41 CFR 102-117.255 - What actions may I take if the TSP's performance is not satisfactory?

Code of Federal Regulations, 2010 CFR

2010-07-01

... 41 Public Contracts and Property Management 3 2010-07-01 2010-07-01 false What actions may I take if the TSP's performance is not satisfactory? 102-117.255 Section 102-117.255 Public Contracts and... may I take if the TSP's performance is not satisfactory? If the TSP's performance is not satisfactory...

Analysis of polymeric phenolics in red wines using different techniques combined with gel permeation chromatography fractionation.

PubMed

Guadalupe, Zenaida; Soldevilla, Alberto; Sáenz-Navajas, María-Pilar; Ayestarán, Belén

2006-04-21

A multiple-step analytical method was developed to improve the analysis of polymeric phenolics in red wines. With a common initial step based on the fractionation of wine phenolics by gel permeation chromatography (GPC), different analytical techniques were used: high-performance liquid chromatography-diode array detection (HPLC-DAD), HPLC-mass spectrometry (MS), capillary zone electrophoresis (CZE) and spectrophotometry. This method proved to be valid for analyzing different families of phenolic compounds, such as monomeric phenolics and their derivatives, polymeric pigments and proanthocyanidins. The analytical characteristics of fractionation by GPC were studied and the method was fully validated, yielding satisfactory statistical results. GPC fractionation substantially improved the analysis of polymeric pigments by CZE, in terms of response, repeatability and reproducibility. It also represented an improvement in the traditional vanillin assay used for proanthocyanidin (PA) quantification. Astringent proanthocyanidins were also analyzed using a simple combined method that allowed these compounds, for which only general indexes were available, to be quantified.

A rapid and sensitive assay of perfluorocarboxylic acids in aqueous matrices by headspace solid phase microextraction-gas chromatography-triple quadrupole mass spectrometry.

PubMed

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

2012-08-17

The work aims at developing a rapid and sensitive method for the quantification of perfluorocarboxylic acids in aqueous matrices. The proposed analytical approach is based on the use of solid phase microextraction in headspace mode after a fast derivatization of the carboxylate function by propylchloroformate/propanol mixture. Several fibers were evaluated and the optimization of the parameters affecting the SPME process was carried out using a central composite design. The optimum working conditions in terms of response values were achieved by performing analysis with CAR/PDMS fiber at room temperature, without addition of NaCl, with a sample volume of 6 ml and an extraction time of 10 min. Assay of PFCAs was performed by using a gas chromatography-triple quadrupole mass spectrometry (GC-QqQ MS) system in negative chemical ionization mode with ammonia as reagent gas. An overall evaluation of all analytical parameters shows that the proposed method provides satisfactory results. In particular, the observed accuracies, ranging from 84.4% to 116.8%, and the RSD values in the range 0.4% and 14.5% confirm the effectiveness of the developed protocol in the assay of PFCAs content in aqueous matrices. Moreover, LOD and LOQ values ranging from 0.08 to 6.6 ng l(-1) and from 0.17 to 14.3 ng l(-1), respectively, can be considered very satisfactory. None of the compounds were detected in six samples of river collected in Calabria. Copyright © 2012 Elsevier B.V. All rights reserved.

Comparison of two thin-film microextractions for the analysis of estrogens in aqueous tea extract and environmental water samples by high performance liquid chromatography-ultraviolet detection.

PubMed

Cai, Pei-Shan; Li, Dan; Chen, Jing; Xiong, Chao-Mei; Ruan, Jin-Lan

2015-04-15

Two thin-film microextractions (TFME), octadecylsilane (ODS)-polyacrylonitrile (PAN)-TFME and polar enhanced phase (PEP)-PAN-TFME have been proposed for the analysis of bisphenol-A, diethylstilbestrol and 17β-estradiol in aqueous tea extract and environmental water samples followed by high performance liquid chromatography-ultraviolet detection. Both thin-films were prepared by spraying. The influencing factors including pH, extraction time, desorption solvent, desorption volume, desorption time, ion strength and reusability were investigated. Under the optimal conditions, the two TFME methods are similar in terms of the analytical performance evaluated by standard addition method. The limits of detection for three estrogens in environmental water and aqueous tea extract matrix ranged from 1.3 to 1.6 and 2.8 to 7.1 ng mL(-1) by the two TFME methods, respectively. Both approaches were applied for the analysis of analytes in real aqueous tea extract and environmental water samples, presenting satisfactory recoveries ranged from 87.3% to 109.4% for the spiked samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

Automation effects in a stereotypical multiloop manual control system. [for aircraft

NASA Technical Reports Server (NTRS)

Hess, R. A.; Mcnally, B. D.

1984-01-01

The increasing reliance of state-of-the art, high performance aircraft on high authority stability and command augmentation systems, in order to obtain satisfactory performance and handling qualities, has made critical the achievement of a better understanding of human capabilities, limitations, and preferences during interactions with complex dynamic systems that involve task allocation between man and machine. An analytical and experimental study has been undertaken to investigate human interaction with a simple, multiloop dynamic system in which human activity was systematically varied by changing the levels of automation. Task definition has led to a control loop structure which parallels that for any multiloop manual control system, and may therefore be considered a stereotype.

Simultaneous determination of active ingredients in Erigeron breviscapus (Vant.) Hand-Mazz. by capillary electrophoresis with electrochemical detection.

PubMed

Chu, Qingcui; Wu, Ting; Fu, Liang; Ye, Jiannong

2005-03-09

A high-performance capillary electrophoresis (CE) with electrochemical detection (ED) method was developed for the determination of the pharmacologically active ingredients in Erigeron breviscapus (Vant.) Hand-Mazz. and its extract phytopharmaceuticals in this work. Under the optimum conditions, nine analytes, baicalein, naringenin, scopoletin, kaempferol, apigenin, scutellarin, luteolin, caffeic acid and protocatechuic acid were separated within 24 min in a borax buffer (pH 8.7). Notably, excellent linearity was obtained over two orders of magnitude with detection limits (S/N=3) ranged from 1.0 x 10(-7) g/mL to 5.6 x 10(-7) g/mL for all nine analytes. This method was successfully used in the analysis of E. breviscapus (Vant.) Hand-Mazz. and its phytopharmaceuticals with a relatively simple extraction procedure, and the assay results were satisfactory.

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.

Dispersive liquid-liquid microextraction applied to isolation and concentration of alkylphenols and their short-chained ethoxylates in water samples.

PubMed

Zgoła-Grześkowiak, Agnieszka

2010-03-12

Dispersive liquid-liquid microextraction (DLLME) coupled with high-performance liquid chromatography with fluorescence detector was applied for the determination of alkylphenols and their short-chained ethoxylates in water samples. Development of DLLME procedure included optimisation of some important parameters such as kind and volume of extracting and dispersing solvents. Under optimised conditions 50 microL of trichloroethylene in 1.5 mL of acetone were rapidly injected into 5 mL of a water sample. After centrifuging the organic phase containing the analytes was taken for evaporation with a gentle nitrogen purge and reconstituted to 50 microL of acetonitrile. The aliquot of this solution was analysed with the use of HPLC. For octylphenol (OP) and octylphenol ethoxylates (OPEOs) linearity was satisfactory in the range 8-1000 microg L(-1) and for nonylphenol (NP) and nonylphenol ethoxylates (NPEOs) linearity was in the range from 50 to about 3000 microg L(-1). Limit of quantitation was 0.1 microg L(-1) for OP and OPEOs and 0.3 microg L(-1) for NP and NPEOs. Satisfactory recoveries between 66 and 79% were obtained for environmental samples. The results showed that DLLME is a simple, rapid and sensitive analytical method for the preconcentration of trace amounts of alkylphenols and their ethoxylates in environmental water samples. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Immobilization of Glucose Oxidase on a Carbon Nanotubes/Dendrimer-Ferrocene Modified Electrode for Reagentless Glucose Biosensing.

PubMed

Zhou, Juan; Li, Huan; Yang, Huasong; Cheng, Hui; Lai, Guosong

2017-01-01

Ferrocene-grafted dendrimer was covalently linked to the surface of a carbon nanotubes (CNTs)-chitosan (CS) nanocomposite modified electrode for immobilizing high-content glucose oxidase (GOx), which resulted in the successful development a novel reagentless glucose biosensor. Electrochemical impedance spectroscopy, cyclic voltammetry, and amperometry were used to characterize the preparation process and the enzymatically catalytic response of this biosensor. Due to the excellent electron transfer acceleration of the CNTs and the high-content loading of the GOx biomolecule and ferrocene mediator on the electrode matrix, this biosensor showed excellent analytical performance such as fast response time less than 10 s, wide linear range from 0.02 to 2.91 mM and low detection limit down to 7.5 μM as well as satisfactory stability and reproducibility toward the amperometric glucose determination. In addition, satisfactory result was obtained when it was used for the glucose measurements in human blood samples. Thus this biosensor provides great potentials for practical applications.

Reliable determination of new lipid peroxidation compounds as potential early Alzheimer Disease biomarkers.

PubMed

García-Blanco, Ana; Peña-Bautista, Carmen; Oger, Camille; Vigor, Claire; Galano, Jean-Marie; Durand, Thierry; Martín-Ibáñez, Nuria; Baquero, Miguel; Vento, Máximo; Cháfer-Pericás, Consuelo

2018-07-01

Lipid peroxidation plays an important role in Alzheimer Disease, so corresponding metabolites found in urine samples could be potential biomarkers. The aim of this work is to develop a reliable ultra-performance liquid chromatography-tandem mass spectrometry analytical method to determine a new set of lipid peroxidation compounds in urine samples. Excellent sensitivity was achieved with limits of detection between 0.08 and 17 nmol L -1 , which renders this method suitable to monitor analytes concentrations in real samples. The method's precision was satisfactory with coefficients of variation around 5-17% (intra-day) and 8-19% (inter-day). The accuracy of the method was assessed by analysis of spiked urine samples obtaining recoveries between 70% and 120% for most of the analytes. The utility of the described method was tested by analyzing urine samples from patients early diagnosed with mild cognitive impairment or mild dementia Alzheimer Disease following the clinical standard criteria. As preliminary results, some analytes (17(RS)-10-epi-SC-Δ 15 -11-dihomo-IsoF, PGE 2 ) and total parameters (Neuroprostanes, Isoprostanes, Isofurans) show differences between the control and the clinical groups. So, these analytes could be potential early Alzheimer Disease biomarkers assessing the patients' pro-oxidant condition. Copyright © 2018 Elsevier B.V. All rights reserved.

Extraction, isolation, and purification of analytes from samples of marine origin--a multivariate task.

PubMed

Liguori, Lucia; Bjørsvik, Hans-René

2012-12-01

The development of a multivariate study for a quantitative analysis of six different polybrominated diphenyl ethers (PBDEs) in tissue of Atlantic Salmo salar L. is reported. An extraction, isolation, and purification process based on an accelerated solvent extraction system was designed, investigated, and optimized by means of statistical experimental design and multivariate data analysis and regression. An accompanying gas chromatography-mass spectrometry analytical method was developed for the identification and quantification of the analytes, BDE 28, BDE 47, BDE 99, BDE 100, BDE 153, and BDE 154. These PBDEs have been used in commercial blends that were used as flame-retardants for a variety of materials, including electronic devices, synthetic polymers and textiles. The present study revealed that an extracting solvent mixture composed of hexane and CH₂Cl₂ (10:90) provided excellent recoveries of all of the six PBDEs studied herein. A somewhat lower polarity in the extracting solvent, hexane and CH₂Cl₂ (40:60) decreased the analyte %-recoveries, which still remain acceptable and satisfactory. The study demonstrates the necessity to perform an intimately investigation of the extraction and purification process in order to achieve quantitative isolation of the analytes from the specific matrix. Copyright © 2012 Elsevier B.V. All rights reserved.

Development of a plasma sprayed ceramic gas path seal for high pressure turbine applications

NASA Technical Reports Server (NTRS)

Shiembob, L. T.

1977-01-01

The plasma sprayed graded layered yittria stabilized zirconia (ZrO2)/metal(CoCrAlY) seal system for gas turbine blade tip applications up to 1589 K (2400 F) seal temperatures was studied. Abradability, erosion, and thermal fatigue characteristics of the graded layered system were evaluated by rig tests. Satisfactory abradability and erosion resistance was demonstrated. Encouraging thermal fatigue tolerance was shown. Initial properties for the plasma sprayed materials in the graded, layered seal system was obtained, and thermal stress analyses were performed. Sprayed residual stresses were determined. Thermal stability of the sprayed layer materials was evaluated at estimated maximum operating temperatures in each layer. Anisotropic behavior in the layer thickness direction was demonstrated by all layers. Residual stresses and thermal stability effects were not included in the analyses. Analytical results correlated reasonably well with results of the thermal fatigue tests. Analytical application of the seal system to a typical gas turbine engine application predicted performance similar to rig specimen thermal fatigue performance. A model for predicting crack propagation in the sprayed ZrO2/CoCrAlY seal system was proposed, and recommendations for improving thermal fatigue resistance were made. Seal system layer thicknesses were analytically optimized to minimize thermal stresses in the abradability specimen during thermal fatigue testing. Rig tests on the optimized seal configuration demonstrated some improvement in thermal fatigue characteristics.

Portable Solid Phase Micro-Extraction Coupled with Ion Mobility Spectrometry System for On-Site Analysis of Chemical Warfare Agents and Simulants in Water Samples

PubMed Central

Yang, Liu; Han, Qiang; Cao, Shuya; Yang, Jie; Yang, Junchao; Ding, Mingyu

2014-01-01

On-site analysis is an efficient approach to facilitate analysis at the location of the system under investigation as it can result in more accurate, more precise and quickly available analytical data. In our work, a novel self-made thermal desorption based interface was fabricated to couple solid-phase microextraction with ion mobility spectrometry for on-site water analysis. The portable interface can be connected with the front-end of an ion mobility spectrometer directly without other modifications. The analytical performance was evaluated via the extraction of chemical warfare agents and simulants in water samples. Several parameters including ionic strength and extraction time have been investigated in detail. The application of the developed method afforded satisfactory recoveries ranging from 72.9% to 114.4% when applied to the analysis of real water samples. PMID:25384006

A low-cost biosorbent-based coating for the highly sensitive determination of organochlorine pesticides by solid-phase microextraction and gas chromatography-electron capture detection.

PubMed

do Carmo, Sângela Nascimento; Merib, Josias; Dias, Adriana Neves; Stolberg, Joni; Budziak, Dilma; Carasek, Eduardo

2017-11-24

In this study, an environmentally friendly and low-cost biosorbent coating was evaluated, for the first time, as the extraction phase for solid-phase microextraction (SPME) supported on a nitinol alloy. The characterization of the new fiber was performed by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The applicability of the biosorbent-based fiber in the determination of δ-hexachlorocyclohexane, aldrin, heptachlor epoxide, α-endosulfan, endrin and 4,4'-DDD in water samples was verified, with separation/detection by gas chromatography coupled to electron capture detection (GC-ECD). The influencing parameters (temperature, extraction time and ionic strength) were optimized simultaneously using a central composite design. The optimum conditions were: extraction time of 80min at 80°C and sodium chloride concentration of 15% (w/v). Satisfactory analytical performance was achieved with limits of detection (LOD) between 0.19 and 0.71ngL -1 and limits of quantification (LOQ) between 0.65 and 2.38ngL -1 . The relative recoveries for the analytes were determined using river and lake water samples spiked at different concentrations and ranged from 60% for α-endosulfan to 113% for δ-hexachlorocyclohexane, with relative standard deviations (RSD) lower than 21%. The fiber-to-fiber reproducibility (n=3) was also evaluated and the RSD was lower than 14%. The extraction efficiency obtained for the proposed biosorbent coating was compared to a commercially available DVB/Car/PDMS coating. The proposed fiber provided very promising results, including LODs at the level of parts per trillion and highly satisfactory thermal and mechanical stability. Copyright © 2017 Elsevier B.V. All rights reserved.

Optimization of an Indirect Enzymatic Method for the Simultaneous Analysis of 3-MCPD, 2-MCPD, and Glycidyl Esters in Edible Oils.

PubMed

Koyama, Kazuo; Miyazaki, Kinuko; Abe, Kousuke; Ikuta, Keiich; Egawa, Yoshitsugu; Kitta, Tadashi; Kido, Hirotsugu; Sano, Takashi; Takahashi, Yukinari; Nezu, Toru; Nohara, Hidenori; Miyashita, Takashi; Yada, Hiroshi; Yamazaki, Kumiko; Watanabe, Yomi

2015-01-01

We developed a novel, indirect enzymatic method for the analysis of fatty acid esters of 3-monochloro-1,2-propanediol (3-MCPD), 2-monochloro-1,3-propanediol (2-MCPD), and glycidol (Gly) in edible oils and fats. Using this method, the ester analytes were rapidly cleavaged by Candida rugosa lipase at room temperature for 0.5 h. As a result of the simultaneous hydrolysis and bromination steps, 3-MCPD esters, 2-MCPD esters, and glycidyl esters were converted to free 3-MCPD, 2-MCPD, and 3-monobromo-1,2-propanediol (3-MBPD), respectively. After the addition of internal standards, the mixtures were washed with hexane, derivatized with phenylboronic acid, and analyzed by gas chromatography-mass spectrometer (GC-MS). The analytical method was evaluated in preliminary and feasibility studies performed by 13 laboratories. The preliminary study from 4 laboratories showed the reproducibility (RSD R ) of < 10% and recoveries in the range of 102-111% for the spiked 3-MCPD and 2-MCPD in extra virgin olive (EVO) oil, semi-solid palm oil, and solid palm oil. However, the RSDR and recoveries of Gly in the palm oil samples were not satisfactory. The Gly content of refrigerated palm oil samples decreased whereas the samples at room temperature were stable for three months, and this may be due to the depletion of Gly during cold storage. The feasibility studies performed by all 13 laboratories were conducted based on modifications of the shaking conditions for ester cleavage, the conditions of Gly bromination, and the removal of gel formed by residual lipase. Satisfactory RSDR were obtained for EVO oil samples spiked with standard esters (4.4% for 3-MCPD, 11.2% for 2-MCPD, and 6.6% for Gly).

