive analytical method for determination of total cesium (Cs) in highly active liquid waste (HALW) by using modified liquid electrode plasma optical emission spectrometry (LEP-OES) is developed in this study. The instrument is modified to measure radioactive samples in a glove box. The effects of important factors, including pulsed voltage sequence and nitric acid concentration, on the emission of Cs are investigated. The limit of detection (LOD) and limit of quantification (LOQ) are 0.005 mg/L and 0.02 mg/L, respectively. The achieved LOD is one order lower than that of recently developed spectroscopic methods using liquid discharge plasma. The developed method is validated by subjecting a simulated HALW sample to inductively coupled plasma mass spectrometry (ICP-MS). The recoveries obtained from a spike-and-recovery test are 96-102%, implying good accuracy. The method is successfully applied to the quantification of Cs in a real HALW sample at the Tokai reprocessing plant in Japan. Apart from dilution and filtration of the HALW sample, no other pre-treatment process is required. The results agree well with the values obtained using gamma spectrometry. The developed method offers a reliable technique for rapid analysis of total Cs in HALW samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Sensor-Based Inspection of the Formation Accuracy in Ultra-Precision Grinding (UPG) of Aspheric Surface Considering the Chatter Vibration

NASA Astrophysics Data System (ADS)

Lei, Yao; Bai, Yue; Xu, Zhijun

2018-06-01

This paper proposes an experimental approach for monitoring and inspection of the formation accuracy in ultra-precision grinding (UPG) with respect to the chatter vibration. Two factors related to the grinding progress, the grinding speed of grinding wheel and spindle, and the oil pressure of the hydrostatic bearing are taken into account to determining the accuracy. In the meantime, a mathematical model of the radius deviation caused by the micro vibration is also established and applied in the experiments. The results show that the accuracy is sensitive to the vibration and the forming accuracy is much improved with proper processing parameters. It is found that the accuracy of aspheric surface can be less than 4 μm when the grinding speed is 1400 r/min and the wheel speed is 100 r/min with the oil pressure being 1.1 MPa.

Revisiting a possible relationship between solar activity and Earth rotation variability

NASA Astrophysics Data System (ADS)

Abarca del Rio, R.; Gambis, D.

2011-10-01

A variety of studies have searched to establish a possible relationship between the solar activity and earth variations (Danjon, 1958-1962; Challinor, 1971; Currie, 1980, Gambis, 1990). We are revisiting previous studies (Bourget et al, 1992, Abarca del Rio et al, 2003, Marris et al, 2004) concerning the possible relationship between solar activity variability and length of day (LOD) variations at decadal time scales. Assuming that changes in AAM for the entire atmosphere are accompanied by equal, but opposite, changes in the angular momentum of the earth it is possible to infer changes in LOD from global AAM time series, through the relation : delta (LOD) (ms) = 1.68 10^29 delta(AAM) (kgm2/s) (Rosen and Salstein, 1983), where δ(LOD) is given in milliseconds. Given the close relationship at seasonal to interannual time's scales between LOD and the Atmospheric Angular Momentum (AAM) (see Abarca del Rio et al., 2003) it is possible to infer from century long atmospheric simulations what may have been the variability in the associated LOD variability throughout the last century. In the absence of a homogeneous century long LOD time series, we take advantage of the recent atmospheric reanalyzes extending since 1871 (Compo, Whitaker and Sardeshmukh, 2006). The atmospheric data (winds) of these reanalyzes allow computing AAM up to the top of the atmosphere; though here only troposphere data (up to 100 hPa) was taken into account.

Use of single-representative reverse-engineered surface-models for RSA does not affect measurement accuracy and precision.

PubMed

Seehaus, Frank; Schwarze, Michael; Flörkemeier, Thilo; von Lewinski, Gabriela; Kaptein, Bart L; Jakubowitz, Eike; Hurschler, Christof

2016-05-01

Implant migration can be accurately quantified by model-based Roentgen stereophotogrammetric analysis (RSA), using an implant surface model to locate the implant relative to the bone. In a clinical situation, a single reverse engineering (RE) model for each implant type and size is used. It is unclear to what extent the accuracy and precision of migration measurement is affected by implant manufacturing variability unaccounted for by a single representative model. Individual RE models were generated for five short-stem hip implants of the same type and size. Two phantom analyses and one clinical analysis were performed: "Accuracy-matched models": one stem was assessed, and the results from the original RE model were compared with randomly selected models. "Accuracy-random model": each of the five stems was assessed and analyzed using one randomly selected RE model. "Precision-clinical setting": implant migration was calculated for eight patients, and all five available RE models were applied to each case. For the two phantom experiments, the 95%CI of the bias ranged from -0.28 mm to 0.30 mm for translation and -2.3° to 2.5° for rotation. In the clinical setting, precision is less than 0.5 mm and 1.2° for translation and rotation, respectively, except for rotations about the proximodistal axis (<4.1°). High accuracy and precision of model-based RSA can be achieved and are not biased by using a single representative RE model. At least for implants similar in shape to the investigated short-stem, individual models are not necessary. © 2015 Orthopaedic Research Society. Published by Wiley Periodicals, Inc. J Orthop Res 34:903-910, 2016. © 2015 Orthopaedic Research Society. Published by Wiley Periodicals, Inc.

A literature review of anthropometric studies of school students for ergonomics purposes: Are accuracy, precision and reliability being considered?

PubMed

Bravo, G; Bragança, S; Arezes, P M; Molenbroek, J F M; Castellucci, H I

2018-05-22

Despite offering many benefits, direct manual anthropometric measurement method can be problematic due to their vulnerability to measurement errors. The purpose of this literature review was to determine, whether or not the currently published anthropometric studies of school children, related to ergonomics, mentioned or evaluated the variables precision, reliability or accuracy in the direct manual measurement method. Two bibliographic databases, and the bibliographic references of all the selected papers were used for finding relevant published papers in the fields considered in this study. Forty-six (46) studies met the criteria previously defined for this literature review. However, only ten (10) studies mentioned at least one of the analyzed variables, and none has evaluated all of them. Only reliability was assessed by three papers. Moreover, in what regards the factors that affect precision, reliability and accuracy, the reviewed papers presented large differences. This was particularly clear in the instruments used for the measurements, which were not consistent throughout the studies. Additionally, it was also clear that there was a lack of information regarding the evaluators' training and procedures for anthropometric data collection, which are assumed to be the most important issues that affect precision, reliability and accuracy. Based on the review of the literature, it was possible to conclude that the considered anthropometric studies had not focused their attention to the analysis of precision, reliability and accuracy of the manual measurement methods. Hence, and with the aim of avoiding measurement errors and misleading data, anthropometric studies should put more efforts and care on testing measurement error and defining the procedures used to collect anthropometric data.