Quality performance of laboratory testing in pharmacies: a collaborative evaluation.

PubMed

Zaninotto, Martina; Miolo, Giorgia; Guiotto, Adriano; Marton, Silvia; Plebani, Mario

2016-11-01

The quality performance and the comparability between results of pharmacies point-of-care-testing (POCT) and institutional laboratories have been evaluated. Eight pharmacies participated in the project: a capillary specimen collected by the pharmacist and, simultaneously, a lithium-heparin sample drawn by a physician of laboratory medicine for the pharmacy customers (n=106) were analyzed in the pharmacy and in the laboratory, respectively. Glucose, cholesterol, HDL-cholesterol, triglycerides, creatinine, uric acid, aspartate aminotransferase, alanine aminotransferase, were measured using: Reflotron, n=5; Samsung, n=1; Cardiocheck PA, n=1; Cholestech LDX, n=1 and Cobas 8000. The POCT analytical performance only (phase 2) were evaluated testing, in pharmacies and in the laboratory, the lithium heparin samples from a female drawn fasting daily in a week, and a control sample containing high concentrations of glucose, cholesterol and triglycerides. For all parameters, except triglycerides, the slopes showed a satisfactory correlation. For triglycerides, a median value higher in POCT in comparison to the laboratory (1.627 mmol/L vs. 0.950 mmol/L) has been observed. The agreement in the subjects classification, demonstrates that for glucose, 70% of the subjects show concentrations below the POCT recommended level (5.8-6.1 mmol/L), while 56% are according to the laboratory limit (<5.6 mmol/L). Total cholesterol exhibits a similar trend while POCT triglycerides show a greater percentage of increased values (21% vs. 9%). The reduction in triglycerides bias (phase 2) suggests that differences between POCT and central laboratory is attributable to a pre-analytical problem. The results confirm the acceptable analytical performance of POCT pharmacies and specific criticisms in the pre- and post-analytical phases.

Development of a simple and valid method for the trace determination of phthalate esters in human plasma using dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry.

PubMed

Ebrahim, Karim; Poursafa, Parinaz; Amin, Mohammad Mehdi

2017-11-01

A new method was developed for the trace determination of phthalic acid esters in plasma using dispersive liquid-liquid microextraction and gas chromatography with mass spectrometry analysis. Plasma proteins were efficiently precipitated by trichloroacetic acid and then a mixture of chlorobenzene (as extraction solvent) and acetonitrile (as dispersive solvent) rapidly injected to clear supernatant using a syringe. After centrifuging, chlorobenzene sedimented at the bottom of the test tube. 1 μL of this sedimented phase was injected into the gas chromatograph for phthalic acid esters analysis. Different factors affecting the extraction performance, such as the type of extraction and dispersive solvent, their volume, extraction time, and the effects of salt addition were investigated and optimized. Under the optimum conditions, the enrichment factors and extraction recoveries were satisfactory and ranged between 820-1020 and 91-97%, respectively. The linear range was wide (50-1000 ng/mL) and limit of detection was very low (1.5-2.5 ng/mL for all analytes). The relative standard deviations for analysis of 1 μg/mL of the analytes were between 3.2-6.1%. Salt addition showed no significant effect on extraction recovery. Finally, the proposed method was successfully utilized for the extraction and determination of the phthalic acid esters in human plasma samples and satisfactory results were obtained. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

36 CFR 51.48 - What happens to a right of preference in the event of termination of a concession contract for...

Code of Federal Regulations, 2010 CFR

2010-07-01

... its terms at any time for less than satisfactory performance or otherwise. If a concession contract is terminated for less than satisfactory performance or other breach, the terminated concessioner, even if... terminated a concession contract for less than satisfactory performance or other breach will not limit the...

41 CFR 102-117.285 - What are my choices if a TSP's performance is not satisfactory?

Code of Federal Regulations, 2010 CFR

2010-07-01

... 41 Public Contracts and Property Management 3 2010-07-01 2010-07-01 false What are my choices if a TSP's performance is not satisfactory? 102-117.285 Section 102-117.285 Public Contracts and Property... are my choices if a TSP's performance is not satisfactory? You may choose to place a TSP in temporary...

34 CFR 361.89 - Enforcement procedures.

Code of Federal Regulations, 2010 CFR

2010-07-01

... revisions until the DSU sustains satisfactory performance based on the current performance levels over a period of more than 1 year. (d) If the Secretary determines that a DSU with less than satisfactory... satisfactory level on the compliance indicators. (Approved by the Office of Management and Budget under control...

13 CFR 120.434 - What are SBA's requirements for loan pledges?

Code of Federal Regulations, 2010 CFR

2010-01-01

... satisfactory SBA performance, as determined by SBA in its discretion. The Lender's Risk Rating, among other factors, will be considered in determining satisfactory SBA performance. Other factors may include, but...); (d) All loan documents must be satisfactory to SBA and must include a multi-party agreement among SBA...

Simultaneous determination of thirteen different steroid hormones using micro UHPLC-MS/MS with on-line SPE system.

PubMed

Márta, Zoltán; Bobály, Balázs; Fekete, Jenő; Magda, Balázs; Imre, Tímea; Mészáros, Katalin Viola; Bálint, Mária; Szabó, Pál Tamás

2018-02-20

Ultratrace analysis of sample components requires excellent analytical performance in terms of limits of quantitation (LOQ). Micro UHPLC coupled to sensitive tandem mass spectrometry provides state of the art solution for such analytical problems. Using on-line SPE with column switching on a micro UHPLC-MS/MS system allowed to decrease LOQ without any complex sample preparation protocol. The presented method is capable of reaching satisfactory low LOQ values for analysis of thirteen different steroid molecules from human plasma without the most commonly used off-line SPE or compound derivatization. Steroids were determined by using two simple sample preparation methods, based on lower and higher plasma steroid concentrations. In the first method, higher analyte concentrations were directly determined after protein precipitation with methanol. The organic phase obtained from the precipitation was diluted with water and directly injected into the LC-MS system. In the second method, low steroid levels were determined by concentrating the organic phase after steroid extraction. In this case, analytes were extracted with ethyl acetate and reconstituted in 90/10 water/acetonitrile following evaporation to dryness. This step provided much lower LOQs, outperforming previously published values. The method has been validated and subsequently applied to clinical laboratory measurement. Copyright © 2017 Elsevier B.V. All rights reserved.

The Empower project - a new way of assessing and monitoring test comparability and stability.

PubMed

De Grande, Linde A C; Goossens, Kenneth; Van Uytfanghe, Katleen; Stöckl, Dietmar; Thienpont, Linda M

2015-07-01

Manufacturers and laboratories might benefit from using a modern integrated tool for quality management/assurance. The tool should not be confounded by commutability issues and focus on the intrinsic analytical quality and comparability of assays as performed in routine laboratories. In addition, it should enable monitoring of long-term stability of performance, with the possibility to quasi "real-time" remedial action. Therefore, we developed the "Empower" project. The project comprises four pillars: (i) master comparisons with panels of frozen single-donation samples, (ii) monitoring of patient percentiles and (iii) internal quality control data, and (iv) conceptual and statistical education about analytical quality. In the pillars described here (i and ii), state-of-the-art as well as biologically derived specifications are used. In the 2014 master comparisons survey, 125 laboratories forming 8 peer groups participated. It showed not only good intrinsic analytical quality of assays but also assay biases/non-comparability. Although laboratory performance was mostly satisfactory, sometimes huge between-laboratory differences were observed. In patient percentile monitoring, currently, 100 laboratories participate with 182 devices. Particularly, laboratories with a high daily throughput and low patient population variation show a stable moving median in time with good between-instrument concordance. Shifts/drifts due to lot changes are sometimes revealed. There is evidence that outpatient medians mirror the calibration set-points shown in the master comparisons. The Empower project gives manufacturers and laboratories a realistic view on assay quality/comparability as well as stability of performance and/or the reasons for increased variation. Therefore, it is a modern tool for quality management/assurance toward improved patient care.

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

Batcheller, Thomas Aquinas; Taylor, Dean Dalton

Idaho Nuclear Technology and Engineering Center 300,000-gallon vessel WM-189 was filled in late 2001 with concentrated sodium bearing waste (SBW). Three airlifted liquid samples and a steam jetted slurry sample were obtained for quantitative analysis and characterization of WM-189 liquid phase SBW and tank heel sludge. Estimates were provided for most of the reported data values, based on the greater of (a) analytical uncertainty, and (b) variation of analytical results between nominally similar samples. A consistency check on the data was performed by comparing the total mass of dissolved solids in the liquid, as measured gravimetrically from a dried sample,more » with the corresponding value obtained by summing the masses of cations and anions in the liquid, based on the reported analytical data. After reasonable adjustments to the nitrate and oxygen concentrations, satisfactory consistency between the two results was obtained. A similar consistency check was performed on the reported compositional data for sludge solids from the steam jetted sample. In addition to the compositional data, various other analyses were performed: particle size distribution was measured for the sludge solids, sludge settling tests were performed, and viscosity measurements were made. WM-189 characterization results were compared with those for WM-180, and other Tank Farm Facility tank characterization data. A 2-liter batch of WM-189 simulant was prepared and a clear, stable solution was obtained, based on a general procedure for mixing SBW simulant that was develop by Dr. Jerry Christian. This WM-189 SBW simulant is considered suitable for laboratory testing for process development.« less

Quality specification and status of internal quality control of cardiac biomarkers in China from 2011 to 2016.

PubMed

Li, Tingting; Wang, Wei; Zhao, Haijian; He, Falin; Zhong, Kun; Yuan, Shuai; Wang, Zhiguo

2017-09-07

This study aimed to investigate the status of internal quality control (IQC) for cardiac biomarkers from 2011 to 2016 so that we can have overall knowledge of the precision level of measurements in China and set appropriate precision specifications. Internal quality control data of cardiac biomarkers, including creatinine kinase MB (CK-MB) (μg/L), CK-MB(U/L), myoglobin (Mb), cardiac troponin I (cTnI), cardiac troponin T (cTnT), and homocysteines (HCY), were collected by a web-based external quality assessment (EQA) system. Percentages of laboratories meeting five precision quality specifications for current coefficient of variations (CVs) were calculated. Then, appropriate precision specifications were chosen for these six analytes. Finally, the CVs and IQC practice were further analyzed with different grouping methods. The current CVs remained nearly constant for 6 years. cTnT had the highest pass rates every year against five specifications, whereas HCY had the lowest pass rates. Overall, most analytes had a satisfactory performance (pass rates >80%), except for HCY, if one-third TEa or the minimum specification were employed. When the optimal specification was applied, the performance of most analytes was frustrating (pass rates < 60%) except for cTnT. The appropriate precision specifications of Mb, cTnI, cTnT and HCY were set as current CVs less than 9.20%, 9.90%, 7.50%, 10.54%, 7.63%, and 6.67%, respectively. The data of IQC practices indicated wide variation and substantial progress. The precision performance of cTnT was already satisfying, while the other five analytes, especially HCY, were still frustrating; thus, ongoing investigation and continuous improvement for IQC are still needed. © 2017 Wiley Periodicals, Inc.

Simultaneous determination of eight flavonoids in propolis using chemometrics-assisted high performance liquid chromatography-diode array detection.

PubMed

Sun, Yan-Mei; Wu, Hai-Long; Wang, Jian-Yao; Liu, Zhi; Zhai, Min; Yu, Ru-Qin

2014-07-01

A fast analytical strategy of second-order calibration method based on the alternating trilinear decomposition algorithm (ATLD)-assisted high performance liquid chromatography coupled with a diode array detector (HPLC-DAD) was established for the simultaneous determination of eight flavonoids (rutin, quercetin, luteolin, kaempferol, isorhamnetin, apigenin, galangin and chrysin) in propolis capsules samples. The chromatographic separation was implemented on a Wondasil™ C18 column (250mm×4.6mm, 5μm) within 13min with a binary mobile phase composed of water with 1% formic acid and methanol at a flow rate of 1.0mLmin(-1) after flavonoids were only extracted with methanol by ultrasound extraction for 15min. The baseline problem was overcome by considering background drift as additional compositions or factors as well as the target analytes, and ATLD was employed to handle the overlapping peaks from analytes of interest or from analytes and co-eluting matrix compounds. The linearity was good with the correlation coefficients no less than 0.9947; the limit of detections (LODs) within the range of 3.39-33.05ngmL(-1) were low enough; the accuracy was confirmed by the recoveries ranged from 91.9% to 110.2% and the root-mean-square-error of predictions (RMSEPs) less than 1.1μg/mL. The results indicated that the chromatographic method with the aid of ATLD is efficient, sensitive and cost-effective and can realize the resolution and accurate quantification of flavonoids even in the presence of interferences, thus providing an alternative method for accurate quantification of analytes especially when the complete separation is not easily accomplished. The method was successfully applied to propolis capsules samples and the satisfactory results were obtained. Copyright © 2014 Elsevier B.V. All rights reserved.

A sustainable on-line CapLC method for quantifying antifouling agents like irgarol-1051 and diuron in water samples: Estimation of the carbon footprint.

PubMed

Pla-Tolós, J; Serra-Mora, P; Hakobyan, L; Molins-Legua, C; Moliner-Martinez, Y; Campins-Falcó, P

2016-11-01

In this work, in-tube solid phase microextraction (in-tube SPME) coupled to capillary LC (CapLC) with diode array detection has been reported, for on-line extraction and enrichment of booster biocides (irgarol-1051 and diuron) included in Water Frame Directive 2013/39/UE (WFD). The analytical performance has been successfully demonstrated. Furthermore, in the present work, the environmental friendliness of the procedure has been quantified by means of the implementation of the carbon footprint calculation of the analytical procedure and the comparison with other methodologies previously reported. Under the optimum conditions, the method presents good linearity over the range assayed, 0.05-10μg/L for irgarol-1051 and 0.7-10μg/L for diuron. The LODs were 0.015μg/L and 0.2μg/L for irgarol-1051 and diuron, respectively. Precision was also satisfactory (relative standard deviation, RSD<3.5%). The proposed methodology was applied to monitor water samples, taking into account the EQS standards for these compounds. The carbon footprint values for the proposed procedure consolidate the operational efficiency (analytical and environmental performance) of in-tube SPME-CapLC-DAD, in general, and in particular for determining irgarol-1051 and diuron in water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Potential of dynamically harmonized Fourier transform ion cyclotron resonance cell for high-throughput metabolomics fingerprinting: control of data quality.

PubMed

Habchi, Baninia; Alves, Sandra; Jouan-Rimbaud Bouveresse, Delphine; Appenzeller, Brice; Paris, Alain; Rutledge, Douglas N; Rathahao-Paris, Estelle

2018-01-01

Due to the presence of pollutants in the environment and food, the assessment of human exposure is required. This necessitates high-throughput approaches enabling large-scale analysis and, as a consequence, the use of high-performance analytical instruments to obtain highly informative metabolomic profiles. In this study, direct introduction mass spectrometry (DIMS) was performed using a Fourier transform ion cyclotron resonance (FT-ICR) instrument equipped with a dynamically harmonized cell. Data quality was evaluated based on mass resolving power (RP), mass measurement accuracy, and ion intensity drifts from the repeated injections of quality control sample (QC) along the analytical process. The large DIMS data size entails the use of bioinformatic tools for the automatic selection of common ions found in all QC injections and for robustness assessment and correction of eventual technical drifts. RP values greater than 10 6 and mass measurement accuracy of lower than 1 ppm were obtained using broadband mode resulting in the detection of isotopic fine structure. Hence, a very accurate relative isotopic mass defect (RΔm) value was calculated. This reduces significantly the number of elemental composition (EC) candidates and greatly improves compound annotation. A very satisfactory estimate of repeatability of both peak intensity and mass measurement was demonstrated. Although, a non negligible ion intensity drift was observed for negative ion mode data, a normalization procedure was easily applied to correct this phenomenon. This study illustrates the performance and robustness of the dynamically harmonized FT-ICR cell to perform large-scale high-throughput metabolomic analyses in routine conditions. Graphical abstract Analytical performance of FT-ICR instrument equipped with a dynamically harmonized cell.

Evaluation of a recent product to remove lipids and other matrix co-extractives in the analysis of pesticide residues and environmental contaminants in foods.

PubMed

Han, Lijun; Matarrita, Jessie; Sapozhnikova, Yelena; Lehotay, Steven J

2016-06-03

This study demonstrates the application of a novel lipid removal product to the residue analysis of 65 pesticides and 52 environmental contaminants in kale, pork, salmon, and avocado by fast, low pressure gas chromatography - tandem mass spectrometry (LPGC-MS/MS). Sample preparation involves QuEChERS extraction followed by use of EMR-Lipid ("enhanced matrix removal of lipids") and an additional salting out step for cleanup. The optimal amount of EMR-Lipid was determined to be 500mg for 2.5mL extracts for most of the analytes. The co-extractive removal efficiency by the EMR-Lipid cleanup step was 83-98% for fatty samples and 79% for kale, including 76% removal of chlorophyll. Matrix effects were typically less than ±20%, in part because analyte protectants were used in the LPGC-MS/MS analysis. The recoveries of polycyclic aromatic hydrocarbons and diverse pesticides were mostly 70-120%, whereas recoveries of nonpolar polybrominated diphenyl ethers and polychlorinated biphenyls were mostly lower than 70% through the cleanup procedure. With the use of internal standards, method validation results showed that 76-85 of the 117 analytes achieved satisfactory results (recoveries of 70-120% and RSD≤20%) in pork, avocado, and kale, while 53 analytes had satisfactory results in salmon. Detection limits were 5-10ng/g for all but a few analytes. EMR-Lipid is a new sample preparation tool that serves as another useful option for cleanup in multiresidue analysis, particularly of fatty foods. Published by Elsevier B.V.

An Improved Call Admission Control Mechanism with Prioritized Handoff Queuing Scheme for BWA Networks

NASA Astrophysics Data System (ADS)

Chowdhury, Prasun; Saha Misra, Iti

2014-10-01

Nowadays, due to increased demand for using the Broadband Wireless Access (BWA) networks in a satisfactory manner a promised Quality of Service (QoS) is required to manage the seamless transmission of the heterogeneous handoff calls. To this end, this paper proposes an improved Call Admission Control (CAC) mechanism with prioritized handoff queuing scheme that aims to reduce dropping probability of handoff calls. Handoff calls are queued when no bandwidth is available even after the allowable bandwidth degradation of the ongoing calls and get admitted into the network when an ongoing call is terminated with a higher priority than the newly originated call. An analytical Markov model for the proposed CAC mechanism is developed to analyze various performance parameters. Analytical results show that our proposed CAC with handoff queuing scheme prioritizes the handoff calls effectively and reduces dropping probability of the system by 78.57% for real-time traffic without degrading the number of failed new call attempts. This results in the increased bandwidth utilization of the network.

Determination of carbohydrates in honey and milk by capillary electrophoresis in combination with graphene-cobalt microsphere hybrid paste electrodes.

PubMed

Liang, Peipei; Sun, Motao; He, Peimin; Zhang, Luyan; Chen, Gang

2016-01-01

A graphene-cobalt microsphere (CoMS) hybrid paste electrode was developed for the determination of carbohydrates in honey and milk in combination with capillary electrophoresis (CE). The performance of the electrodes was demonstrated by detecting mannitol, sucrose, lactose, glucose, and fructose after CE separation. The five analytes were well separated within 9 min in a 40 cm long capillary at a separation voltage of 12 kV. The electrodes exhibited pronounced electrocatalytic activity, lower detection potentials, enhanced signal-to-noise characteristics, and higher reproducibility. The relation between peak current and analyte concentration was linear over about three orders of magnitude. The proposed method had been employed to determine lactose in bovine milk and glucose and fructose in honey with satisfactory results. Because only electroactive substances in the samples could be detected on the paste electrode, the electropherograms of both food samples were simplified to some extent. Copyright © 2015 Elsevier Ltd. All rights reserved.

Sustained prediction ability of net analyte preprocessing methods using reduced calibration sets. Theoretical and experimental study involving the spectrophotometric analysis of multicomponent mixtures.

PubMed

Goicoechea, H C; Olivieri, A C

2001-07-01

A newly developed multivariate method involving net analyte preprocessing (NAP) was tested using central composite calibration designs of progressively decreasing size regarding the multivariate simultaneous spectrophotometric determination of three active components (phenylephrine, diphenhydramine and naphazoline) and one excipient (methylparaben) in nasal solutions. Its performance was evaluated and compared with that of partial least-squares (PLS-1). Minimisation of the calibration predicted error sum of squares (PRESS) as a function of a moving spectral window helped to select appropriate working spectral ranges for both methods. The comparison of NAP and PLS results was carried out using two tests: (1) the elliptical joint confidence region for the slope and intercept of a predicted versus actual concentrations plot for a large validation set of samples and (2) the D-optimality criterion concerning the information content of the calibration data matrix. Extensive simulations and experimental validation showed that, unlike PLS, the NAP method is able to furnish highly satisfactory results when the calibration set is reduced from a full four-component central composite to a fractional central composite, as expected from the modelling requirements of net analyte based methods.

Investigating the Mobility of Trilayer Graphene Nanoribbon in Nanoscale FETs

NASA Astrophysics Data System (ADS)

Rahmani, Meisam; Ghafoori Fard, Hassan; Ahmadi, Mohammad Taghi; Rahbarpour, Saeideh; Habibiyan, Hamidreza; Varmazyari, Vali; Rahmani, Komeil

2017-10-01

The aim of the present paper is to investigate the scaling behaviors of charge carrier mobility as one of the most remarkable characteristics for modeling of nanoscale field-effect transistors (FETs). Many research groups in academia and industry are contributing to the model development and experimental identification of multi-layer graphene FET-based devices. The approach in the present work is to provide an analytical model for carrier mobility of tri-layer graphene nanoribbon (TGN) FET. In order to do so, one starts by identifying the analytical modeling of TGN carrier velocity and ballistic conductance. At the end, a model of charge carrier mobility with numerical solution is analytically derived for TGN FET, in which the carrier concentration, temperature and channel length characteristics dependence are highlighted. Moreover, variation of band gap and gate voltage during the proposed device operation and its effect on carrier mobility is investigated. To evaluate the nanoscale FET performance, the carrier mobility model is also adopted to obtain the I-V characteristics of the device. In order to verify the accuracy of the proposed analytical model for TGN mobility, it is compared to the existing experimental data, and a satisfactory agreement is reported for analogous ambient conditions. Moreover, the proposed model is compared with the published data of single-layer graphene and bi-layer graphene, in which the obtained results demonstrate significant insights into the importance of charge carrier mobility impact in high-performance TGN FET. The work presented here is one step towards an applicable model for real-world nanoscale FETs.

Optimization and validation of the reversed-phase high-performance liquid chromatography with fluorescence detection method for the separation of tocopherol and tocotrienol isomers in cereals, employing a novel sorbent material.

PubMed

Irakli, Maria N; Samanidou, Victoria F; Papadoyannis, Ioannis N

2012-03-07

The separation and determination of tocopherols (Ts) and tocotrienols (T3s) by reversed-phase high-performance liquid chromatography with fluorescence detection has been developed and validated after optimization of various chromatographic conditions and other experimental parameters. Analytes were separated on a PerfectSil Target ODS-3 (250 × 4.6 mm, 3 μm) column filled with a novel sorbent material of ultrapure silica gel. The separation of Ts and T3s was optimized in terms of mobile-phase composition and column temperature on the basis of the best compromise among efficiency, resolution, and analysis time. Using a gradient elution of mobile phase composed of isopropanol/water and 7 °C column temperature, a satisfactory resolution was achieved within 62 min. For the quantitative determination, α-T acetate (50 μg/mL) was used as the internal standard. Detection limits ranged from 0.27 μg/mL (γ-T) to 0.76 μg/mL (γ-T3). The validation of the method was examined performing intraday (n = 5) and interday (n = 3) assays and was found to be satisfactory, with high accuracy and precision results. Solid-phase extraction provided high relative extraction recoveries from cereal samples: 87.0% for γ-T3 and 115.5% for δ-T. The method was successfully applied to cereals, such as durum wheat, bread wheat, rice, barley, oat, rye, and corn.

[Monitoring method for macroporous resin column chromatography process of salvianolic acids based on near infrared spectroscopy].

PubMed

Hou, Xiang-Mei; Zhang, Lei; Yue, Hong-Shui; Ju, Ai-Chun; Ye, Zheng-Liang

2016-07-01

To study and establish a monitoring method for macroporous resin column chromatography process of salvianolic acids by using near infrared spectroscopy (NIR) as a process analytical technology (PAT).The multivariate statistical process control (MSPC) model was developed based on 7 normal operation batches, and 2 test batches (including one normal operation batch and one abnormal operation batch) were used to verify the monitoring performance of this model. The results showed that MSPC model had a good monitoring ability for the column chromatography process. Meanwhile, NIR quantitative calibration model was established for three key quality indexes (rosmarinic acid, lithospermic acid and salvianolic acid B) by using partial least squares (PLS) algorithm. The verification results demonstrated that this model had satisfactory prediction performance. The combined application of the above two models could effectively achieve real-time monitoring for macroporous resin column chromatography process of salvianolic acids, and can be used to conduct on-line analysis of key quality indexes. This established process monitoring method could provide reference for the development of process analytical technology for traditional Chinese medicines manufacturing. Copyright© by the Chinese Pharmaceutical Association.

Rapid and reliable QuEChERS-based LC-MS/MS method for determination of acrylamide in potato chips and roasted coffee

NASA Astrophysics Data System (ADS)

Stefanović, S.; Đorđevic, V.; Jelušić, V.

2017-09-01

The aim of this paper is to verify the performance characteristics and fitness for purpose of rapid and simple QuEChERS-based LC-MS/MS method for determination of acrylamide in potato chips and coffee. LC-MS/MS is by far the most suitable analytical technique for acrylamide measurements given its inherent sensitivity and selectivity, as well as capability of analyzing underivatized molecule. Acrylamide in roasted coffee and potato chips wasextracted with water:acetonitrile mixture using NaCl and MgSO4. Cleanup was carried out with MgSO4 and PSA. Obtained results were satisfactory. Recoveries were in the range of 85-112%, interlaboratory reproducibility (Cv) was 5.8-7.6% and linearity (R2) was in the range of 0.995-0.999. LoQ was 35 μg kg-1 for coffee and 20 μg kg-1 for potato chips. Performance characteristic of the method are compliant with criteria for analytical methods validation. Presented method for quantitative determination of acrylamide in roasted coffee and potato chips is fit for purposes of self-control in food industry as well as regulatory controls carried out by the governmental agencies.

Ultra-high performance liquid chromatography with fluorescence detection following salting-out assisted liquid-liquid extraction for the analysis of benzimidazole residues in farm fish samples.

PubMed

Tejada-Casado, Carmen; Lara, Francisco J; García-Campaña, Ana M; Del Olmo-Iruela, Monsalud

2018-03-30

Ultra-high performance liquid chromatography (UHPLC) coupled with fluorescence detection (FL) has been proposed for the first time to determine thirteen benzimidazoles (BZs) in farmed fish samples. In order to optimize the chromatographic separation, parameters such as mobile phase composition and flow rate were carefully studied, establishing a gradient mode with a mobile phase consisted of water (solvent A) and acetonitrile (solvent B) at a flow rate of 0.4 mL/min. The separation was performed on a Zorbax Eclipse Plus RRHD C 18 column (50 × 2.1 mm, 1.8 μm), involving a total analysis time lower than 12 min. Salting-out assisted liquid-liquid extraction (SALLE) was applied as sample treatment to different types of farmed fish (trout, sea bream and sea bass). To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized including the amount of sample, type and volume of the extraction solvent, and the nature and amount of the salt used. Characterization of the method in terms of performance characteristics was carried out, obtaining satisfactory results for the linearity (R 2  ≥ 0.997), repeatability (RSD ≤ 6.1%), reproducibility (RSD ≤ 10.8%) and recoveries (R ≥ 79%; RSD ≤ 7.8%). Detection limits between 0.04-29.9 μg kg -1 were obtained, demonstrating the applicability of this fast, simple and environmentally friendly method. Copyright © 2018 Elsevier B.V. All rights reserved.

Mixed hemimicelles solid-phase extraction based on ionic liquid-coated Fe3O4/SiO2 nanoparticles for the determination of flavonoids in bio-matrix samples coupled with high performance liquid chromatography.

PubMed

He, Huan; Yuan, Danhua; Gao, Zhanqi; Xiao, Deli; He, Hua; Dai, Hao; Peng, Jun; Li, Nan

2014-01-10

A novel magnetic solid-phase extraction (MSPE) method based on mixed hemimicelles of room temperature ionic liquids (RTILs) coated Fe3O4/SiO2 nanoparticles (NPs) was developed for simultaneous extraction of trace amounts of flavonoids in bio-matrix samples. A comparative study on the use of RTILs (C16mimBr) and CTAB-coated Fe3O4/SiO2 NPs as sorbents was presented. Owing to bigger adsorption amounts for analytes, RTILs-coated Fe3O4/SiO2 NPs was selected as MSPE materials and three analytes luteolin, quercetin and kaempferol can be quantitatively extracted and simultaneously determined coupled with high performance liquid chromatography (HPLC) in urine samples. No interferences were caused by proteins or endogenous compounds. Good linearity (R(2)>0.9993) for all calibration curves was obtained, and the limits of detection (LOD) for luteolin, quercetin and kaempferol were 0.10 ng/mL, 0.50 ng/mL and 0.20 ng/mL in urine samples, respectively. Satisfactory recoveries (93.5-97.6%, 90.1-95.4% and 93.3-96.6% for luteolin, quercetin and kaempferol) in biological matrices were achieved. It was notable that while using a small amount of Fe3O4/SiO2 NPs (4.0 mg) and C16mimBr (1.0 mg), satisfactory preconcentration factors and extraction recoveries for the three flavonoids were obtained. To the best of our knowledge, this is the first time a mixed hemimicelles MSPE method based on RTILs and Fe3O4/SiO2 NPs magnetic separation has ever been used for pretreatment of complex biological samples. Copyright © 2013 Elsevier B.V. All rights reserved.

One-pot preparation of magnetic carbon adsorbent derived from pomelo peel for magnetic solid-phase extraction of pollutants in environmental waters.

PubMed

Huang, Youfang; Peng, Jinghe; Huang, Xiaojia

2018-04-20

In this work, magnetic carbon material derived from pomelo peels (MCMPs) was conveniently fabricated utilizing one-pot synthesis method and employed as adsorbent of magnetic solid-phase extraction (MSPE). Several characterized measures including infrared spectroscopy, scanning electron microscopy, transmission electron microscopy and vibrating sample magnetometer were used to investigate the morphology, spectroscopic and magnetic properties of prepared adsorbent. Apolar parabens and polar fluoroquinolones (FQs) were used to investigate the extraction performance of MCMPs. Under the optimized extraction conditions, the MCMPs displayed satisfactory extraction performance for target analytes. At the same time, the MCMPs/MSPE was combined with HPLC-DAD for the sensitive determination of parabens and FQs in real-life water samples. Results showed that the limits of detection (S/N = 3) for parabens and FQs were in the ranges of 0.011-0.053 μg/L and 0.012-0.46 μg/L, respectively. The spiked recoveries were in the range of 76.6-116% for parabens and 80.2-114% for FQs with good repeatability (relative standard deviations less than 10%). In comparison to reported methods, the developed MCMPs/MSPE-HPLC-DAD showed some merits including low-cost, simplicity, satisfactory sensitivity and green non-pollution. Copyright © 2018 Elsevier B.V. All rights reserved.

Configuration and validation of an analytical model predicting secondary neutron radiation in proton therapy using Monte Carlo simulations and experimental measurements.

PubMed

Farah, J; Bonfrate, A; De Marzi, L; De Oliveira, A; Delacroix, S; Martinetti, F; Trompier, F; Clairand, I

2015-05-01

This study focuses on the configuration and validation of an analytical model predicting leakage neutron doses in proton therapy. Using Monte Carlo (MC) calculations, a facility-specific analytical model was built to reproduce out-of-field neutron doses while separately accounting for the contribution of intra-nuclear cascade, evaporation, epithermal and thermal neutrons. This model was first trained to reproduce in-water neutron absorbed doses and in-air neutron ambient dose equivalents, H*(10), calculated using MCNPX. Its capacity in predicting out-of-field doses at any position not involved in the training phase was also checked. The model was next expanded to enable a full 3D mapping of H*(10) inside the treatment room, tested in a clinically relevant configuration and finally consolidated with experimental measurements. Following the literature approach, the work first proved that it is possible to build a facility-specific analytical model that efficiently reproduces in-water neutron doses and in-air H*(10) values with a maximum difference less than 25%. In addition, the analytical model succeeded in predicting out-of-field neutron doses in the lateral and vertical direction. Testing the analytical model in clinical configurations proved the need to separate the contribution of internal and external neutrons. The impact of modulation width on stray neutrons was found to be easily adjustable while beam collimation remains a challenging issue. Finally, the model performance agreed with experimental measurements with satisfactory results considering measurement and simulation uncertainties. Analytical models represent a promising solution that substitutes for time-consuming MC calculations when assessing doses to healthy organs. Copyright © 2015 Associazione Italiana di Fisica Medica. Published by Elsevier Ltd. All rights reserved.

An analytical approach to top predator interference on the dynamics of a food chain model

NASA Astrophysics Data System (ADS)

Senthamarai, R.; Vijayalakshmi, T.

2018-04-01

In this paper, a nonlinear mathematical model is proposed and analyzed to study of top predator interference on the dynamics of a food chain model. The mathematical model is formulated using the system of non-linear ordinary differential equations. In this model, there are three state dimensionless variables, viz, size of prey population x, size of intermediate predator y and size of top predator population z. The analytical results are compared with the numerical simulation using MATLAB software and satisfactory results are noticed.

Liquid chromatography-tandem mass spectrometry multiresidue method for the analysis of quaternary ammonium compounds in cheese and milk products: Development and validation using the total error approach.

PubMed

Slimani, Kahina; Féret, Aurélie; Pirotais, Yvette; Maris, Pierre; Abjean, Jean-Pierre; Hurtaud-Pessel, Dominique

2017-09-29

Quaternary ammonium compounds (QACs) are both cationic surfactants and biocidal substances widely used as disinfectants in the food industry. A sensitive and reliable method for the analysis of benzalkonium chlorides (BACs) and dialkyldimethylammonium chlorides (DDACs) has been developed that enables the simultaneous quantitative determination of ten quaternary ammonium residues in dairy products below the provisional maximum residue level (MRL), set at 0.1mgkg -1 . To the best of our knowledge, this method could be the one applicable to milk and to three major processed milk products selected, namely processed or hard pressed cheeses, and whole milk powder. The method comprises solvent extraction using a mixture of acetonitrile and ethyl acetate, without any further clean-up. Analyses were performed by liquid chromatography coupled with electrospray tandem mass spectrometry detection (LC-ESI-MS/MS) operating in positive mode. A C18 analytical column was used for chromatographic separation, with a mobile phase composed of acetonitrile and water both containing 0.3% formic acid; and methanol in the gradient mode. Five deuterated internal standards were added to obtain the most accurate quantification. Extraction recoveries were satisfactory and no matrix effects were observed. The method was validated using the total error approach in accordance with the NF V03-110 standard in order to characterize the trueness, repeatability, intermediate precision and analytical limits within the range of 5-150μgkg -1 for all matrices. These performance criteria, calculated by e.noval ® 3.0 software, were satisfactory and in full accordance with the proposed provisional MRL and with the recommendations in the European Union SANTE/11945/2015 regulatory guidelines. The limit of detection (LOD) was low (<1.9μgkg -1 ) and the limit of quantification (LOQ) ranged from 5μgkg -1 to 35μgkg -1 for all matrices depending on the analytes. The validation results proved that the method is suitable for quantifying quaternary ammoniums in foodstuffs from dairy industries at residue levels, and could be used for biocide residues monitoring plans and to measure the exposition consumer to biocides products. Copyright © 2017 Elsevier B.V. All rights reserved.