The Use of Daily Geodetic UT1 and LOD Data in the Optimal Estimation of UT1 and LOD With the JPL Kalman Earth Orientation Filter

NASA Technical Reports Server (NTRS)

Freedman, A. P.; Steppe, J. A.

1995-01-01

The Jet Propulsion Laboratory Kalman Earth Orientation Filter (KEOF) uses several of the Earth rotation data sets available to generate optimally interpolated UT1 and LOD series to support spacecraft navigation. This paper compares use of various data sets within KEOF.

Determining the 95% limit of detection for waterborne pathogen analyses from primary concentration to qPCR

USDA-ARS?s Scientific Manuscript database

The limit of detection (LOD) for qPCR-based analyses is not consistently defined or determined in studies on waterborne pathogens. Moreover, the LODs reported often reflect the qPCR assay rather than the entire sample process. Our objective was to develop a method to determine the 95% LOD (lowest co...

A Comparative Study of Precise Point Positioning (PPP) Accuracy Using Online Services

NASA Astrophysics Data System (ADS)

Malinowski, Marcin; Kwiecień, Janusz

2016-12-01

Precise Point Positioning (PPP) is a technique used to determine the position of receiver antenna without communication with the reference station. It may be an alternative solution to differential measurements, where maintaining a connection with a single RTK station or a regional network of reference stations RTN is necessary. This situation is especially common in areas with poorly developed infrastructure of ground stations. A lot of research conducted so far on the use of the PPP technique has been concerned about the development of entire day observation sessions. However, this paper presents the results of a comparative analysis of accuracy of absolute determination of position from observations which last between 1 to 7 hours with the use of four permanent services which execute calculations with PPP technique such as: Automatic Precise Positioning Service (APPS), Canadian Spatial Reference System Precise Point Positioning (CSRS-PPP), GNSS Analysis and Positioning Software (GAPS) and magicPPP - Precise Point Positioning Solution (magicGNSS). On the basis of acquired results of measurements, it can be concluded that at least two-hour long measurements allow acquiring an absolute position with an accuracy of 2-4 cm. An evaluation of the impact on the accuracy of simultaneous positioning of three points test network on the change of the horizontal distance and the relative height difference between measured triangle vertices was also conducted. Distances and relative height differences between points of the triangular test network measured with a laser station Leica TDRA6000 were adopted as references. The analyses of results show that at least two hours long measurement sessions can be used to determine the horizontal distance or the difference in height with an accuracy of 1-2 cm. Rapid products employed in calculations conducted with PPP technique reached the accuracy of determining coordinates on a close level as in elaborations which employ Final products.

Electromagnetic tracking (EMT) technology for improved treatment quality assurance in interstitial brachytherapy.

PubMed

Kellermeier, Markus; Herbolzheimer, Jens; Kreppner, Stephan; Lotter, Michael; Strnad, Vratislav; Bert, Christoph

2017-01-01

Electromagnetic Tracking (EMT) is a novel technique for error detection and quality assurance (QA) in interstitial high dose rate brachytherapy (HDR-iBT). The purpose of this study is to provide a concept for data acquisition developed as part of a clinical evaluation study on the use of EMT during interstitial treatment of breast cancer patients. The stability, accuracy, and precision of EMT-determined dwell positions were quantified. Dwell position reconstruction based on EMT was investigated on CT table, HDR table and PDR bed to examine the influence on precision and accuracy in a typical clinical workflow. All investigations were performed using a precise PMMA phantom. The track of catheters inserted in that phantom was measured by manually inserting a 5 degree of freedom (DoF) sensor while recording the position of three 6DoF fiducial sensors on the phantom surface to correct motion influences. From the corrected data, dwell positions were reconstructed along the catheter's track. The accuracy of the EMT-determined dwell positions was quantified by the residual distances to reference dwell positions after using a rigid registration. Precision and accuracy were investigated for different phantom-table and sensor-field generator (FG) distances. The measured precision of the EMT-determined dwell positions was ≤ 0.28 mm (95th percentile). Stability tests showed a drift of 0.03 mm in the first 20 min of use. Sudden shaking of the FG or (large) metallic objects close to the FG degrade the precision. The accuracy with respect to the reference dwell positions was on all clinical tables < 1 mm at 200 mm FG distance and 120 mm phantom-table distance. Phantom measurements showed that EMT-determined localization of dwell positions in HDR-iBT is stable, precise, and sufficiently accurate for clinical assessment. The presented method may be viable for clinical applications in HDR-iBT, like implant definition, error detection or quantification of uncertainties. Further clinical investigations are needed. © 2017 The Authors. Journal of Applied Clinical Medical Physics published by Wiley Periodicals, Inc. on behalf of American Association of Physicists in Medicine.

Evaluation of carbon aerogel-based solid-phase extraction sorbent for the analysis of sulfur mustard degradation products in environmental water samples.

PubMed

Jõul, Piia; Vaher, Merike; Kuhtinskaja, Maria

2018-05-01

In this study, SPE method using a carbon aerogel(CA)-based sorbent was developed and evaluated for the simultaneous extraction of sulfur mustard (HD) degradation products from environmental water samples. Applied CAs proved to be very promising materials for use as SPE sorbents, due to their high porosity, very low density and a large specific surface area. 10 degradation products of HD, both aliphatic and cyclic (thiodiglycol (TDG), TDG sulfoxide, TDG sulfone, 3,5-dithia-1,7-heptanediol, 3,6-dithia-1,8-octanediol, 1,4-thioxane, 1,3-dithiolane, 1,4-dithiane, 1,2,5-trithiepane, and 1,4,5-oxadithiepane) were extracted on a CA-based SPE cartridge. The concentrations of target analytes in the eluate were determined by HPLC-DAD and CE-DAD. Several parameters affecting the extraction efficiency, including the kind and volume of the eluting solvent, sample loading flow rate, volume and ionic strength as well as the reusability of the cartridge, were investigated and optimized to achieve the best performance for the analytes. A series of quantitative parameters such as linear range, coefficient of determination, LOD, LOQ and precision were examined under the optimized conditions. High sensitivity (LODs 0.17-0.50 μM) and high precision (intraday RSD = 2.0-7.7% and interday RSD = 2.7-9.9%) for all the analytes were achieved. The performance of the CA-based sorbent was compared with that of commonly used SPE sorbents. Applied for the analysis of spiked pore water samples collected from the Bornholm Basin, one of the largest chemical warfare dumping sites in the Baltic Sea, the proposed method allowed high SPE recoveries of all the analytes ranging from 83.5 to 99.7% to be obtained. Copyright © 2018 Elsevier Ltd. All rights reserved.

Further evidence for the increased power of LOD scores compared with nonparametric methods.

PubMed

Durner, M; Vieland, V J; Greenberg, D A

1999-01-01

In genetic analysis of diseases in which the underlying model is unknown, "model free" methods-such as affected sib pair (ASP) tests-are often preferred over LOD-score methods, although LOD-score methods under the correct or even approximately correct model are more powerful than ASP tests. However, there might be circumstances in which nonparametric methods will outperform LOD-score methods. Recently, Dizier et al. reported that, in some complex two-locus (2L) models, LOD-score methods with segregation analysis-derived parameters had less power to detect linkage than ASP tests. We investigated whether these particular models, in fact, represent a situation that ASP tests are more powerful than LOD scores. We simulated data according to the parameters specified by Dizier et al. and analyzed the data by using a (a) single locus (SL) LOD-score analysis performed twice, under a simple dominant and a recessive mode of inheritance (MOI), (b) ASP methods, and (c) nonparametric linkage (NPL) analysis. We show that SL analysis performed twice and corrected for the type I-error increase due to multiple testing yields almost as much linkage information as does an analysis under the correct 2L model and is more powerful than either the ASP method or the NPL method. We demonstrate that, even for complex genetic models, the most important condition for linkage analysis is that the assumed MOI at the disease locus being tested is approximately correct, not that the inheritance of the disease per se is correctly specified. In the analysis by Dizier et al., segregation analysis led to estimates of dominance parameters that were grossly misspecified for the locus tested in those models in which ASP tests appeared to be more powerful than LOD-score analyses.

Melancholia in later life: late and early onset differences in presentation, course, and dementia risk.

PubMed

Sachs-Ericsson, Natalie; Moxley, Jerad H; Corsentino, Elizabeth; Rushing, Nicole Collins; Sheffler, Julia; Selby, Edward A; Gotlib, Ian; Steffens, David C

2014-09-01

Depression is a risk factor for cognitive decline and dementia. This risk may vary with age of onset and depression subtype. Late onset depression (LOD, 60 years and older) is associated with more cognitive decline, whereas early onset depression (EOD, before 60 years) is associated with more residual depressive symptoms. Potential differences may reflect divergent etiologies. These onset differences, however, have not been examined in the melancholic subtype of depression in older adults. Data were obtained from the Neurocognitive Outcomes of Depression in the Elderly study. Participants (N = 284, 73% EOD-melancholic (EOD-M) and 27% LOD-melancholic (LOD-M)) were followed up over 3 years. Factor analyses examined differences in baseline depressive symptoms. Hierarchical linear growth curve models examined changes in depressive symptoms (Montgomery-Asberg Depression Rating Scale) and cognition (mini mental state examination). An annual clinical review panel assigned diagnoses of dementia. The LOD-M participants had more vegetative symptoms at baseline. LOD-M exhibited greater cognitive decline but fewer residual depressive symptoms than EOD-M. Among participants who remained in the study for at least 1 year, in uncontrolled analyses, a greater percentage of LOD-M compared with EOD-M developed dementia (23.0% vs. 7.8%). Whereas in logistic analyses, controlling for baseline demographics, age at onset remained a predictor of dementia, the odds ratio suggested that the effect was relatively small. The EOD-M and LOD-M participants have a different presentation and course. LOD-M may represent a syndrome of neuropsychiatric deterioration with expression of both depressive symptoms and cognitive decline. Copyright © 2014 John Wiley & Sons, Ltd.

Evidence for a gene influencing the TG/HDL-C ratio on chromosome 7q32.3-qter: a genome-wide scan in the Framingham study.

PubMed

Shearman, A M; Ordovas, J M; Cupples, L A; Schaefer, E J; Harmon, M D; Shao, Y; Keen, J D; DeStefano, A L; Joost, O; Wilson, P W; Housman, D E; Myers, R H

2000-05-22

Some studies show that plasma triglyceride (TG) levels are a significant independent risk factor for cardiovascular disease (CVD). TG levels are inversely correlated with high density lipoprotein cholesterol (HDL-C) levels, and their metabolism may be closely interrelated. Therefore, the TG/HDL-C ratio may be a relevant CVD risk factor. Our analysis of families in the Framingham Heart Study gave a genetic heritability estimate for log(TG) of 0.40 and for log(TG/HDL-C) of 0.49, demonstrating an important genetic component for both. A 10 cM genome-wide scan for log(TG) level and log(TG/HDL-C) was carried out for the largest 332 extended families of the Framingham Heart Study (1702 genotyped individuals). The highest multipoint variance component LOD scores obtained for both log(TG) and log(TG/HDL-C) were on chromosome 7 (at 155 cM), where the results for the two phenotypes were 1.8 and 2.5, respectively. The 7q32.3-qter region contains several candidate genes. Four other regions with multipoint LOD scores greater than one were identified on chromosome 3 [LOD score for log(TG/HDL-C) = 1.8 at 140 cM], chromosome 11 [LOD score for log(TG/HDL-C) = 1.1 at 125 cM], chromosome 16 [LOD score for log(TG) = 1.5 at 70 cM, LOD score for log(TG/HDL-C) = 1.1 at 75 cM] and chromosome 20 [LOD score for log(TG/HDL-C) = 1.7 at 35 cM, LOD score for log(TG) = 1.3 at 40 cM]. These results identify loci worthy of further study.

Forecasting irregular variations of UT1-UTC and LOD data caused by ENSO

NASA Astrophysics Data System (ADS)

Niedzielski, T.; Kosek, W.

2008-04-01

The research focuses on prediction of LOD and UT1-UTC time series up to one-year in the future with the particular emphasis on the prediction improvement during El Nĩ o or La Nĩ a n n events. The polynomial-harmonic least-squares model is applied to fit the deterministic function to LOD data. The stochastic residuals computed as the difference between LOD data and the polynomial- harmonic model reveal the extreme values driven by El Nĩ o or La Nĩ a. These peaks are modeled by the n n stochastic bivariate autoregressive prediction. This approach focuses on the auto- and cross-correlations between LOD and the axial component of the atmospheric angular momentum. This technique allows one to derive more accurate predictions than purely univariate forecasts, particularly during El Nĩ o/La n Nĩ a events. n

Changes in ovarian reserve and ovarian blood flow in patients with polycystic ovary syndrome following laparoscopic ovarian drilling.