Model of critical diagnostic reasoning: achieving expert clinician performance.

PubMed

Harjai, Prashant Kumar; Tiwari, Ruby

2009-01-01

Diagnostic reasoning refers to the analytical processes used to determine patient health problems. While the education curriculum and health care system focus on training nurse clinicians to accurately recognize and rescue clinical situations, assessments of non-expert nurses have yielded less than satisfactory data on diagnostic competency. The contrast between the expert and non-expert nurse clinician raises the important question of how differences in thinking may contribute to a large divergence in accurate diagnostic reasoning. This article recognizes superior organization of one's knowledge base, using prototypes, and quick retrieval of pertinent information, using similarity recognition as two reasons for the expert's superior diagnostic performance. A model of critical diagnostic reasoning, using prototypes and similarity recognition, is proposed and elucidated using case studies. This model serves as a starting point toward bridging the gap between clinical data and accurate problem identification, verification, and management while providing a structure for a knowledge exchange between expert and non-expert clinicians.

Low Density Solvent-Based Dispersive Liquid-Liquid Microextraction for the Determination of Synthetic Antioxidants in Beverages by High-Performance Liquid Chromatography

PubMed Central

Çabuk, Hasan; Köktürk, Mustafa

2013-01-01

A simple and efficient method was established for the determination of synthetic antioxidants in beverages by using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection. Butylated hydroxy toluene, butylated hydroxy anisole, and tert-butylhydroquinone were the antioxidants evaluated. Experimental parameters including extraction solvent, dispersive solvent, pH of sample solution, salt concentration, and extraction time were optimized. Under optimal conditions, the extraction recoveries ranged from 53 to 96%. Good linearity was observed by the square of correlation coefficients ranging from 0.9975 to 0.9997. The relative standard deviations ranged from 1.0 to 5.2% for all of the analytes. Limits of detection ranged from 0.85 to 2.73 ng mL−1. The method was successfully applied for determination of synthetic antioxidants in undiluted beverage samples with satisfactory recoveries. PMID:23853535

Evaluation of neutron thermalization parameters and benchmark reactor calculations using a synthetic scattering function for molecular gases

NASA Astrophysics Data System (ADS)

Gillette, V. H.; Patiño, N. E.; Granada, J. R.; Mayer, R. E.

1989-08-01

Using a synthetic incoherent scattering function which describes the interaction of neutrons with molecular gases we provide analytical expressions for zero- and first-order scattering kernels, σ0( E0 → E), σ1( E0 → E), and total cross section σ0( E0). Based on these quantities, we have performed calculations of thermalization parameters and transport coefficients for H 2O, D 2O, C 6H 6 and (CH 2) n at room temperature. Comparison of such values with available experimental data and other calculations is satisfactory. We also generated nuclear data libraries for H 2O with 47 thermal groups at 300 K and performed some benchmark calculations ( 235U, 239Pu, PWR cell and typical APWR cell); the resulting reactivities are compared with experimental data and ENDF/B-IV calculations.

Rapid determination of residues of pesticides in honey by µGC-ECD and GC-MS/MS: Method validation and estimation of measurement uncertainty according to document No. SANCO/12571/2013.

PubMed

Paoloni, Angela; Alunni, Sabrina; Pelliccia, Alessandro; Pecorelli, Ivan

2016-01-01

A simple and straightforward method for simultaneous determination of residues of 13 pesticides in honey samples (acrinathrin, bifenthrin, bromopropylate, cyhalothrin-lambda, cypermethrin, chlorfenvinphos, chlorpyrifos, coumaphos, deltamethrin, fluvalinate-tau, malathion, permethrin and tetradifon) from different pesticide classes has been developed and validated. The analytical method provides dissolution of honey in water and an extraction of pesticide residues by n-Hexane followed by clean-up on a Florisil SPE column. The extract was evaporated and taken up by a solution of an injection internal standard (I-IS), ethion, and finally analyzed by capillary gas chromatography with electron capture detection (GC-µECD). Identification for qualitative purpose was conducted by gas chromatography with triple quadrupole mass spectrometer (GC-MS/MS). A matrix-matched calibration curve was performed for quantitative purposes by plotting the area ratio (analyte/I-IS) against concentration using a GC-µECD instrument. According to document No. SANCO/12571/2013, the method was validated by testing the following parameters: linearity, matrix effect, specificity, precision, trueness (bias) and measurement uncertainty. The analytical process was validated analyzing blank honey samples spiked at levels equal to and greater than 0.010 mg/kg (limit of quantification). All parameters were satisfactorily compared with the values established by document No. SANCO/12571/2013. The analytical performance was verified by participating in eight multi-residue proficiency tests organized by BIPEA, obtaining satisfactory z-scores in all 70 determinations. Measurement uncertainty was estimated according to the top-down approaches described in Appendix C of the SANCO document using the within-laboratory reproducibility relative standard deviation combined with laboratory bias using the proficiency test data.

Social Support, Network Structure, and the Inventory of Socially Supportive Behaviors.

ERIC Educational Resources Information Center

Stokes, Joseph P.; Wilson, Diane Grimard

The Inventory of Socially Supportive Behaviors (ISSB) appears to be a satisfactory measure of social support with good reliability and some evidence of validity. To investigate the dimensionality of the ISSB through factor analytic procedures and to predict social support from social network variables, 179 college students (97 male, 82 female)…

Microemulsification: an approach for analytical determinations.

PubMed

Lima, Renato S; Shiroma, Leandro Y; Teixeira, Alvaro V N C; de Toledo, José R; do Couto, Bruno C; de Carvalho, Rogério M; Carrilho, Emanuel; Kubota, Lauro T; Gobbi, Angelo L

2014-09-16

We address a novel method for analytical determinations that combines simplicity, rapidity, low consumption of chemicals, and portability with high analytical performance taking into account parameters such as precision, linearity, robustness, and accuracy. This approach relies on the effect of the analyte content over the Gibbs free energy of dispersions, affecting the thermodynamic stabilization of emulsions or Winsor systems to form microemulsions (MEs). Such phenomenon was expressed by the minimum volume fraction of amphiphile required to form microemulsion (Φ(ME)), which was the analytical signal of the method. Thus, the measurements can be taken by visually monitoring the transition of the dispersions from cloudy to transparent during the microemulsification, like a titration. It bypasses the employment of electric energy. The performed studies were: phase behavior, droplet dimension by dynamic light scattering, analytical curve, and robustness tests. The reliability of the method was evaluated by determining water in ethanol fuels and monoethylene glycol in complex samples of liquefied natural gas. The dispersions were composed of water-chlorobenzene (water analysis) and water-oleic acid (monoethylene glycol analysis) with ethanol as the hydrotrope phase. The mean hydrodynamic diameter values for the nanostructures in the droplet-based water-chlorobenzene MEs were in the range of 1 to 11 nm. The procedures of microemulsification were conducted by adding ethanol to water-oleic acid (W-O) mixtures with the aid of micropipette and shaking. The Φ(ME) measurements were performed in a thermostatic water bath at 23 °C by direct observation that is based on the visual analyses of the media. The experiments to determine water demonstrated that the analytical performance depends on the composition of ME. It shows flexibility in the developed method. The linear range was fairly broad with limits of linearity up to 70.00% water in ethanol. For monoethylene glycol in water, in turn, the linear range was observed throughout the volume fraction of analyte. The best limits of detection were 0.32% v/v water to ethanol and 0.30% v/v monoethylene glycol to water. Furthermore, the accuracy was highly satisfactory. The natural gas samples provided by the Petrobras exhibited color, particulate material, high ionic strength, and diverse compounds as metals, carboxylic acids, and anions. These samples had a conductivity of up to 2630 μS cm(-1); the conductivity of pure monoethylene glycol was only 0.30 μS cm(-1). Despite such downsides, the method allowed accurate measures bypassing steps such as extraction, preconcentration, and dilution of the sample. In addition, the levels of robustness were promising. This parameter was evaluated by investigating the effect of (i) deviations in volumetric preparation of the dispersions and (ii) changes in temperature over the analyte contents recorded by the method.

Determination of atenolol in human plasma using ionic-liquid-based ultrasound-assisted in situ solvent formation microextraction followed by high-performance liquid chromatography.

PubMed

Zeeb, Mohsen; Farahani, Hadi; Papan, Mohammad Kazem

2016-06-01

An efficient analytical method called ionic-liquid-based ultrasound-assisted in situ solvent formation microextraction followed by high-performance liquid chromatography was developed for the determination of atenolol in human plasma. A hydrophobic ionic liquid (1-butyl-3-methylimidazolium hexafluorophosphate) was formed by the addition of a hydrophilic ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate) to a sample solution containing an ion-pairing agent during microextraction. The analyte was extracted into the ionic liquid phase while the microextraction solvent was dispersed throughout the sample by utilizing ultrasound. The sample was then centrifuged, and the extracting phase retracted into the microsyringe and injected to liquid chromatography. After optimization, the calibration curve showed linearity in the range of 2-750 ng/mL with the regression coefficient corresponding to 0.998. The limits of detection (S/N = 3) and quantification (S/N = 10) were 0.5 and 2 ng/mL, respectively. A reasonable relative recovery range of 90-96.7% and satisfactory intra-assay (4.8-5.1%, n = 6) and interassay (5.0-5.6%, n = 9) precision along with a substantial sample clean-up demonstrated good performance of the procedure. It was applied for the determination of atenolol in human plasma after oral administration and some pharmacokinetic data were obtained. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Early warning systems for the management of chronic heart failure: a systematic literature review of cost-effectiveness models.

PubMed

Albuquerque De Almeida, Fernando; Al, Maiwenn; Koymans, Ron; Caliskan, Kadir; Kerstens, Ankie; Severens, Johan L

2018-04-01

Describing the general and methodological characteristics of decision-analytical models used in the economic evaluation of early warning systems for the management of chronic heart failure patients and performing a quality assessment of their methodological characteristics is expected to provide concise and useful insight to inform the future development of decision-analytical models in the field of heart failure management. Areas covered: The literature on decision-analytical models for the economic evaluation of early warning systems for the management of chronic heart failure patients was systematically reviewed. Nine electronic databases were searched through the combination of synonyms for heart failure and sensitive filters for cost-effectiveness and early warning systems. Expert commentary: The retrieved models show some variability with regards to their general study characteristics. Overall, they display satisfactory methodological quality, even though some points could be improved, namely on the consideration and discussion of any competing theories regarding model structure and disease progression, identification of key parameters and the use of expert opinion, and uncertainty analyses. A comprehensive definition of early warning systems and further research under this label should be pursued. To improve the transparency of economic evaluation publications, authors should make available detailed technical information regarding the published models.

Development of a fast liquid chromatography-tandem mass spectrometry method for the determination of endocrine-disrupting compounds in waters.

PubMed

Di Carro, Marina; Scapolla, Carlo; Liscio, Camilla; Magi, Emanuele

2010-09-01

A fast liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS-MS) method was developed to study five endocrine-disrupting compounds (4-n-nonylphenol, bisphenol A, estrone, 17β-estradiol and 17α-ethinylestradiol) in water. Different columns were tested; the chromatographic separation of the analytes was optimized on a Pinnacle DB biphenylic column with a water-acetonitrile gradient elution, which allowed the separation of the selected endocrine-disrupting compounds (EDCs) in less than 6 min. Quantitative analysis was performed in selected reaction monitoring (SRM) mode; two transitions were chosen for each compound, using the most abundant for quantitation. Calibration curves using bisphenol A-d (16) as internal standard were drawn, showing good correlation coefficients (0.9993-0.9998). All figures of merit of the method were satisfactory; limits of detection were in the low pg range for all analytes. The method was then applied to the determination of the analytes in real water samples: to this aim, polar organic chemical integrative samplers (POCIS) were deployed in the influent and in the effluent of a drinking water treatment plant in Liguria (Italy). The EDC level was rather low in the influent and negligible in the outlet, reflecting the expected function of the treatment plant.

Analytical design of modified Smith predictor for unstable second-order processes with time delay

NASA Astrophysics Data System (ADS)

Ajmeri, Moina; Ali, Ahmad

2017-06-01

In this paper, a modified Smith predictor using three controllers, namely, stabilising (Gc), set-point tracking (Gc1), and load disturbance rejection (Gc2) controllers is proposed for second-order unstable processes with time delay. Controllers of the proposed structure are tuned using direct synthesis approach as this method enables the user to achieve a trade-off between the performance and robustness by adjusting a single design parameter. Furthermore, suitable values of the tuning parameters are recommended after studying their effect on the closed-loop performance and robustness. This is the main advantage of the proposed work over other recently published manuscripts, where authors provide only suitable ranges for the tuning parameters in spite of giving their suitable values. Simulation studies show that the proposed method results in satisfactory performance and improved robustness as compared to the recently reported control schemes. It is observed that the proposed scheme is able to work in the noisy environment also.

Antimisting kerosene JT3 engine fuel system integration study

NASA Technical Reports Server (NTRS)

Fiorentino, A.

1987-01-01

An analytical study and laboratory tests were conducted to assist NASA in determining the safety and mission suitability of the modified fuel system and flight tests for the Full-Scale Transport Controlled Impact Demonstration (CID) program. This twelve-month study reviewed and analyzed both the use of antimisting kerosene (AMK) fuel and the incorporation of a fuel degrader on the operational and performance characteristics of the engines tested. Potential deficiencies and/or failures were identified and approaches to accommodate these deficiencies were recommended to NASA Ames -Dryden Flight Research Facility. The result of flow characterization tests on degraded AMK fuel samples indicated levels of degradation satisfactory for the planned missions of the B-720 aircraft. The operability and performance with the AMK in a ground test engine and in the aircraft engines during the test flights were comparable to those with unmodified Jet A. For the final CID test, the JT-3C-7 engines performed satisfactorily while operating on AMK right up to impact.

Pressurized hot water extraction followed by miniaturized membrane assisted solvent extraction for the green analysis of alkylphenols in sediments.

PubMed

Salgueiro-González, N; Turnes-Carou, I; Muniategui-Lorenzo, S; López-Mahía, P; Prada-Rodríguez, D

2015-02-27

A novel and Green analytical methodology for the determination of alkylphenols (4-tert-octylphenol, 4-n-octylphenol, 4-n-nonylphenol, nonylphenol) in sediments was developed and validated. The method was based on pressurized hot water extraction (PHWE) followed by miniaturized membrane assisted solvent extraction (MASE) and liquid chromatography-electrospray ionization tandem mass spectrometry detection (LC-ESI-MS/MS). The extraction conditions were optimized by a Plackett-Burman design in order to minimize the number of assays according to Green principles. Matrix effect was studied and compensated using deuterated labeled standards as surrogate standards for the quantitation of the target compounds. The analytical features of the method were satisfactory: relative recoveries varied between 92 and 103% and repeatability and intermediate precision were <9% for all compounds. Quantitation limits of the method (MQL) ranged from 0.061 (4-n-nonylphenol) to 1.7ngg(-1) dry weight (nonylphenol). Sensitivity, selectivity, automaticity and fastness are the main advantages of the exposed methodology. Reagent consumption, analysis time and waste generation were minimized. The "greenness" of the proposed method was evaluated using an analytical Eco-Scale approach and satisfactory results were obtained. The applicability of the proposed method was demonstrated analysing sediment samples of Galicia coast (NW of Spain) and the ubiquity of alkylphenols in the environment was demonstrated. Copyright © 2015 Elsevier B.V. All rights reserved.

Conductive hydrogel composed of 1,3,5-benzenetricarboxylic acid and Fe3+ used as enhanced electrochemical immunosensing substrate for tumor biomarker.

PubMed

Wang, Huiqiang; Han, Hongliang; Ma, Zhanfang

2017-04-01

In this work, a new conductive hydrogel was prepared by a simple cross-linking coordination method using 1,3,5-benzenetricarboxylic acid as the ligand and Fe 3+ as the metal ion. The hydrogel film was formed on a glassy carbon electrode (GCE) by a drop coating method, which can dramatically facilitate the transport of electrons. A sensitive label-free electrochemical immunosensor was fabricated following electrodeposition of gold nanoparticles (AuNPs) on a hydrogel film and immobilization of an antibody. Neuron-specific enolase (NSE), a lung cancer biomarker, was used as the model analyte to be detected. The proposed immunosensor exhibited a wide linear detection range of 1pgmL -1 to 200ngmL -1 and a limit of detection of 0.26pgmL -1 (the ratio of signal to noise (S/N)=3). Moreover, the detection of NSE in human serum samples showed satisfactory accuracy compared with the data determined by enzyme-linked immunosorbent assay (ELISA), indicating good analytical performance of the immunoassay. Copyright © 2016 Elsevier B.V. All rights reserved.

Temperature field for radiative tomato peeling

NASA Astrophysics Data System (ADS)

Cuccurullo, G.; Giordano, L.

2017-01-01

Nowadays peeling of tomatoes is performed by using steam or lye, which are expensive and polluting techniques, thus sustainable alternatives are searched for dry peeling and, among that, radiative heating seems to be a fairly promising method. This paper aims to speed up the prediction of surface temperatures useful for realizing dry-peeling, thus a 1D-analytical model for the unsteady temperature field in a rotating tomato exposed to a radiative heating source is presented. Since only short times are of interest for the problem at hand, the model involves a semi-infinite slab cooled by convective heat transfer while heated by a pulsating heat source. The model being linear, the solution is derived following the Laplace Transform method. A 3D finite element model of the rotating tomato is introduced as well in order to validate the analytical solution. A satisfactory agreement is attained. Therefore, two different ways to predict the onset of the peeling conditions are available which can be of help for proper design of peeling plants. Particular attention is paid to study surface temperature uniformity, that being a critical parameter for realizing an easy tomato peeling.

[Determination of triclosan and triclocarban in human breast milk by solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry].