PubMed

Kamal, Nasser; Sanad, Zakaria; Elkelani, Osama; Rezk, Mohamed; Shawky, Mohamed; Sharaf, Abd-Elbar

2018-04-10

This prospective cohort study was conducted on 80 patients with clomiphene citrate (CC)-resistant polycystic ovary syndrome undergoing laparoscopic ovarian drilling (LOD). Pre- and post-LOD ovarian reserve parameters (anti-Mullerian hormone: AMH, ovarian volume: OV, and antral follicle count: AFC) and ovarian stromal blood flow indices (Vascularization index: VI, flow index: FI, and vascularization flow index: VFI) were measured to explore the effect of LOD and to find out the correlation between serum AMH and different clinical, hormonal, and ultrasonic variables. There was a highly significant reduction of the serum AMH (p < .001) after LOD with significant reduction in OV, AFC and vascular indices (VI, FI and VFI) of the right and left ovaries (p < .05). LOD significantly reduced ovarian reserve parameters (AMH, OV and AFC) and ovarian stromal blood flow indices (VI, FI and VFI) with no observed correlation between AMH levels and Doppler indices.

Improving multi-GNSS ultra-rapid orbit determination for real-time precise point positioning

NASA Astrophysics Data System (ADS)

Li, Xingxing; Chen, Xinghan; Ge, Maorong; Schuh, Harald

2018-03-01

Currently, with the rapid development of multi-constellation Global Navigation Satellite Systems (GNSS), the real-time positioning and navigation are undergoing dramatic changes with potential for a better performance. To provide more precise and reliable ultra-rapid orbits is critical for multi-GNSS real-time positioning, especially for the three merging constellations Beidou, Galileo and QZSS which are still under construction. In this contribution, we present a five-system precise orbit determination (POD) strategy to fully exploit the GPS + GLONASS + BDS + Galileo + QZSS observations from CDDIS + IGN + BKG archives for the realization of hourly five-constellation ultra-rapid orbit update. After adopting the optimized 2-day POD solution (updated every hour), the predicted orbit accuracy can be obviously improved for all the five satellite systems in comparison to the conventional 1-day POD solution (updated every 3 h). The orbit accuracy for the BDS IGSO satellites can be improved by about 80, 45 and 50% in the radial, cross and along directions, respectively, while the corresponding accuracy improvement for the BDS MEO satellites reaches about 50, 20 and 50% in the three directions, respectively. Furthermore, the multi-GNSS real-time precise point positioning (PPP) ambiguity resolution has been performed by using the improved precise satellite orbits. Numerous results indicate that combined GPS + BDS + GLONASS + Galileo (GCRE) kinematic PPP ambiguity resolution (AR) solutions can achieve the shortest time to first fix (TTFF) and highest positioning accuracy in all coordinate components. With the addition of the BDS, GLONASS and Galileo observations to the GPS-only processing, the GCRE PPP AR solution achieves the shortest average TTFF of 11 min with 7{°} cutoff elevation, while the TTFF of GPS-only, GR, GE and GC PPP AR solution is 28, 15, 20 and 17 min, respectively. As the cutoff elevation increases, the reliability and accuracy of GPS-only PPP AR solutions decrease dramatically, but there is no evident decrease for the accuracy of GCRE fixed solutions which can still achieve an accuracy of a few centimeters in the east and north components.

Calorimetry of low mass Pu239 items

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cremers, Teresa L; Sampson, Thomas E

2010-01-01

Calorimetric assay has the reputation of providing the highest precision and accuracy of all nondestructive assay measurements. Unfortunately, non-destructive assay practitioners and measurement consumers often extend, inappropriately, the high precision and accuracy of calorimetric assay to very low mass items. One purpose of this document is to present more realistic expectations for the random uncertainties associated with calorimetric assay for weapons grade plutonium items with masses of 200 grams or less.

Location Technologies for Apparel Assembly

DTIC Science & Technology

1991-09-01

ADDRESS (Stry, State, and ZIP Code) School of Textile & Fiber Engineering Georgia Institute of Technology Atlanta, Georgia 30332-0295 206 O’Keefe...at a cost of less than $500. A review is also given of state-of-the- art vision systems. These systems have the nccessry- accuracy and precision for...of state-of-the- art vision systems. These systems have the necessary accuracy and precision for apparel manufacturing applications and could

Measuring changes in Plasmodium falciparum transmission: Precision, accuracy and costs of metrics

PubMed Central

Tusting, Lucy S.; Bousema, Teun; Smith, David L.; Drakeley, Chris

2016-01-01

As malaria declines in parts of Africa and elsewhere, and as more countries move towards elimination, it is necessary to robustly evaluate the effect of interventions and control programmes on malaria transmission. To help guide the appropriate design of trials to evaluate transmission-reducing interventions, we review eleven metrics of malaria transmission, discussing their accuracy, precision, collection methods and costs, and presenting an overall critique. We also review the non-linear scaling relationships between five metrics of malaria transmission; the entomological inoculation rate, force of infection, sporozoite rate, parasite rate and the basic reproductive number, R0. Our review highlights that while the entomological inoculation rate is widely considered the gold standard metric of malaria transmission and may be necessary for measuring changes in transmission in highly endemic areas, it has limited precision and accuracy and more standardised methods for its collection are required. In areas of low transmission, parasite rate, sero-conversion rates and molecular metrics including MOI and mFOI may be most appropriate. When assessing a specific intervention, the most relevant effects will be detected by examining the metrics most directly affected by that intervention. Future work should aim to better quantify the precision and accuracy of malaria metrics and to improve methods for their collection. PMID:24480314

[Precision and accuracy of "a pocket" pulse oximeter in Mexico City].

PubMed

Torre-Bouscoulet, Luis; Chávez-Plascencia, Elizabeth; Vázquez-García, Juan Carlos; Pérez-Padilla, Rogelio

2006-01-01

Pulse oximeters are frequently used in the clinical practice and we must known their precision and accuracy. The objective was to evaluate the precision and accuracy of a "pocket" pulse oximeter at an altitude of 2,240 m above sea level. We tested miniature pulse oximeters (Onyx 9,500, Nonin Finger Pulse Oximeter) in 96 patients sent to the pulmonary laboratory for an arterial blood sample. Patients were tested with 5 pulse oximeters placed in each of the fingers of the hand oposite to that used for the arterial puncture. The gold standard was the oxygen saturation of the arterial blood sample. Blood samples had SaO2 of 87.2 +/- 11.0 (between 42.2 and 97.9%). Pulse oximeters had a mean error of 0.28 +/- 3.1%. SaO2 = (1.204 x SpO2) - 17.45966 (r = 0.92, p < 0.0001). Intraclass correlation coefficient between each of five pulse oximeters against the arterial blood standard ranged between 0.87 and 0.99. HbCO (2.4 +/- 0.6) did not affect the accuracy. The miniature oximeter Nonin is precise and accurate at 2,240 m of altitude. The observed levels of HbCO did not affect the performance of the equipment. The oximeter good performance, small size and low cost enhances its clinical usefulness.

Sex differences in accuracy and precision when judging time to arrival: data from two Internet studies.

PubMed

Sanders, Geoff; Sinclair, Kamila

2011-12-01

We report two Internet studies that investigated sex differences in the accuracy and precision of judging time to arrival. We used accuracy to mean the ability to match the actual time to arrival and precision to mean the consistency with which each participant made their judgments. Our task was presented as a computer game in which a toy UFO moved obliquely towards the participant through a virtual three-dimensional space on route to a docking station. The UFO disappeared before docking and participants pressed their space bar at the precise moment they thought the UFO would have docked. Study 1 showed it was possible to conduct quantitative studies of spatiotemporal judgments in virtual reality via the Internet and confirmed reports that men are more accurate because women underestimate, but found no difference in precision measured as intra-participant variation. Study 2 repeated Study 1 with five additional presentations of one condition to provide a better measure of precision. Again, men were more accurate than women but there were no sex differences in precision. However, within the coincidence-anticipation timing (CAT) literature, of those studies that report sex differences, a majority found that males are both more accurate and more precise than females. Noting that many CAT studies report no sex differences, we discuss appropriate interpretations of such null findings. While acknowledging that CAT performance may be influenced by experience we suggest that the sex difference may have originated among our ancestors with the evolutionary selection of men for hunting and women for gathering.

The dynamic system corresponding to LOD and AAM.

NASA Astrophysics Data System (ADS)

Liu, Shida; Liu, Shikuo; Chen, Jiong

2000-02-01

Using wavelet transform, the authors can reconstruct the 1-D map of a multifractal object. The wavelet transform of LOD and AAM shows that at 20 years scale, annual scale and 2 - 3 years scale, the jump points of LOD and AAM accord with each other very well, and their reconstructing 1-D mapping dynamic system are also very similar.

Cycles, scaling and crossover phenomenon in length of the day (LOD) time series

NASA Astrophysics Data System (ADS)

Telesca, Luciano

2007-06-01

The dynamics of the temporal fluctuations of the length of the day (LOD) time series from January 1, 1962 to November 2, 2006 were investigated. The power spectrum of the whole time series has revealed annual, semi-annual, decadal and daily oscillatory behaviors, correlated with oceanic-atmospheric processes and interactions. The scaling behavior was analyzed by using the detrended fluctuation analysis (DFA), which has revealed two different scaling regimes, separated by a crossover timescale at approximately 23 days. Flicker-noise process can describe the dynamics of the LOD time regime involving intermediate and long timescales, while Brownian dynamics characterizes the LOD time series for small timescales.

High precision during food recruitment of experienced (reactivated) foragers in the stingless bee Scaptotrigona mexicana (Apidae, Meliponini)

NASA Astrophysics Data System (ADS)

Sánchez, Daniel; Nieh, James C.; Hénaut, Yann; Cruz, Leopoldo; Vandame, Rémy

Several studies have examined the existence of recruitment communication mechanisms in stingless bees. However, the spatial accuracy of location-specific recruitment has not been examined. Moreover, the location-specific recruitment of reactivated foragers, i.e., foragers that have previously experienced the same food source at a different location and time, has not been explicitly examined. However, such foragers may also play a significant role in colony foraging, particularly in small colonies. Here we report that reactivated Scaptotrigona mexicana foragers can recruit with high precision to a specific food location. The recruitment precision of reactivated foragers was evaluated by placing control feeders to the left and the right of the training feeder (direction-precision tests) and between the nest and the training feeder and beyond it (distance-precision tests). Reactivated foragers arrived at the correct location with high precision: 98.44% arrived at the training feeder in the direction trials (five-feeder fan-shaped array, accuracy of at least +/-6° of azimuth at 50 m from the nest), and 88.62% arrived at the training feeder in the distance trials (five-feeder linear array, accuracy of at least +/-5 m or +/-10% at 50 m from the nest). Thus, S. mexicana reactivated foragers can find the indicated food source at a specific distance and direction with high precision, higher than that shown by honeybees, Apis mellifera, which do not communicate food location at such close distances to the nest.

Supercritical fluid extraction of selected pharmaceuticals from water and serum.

PubMed

Simmons, B R; Stewart, J T

1997-01-24

Selected drugs from benzodiazepine, anabolic agent and non-steroidal anti-inflammatory drug (NSAID) therapeutic classes were extracted from water and serum using a supercritical CO2 mobile phase. The samples were extracted at a pump pressure of 329 MPa, an extraction chamber temperature of 45 degrees C, and a restrictor temperature of 60 degrees C. The static extraction time for all samples was 2.5 min and the dynamic extraction time ranged from 5 to 20 min. The analytes were collected in appropriate solvent traps and assayed by modified literature HPLC procedures. Analyte recoveries were calculated based on peak height measurements of extracted vs. unextracted analyte. The recovery of the benzodiazepines ranged from 80 to 98% in water and from 75 to 94% in serum. Anabolic drug recoveries from water and serum ranged from 67 to 100% and 70 to 100%, respectively. The NSAIDs were recovered from water in the 76 to 97% range and in the 76 to 100% range from serum. Accuracy, precision and endogenous peak interference, if any, were determined for blank and spiked serum extractions and compared with classical sample preparation techniques of liquid-liquid and solid-phase extraction reported in the literature. For the benzodiazepines, accuracy and precision for supercritical fluid extraction (SFE) ranged from 1.95 to 3.31 and 0.57 to 1.25%, respectively (n = 3). The SFE accuracy and precision data for the anabolic agents ranged from 4.03 to 7.84 and 0.66 to 2.78%, respectively (n = 3). The accuracy and precision data reported for the SFE of the NSAIDs ranged from 2.79 to 3.79 and 0.33 to 1.27%, respectively (n = 3). The precision of the SFE method from serum was shown to be comparable to the precision obtained with other classical preparation techniques.