PubMed

Zhang, Pin; Zhang, Jing; Shi, Ying; Shao, Bing

2015-03-01

An analytical method was developed to simultaneously detect triclosan (TCS) and triclocarban (TCC) in human breast milk using solid-phase extraction (SPE) with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples were extracted by acetonitrile and purified with C -18 SPE cartridge after enzymolysis with β-glucuronidase/arylsulfatase. The chromatographic separation was performed on a Waters ACQUITY UPLC™ HSS T3 column (100 mm x 2. 1 mm, 1. 8 µm) with gradient elution using methanol and water at a flow rate of 0. 3 ml/min. The target analytes were assayed by triple quadrupole mass spectrometer operating in the negative ion mode. Quantification was performed by isotopic internal standard calibration. Satisfactory linearity (r2 > 0. 999) was obtained over the range of 0. 2 - 20. 0 µg/L and 0. 02 - 2. 0 µg/L for triclosan and triclocarban, respectively, with the limits of quantifications (LOQs) of 0. 41 and 0. 03 µg/kg. Average recoveries of two target compounds (spiked at three concentration levels) ranged from 100. 2% to 119. 3%, with the relative standard deviations (RSDs) between 5. 91% and 11. 31% (n =6). Twenty-five real samples (n = 25) were detected containing TCS and TCC at concentrations of < LOQ - 0. 77 µg/kg and < LOQ - 4. 28 µg/kg, respectively. Due to its high sensitivity and good reproductivity, this method can be applied to analyze TCS and TCC in human breast milk.

Biological diagnosis of von Willebrand disease: analytical characteristics of Innovance vWF:Ac assay kit on STA-R Evolution Expert series analyzer (Stago).

PubMed

Florin, Cécile; Garraud, Olivier; Molliex, Serge; Tardy, Brigitte; Campos, Lydia; Scherrer, Carine

2016-06-01

The Innovance VWF:Ac test (Siemens) has the particularity to assess the binding capacity of von Willebrand factor (VWF) to recombinant platelet GPIb mutated in the absence of ristocetin. Our study aimed to evaluate and validate according to standard NF EN ISO 15189 the original protocol adaptation on STA-R Evolution series analyser (Diagnostica Stago). We evaluated the performance in terms of imprecision and we validate additional parameters necessary in range B as recommended by the SH GTA 04 (Cofrac). We compared the new assay with the reference assay: ristocetin cofactor activity (VWF:RCo) performed on the BCS-XP analyser by testing retrospectively samples from 82 healthy normal subjects and 61 patients with von Willebrand disease (VWD). This new assay is consistent with objectives set in terms of imprecision with CV around 4%. Excepted limit of quantification higher, additional parameters evaluated in range B have been validated. The Innovance VWF: Ac assay allowed the detection of all deficits of VWF already detected by the VWF:RCo test on the BCS-XP. This adjustment on STA-R analyser therefore has satisfactory analytical performance criteria. Apart from the limit of quantification, this reagent can be used according to the recommendations specified in the original protocol adaptation. Its performance and compatibility with the spot measurement allow the diagnosis and therapeutic monitoring of VWD according to current requirements and guidelines.

Headspace sorptive solid phase microextraction (HS-SPME) combined with a spectrophotometry system: A simple glass devise for extraction and simultaneous determination of cyanide and thiocyanate in environmental and biological samples.

PubMed

Al-Saidi, H M; Al-Harbi, Sami A; Aljuhani, E H; El-Shahawi, M S

2016-10-01

A simple, low cost and efficient headspace sorptive solid phase microextraction (HS-SPME) method for determination of cyanide has been developed. The system comprises of a glass tube with two valves and a moveable glass slide fixed at its centre. It includes an acceptor phase polyurethane foam treated mercury (II) dithizonate [Hg(HDz)2-PUF] complex fixed inside by a septum cap in a cylindrical configuration (5.0cm length and 1.0cm diameter). The extraction is based upon the contact of the acceptor phase to the headspace and subsequently measuring the absorbance of the recovered mercury (II) dithizonate from PUFs sorbent. Unlike other HSSE, extraction and back - extractions was carried out in a closed system, thereby improving the analytical performance by preventing the analyte loss. Under the optimized conditions, a linear calibration plot in the range of 1.0-50.0µmolL(-1) was achieved with limits of detection (LOD) and quantification (LOQ) of 0.34, 1.2µmolL(-1) CN(-), respectively. Simultaneous analysis of cyanide and thiocyanate in saliva was also performed with satisfactory recoveries. Copyright © 2016. Published by Elsevier B.V.

Critical assessment of three high performance liquid chromatography analytical methods for food carotenoid quantification.

PubMed

Dias, M Graça; Oliveira, Luísa; Camões, M Filomena G F C; Nunes, Baltazar; Versloot, Pieter; Hulshof, Paul J M

2010-05-21

Three sets of extraction/saponification/HPLC conditions for food carotenoid quantification were technically and economically compared. Samples were analysed for carotenoids alpha-carotene, beta-carotene, beta-cryptoxanthin, lutein, lycopene, and zeaxanthin. All methods demonstrated good performance in the analysis of a composite food standard reference material for the analytes they are applicable to. Methods using two serial connected C(18) columns and a mobile phase based on acetonitrile, achieved a better carotenoid separation than the method using a mobile phase based on methanol and one C(18)-column. Carotenoids from leafy green vegetable matrices appeared to be better extracted with a mixture of methanol and tetrahydrofuran than with tetrahydrofuran alone. Costs of carotenoid determination in foods were lower for the method with mobile phase based on methanol. However for some food matrices and in the case of E-Z isomer separations, this was not technically satisfactory. Food extraction with methanol and tetrahydrofuran with direct evaporation of these solvents, and saponification (when needed) using pyrogallol as antioxidant, combined with a HPLC system using a slight gradient mobile phase based on acetonitrile and a stationary phase composed by two serial connected C(18) columns was the most technically and economically favourable method. 2010. Published by Elsevier B.V.

Extraction of triazole fungicides in environmental waters utilizing poly (ionic liquid)-functionalized magnetic adsorbent.

PubMed

Liu, Cheng; Liao, Yingmin; Huang, Xiaojia

2017-11-17

This work prepared a new poly (ionic liquid)-functionalized magnetic adsorbent (PFMA) for the extraction of triazole fungicides (TFs) in environmental waters prior to determination by high performance liquid chromatography/diode array detection (HPLC-DAD). A polymerizable ionic liquid, 1-methyl-3-allylimidazolium bis(trifluoromethylsulfonyl)imide was employed to copolymerize with divinylbenzene on the surface of modified magnetite to fabricate the PFMA. The morphology, spectroscopic and magnetic properties of the new adsorbent were investigated by different techniques. A series of key parameters that influence the extraction performance including the amount of PFMA, desorption solvent, adsorption and desorption time, sample pH value and ionic strength were optimized in detail. Under the optimum conditions, the prepared PFMA could extract targeted TFs effectively and quickly under the format of magnetic solid-phase extraction (MSPE). Satisfactory linearities were achieved in the range of 0.1-200.0μg/L for triadimenol and 0.05-200.0μg/L for other TFs with good coefficients of determination above 0.99 for all analytes. The limits of detection (S/N=3) and limits of quantification (S/N=10) for TFs were in the range of 0.0050-0.0078μg/L and 0.017-0.026μg/L, respectively. Environmental waters including lake, river and well waters were used to demonstrate the applicability of developed MSPE-HPLC-DAD method, and satisfactory recoveries and repeatability were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.

A steering law for a roof-type configuration for a single-gimbal control moment gyro system

NASA Technical Reports Server (NTRS)

Yoshikawa, T.

1974-01-01

Single-Gimbal Control Moment Gyro (SGCMG) systems have been investigated for attitude control of the Large Space Telescope (LST) and the High Energy Astronomy Observatory (HEAO). However, various proposed steering laws for the SGCMG systems thus far have some defects because of singular states of the system. In this report, a steering law for a roof-type SGCMG system is proposed which is based on a new momentum distribution scheme that makes all the singular states unstable. This momentum distribution scheme is formulated by a treatment of the system as a sampled-data system. From analytical considerations, it is shown that this steering law gives control performance which is satisfactory for practical applications. Results of the preliminary computer simulation entirely support this premise.

Thermal shock fracture in cross-ply fibre-reinforced ceramic-matrix composites

NASA Astrophysics Data System (ADS)

Kastritseas, C.; Smith, P. A.; Yeomans, J. A.

2010-11-01

The onset of matrix cracking due to thermal shock in a range of simple and multi-layer cross-ply laminates comprising a calcium aluminosilicate (CAS) matrix reinforced with Nicalon® fibres is investigated analytically. A comprehensive stress analysis under conditions of thermal shock, ignoring transient effects, is performed and fracture criteria based on either a recently derived model for the thermal shock resistance of unidirectional Nicalon®/glass ceramic-matrix composites or fracture mechanics considerations are formulated. The effect of material thickness on the apparent thermal shock resistance is also modelled. Comparison with experimental results reveals that the accuracy of the predictions is satisfactory and the reasons for some discrepancies are discussed. In addition, a theoretical argument based on thermal shock theory is formulated to explain the observed cracking patterns.

Experimental control in software reliability certification

NASA Technical Reports Server (NTRS)

Trammell, Carmen J.; Poore, Jesse H.

1994-01-01

There is growing interest in software 'certification', i.e., confirmation that software has performed satisfactorily under a defined certification protocol. Regulatory agencies, customers, and prospective reusers all want assurance that a defined product standard has been met. In other industries, products are typically certified under protocols in which random samples of the product are drawn, tests characteristic of operational use are applied, analytical or statistical inferences are made, and products meeting a standard are 'certified' as fit for use. A warranty statement is often issued upon satisfactory completion of a certification protocol. This paper outlines specific engineering practices that must be used to preserve the validity of the statistical certification testing protocol. The assumptions associated with a statistical experiment are given, and their implications for statistical testing of software are described.

Direct electron transfer of glucose oxidase and biosensing for glucose based on PDDA-capped gold nanoparticle modified graphene/multi-walled carbon nanotubes electrode.

PubMed

Yu, Yanyan; Chen, Zuanguang; He, Sijing; Zhang, Beibei; Li, Xinchun; Yao, Meicun

2014-02-15

In this work, poly (diallyldimethylammonium chloride) (PDDA)-capped gold nanoparticles (AuNPs) functionalized graphene (G)/multi-walled carbon nanotubes (MWCNTs) nanocomposites were fabricated. Based on the electrostatic attraction, the G/MWCNTs hybrid material can be decorated with AuNPs uniformly and densely. The new hierarchical nanostructure can provide a larger surface area and a more favorable microenvironment for electron transfer. The AuNPs/G/MWCNTs nanocomposite was used as a novel immobilization platform for glucose oxidase (GOD). Direct electron transfer (DET) was achieved between GOD and the electrode. Field emission scanning electron microscopy (FESEM), UV-vis spectroscopy and cyclic voltammetry (CV) were used to characterize the electrochemical biosensor. The glucose biosensor fabricated based on GOD electrode modified with AuNPs/G/MWCNTs demonstrated satisfactory analytical performance with high sensitivity (29.72mAM(-1)cm(-2)) and low limit of detection (4.8 µM). The heterogeneous electron transfer rate constant (ΚS) and the apparent Michaelis-Menten constant (Km) of GOD were calculated to be 11.18s(-1) and 2.09 mM, respectively. With satisfactory selectivity, reproducibility, and stability, the nanostructure we proposed offered an alternative for electrode fabricating and glucose biosensing. © 2013 Elsevier B.V. All rights reserved.

Determination of phenolic constituents of biological interest in red wine by capillary electrophoresis with electrochemical detection.

PubMed

Peng, Youyuan; Chu, Qingcui; Liu, Fanghua; Ye, Jiannong

2004-01-28

A simultaneous determination of trans-resveratrol, (-)-epicatechin, and (+)-catechin in red wine by capillary electrophoresis with electrochemical detection (CE-ED) is reported. The effects of the potential of the working electrode, pH and concentration of running buffer, separation voltage, and injection time on CE-ED were investigated. Under the optimum conditions, the analytes could be separated in a 100 mmol/L borate buffer (pH 9.2) within 20 min. A 300 microm diameter carbon disk electrode has a good response at +0.85 V (vs SCE) for all analytes. The response was linear over 3 orders of magnitude with detection limit (S/N = 3) ranging from 2 x 10(-7) to 5 x 10(-7) g/mL for all analytes. This method has been used for the determination of these analytes in red wine without enrichment, and the assay result was satisfactory.

Limitless Analytic Elements

NASA Astrophysics Data System (ADS)

Strack, O. D. L.

2018-02-01

We present equations for new limitless analytic line elements. These elements possess a virtually unlimited number of degrees of freedom. We apply these new limitless analytic elements to head-specified boundaries and to problems with inhomogeneities in hydraulic conductivity. Applications of these new analytic elements to practical problems involving head-specified boundaries require the solution of a very large number of equations. To make the new elements useful in practice, an efficient iterative scheme is required. We present an improved version of the scheme presented by Bandilla et al. (2007), based on the application of Cauchy integrals. The limitless analytic elements are useful when modeling strings of elements, rivers for example, where local conditions are difficult to model, e.g., when a well is close to a river. The solution of such problems is facilitated by increasing the order of the elements to obtain a good solution. This makes it unnecessary to resort to dividing the element in question into many smaller elements to obtain a satisfactory solution.

Fast determination of pyrethroid pesticides in tobacco by GC-MS-SIM coupled with modified QuEChERS sample preparation procedure.

PubMed

Gao, Yan; Sun, Ying; Jiang, Chunzhu; Yu, Xi; Wang, Yuanpeng; Zhang, Hanqi; Song, Daqian

2013-01-01

An analytical method was developed for the extraction and determination of pyrethroid pesticide residues in tobacco. The modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method was applied for preparing samples. In this study, methyl cyanide (MeCN)-saturated salt aqueous was used as the two-phase extraction solvent for the first time, and a vortex shaker was used for the simultaneous shaking and concentration of the analytes. The effects of experimental parameters on extraction and clean-up efficiency were investigated and optimized. The analytes were determined by gas chromatography-mass spectrometry-selected ion monitoring (GC-MS-SIM). The obtained recoveries of the analytes at three different fortification levels were 76.85-114.1% and relative standard deviations (RSDs) were lower than 15.7%. The limits of quantification (LOQs) were from 1.28 to 26.6 μg kg(-1). This method was also applied to the analysis of actual commercial tobacco products and the analytical results were satisfactory.

Fast determination of alkylphenol ethoxylates in leafy vegetables using a modified quick, easy, cheap, effective, rugged, and safe method and ultra-high performance supercritical fluid chromatography-tandem mass spectrometry.

PubMed

Jiang, Ze-Jun; Cao, Xiao-Lin; Li, Hui; Zhang, Chan; Abd El-Aty, A M; Jin, Fen; Shao, Hua; Jin, Mao-Jun; Wang, Shan-Shan; She, Yong-Xin; Wang, Jing

2017-11-24

In the present study, a quick and sensitive method was developed for simultaneous determination of nonylphenol ethoxylates (NPxEOs) and octylphenol ethoxylates (OPxEOs) (x=2-20) in three leafy vegetables, including cabbage, lettuce, and spinach using a modified "QuEChERS" method and ultra-high performance supercritical fluid chromatography-tandem mass spectrometry (UHPSFC-MS/MS) with scheduled multiple reaction monitoring (MRM). Under optimized conditions, the 38 target analytes were analyzed within a short period of time (5 min). The linearities of the matrix-matched standard calibrations were satisfactory with coefficients of determination (R 2 )>0.99 and the limits of detection (LOD) and quantification (LOQ) were in between 0.02-0.27 and 0.18-1.75μgkg -1 , respectively. The recovery of all target analytes spiked at three (low, medium, and high) fortification levels in various leafy vegetables were ranged from 72.8-122.6% with relative standard deviation (RSD) ≤18.3%. The method was successfully applied to market samples and the target analytes were found in all monitored samples, with total concentrations of 0-8.67μgkg -1 and 15.75-95.75μgkg -1 for OPxEOs and NPxEOs (x=2-20), respectively. In conclusion, the newly developed UHPSFC-ESI-MS/MS method is rapid and versatile and could be extrapolated for qualitative and quantitative analysis of APxEOs in other leafy vegetables. Copyright © 2017 Elsevier B.V. All rights reserved.

Dicationic polymeric ionic-liquid-based magnetic material as an adsorbent for the magnetic solid-phase extraction of organophosphate pesticides and polycyclic aromatic hydrocarbons.

PubMed

Jiang, Qiong; Liu, Qin; Chen, Qiliang; Zhao, Wenjie; Xiang, Guoqiang; He, Lijun; Jiang, Xiuming; Zhang, Shusheng

2016-08-01

Magnetic particles modified with a dicationic polymeric ionic liquid are described as a new adsorbent in magnetic solid-phase extraction. They were obtained through the copolymerization of a 1,8-di(3-vinylimidazolium)octane-based ionic liquid with vinyl-modified SiO2 @Fe3 O4 , and were characterized by FTIR spectroscopy, X-ray diffraction, and vibrating sample magnetometry. The modified magnetic particles are effective in the extraction of organophosphate pesticides and polycyclic aromatic hydrocarbons. Also, they can provide different extraction performance for the selected analytes including fenitrothion, parathion, fenthion, phoxim, phenanthrene, and fluoranthene, where the extraction efficiency is found to be in agreement with the hydrophobicity of analytes. Various factors influencing the extraction efficiency, such as, the amount of adsorbent, extraction, and desorption time, and type and volume of the desorption solvent, were optimized. Under the optimized conditions, a good linearity ranging from 1-100 μg/L is obtained for all analytes, except for parathion (2-200 μg/L), where the correlation coefficients varied from 0.9960 to 0.9998. The limits of detection are 0.2-0.8 μg/L, and intraday and interday relative standard deviations are 1.7-7.4% (n = 5) and 3.8-8.0% (n = 3), respectively. The magnetic solid-phase extraction combined with high-performance liquid chromatography can be applied for the detection of trace targets in real water samples with satisfactory relative recoveries and relative standard deviations. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Multiple monolithic fiber solid-phase microextraction based on a polymeric ionic liquid with high-performance liquid chromatography for the determination of steroid sex hormones in water and urine.