Preliminary Figures of Merit for Isotope Ratio Measurements: The Liquid Sampling-Atmospheric Pressure Glow Discharge Microplasma Ionization Source Coupled to an Orbitrap Mass Analyzer

NASA Astrophysics Data System (ADS)

Hoegg, Edward D.; Barinaga, Charles J.; Hager, George J.; Hart, Garret L.; Koppenaal, David W.; Marcus, R. Kenneth

2016-08-01

In order to meet a growing need for fieldable mass spectrometer systems for precise elemental and isotopic analyses, the liquid sampling-atmospheric pressure glow discharge (LS-APGD) has a number of very promising characteristics. One key set of attributes that await validation deals with the performance characteristics relative to isotope ratio precision and accuracy. Owing to its availability and prior experience with this research team, the initial evaluation of isotope ratio (IR) performance was performed on a Thermo Scientific Exactive Orbitrap instrument. While the mass accuracy and resolution performance for Orbitrap analyzers are well-documented, no detailed evaluations of the IR performance have been published. Efforts described here involve two variables: the inherent IR precision and accuracy delivered by the LS-APGD microplasma and the inherent IR measurement qualities of Orbitrap analyzers. Important to the IR performance, the various operating parameters of the Orbitrap sampling interface, high-energy collisional dissociation (HCD) stage, and ion injection/data acquisition have been evaluated. The IR performance for a range of other elements, including natural, depleted, and enriched uranium isotopes was determined. In all cases, the precision and accuracy are degraded when measuring low abundance (<0.1% isotope fractions). In the best case, IR precision on the order of 0.1% RSD can be achieved, with values of 1%-3% RSD observed for low-abundance species. The results suggest that the LS-APGD is a promising candidate for field deployable MS analysis and that the high resolving powers of the Orbitrap may be complemented with a here-to-fore unknown capacity to deliver high-precision IRs.

Spectrophotometric determination of certain CNS stimulants in dosage forms and spiked human urine via derivatization with 2,4-Dinitrofluorobenzene

PubMed Central

2011-01-01

A new spectrophotometric method is developed for the determination of phenylpropanolamine HCl (PPA), ephedrine HCl (EPH) and pseudoephedrine HCl (PSE) in pharmaceutical preparations and spiked human urine. The method involved heat-catalyzed derivatization of the three drugs with 2,4-dinitrofluorobenzene (DNFB) producing a yellow colored product peaking at 370 nm for PPA and 380 nm for EPH and PSE, respectively. The absorbance concentration plots were rectilinear over the range of 2-20 for PPA and 1-14 μg/mL for both of EPH and PSE, respectively. The limit of detection (LOD) values were 0.20, 0.13 and 0.20 μg/mL for PPA, EPH and PSE, respectively and limit of quantitation (LOQ) values of 0.60 and 0.40 and 0.59 μg/mL for PPA, EPH and PSE, respectively. The analytical performance of the method was fully validated and the results were satisfactory. The proposed method was successfully applied to the determination of the three studied drugs in their commercial dosage forms including tablets, capsules and ampoules with good percentage recoveries. The proposed method was further applied for the determination of PSE in spiked human urine with a mean percentage recovery of 108.17 ± 1.60 for (n = 3). Statistical comparison of the results obtained with those of the comparison methods showed good agreement and proved that there was no significant difference in the accuracy and precision between the two methods. The mechanism of the reaction pathway was postulated. PMID:22032335

A Simple and High-Throughput Analysis of Amatoxins and Phallotoxins in Human Plasma, Serum and Urine Using UPLC-MS/MS Combined with PRiME HLB μElution Platform

PubMed Central

Zhang, Shuo; Zhao, Yunfeng; Li, Haijiao; Zhou, Shuang; Chen, Dawei; Zhang, Yizhe; Yao, Qunmei; Sun, Chengye

2016-01-01

Amatoxins and phallotoxins are toxic cyclopeptides found in the genus Amanita and are among the predominant causes of fatal food poisoning in China. In the treatment of Amanita mushroom poisoning, an early and definite diagnosis is necessary for a successful outcome, which has prompted the development of protocols for the fast and confirmatory determination of amatoxins and phallotoxins in human biological fluids. For this purpose, a simple, rapid and sensitive multiresidue UPLC-MS/MS method for the simultaneous determination of α-amanitin, β-amanitin, γ-amanitin, phalloidin (PHD) and phallacidin (PCD) in human plasma, serum and urine was developed and validated. The diluted plasma, serum and urine samples were directly purified with a novel PRiME technique on a 96-well μElution plate platform, which allowed high-throughput sample processing and low reagent consumption. After purification, a UPLC-MS/MS analysis was performed using positive electrospray ionization (ESI+) in multiple reaction monitoring (MRM) mode. This method fulfilled the requirements of a validation test, with good results for the limit of detection (LOD), lower limit of quantification (LLOQ), accuracy, intra- and inter-assay precision, recovery and matrix effects. All of the analytes were confirmed and quantified in authentic plasma, serum and urine samples obtained from cases of poisoning using this method. Using the PRiME μElution technique for quantification reduces labor and time costs and represents a suitable method for routine toxicological and clinical emergency analysis. PMID:27153089

Determination of ten monohydroxylated polycyclic aromatic hydrocarbons by liquid-liquid extraction and liquid chromatography/tandem mass spectrometry.

PubMed

Fan, Ruifang; Ramage, Robert; Wang, Dongli; Zhou, Junqiang; She, Jianwen

2012-05-15

The aim of this study is to develop and validate an analytical method for the quantitation of ten urinary monohydroxylated polycyclic aromatic hydrocarbons (OH-PAHs) through high pressure liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). After enzymatic deconjugation, urine samples were extracted by liquid-liquid extraction (LLE) and OH-PAHs were analyzed by HPLC/MS/MS operated in negative electrospray ionization (ESI) and multiple reaction monitoring (MRM) mode. LLE was conducted with the solvent mixture of pentane and toluene, which reduced the matrix interferences and enhanced the method sensitivity significantly. Deuterated and (13)C-labeled analogs are used as internal standards. Calibration curves of all target analytes shows favorable linearity within the concentration range of 5.9-15,000.0 ng/L for different OH-PAHs with the regression coefficients above 0.993. The limits of detection (LODs) in pooled urine ranged from 1.72 to 17.47 ng/L, which were much lower than those obtained by a gas chromatography/high resolution mass spectrometry (GC/HRMS) method. The method shows satisfactory accuracy and precision when analyzing three different levels of OH-PAHs spiked in pooled urine. Except for 1-hydroxynaphthalene, recoveries of other OH-PAHs were in the range of 100 ± 20% with a variation coefficient of less than 13%. The measurement of OH-PAHs from a QC sample of the Centers for Disease Control and Prevention (CDC) generated results close to the values measured by CDC. This method has been successfully employed in the California Biomonitoring Program. Published by Elsevier B.V.

Sensitive determination of four tetracycline antibiotics in pig plasma by field-amplified sample stacking open-tubular capillary electrochromatography with dimethylethanolamine aminated polychloromethyl styrene nano-latex coated capillary column.

PubMed

Guo, Yaxiao; Meng, Lei; Zhang, Yanhao; Tang, Wei; Zhang, Wenfen; Xia, Yan; Ban, Fuguo; Wu, Ningpeng; Zhang, Shusheng

2013-12-30

This paper described the preparation and application of a new dimethylethanolamine aminated polychloromethyl styrene nano-latex (DMEAPL) coated capillary column (ccc-DMEAPL) in the determination of four tetracycline antibiotics (TCA) including tetracycline (TC), oxytetracycline (OTC), doxycycline (DC) and chlorotetracycline (CTC) in pig plasma. The ccc-DMEAPL column was characterized with steady EOF values of ca. 1.5-5.2×10(-5)cm(2)/Vs at pH 1.8-6.3. The optimized conditions for field-amplified sample stacking open-tubular capillary electrochromatography (FASS-OT-CEC) were as following: background electrolyte, 10mmol/L Na2HPO4+15mmol/L citric acid (pH 3.2); ccc-DMEAPL, 50μm i.d.×50cm (effective length 41.5cm), separation voltage, 18kV; column temperature, 25°C; UV detection wavelength, 270nm; water-plug injection: 30mbar×10s; sample electrokinetic injection, 10kV×20s. The four TCA were extracted with the solution of 10mmol/L Na2HPO4+15mmol/L citric acid+4g/L EDTA-2Na (pH 3.2). The FASS-OT-CEC method was validated in terms of linearity, sensitivity, selectivity, precision and accuracy. The LODs ranged from 3 to 7ng/mL, the recoveries for the four TCA were all more than 80%. The developed method was successfully applied for the determination of TCs in the actual pig plasma samples. Copyright © 2013 Elsevier B.V. All rights reserved.

New validated high-performance liquid chromatographic method for simultaneous analysis of ten flavonoid aglycones in plant extracts using a C18 fused-core column and acetonitrile-tetrahydrofuran gradient.

PubMed

Olszewska, Monika A

2012-09-01

An HPLC method of high resolution has been developed and validated for the simultaneous determination of ten prominent flavonoid aglycones in plant materials using a fused-core C18-silica column (Ascentis® Express, 4.6 mm × 150 mm, 2.7 μm). The separation was accomplished with an acetonitrile-tetrahydrofuran gradient elution at a flow rate of 1 mL/min and temperature of 30°C. UV spectrophotometric detection was employed at 370 nm for flavonols (quercetin [QU], myricetin [MY], isorhamnetin [IS], kaempferol [KA], sexangularetin [SX], and limocitrin [LM]) and 340 nm for flavones (apigenin [AP], acacetin [AC], chrysoeriol [CH], and luteolin [LU]). The high resolution of critical pairs QU/LU (10.50), QU/CH (3.40), AP/CH (2.51), SX/LM (2.30), and IS/KA (2.70) was achieved within 30.3 min. The observed column back pressure was less than 4300 psi, thus acceptable for conventional HPLC equipment. The method was sensitive enough having LODs of 0.115-0.525 ng and good linearity (r > 0.9999) over the test range. The precision values, expressed as RSD values, were <7.5%, and the accuracy was in the range of 95.3-100.2% for all analytes except MY (73.8%). The method was successfully employed for the determination of flavonoids in several medicinal plants, such as Ginkgo biloba, Betula pendula, and a variety of Sorbus species. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Derivative spectrophotometric method for simultaneous determination of zofenopril and fluvastatin in mixtures and pharmaceutical dosage forms.

PubMed

Stolarczyk, Mariusz; Maślanka, Anna; Apola, Anna; Rybak, Wojciech; Krzek, Jan

2015-09-05

Fast, accurate and precise method for the determination of zofenopril and fluvastatin was developed using spectrophotometry of the first (D1), second (D2), and third (D3) order derivatives in two-component mixtures and in pharmaceutical preparations. It was shown, that the developed method allows for the determination of the tested components in a direct manner, despite the apparent interference of the absorption spectra in the UV range. For quantitative determinations, "zero-crossing" method was chosen, appropriate wavelengths for zofenopril were: D1 λ=270.85 nm, D2 λ=286.38 nm, D3 λ=253.90 nm. Fluvastatin was determined at wavelengths: D1 λ=339.03 nm, D2 λ=252.57 nm, D3 λ=258.50 nm, respectively. The method was characterized by high sensitivity and accuracy, for zofenopril LOD was in the range of 0.19-0.87 μg mL(-1), for fluvastatin 0.51-1.18 μg mL(-1), depending on the class of derivative, and for zofenopril and fluvastatin LOQ was 0.57-2.64 μg mL(-1) and 1.56-3.57 μg mL(-1), respectively. The recovery of individual components was within the range of 100±5%. For zofenopril, the linearity range was estimated between 7.65 μg mL(-1) and 22.94 μg mL(-1), and for fluvastatin between 5.60 μg mL(-1) and 28.00 μg mL(-1). Copyright © 2015 Elsevier B.V. All rights reserved.

Development and validation of rapid and simultaneous method for determination of 12 hair-growth compounds in adulterated products by UHPLC-MS/MS.

PubMed

Park, Han Na; Lee, Ji Hyun; Park, Sung-Kwan; Baek, Sun Young; Lee, Yong-Moon; Kang, Hoil

2018-03-01

Synthetic hair-growth compounds have been illegally used in diverse products to enhance the short-term efficacy of these products. In this study, a rapid and simultaneous method for the determination of hair-growth compounds in adulterated products based on ultra high pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed and validated. The limit of detection (LOD) and limit of quantitation (LOQs) of the method were 0.08-43.6ng/mL and 0.27-145ng/mL for the solid-, liquid-, and cream-type samples, respectively. Good calibration linearity for all compounds was demonstrated with a correlation coefficient (r 2 ) higher than 0.997. The intra- and inter-assay precisions were within 11%. The corresponding accuracies were 86-117% and 81-113%, respectively. The mean recoveries obtained for the solid-, liquid, and cream-type samples ranged from 87 to 114%, with a relative standard deviation (RSD) within 6%. The RSD of the stability evaluated at 4°C for 48h was less than 6%. The established method was used to screen 76 samples advertised as hair-growth treatments, from online and offline markets, over the course of two years. In 10% of the samples, four compounds, including triaminodil, minoxidil, finasteride, methyltestosterone, and testosterone-propionate were detected. The concentrations were in the range of 0.5-16.4mg/g. This technique provides a reliable platform for technical analysis for continuous monitoring of adulterated products to protect public health. Copyright © 2018 Elsevier B.V. All rights reserved.