PubMed

Liao, Keren; Mei, Meng; Li, Haonan; Huang, Xiaojia; Wu, Cuiqin

2016-02-01

The development of a simple and sensitive analytical approach that combines multiple monolithic fiber solid-phase microextraction with liquid desorption followed by high-performance liquid chromatography with diode array detection is proposed for the determination of trace levels of seven steroid sex hormones (estriol, 17β-estradiol, testosterone, ethinylestradiol, estrone, progesterone and mestranol) in water and urine matrices. To extract the target analytes effectively, multiple monolithic fiber solid-phase microextraction based on a polymeric ionic liquid was used to concentrate hormones. Several key extraction parameters including desorption solvent, extraction and desorption time, pH value and ionic strength in sample matrix were investigated in detail. Under the optimal experimental conditions, the limits of detection were found to be in the range of 0.027-0.12 μg/L. The linear range was 0.10-200 μg/L for 17β-estradiol, 0.25-200 μg/L estriol, ethinylestradiol and estrone, and 0.50-200 μg/L for the other hormones. Satisfactory linearities were achieved for analytes with the correlation coefficients above 0.99. Acceptable method reproducibility was achieved by evaluating the repeatability and intermediate precision with relative standard deviations of both less than 8%. The enrichment factors ranged from 54- to 74-fold. Finally, the proposed method was successfully applied to the analysis of steroid sex hormones in environmental water samples and human urines with spiking recoveries ranged from 75.6 to 116%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Avoiding pitfalls in the determination of halocarboxylic acids: the photochemistry of methylation.

PubMed

Rubio, F J; Urbansky, E T; Magnuson, M L

2000-06-01

Haloethanoic (haloacetic) acids are formed during chlorination of drinking water and are regulated by the Environmental Protection Agency (EPA). These compounds are normally quantified by gas chromatography with electron capture detection (GC-ECD) as the methyl esters. EPA Method 552 uses diazomethane (CH2N2) for this purpose, but has only been validated by EPA for HAA6: chloro-, dichloro-, bromo-, dibromo-, bromochloro- and trichloroacetic acids. EPA Method 552.2 was developed and validated for all nine analytes (HAA9 = HAA6 + dibromochloro-, bromodichloro- and tribromoethanoic acids). Since the promulgation of Method 552.2, which uses acidic methanol, a debate has ensued over discrepancies observed by various laboratories when using diazomethane instead. In an effort to identify and eliminate potential sources for these discrepancies, a comparative study was undertaken for HAA9. Better accuracy and precision were observed for all HAA9 species by Method 552.2; recoveries were satisfactory in de-ionized and tap water. Method 552 remains satisfactory for HAA6. Systematic differences in instrumental response are observed for the two methods, but these are precise and may be accounted for using similarly treated standards and analyte-fortified (spiked) samples. That notwithstanding, Method 552 (CH2N2) was shown to be unsuitable for dibromochloro-, bromodichloro- and tribromoethanoic acids (HAA9-6). The primary problem appears to be a photoactivated reaction between diazomethane and the HAA9-6 analytes; however, side reactions were found to occur even in the dark. Analyte loss is most pronounced under typical laboratory lighting (white F40 fluorescent lamps + sunlight), but it is also observed under Philips gold F40 lamps (lambda > or = 520 nm), and in the dark.

Identifying Gaps in the Performance of Pediatric Trainees Who Receive Marginal/Unsatisfactory Ratings.

PubMed

Li, Su-Ting T; Tancredi, Daniel J; Schwartz, Alan; Guillot, Ann; Burke, Ann; Trimm, R Franklin; Guralnick, Susan; Mahan, John D; Gifford, Kimberly A

2018-01-01

To perform a derivation study to determine in which subcompetencies marginal/unsatisfactory pediatric residents had the greatest deficits compared with their satisfactorily performing peers and which subcompetencies best discriminated between marginal/unsatisfactory and satisfactorily performing residents. Multi-institutional cohort study of all 21 milestones (rated on four or five levels) reported to the Accreditation Council for Graduate Medical Education, and global marginal/unsatisfactory versus satisfactory performance reported to the American Board of Pediatrics. Data were gathered in 2013-2014. For each level of training (postgraduate year [PGY] 1, 2, and 3), mean differences between milestone levels of residents with marginal/unsatisfactory and satisfactory performance adjusted for clustering by program and C-statistics (area under receiver operating characteristic curve) were calculated. A Bonferroni-corrected significance threshold of .0007963 was used to account for multiple comparisons. Milestone and overall performance evaluations for 1,704 pediatric residents in 41 programs were obtained. For PGY1s, two subcompetencies had almost a one-point difference in milestone levels between marginal/unsatisfactory and satisfactory trainees and outstanding discrimination (≥ 0.90): organize/prioritize (0.93; C-statistic: 0.91) and transfer of care (0.97; C-statistic: 0.90). The largest difference between marginal/unsatisfactory and satisfactory PGY2s was trustworthiness (0.78). The largest differences between marginal/unsatisfactory and satisfactory PGY3s were ethical behavior (1.17), incorporating feedback (1.03), and professionalization (0.96). For PGY2s and PGY3s, no subcompetencies had outstanding discrimination. Marginal/unsatisfactory pediatric residents had different subcompetency gaps at different training levels. While PGY1s may have global deficits, senior residents may have different performance deficiencies requiring individualized counseling and targeted performance improvement plans.

Enhancement for trace analysis of sulfonamide antibiotics in water matrices using bar adsorptive microextraction (BAμE).

PubMed

Ide, A H; Ahmad, S M; Neng, N R; Nogueira, J M F

2016-09-10

In this study, the enhancement for trace analysis of sulfonamide antibiotics (sulfathiazole, sulfamethoxazole and sulfadimethoxine) and trimethoprim in water matrices is proposed using bar adsorptive microextraction combined with micro-liquid desorption followed by high-performance liquid chromatography with diode array detection (BAμE-μLD/HPLC-DAD). By comparing different polymers and activated carbons as sorbent coatings for BAμE, the polystyrene-divinylbenzene polymer (PS-DVB) showed the best selectivity for the compounds under study. Assays performed through BAμE(PS-DVB)-μLD on 25mL of ultrapure water samples spiked at the 8.0μgL(-1) level showed recoveries ranging from 63.8±1.5% to 84.2±1.9%, under optimized experimental conditions. The validated method provided satisfactory limits of detection (0.08-0.16μgL(-1)) and good linear dynamic ranges (0.16-8.00μgL(-1)) with determination coefficients higher than 0.9958. The proposed analytical methodology was applied to real matrices, such as tap, estuarine and wastewater samples using the standard addition method. It showed to be easy to implement, with good reproducibility, sensitivity and requiring small amount of sample. Furthermore, negligible consumption of organic solvents was used in compliance with the green analytical chemistry principles. When compared to other well-established microextraction approaches, BAμE demonstrated better performance concerning recovery yields and sensitivity. Copyright © 2016 Elsevier B.V. All rights reserved.

Ultra-high performance liquid chromatography with tandem mass spectrometry method for the simultaneous quantitation of five phthalides in rat plasma: Application to a comparative pharmacokinetic study of Huo Luo Xiao Ling Dan and herb-pair extract.

PubMed

Ma, Wen; Wang, Weihui; Peng, Yan; Bian, Qiaoxia; Wang, Nannan; Lee, David Y-W; Dai, Ronghua

2016-06-01

A fast, sensitive, and reliable ultra-high performance liquid chromatography with tandem mass spectrometry method has been developed and validated for the simultaneous quantitation and pharmacokinetic study of five phthalides (senkyunolide A, ligustilide, butylidenephthalide, 3-butylphthalide, and levistilide A) in rat plasma after oral administration of Huo Luo Xiao Ling Dan (HLXLD) or Angelica sinensis--Ligusticum chuanxiong herb pair (DG-CX) between normal and arthritis rats. After extraction from blood, the analytes and internal standard were subjected to ultra-high performance liquid chromatography with a Shim-pack XR-ODS column (75 × 3.0 mm(2) , 2.2 μm particles) and mobile phase was composed of methanol and water (containing 0.05% formic acid) under gradient elution conditions, with an electrospray ionization source in the positive ionization and multiple reaction monitoring mode. The lower limits of quantification were 0.192-0.800 ng/mL for all the analytes. Satisfactory linearity, precision, accuracy, mean extraction recovery, and acceptable matrix effect have been achieved. The validated method was successfully applied to a comparative pharmacokinetic study of five bioactive components in rat plasma after oral administration of HLXLD or DG-CX alone, respectively, between normal and arthritic rats. The results showed that there were unlike characters of pharmacokinetics among different groups. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of organophosphorus pesticides and their major degradation product residues in food samples by HPLC-UV.

PubMed

Peng, Guilong; He, Qiang; Lu, Ying; Mmereki, Daniel; Zhong, Zhihui

2016-10-01

A simple method based on dispersive solid-phase extraction (DSPE) and dispersive liquid-liquid microextraction method based on solidification of floating organic droplets (DLLME-SFO) was developed for the extraction of chlorpyrifos (CP), chlorpyrifos-methyl (CPM), and their main degradation product 3,5,6-trichloro-2-pyridinol (TCP) in tomato and cucumber samples. The determination was carried out by high performance liquid chromatography with ultraviolet detection (HPLC-UV). In the DSPE-DLLME-SFO, the analytes were first extracted with acetone. The clean-up of the extract by DSPE was carried out by directly adding activated carbon sorbent into the extract solution, followed by shaking and filtration. Under the optimum conditions, the proposed method was sensitive and showed a good linearity within a range of 2-500 ng/g, with the correlation coefficients (r) varying from 0.9991 to 0.9996. The enrichment factors ranged from 127 to 138. The limit of detections (LODs) were in the range of 0.12-0.68 ng/g, and the relative standard deviations (RSDs) for 50 ng/g of each analytes in tomato samples were in the range of 3.25-6.26 % (n = 5). The proposed method was successfully applied for the extraction and determination of the mentioned analytes residues in tomato and cucumber samples, and satisfactory results were obtained.

Numerical design of streamlined tunnel walls for a two-dimensional transonic test

NASA Technical Reports Server (NTRS)

Newman, P. A.; Anderson, E. C.

1978-01-01

An analytical procedure is discussed for designing wall shapes for streamlined, nonporous, two-dimensional, transonic wind tunnels. It is based upon currently available 2-D inviscid transonic and boundary layer analysis computer programs. Predicted wall shapes are compared with experimental data obtained from the NASA Langley 6 by 19 inch Transonic Tunnel where the slotted walls were replaced by flexible nonporous walls. Comparisons are presented for the empty tunnel operating at a Mach number of 0.9 and for a supercritical test of an NACA 0012 airfoil at zero lift. Satisfactory agreement is obtained between the analytically and experimentally determined wall shapes.

Simulations of solid lumber strength property monitoring tests

Treesearch

Steve Verrill; David E. Kretschmann; James W. Evans

2017-01-01

Dimension lumber, visually graded in accordance with the National Grading Rule and assigned design values derived in accordance with procedures found in ASTM D 1990, has provided satisfactory performance in homes and other structural applications for many years. This ongoing satisfactory performance depends upon a recognition that all standards are living documents...

48 CFR 9.104-1 - General standards.

Code of Federal Regulations, 2010 CFR

2010-10-01

... business commitments; (c) Have a satisfactory performance record (see 48 CFR 9.104-3(b) and part 42... the basis of a lack of relevant performance history, except as provided in 9.104-2; (d) Have a satisfactory record of integrity and business ethics (for example, see Subpart 42.15). (e) Have the necessary...

A simple sample preparation for simultaneous determination of chloramphenicol and its succinate esters in food products using high-performance liquid chromatography/high-resolution mass spectrometry.

PubMed

Amelin, Vasiliy; Korotkov, Anton

2017-02-01

A simple method is described for the determination of chloramphenicol and its succinate esters in food products. Examination of food products using high-performance liquid chromatography/high-resolution mass spectrometry showed the presence not only of chloramphenicol but also of its succinate forms. A scheme is proposed for determining chloramphenicol and its succinate esters (calculated as chloramphenicol) in meat (beef, pork, poultry), milk, liver, kidney, eggs, fish and honey. Analytes are extracted from a 1.0 g sample with 5 ml acetonitrile. It was found that using the method of standard addition and diluting the extract with water leads to the elimination of matrix effects and also eliminates errors associated with peak splitting due to the separate elution of the differing forms of the analyte. Validation results were satisfactory, with recoveries from 85% to 111% (meat, milk, liver, kidney, eggs, fish and honey) and a relative standard deviation (RSD) lower than 13% for spiked levels of 0.3, 1.0 and 5 µg kg - 1 . The limits of detection and quantification (calculated as chloramphenicol for all forms) were 0.1 and 0.3 µg kg - 1 , respectively. The RSD of the results of the analysis was < 10%. The duration of the analysis was less than 1 h.

Novel approach to high-throughput determination of endocrine disruptors using recycled diatomaceous earth as a green sorbent phase for thin-film solid-phase microextraction combined with 96-well plate system.

PubMed

Kirschner, Nicolas; Dias, Adriana Neves; Budziak, Dilma; da Silveira, Cristian Berto; Merib, Josias; Carasek, Eduardo

2017-12-15

A sustainable approach to TF-SPME is presented using recycled diatomaceous earth, obtained from a beer purification process, as a green sorbent phase for the determination of bisphenol A (BPA), benzophenone (BzP), triclocarban (TCC), 4-methylbenzylidene camphor (4-MBC) and 2-ethylhexyl-p-methoxycinnamate (EHMC) in environmental water samples. TF-SPME was combined with a 96-well plate system allowing for high-throughput analysis due to the simultaneous extraction/desorption up to 96 samples. The proposed sorbent phase exhibited good stability in organic solvents, as well as satisfactory analytical performance. The optimized method consisted of 240 min of extraction at pH 6 with the addition of NaCl (15% w/v). A mixture of MeOH:ACN (50:50 v/v) was used for the desorption the analytes, using a time of 30 min. Limits of detection varied from 1 μg L -1 for BzP and TCC to 8 μg L -1 for the other analytes, and R 2 ranged from 0.9926 for 4-MBC to 0.9988 for BPA. This novel and straightforward approach offers an environmentally-friendly and very promising alternative for routine analysis. . The total sample preparation time per sample was approximately 2.8 min, which is a significant advantage when a large number of analytical run is required. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of Anti-Loosening Performance of Hyper Lock Nut

NASA Astrophysics Data System (ADS)

Nishiyama, Shuji; Migita, Hiroaki; Kataoka, Mitumasa; Nakasaki, Nobuyuki; Murano, Kohshi

Bolted joints are widely used in mechanical structures as they allow easy disassembly for maintenance without high cost. However, vibration-induced loosening due to dynamic loading remains a long-unresolved issue. We have developed a new type of nut named the hyper lock nut (HLN) that offers anti-loosening performance without a complicated tightening process and tools. In this study, we investigated the mechanisms of joints bolted with the HLN, and tightening behavior was analyzed using the three-dimensional finite element method. The analytical results were compared with the experimental results for the HLN, and close qualitative agreement was observed between the two with respect to displacement, tightening force and tightening torque. We found a number of new aspects and plus points for joints bolted with the HLN in comparison to those fastened with JIS standard nuts. It was found that the tightening torque of the HLN is higher than that of JIS standard nuts, and that satisfactory anti-loosening performance can be realized through the thread contact force at the slit region and the angular face of the bearing surface.

Dissipation kinetics of alpha-cypermethrin and lambda-cyhalothrin residues in aboveground part of white mustard (Sinapis alba L.).

PubMed

Słowik-Borowiec, Magdalena

2016-09-01

Dissipation of simultaneously applied insecticides alpha-cypermethrin and lambda-cyhalothrin was studied in a minor crop, aboveground part of white mustard (Sinapis alba L.). A validated gas chromatographic method (GC-ECD/NPD) was used to determine insecticide residues. Analytical performances were very satisfactory, with expanded uncertainties not higher than 14% (coverage factor k = 2, confidence level 95%). Dissipation of alpha-cypermethrin and lambda-cyhalothrin in white mustard followed first-order kinetics (R(2) between 0.953 and 0.995), with half-lives of 3.1-4.6 and 2.9-3.7 days respectively. Based on the results of this two-year study and the relevant residue regulation, alpha-cypermethrin and lambda-cyhalothrin treatments can be considered safe for crop protection, feeding animals and the environment.

Large-scale dialysis of sample lipids

USGS Publications Warehouse

Meadows, Jill; Tillitt, Donald E.; Huckins, James; Schroeder, D.

1993-01-01

The use of a semipermeable membrane device (SPMD) for dialysis in an organic solvent phase is an efficient alternative approach to separation of contaminants from large amounts of lipid (up to 50 grams or more) prior to organic chemical analysis. Passive separation of contaminants can be accomplished with a minimum of equipment and a comparatively small volume of solvent. This study examines the effects of factors such as dialytic solvent, lipid type, dialytic solvent:lipid volume ratio, dialysis time, and temperature on the performance of polyethylene SPMDs during lipid-contaminant separations. The experimental conditions for maximal recoveries of organochlorine pesticides and polychlorinated biphenyls with minimal lipid carryover are determined for the examined variables. When the dialytic procedure is optimized, very satisfactory and highly reproducible analyte recoveries can be obtained in a few days while separating > 90% of the lipid material in a single operation.

Electrochemical impedimetric sensor based on molecularly imprinted polymers/sol-gel chemistry for methidathion organophosphorous insecticide recognition.

PubMed

Bakas, Idriss; Hayat, Akhtar; Piletsky, Sergey; Piletska, Elena; Chehimi, Mohamed M; Noguer, Thierry; Rouillon, Régis

2014-12-01

We report here a novel method to detect methidathion organophosphorous insecticides. The sensing platform was architected by the combination of molecularly imprinted polymers and sol-gel technique on inexpensive, portable and disposable screen printed carbon electrodes. Electrochemical impedimetric detection technique was employed to perform the label free detection of the target analyte on the designed MIP/sol-gel integrated platform. The selection of the target specific monomer by electrochemical impedimetric methods was consistent with the results obtained by the computational modelling method. The prepared electrochemical MIP/sol-gel based sensor exhibited a high recognition capability toward methidathion, as well as a broad linear range and a low detection limit under the optimized conditions. Satisfactory results were also obtained for the methidathion determination in waste water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Analytical excited state forces for the time-dependent density-functional tight-binding method.