UHPLC determination of catechins for the quality control of green tea.

PubMed

Naldi, Marina; Fiori, Jessica; Gotti, Roberto; Périat, Aurélie; Veuthey, Jean-Luc; Guillarme, Davy; Andrisano, Vincenza

2014-01-01

An ultra-high performance liquid chromatography (UHPLC) with UV detection method was developed for the fast quantitation of the most represented and biologically important green tea catechins and caffeine. UHPLC system was equipped with C18 analytical column (50mm×2.1mm, 1.8μm), utilizing a mobile phase composed of pH 2.5 triethanolamine phosphate buffer (0.1M) and acetonitrile in a gradient elution mode; under these conditions six major catechins and caffeine were separated in a 3min run. The method was fully validated in terms of precision, detection and quantification limits, linearity, accuracy, and it was applied to the identification and quantification of catechins and caffeine present in green tea infusions. In particular, commercially available green tea leaves samples of different geographical origin (Sencha, Ceylon Green and Lung Ching) were used for infusion preparations (water at 85°C for 15min). The selectivity of the developed UHPLC method was confirmed by comparison with UHPLC-MS/MS analysis. The recovery of the main six catechins and caffeine on the three analyzed commercial tea samples ranged from 94 to 108% (n=3). Limits of detection (LOD) were comprised in the range 0.1-0.4μgmL(-1). An orthogonal micellar electrokinetic (MEKC) method was applied for comparative purposes on selectivity and quantitative data. The combined use of the results obtained by the two techniques allowed for a fast confirmation on quantitative characterization of commercial samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Direct trace-elemental analysis of urine samples by laser ablation-inductively coupled plasma mass spectrometry after sample deposition on clinical filter papers.

PubMed

Aramendía, Maite; Rello, Luis; Vanhaecke, Frank; Resano, Martín

2012-10-16

Collection of biological fluids on clinical filter papers shows important advantages from a logistic point of view, although analysis of these specimens is far from straightforward. Concerning urine analysis, and particularly when direct trace elemental analysis by laser ablation-inductively coupled plasma mass spectrometry (LA-ICPMS) is aimed at, several problems arise, such as lack of sensitivity or different distribution of the analytes on the filter paper, rendering obtaining reliable quantitative results quite difficult. In this paper, a novel approach for urine collection is proposed, which circumvents many of these problems. This methodology consists on the use of precut filter paper discs where large amounts of sample can be retained upon a single deposition. This provides higher amounts of the target analytes and, thus, sufficient sensitivity, and allows addition of an adequate internal standard at the clinical lab prior to analysis, therefore making it suitable for a strategy based on unsupervised sample collection and ulterior analysis at referral centers. On the basis of this sampling methodology, an analytical method was developed for the direct determination of several elements in urine (Be, Bi, Cd, Co, Cu, Ni, Sb, Sn, Tl, Pb, and V) at the low μg L(-1) level by means of LA-ICPMS. The method developed provides good results in terms of accuracy and LODs (≤1 μg L(-1) for most of the analytes tested), with a precision in the range of 15%, fit-for-purpose for clinical control analysis.

[Rapid simultaneous determination of organophosphorus pesticides in human serum and urine by liquid chromatography-mass spectrometry].

PubMed

Zlatković, Milica; Jovanović, Miodrag; Djordjević, Dragana; Vucinić, Slavica

2010-09-01

Analysis of organophosphosphorus compounds and their metabolites in a biological material includes the use of numerous methods, covering both preparation of samples for analysis and their identification that is considered to be very complex. Low concentrations monitoring requires implementation of highly sensitive analytical techniques. The aim of this study was to develop and validate an original and sensitive method for the detection and quantitation of organophosphorus pesticides (dimethoate, diazinon, malathion and malaoxon) in human biological matrices (serum, urine). This method was based on a solid-phase extraction procedure, a chromatographic separation using an ACQUITY UPLC HSST3 column and mass spectrometric detection in the positive ion mode. Mobile phase: was consited of Solvent A (5 mM ammonium formate pH 3.0) and Solvent B (0.1% acetic formate in methanol), in a linear gradient (constant flow-rate 0.3 mL/min). The standard curve was linear in the range of 0.05-5.00 mg/L for malathion and malaoxon, 0.10-5.00 mg/L for dimethoate and 0.05-2.50 mg/L for diazinon. The correlation coefficient was r > or = 0.99. Extraction recoveries were satisfactory and ranged between 90-99%. The limits of detection (LOD) was between 0.007-0.07 mg/L and the limits of quantitation (LOQ) ranged between 0.022-0.085 mg/L. Intra- and interassay precision and accuracy were satisfactory for all of the pesticides analyzed. The method of liquid chromatography-mass spectrometry is simple, accurate, and useful for the determination of organophosphorus pesticides in both clinical and forensic toxicology.

Ion-Pair Extractive Spectrophotometric Assay of Terbinafine Hydrochloride in Pharmaceuticals and Spiked Urine Using Bromocresol Purple

NASA Astrophysics Data System (ADS)

Salem Qarah, N. A.; Basavaiah, K.; Swamy, N.

2016-09-01

Two simple, rapid, selective, and sensitive methods were developed and validated for the determination of terbinafi ne hydrochloride (TBH) in pharmaceuticals and urine. The fi rst method (method A) is based on the formation of a yellow ion-pair complex of TBH and bromocresol purple (BCP), a sulfonephthalein dye, in Walpole buffer of pH 3.61, which was extracted into chloroform and investigated at 420 nm. For the second method (method B) the drug-dye ion-pair was broken in alkaline KOH medium, and the resulting free dye color was measured at 610 nm. All variables were studied to optimize the reaction conditions. The regression analysis of Beer's law plots showed good correlation in the concentration ranges of 1-10 and 0.1-2.0 μg/mL for method A and method B, respectively. Molar absorptivity values were 2.99 × 104, and 1.51×105 L/(mol × cm) for measurements by these methods. The methods were also validated for limits of detection (LOD) and quantifi cation (LOQ), intra-day and inter-day accuracy and precision, selectivity, robustness and ruggedness. The composition of the ion-pair (drug-dye) used in the method A was found to be 1:1 by both mole-ratio and Job's methods. The developed methods were applied to tablets, and the results were in good agreement with the label claim and those of the reference method. Because of its high sensitivity, method A was applied to spiked human urine with percent recoveries in the range 96.58-107.3 and a standard deviation <2%.