PubMed

Heringer, D; Niehaus, T A; Wanko, M; Frauenheim, Th

2007-12-01

An analytical formulation for the geometrical derivatives of excitation energies within the time-dependent density-functional tight-binding (TD-DFTB) method is presented. The derivation is based on the auxiliary functional approach proposed in [Furche and Ahlrichs, J Chem Phys 2002, 117, 7433]. To validate the quality of the potential energy surfaces provided by the method, adiabatic excitation energies, excited state geometries, and harmonic vibrational frequencies were calculated for a test set of molecules in excited states of different symmetry and multiplicity. According to the results, the TD-DFTB scheme surpasses the performance of configuration interaction singles and the random phase approximation but has a lower quality than ab initio time-dependent density-functional theory. As a consequence of the special form of the approximations made in TD-DFTB, the scaling exponent of the method can be reduced to three, similar to the ground state. The low scaling prefactor and the satisfactory accuracy of the method makes TD-DFTB especially suitable for molecular dynamics simulations of dozens of atoms as well as for the computation of luminescence spectra of systems containing hundreds of atoms. (c) 2007 Wiley Periodicals, Inc.

An Integrated Model for Supplier Selection for a High-Tech Manufacturer

NASA Astrophysics Data System (ADS)

Lee, Amy H. I.; Kang, He-Yau; Lin, Chun-Yu

2011-11-01

Global competitiveness has become the biggest concern of manufacturing companies, especially in high-tech industries. Improving competitive edges in an environment with rapidly changing technological innovations and dynamic customer needs is essential for a firm to survive and to acquire a decent profit. Thus, the introduction of successful new products is a source of new sales and profits and is a necessity in the intense competitive international market. After a product is developed, a firm needs the cooperation of upstream suppliers to provide satisfactory components and parts for manufacturing final products. Therefore, the selection of suitable suppliers has also become a very important decision. In this study, an analytical approach is proposed to select the most appropriate critical-part suppliers in order to maintain a high reliability of the supply chain. A fuzzy analytic network process (FANP) model, which incorporates the benefits, opportunities, costs and risks (BOCR) concept, is constructed to evaluate various aspects of suppliers. The proposed model is adopted in a TFT-LCD manufacturer in Taiwan in evaluating the expected performance of suppliers with respect to each important factor, and an overall ranking of the suppliers can be generated as a result.

Determination of vitamin C in foods: current state of method validation.

PubMed

Spínola, Vítor; Llorent-Martínez, Eulogio J; Castilho, Paula C

2014-11-21

Vitamin C is one of the most important vitamins, so reliable information about its content in foodstuffs is a concern to both consumers and quality control agencies. However, the heterogeneity of food matrixes and the potential degradation of this vitamin during its analysis create enormous challenges. This review addresses the development and validation of high-performance liquid chromatography methods for vitamin C analysis in food commodities, during the period 2000-2014. The main characteristics of vitamin C are mentioned, along with the strategies adopted by most authors during sample preparation (freezing and acidification) to avoid vitamin oxidation. After that, the advantages and handicaps of different analytical methods are discussed. Finally, the main aspects concerning method validation for vitamin C analysis are critically discussed. Parameters such as selectivity, linearity, limit of quantification, and accuracy were studied by most authors. Recovery experiments during accuracy evaluation were in general satisfactory, with usual values between 81 and 109%. However, few methods considered vitamin C stability during the analytical process, and the study of the precision was not always clear or complete. Potential future improvements regarding proper method validation are indicated to conclude this review. Copyright © 2014. Published by Elsevier B.V.

Liquid chromatographic method for the simultaneous determination of cefalexin and trimethoprim in dog plasma and application to the pharmacokinetic studies of a coformulated preparation.

PubMed

Qi, Meiling; Wang, Peng; Sun, Ping; Liu, Xia

2006-03-07

A liquid chromatographic method is described for the simultaneous determination of cefalexin and trimethoprim in dog plasma. A simple protein precipitation procedure was adopted for the sample preparation with satisfactory extraction recoveries for both analytes. Chromatographic separation of the analytes was achieved on a C(18) column using a mixture of 2 mol/l formate buffer (pH 3.5), methanol and acetonitrile (22:7:7, v/v/v) containing a 0.002 mol/l sodium dodecyl sulfate as mobile phase and detection was performed at 240 nm. The linearity was obtained over the concentration ranges of 1.0-100.0 microg/ml for cefalexin and 0.5-50.0 microg/ml for trimethoprim. For each level of QC samples including the lower limit of quantification, both inter- and intra-day precisions (R.S.D.) were < or =14.0% for cefalexin and < or =11.4% for trimethoprim, and accuracy (RE) was -1.4% for cefalexin and -3.0% for trimethoprim. The present LC method was successfully applied to the pharmacokinetic studies of coformulated cefalexin dispersible tablets after oral administration to beagle dogs.

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

Determination of Aluminum in Dialysis Concentrates by Atomic Absorption Spectrometry after Coprecipitation with Lanthanum Phosphate.

PubMed

Selvi, Emine Kılıçkaya; Şahin, Uğur; Şahan, Serkan

2017-01-01

This method was developed for the determination of trace amounts of aluminum(III) in dialysis concentrates using atomic absorption spectrometry after coprecipitation with lanthanum phosphate. The analytical parameters that influenced the quantitative coprecipitation of analyte including amount of lanthanum, amount of phosfate, pH and duration time were optimized. The % recoveries of the analyte ion were in the range of 95-105 % with limit of detection (3s) of 0.5 µg l -1 . Preconcentration factor was found as 1000 and Relative Standard Deviation (RSD) % value obtained from model solutions was 2.5% for 0.02 mg L -1 . The accuracy of the method was evaluated with standard reference material (CWW-TMD Waste Water). The method was also applied to most concentrated acidic and basic dialysis concentrates with satisfactory results.

Knowledge, risk perception and mitigation measures towards Ebola virus disease by potentially exposed bushmeat handlers in north-central Nigeria: Any critical gap?

PubMed

Alhaji, N B; Yatswako, S; Oddoh, E Y

2018-02-01

The bushmeat industry has been a topic of increasing importance among public health officials for its influence on zoonotic diseases transmission, such as Ebola virus disease (EVD), a rare and severe infectious disease of humans and non-human primates. This survey assessed knowledge/awareness, risk perceptions and mitigation practices towards EVD among bushmeat handlers in north-central Nigeria. These characteristics are premise to level of preparedness against appropriate risk prevention and control. A questionnaire-based cross-sectional study was conducted between January and December 2015 on 395 bushmeat handlers. Descriptive and analytical statistical analyses were performed using Epi-Info 3.5.3 software, and p < 0.05 was considered statistical significance in all analyses. Mean age of respondents was 40.9 ± 10.7 years, and most (30.4%) of them were in the age group 40-49 years. Majority (82.8%) of them were males, while most (47.9%) do not possess formal education. Bushmeat hunters, vendors and consumers constituted 17.2%, 28.1% and 54.7% of the respondents, respectively. A majority (85.6%) of the participants had heard about EVD. Bushmeat vendors were more likely (OR 1.96; 95% CI: 1.05-3.65) to have satisfactory knowledge than the hunters. Handlers with tertiary education were more likely (OR 3.22; 95% CI: 1.56-6.67) to possess significant satisfactory knowledge/awareness about EVD. Also, vendors were more likely (OR 1.85; 95% CI: 1.01-3.42) to practice satisfactory mitigation measures than the hunters. Only handlers with tertiary education were more likely (OR 2.48; 95% CI: 1.26-4.89) to significantly practice satisfactory mitigation measures against EVD. Although most of the handlers possessed significant knowledge/awareness about EVD, few applied mitigation measures against its infection, which is the challenging gap. There is a need for collaborations between the public health, veterinary and wildlife authorities in the provision of health information to bushmeat handlers on better management of emerging and re-emerging zoonotic viral diseases of wildlife origin. © 2017 Blackwell Verlag GmbH.

Residue analysis of four diacylhydrazine insecticides in fruits and vegetables by Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method using ultra-performance liquid chromatography coupled to tandem mass spectrometry.

PubMed

Liu, Xingang; Xu, Jun; Dong, Fengshou; Li, Yuanbo; Song, Wenchen; Zheng, Yongquan

2011-08-01

The new analytical method using Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) procedure for simultaneous determination of diacylhydrazine insecticide residues in fruits and vegetables was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS). The four insecticides (tebufenozide, methoxfenozide, chromafenozide, and halofenozide) were extracted from six fruit and vegetable matrices using acetonitrile and subsequently cleaned up using primary secondary amine (PSA) or octadecylsilane (C18) as sorbent prior to UPLC-MS/MS analysis. The determination of the target compounds was achieved in less than 3.0 min using an electrospray ionization source in positive mode (ESI+) for tebufenozide, methoxfenozide, and halofenozide and in negative mode (ESI-) for chromafenozide. The limits of detection were below 0.6 μg kg(-1), while the limit of quantification did not exceed 2 μg kg(-1) in different matrices. The QuEChERS procedure by using two sorbents (PSA and C18) and the matrix-matched standards gave satisfactory recoveries and relative standard deviation (RSD) values in different matrices at four spiked levels (0.01, 0.05, 0.1, and 1 mg kg(-1)). The overall average recoveries for this method in apple, grape, cucumber, tomato, cabbage, and spinach at four levels ranged from 74.2% to 112.5% with RSDs in the range of 1.4-13.8% (n = 5) for all analytes. This study provides a theoretical basis for China to draw up maximum residue limits and analytical method for diacylhydrazine insecticide in vegetables and fruits.

Simultaneous determination of atorvastatin and valsartan in human plasma by solid-based disperser liquid-liquid microextraction followed by high-performance liquid chromatography-diode array detection.

PubMed

Farajzadeh, Mir Ali; Khorram, Parisa; Pazhohan, Azar

2016-04-01

A simple, sensitive, and efficient method has been developed for simultaneous estimation of valsartan and atorvastatin in human plasma by combination of solid-based dispersive liquid-liquid microextraction and high performance liquid chromatography-diode array detection. In the proposed method, 1,2-dibromoethane (extraction solvent) is added on a sugar cube (as a solid disperser) and it is introduced into plasma sample containing the analytes. After manual shaking and centrifugation, the resultant sedimented phase is subjected to back extraction into a small volume of sodium hydrogen carbonate solution using air-assisted liquid-liquid microextraction. Then the cloudy solution is centrifuged and the obtained aqueous phase is transferred into a microtube and analyzed by the separation system. Under the optimal conditions, extraction recoveries are obtained in the range of 81-90%. Calibration curves plotted in drug-free plasma sample are linear in the ranges of 5-5000μgL(-1) for valsartan and 10-5000μgL(-1) for atorvastatin with the coefficients of determination higher than 0.997. Limits of detection and quantification of the studied analytes in plasma sample are 0.30-2.6 and 1.0-8.2μgL(-1), respectively. Intra-day (n=6) and inter-days (n=4) precisions of the method are satisfactory with relative standard deviations less than 7.4% (at three levels of 10, 500, and 2000μgL(-1), each analyte). These data suggest that the method can be successfully applied to determine trace amounts of valsartan and atorvastatin in human plasma samples. Copyright © 2016 Elsevier B.V. All rights reserved.

A multi-targeted liquid chromatography-mass spectrometry screening procedure for the detection in human urine of drugs non-prohibited in sport commonly used by the athletes.

PubMed

Mazzarino, Monica; Cesarei, Lorenzo; de la Torre, Xavier; Fiacco, Ilaria; Robach, Paul; Botrè, Francesco

2016-01-05

This work presents an analytical method for the simultaneous analysis in human urine of 38 pharmacologically active compounds (19 benzodiazepine-like substances, 7 selective serotonin reuptake inhibitors, 4 azole antifungal drugs, 5 inhibitors of the phosphodiesterases type 4 and 3 inhibitors of the phosphodiesterase type 5) by liquid-chromatography coupled with tandem mass spectrometry. The above substances classes include both the most common "non banned" drugs used by the athletes (based on the information reported on the "doping control form") and those drugs who are suspected to be performance enhancing and/or act as masking agents in particular conditions. The chromatographic separation was performed by a reverse-phase octadecyl column using as mobile phases acetonitrile and ultra-purified water, both with 0.1% formic acid. The detection was carried out using a triple quadrupole mass spectrometric analyser, positive electro-spray as ionization source and selected reaction monitoring as acquisition mode. Sample pre-treatment consisted in an enzymatic hydrolysis followed by a liquid-liquid extraction in neutral field using tert-butyl methyl-ether. The analytical procedure, once developed, was validated in terms of sensitivity (lower limits of detection in the range of 1-50 ng mL(-1)), specificity (no interferences were detected at the retention time of all the analytes under investigation), recovery (≥60% with a satisfactory repeatability, CV % lower than 10), matrix effect (lower than 30%) and reproducibility of retention times (CV% lower than 0.1) and of relative abundances (CV% lower than 15). The performance and the applicability of the method was evaluated by analyzing real samples containing benzodiazepines (alprazolam, diazepam, zolpidem or zoplicone) or inhibitors of the phosphodiesterases type 5 (sildenafil or vardenafil) and samples obtained incubating two of the phosphodiesterases type 4 studied (cilomilast or roflumilast) with pooled human liver microsomes. All the parent compounds, together with their main phase I metabolites, were clearly detected using the analytical procedures here developed. Copyright © 2015 Elsevier B.V. All rights reserved.

Collisional evolution - an analytical study for the non steady-state mass distribution.

NASA Astrophysics Data System (ADS)

Vieira Martins, R.

1999-05-01

To study the collisional evolution of asteroidal groups one can use an analytical solution for the self-similar collision cascades. This solution is suitable to study the steady-state mass distribution of the collisional fragmentation. However, out of the steady-state conditions, this solution is not satisfactory for some values of the collisional parameters. In fact, for some values for the exponent of the mass distribution power law of an asteroidal group and its relation to the exponent of the function which describes "how rocks break" the author arrives at singular points for the equation which describes the collisional evolution. These singularities appear since some approximations are usually made in the laborious evaluation of many integrals that appear in the analytical calculations. They concern the cutoff for the smallest and the largest bodies. These singularities set some restrictions to the study of the analytical solution for the collisional equation. To overcome these singularities the author performed an algebraic computation considering the smallest and the largest bodies and he obtained the analytical expressions for the integrals that describe the collisional evolution without restriction on the parameters. However, the new distribution is more sensitive to the values of the collisional parameters. In particular the steady-state solution for the differential mass distribution has exponents slightly different from 11/6 for the usual parameters in the asteroid belt. The sensitivity of this distribution with respect to the parameters is analyzed for the usual values in the asteroidal groups. With an expression for the mass distribution without singularities, one can evaluate also its time evolution. The author arrives at an analytical expression given by a power series of terms constituted by a small parameter multiplied by the mass to an exponent, which depends on the initial power law distribution. This expression is a formal solution for the equation which describes the collisional evolution.

Analytical method for the identification and assay of 12 phthalates in cosmetic products: application of the ISO 12787 international standard "Cosmetics-Analytical methods-Validation criteria for analytical results using chromatographic techniques".

PubMed

Gimeno, Pascal; Maggio, Annie-Françoise; Bousquet, Claudine; Quoirez, Audrey; Civade, Corinne; Bonnet, Pierre-Antoine

2012-08-31

Esters of phthalic acid, more commonly named phthalates, may be present in cosmetic products as ingredients or contaminants. Their presence as contaminant can be due to the manufacturing process, to raw materials used or to the migration of phthalates from packaging when plastic (polyvinyl chloride--PVC) is used. 8 phthalates (DBP, DEHP, BBP, DMEP, DnPP, DiPP, DPP, and DiBP), classified H360 or H361, are forbidden in cosmetics according to the European regulation on cosmetics 1223/2009. A GC/MS method was developed for the assay of 12 phthalates in cosmetics, including the 8 phthalates regulated. Analyses are carried out on a GC/MS system with electron impact ionization mode (EI). The separation of phthalates is obtained on a cross-linked 5%-phenyl/95%-dimethylpolysiloxane capillary column 30 m × 0.25 mm (i.d.) × 0.25 mm film thickness using a temperature gradient. Phthalate quantification is performed by external calibration using an internal standard. Validation elements obtained on standard solutions, highlight a satisfactory system conformity (resolution>1.5), a common quantification limit at 0.25 ng injected, an acceptable linearity between 0.5 μg mL⁻¹ and 5.0 μg mL⁻¹ as well as a precision and an accuracy in agreement with in-house specifications. Cosmetic samples ready for analytical injection are analyzed after a dilution in ethanol whereas more complex cosmetic matrices, like milks and creams, are assayed after a liquid/liquid extraction using ter-butyl methyl ether (TBME). Depending on the type of cosmetics analyzed, the common limits of quantification for the 12 phthalates were set at 0.5 or 2.5 μg g⁻¹. All samples were assayed using the analytical approach described in the ISO 12787 international standard "Cosmetics-Analytical methods-Validation criteria for analytical results using chromatographic techniques". This analytical protocol is particularly adapted when it is not possible to make reconstituted sample matrices. Copyright © 2012 Elsevier B.V. All rights reserved.

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.

Electromembrane extraction of gonadotropin-releasing hormone agonists from plasma and wastewater samples.

PubMed

Nojavan, Saeed; Bidarmanesh, Tina; Mohammadi, Ali; Yaripour, Saeid

2016-03-01

In the present study, for the first time electromembrane extraction followed by high performance liquid chromatography coupled with ultraviolet detection was optimized and validated for quantification of four gonadotropin-releasing hormone agonist anticancer peptides (alarelin, leuprolide, buserelin and triptorelin) in biological and aqueous samples. The parameters influencing electromigration were investigated and optimized. The membrane consists 95% of 1-octanol and 5% di-(2-ethylhexyl)-phosphate immobilized in the pores of a hollow fiber. A 20 V electrical field was applied to make the analytes migrate from sample solution with pH 7.0, through the supported liquid membrane into an acidic acceptor solution with pH 1.0 which was located inside the lumen of hollow fiber. Extraction recoveries in the range of 49 and 71% within 15 min extraction time were obtained in different biological matrices which resulted in preconcentration factors in the range of 82-118 and satisfactory repeatability (7.1 < RSD% < 19.8). The method offers good linearity (2.0-1000 ng/mL) with estimation of regression coefficient higher than 0.998. The procedure allows very low detection and quantitation limits of 0.2 and 0.6 ng/mL, respectively. Finally, it was applied to determination and quantification of peptides in human plasma and wastewater samples and satisfactory results were yielded. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous Determination of Formoterol Fumarate and Budesonide Epimers in Metered Dose Inhaler Using Ion-Pair Chromatography.

PubMed

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

2017-11-01

A simple, accurate and valid ion-pairing chromatographic method was developed for the simultaneous determination of formoterol fumarate (FF) and budesonide (BUD) epimers in metered dose inhaler. The separation was performed on C-18 column using mobile phase consisting of acetonitrile:0.05 M sodium acetate buffer (40:60% v/v) containing 0.03% sodium dodecyl sulfate adjusted to pH 3.1 using increasing volumes of either TEA or orthophosphoric acid isocratically eluted at 1.0 mL/min. Quantitation was achieved with UV detection at 214 nm. The retention times were 3.22, 6.41 and 6.91 min for formoterol fumarate, budesonide epimers B and A, respectively. The linearity range was 0.05-5.0 μg/mL for formoterol fumarate and 0.5-50.0 μg/mL for budesonide. The method was validated for, linearity; lower limit of quantification, lower limit of detection accuracy and precision. The proposed method is rapid (7 min), reproducible (RSD < 2.0%) and achieves satisfactory resolution between FF and BUD B (resolution factor = 12.07). The mean recoveries of the analytes in metered dose inhaler (99.97 and 99.83% for FF and BUD, respectively) were satisfactory. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

A Better Leveled Playing Field for Assessing Satisfactory Job Performance of Superintendents on the Basis of High-Stakes Testing Outcomes

ERIC Educational Resources Information Center

Young, I. Phillip; Cox, Edward P.; Buckman, David G.

2014-01-01

To assess satisfactory job performance of superintendents on the basis of school districts' high-stakes testing outcomes, existing teacher models were reviewed and critiqued as potential options for retrofit. For these models, specific problems were identified relative to the choice of referent groups. An alternate referent group (statewide…

The Shock and Vibration Digest. Volume 12, Number 7,

DTIC Science & Technology

1980-07-01

clearance of the pump [14]. This external damper controls passage of the and the journal bearing have an effect on the stability shaft through...initial Analytical and experimental investigation with the operation of large Deriaz pumps have been studied squeeze- film damper [15, 16] showed the...existence (251; a procedure for satisfactory operation is de- of an intershaft viscous damper instability. The scribed. squeeze- film damper was explored

Externally Pressurized Journal Gas Bearings

NASA Technical Reports Server (NTRS)

Laub, John H.

1959-01-01

Externally pressurized gas-lubricated bearings with multiple orifice feed are investigated. An analytical treatment is developed for a semi-cylindrical bearing with 9 orifices and for a cylindrical journal bearing with 192 radial and 24 axial orifices. Experiments are described on models of the two bearing configurations with specially designed fixtures which incorporate pneumatic loading and means for determining pressure profiles, gas flow and gap height. The correlation between theory and experiment is satisfactory.

Simultaneous and rapid determination of deoxynivalenol and its acetylate derivatives in wheat flour and rice by ultra high performance liquid chromatography with photo diode array detection.

PubMed

Xu, Jiao-Jiao; Zhou, Jian; Huang, Bai-Fen; Cai, Zeng-Xuan; Xu, Xiao-Min; Ren, Yi-Ping

2016-06-01

A simple and reliable method of ultra high performance liquid chromatography coupled with photo-diode array detection has been proposed for the simultaneous determination of deoxynivalenol and its acetylated derivatives in wheat flour and rice, especially focusing on the optimization of sample extraction, cleanup, and chromatographic separation conditions. Sample pretreatment consisted of a first step using a quick, easy, cheap, effective, rugged, and safe based extraction procedure and a subsequent cleanup step based on solid-phase extraction. The method was extensively validated in wheat flour and rice, obtaining satisfactory analytical performance with good linearity (R(2) ≥ 0.999), acceptable recoveries (80.0-104.4%), and repeatability (RSDs 1.3-10.7%). The limits of detection (21.7-57.4 μg/kg) and quantitation (72.3-191.4 μg/kg) for deoxynivalenols were lower than those usually permitted by various countries' legislation in these food matrices. The method was applied to 34 wheat and rice samples. The results were further compared with results of ultra high performance liquid chromatography with electrospray ionization tandem mass spectrometry. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Hierarchically mesostructured porous TiO2 hollow nanofibers for high performance glucose biosensing.

PubMed

Guo, Qiaohui; Liu, Lijuan; Zhang, Man; Hou, Haoqing; Song, Yonghai; Wang, Huadong; Zhong, Baoying; Wang, Li

2017-06-15

Effective immobilization of enzymes on an electrode surface is of great importance for biosensor development, but it still remains challenging because enzymes tend to denaturation and/or form close-packed structures. In this work, a free-standing TiO 2 hollow nanofibers (HNF-TiO 2 ) was successfully prepared by a simple and scalable electrospun nanofiber film template-assisted sol-gel method, and was further explored for glucose oxidase (GOD) immobilization and biosensing. This porous and nanotubular HNF-TiO 2 provides a well-defined hierarchical nanostructure for GOD loading, and the fine TiO 2 nanocrystals facilitate direct electron transfer from GOD to the electrode, also the strong interaction between GOD and HNF-TiO 2 greatly enhances the stability of the biosensor. The as-prepared glucose biosensors show good sensing performances both in O 2 -free and O 2 -containing conditions with good sensitivity, satisfactory selectivity, long-term stability and sound reliability. The novel textile formation, porous and hierarchically mesostructured nature of HNF-TiO 2 with excellent analytical performances make it a superior platform for the construction of high-performance glucose biosensors. Copyright © 2016 Elsevier B.V. All rights reserved.

The Italian pilot external quality assessment program for cystic fibrosis sweat test.

PubMed

Salvatore, Marco; Floridia, Giovanna; Amato, Annalisa; Censi, Federica; Carta, Claudio; de Stefano, Maria Chiara; Ferrari, Gianluca; Tosto, Fabrizio; Capoluongo, Ettore; Caruso, Ubaldo; Castaldo, Giuseppe; Cirilli, Natalia; Corbetta, Carlo; Padoan, Rita; Raia, Valeria; Taruscio, Domenica

2016-05-01

Sweat chloride test is the gold standard test for cystic fibrosis (CF) diagnosis. In 2014 the Istituto Superiore di Sanità established the Italian pilot external quality assessment program for CF sweat test (IEQA-ST). Ten laboratories, included among the 33 Italian CF Referral Centers, were selected and enrolled on the basis of their attitude to perform sweat test (ST) analysis by using methods recommended by the Italian Guidelines. They received three different sweat-like samples (normal, borderline and pathologic chloride concentration), with mock clinical indications, for analysis according to routine procedures. Assessment, performed by a panel of experts, covered analytical performance, interpretation and reporting of results; categories of "poor" and "satisfactory" performance were not defined. All data were managed through a web utility. The program identified important areas of interest and, in some case, of concern. It is important to underline that results are referred to a small proportion, i.e. about 30%, of Italian laboratories performing CF ST in the context of the Referral Centers. Data collected highlight the importance of participation in EQA programs as it may improve laboratory/clinical performance; our study represents a model for the setting up of a large-scale EQA scheme for ST. Copyright © 2016 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Determination of phosphonoformate (foscarnet) in calf and human serum by automated solid-phase extraction and high-performance liquid chromatography with amperometric detection.

PubMed

Ba, B B; Corniot, A G; Ducint, D; Breilh, D; Grellet, J; Saux, M C

1999-03-05

An isocratic high-performance liquid chromatographic method with automated solid-phase extraction has been developed to determine foscarnet in calf and human serums. Extraction was performed with an anion exchanger, SAX, from which the analyte was eluted with a 50 mM potassium pyrophosphate buffer, pH 8.4. The mobile phase consisted of methanol-40 mM disodium hydrogenphosphate, pH 7.6 containing 0.25 mM tetrahexylammonium hydrogensulphate (25:75, v/v). The analyte was separated on a polyether ether ketone (PEEK) column 150x4.6 mm I.D. packed with Kromasil 100 C18, 5 microm. Amperometric detection allowed a quantification limit of 15 microM. The assay was linear from 15 to 240 microM. The recovery of foscarnet from calf serum ranged from 60.65+/-1.89% for 15 microM to 67.45+/-1.24% for 200 microM. The coefficient of variation was < or = 3.73% for intra-assay precision and < or =7.24% for inter-assay precision for calf serum concentrations ranged from 15 to 800 microM. For the same samples, the deviation from the nominal value ranged from -8.97% to +5.40% for same day accuracy and from -4.50% to +2.77% for day-to-day accuracy. Selectivity was satisfactory towards potential co-medications. Replacement of human serum by calf serum for calibration standards and quality control samples was validated. Automation brought more protection against biohazards and increase in productivity for routine monitoring and pharmacokinetic studies.

Optimisation and validation of the analytical procedure for the determination of acrylamide in coffee by LC-MS/MS with SPE clean up.

PubMed

Gielecińska, Iwona; Mojska, Hanna

2013-01-01

Numerous studies have demonstrated acrylamide to be both neurotoxic and carcinogenic. At present it is widely recognised that acrylamide is mainly formed through the Maillard reaction from free asparagine and reducing sugars. The major sources of dietary acrylamide are potato products, processed cereals and coffee. To optimise and validate an analytical method for determining acrylamide in coffee by liquid chromatography and tandem mass spectrometry analysis (LC/MS/MS) using SPE clean-up. Analytical separation of acrylamide from roasted coffee was performed by liquid chromatography using a Hypercarb column followed by LC/MS/MS analysis, with 2,3,3-d3 acrylamide as an internal standard. The method was based on two purification steps: the first with hexane and Carrez solutions in order to remove of fat and to precipitate proteins, respectively; and the second with a solid-phase extraction (SPE) column which proved to be efficient in the elimination of the main chromatographic interferences. Limit of quantification (LOQ) for measuring acrylamide in coffee was 50 microg/kg. The described method demonstrates satisfactory precision (RSD = 2.5%), repeatability (RSD = 9.2%) and accuracy (mean recovery - 97.4%). Our results confirm that LC-MS/MS with SPE clean-up is selective and suitable for determination of acrylamide in coffee. Indeed, this method meets the criteria of EU Commission Recommendations (No. 2007/331/EC and No. 2010/307/EU), on the monitoring of acrylamide levels in food.

Rapid sucrose monitoring in green coffee samples using multienzymatic biosensor.

PubMed

Stredansky, Miroslav; Redivo, Luca; Magdolen, Peter; Stredansky, Adam; Navarini, Luciano

2018-07-15

Amperometric biosensor utilizing FAD-dependent glucose dehydrogenase (FAD-GDH) for a specific sucrose monitoring in green coffee is described. FAD-GDH was co-immobilized with invertase and mutarotase on a thin-layer gold planar electrode using chitosan. The biosensor showed a wide linearity (from 10 to 1200 μM), low detection limit (8.4 μM), fast response time (50 s), and appeared to be O2 independent. In addition the biosensors exhibited a good operational (3 days) and storage (1 year) stability. Finally, the results achieved from the biosensor measurements of sucrose in 17 samples of green coffee (Coffea arabica, C. canephora and C. liberica) were compared with those obtained by the standard HPLC method. The good correlation among results of real samples, satisfactory analytical performance and simple use of the presented biosensor make it suitable for application in coffee industry. Copyright © 2018 Elsevier Ltd. All rights reserved.

Experimental and theoretical studies of near-ground acoustic radiation propagation in the atmosphere

NASA Astrophysics Data System (ADS)

Belov, Vladimir V.; Burkatovskaya, Yuliya B.; Krasnenko, Nikolai P.; Rakov, Aleksandr S.; Rakov, Denis S.; Shamanaeva, Liudmila G.

2017-11-01

Results of experimental and theoretical studies of the process of near-ground propagation of monochromatic acoustic radiation on atmospheric paths from a source to a receiver taking into account the contribution of multiple scattering on fluctuations of atmospheric temperature and wind velocity, refraction of sound on the wind velocity and temperature gradients, and its reflection by the underlying surface for different models of the atmosphere depending the sound frequency, coefficient of reflection from the underlying surface, propagation distance, and source and receiver altitudes are presented. Calculations were performed by the Monte Carlo method using the local estimation algorithm by the computer program developed by the authors. Results of experimental investigations under controllable conditions are compared with theoretical estimates and results of analytical calculations for the Delany-Bazley impedance model. Satisfactory agreement of the data obtained confirms the correctness of the suggested computer program.

Microwave Sanitization of Color Additives Used in Cosmetics: Feasibility Study

PubMed Central

Jasnow, S. B.; Smith, J. L.

1975-01-01

Microwave exposure has been explored as a method of microbiologically sanitizing color additives used in cosmetic products. Selected microbiologically unacceptable cosmetic color additives, D&C red no. 7 Ca lake (certified synthetic organic color), carmine (natural organic color not subject to certification), and chromium hydroxide green (inorganic color not subject to certification), were submitted to microwave exposure. Gram-negative bacteria were eliminated, as verified by enrichment procedures, and levels of gram-positive bacteria were reduced. Generally, analytical and dermal safety studies indicated no significant alterations in physical, chemical, and toxicological properties of the colors. Sanitization was also successfully performed on other colors (D&C red no. 9 Ba lake, D&C red no. 12 Ba lake, D&C green no. 5, and FD&C red no. 4); initial physical and chemical tests were satisfactory. Results indicated that this method of sanitization is feasible and warrants further investigation. PMID:1164010

Analysis and design of optical systems by use of sensitivity analysis of skew ray tracing

NASA Astrophysics Data System (ADS)

Lin, Psang Dain; Lu, Chia-Hung

2004-02-01

Optical systems are conventionally evaluated by ray-tracing techniques that extract performance quantities such as aberration and spot size. Current optical analysis software does not provide satisfactory analytical evaluation functions for the sensitivity of an optical system. Furthermore, when functions oscillate strongly, the results are of low accuracy. Thus this work extends our earlier research on an advanced treatment of reflected or refracted rays, referred to as sensitivity analysis, in which differential changes of reflected or refracted rays are expressed in terms of differential changes of incident rays. The proposed sensitivity analysis methodology for skew ray tracing of reflected or refracted rays that cross spherical or flat boundaries is demonstrated and validated by the application of a cat's eye retroreflector to the design and by the image orientation of a system with noncoplanar optical axes. The proposed sensitivity analysis is projected as the nucleus of other geometrical optical computations.

Analysis and Design of Optical Systems by Use of Sensitivity Analysis of Skew Ray Tracing

NASA Astrophysics Data System (ADS)

Dain Lin, Psang; Lu, Chia-Hung

2004-02-01

Optical systems are conventionally evaluated by ray-tracing techniques that extract performance quantities such as aberration and spot size. Current optical analysis software does not provide satisfactory analytical evaluation functions for the sensitivity of an optical system. Furthermore, when functions oscillate strongly, the results are of low accuracy. Thus this work extends our earlier research on an advanced treatment of reflected or refracted rays, referred to as sensitivity analysis, in which differential changes of reflected or refracted rays are expressed in terms of differential changes of incident rays. The proposed sensitivity analysis methodology for skew ray tracing of reflected or refracted rays that cross spherical or flat boundaries is demonstrated and validated by the application of a cat ?s eye retroreflector to the design and by the image orientation of a system with noncoplanar optical axes. The proposed sensitivity analysis is projected as the nucleus of other geometrical optical computations.

[Amanitine determination as an example of peptide analysis in the biological samples with HPLC-MS technique].

PubMed

Janus, Tomasz; Jasionowicz, Ewa; Potocka-Banaś, Barbara; Borowiak, Krzysztof

Routine toxicological analysis is mostly focused on the identification of non-organic and organic, chemically different compounds, but generally with low mass, usually not greater than 500–600 Da. Peptide compounds with atomic mass higher than 900 Da are a specific analytical group. Several dozen of them are highly-toxic substances well known in toxicological practice, for example mushroom toxin and animal venoms. In the paper the authors present an example of alpha-amanitin to explain the analytical problems and different original solutions in identifying peptides in urine samples with the use of the universal LC MS/MS procedure. The analyzed material was urine samples collected from patients with potential mushroom intoxication, routinely diagnosed for amanitin determination. Ultra filtration with centrifuge filter tubes (limited mass cutoff 3 kDa) was used. Filtrate fluid was directly injected on the chromatographic column and analyzed with a mass detector (MS/MS). The separation of peptides as organic, amphoteric compounds from biological material with the use of the SPE technique is well known but requires dedicated, specific columns. The presented paper proved that with the fast and simple ultra filtration technique amanitin can be effectively isolated from urine, and the procedure offers satisfactory sensitivity of detection and eliminates the influence of the biological matrix on analytical results. Another problem which had to be solved was the non-characteristic fragmentation of peptides in the MS/MS procedure providing non-selective chromatograms. It is possible to use higher collision energies in the analytical procedure, which results in more characteristic mass spectres, although it offers lower sensitivity. The ultra filtration technique as a procedure of sample preparation is effective for the isolation of amanitin from the biological matrix. The monitoring of selected mass corresponding to transition with the loss of water molecule offers satisfactory sensitivity of determination.

Simultaneous determination of 24 personal care products in fish muscle and liver tissues using QuEChERS extraction coupled with ultra pressure liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometer analyses.

PubMed

Yao, Li; Zhao, Jian-Liang; Liu, You-Sheng; Yang, Yuan-Yuan; Liu, Wang-Rong; Ying, Guang-Guo

2016-11-01

A sensitive and selective quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction combined with dispersive solid-phase extraction (d-SPE) cleanup method was developed to simultaneously extract a wide range of personal care products (16 biocides, 4 synthetic musks, and 4 benzotriazoles) in fish muscle and liver tissues. In order to get satisfactory recoveries, different extraction parameters were optimized, including extraction salts and d-SPE materials, extraction solvents and acetic acid contents in organic phase, and the ratios of solvent and water. Ultra pressure liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry were used to analyze the target compounds in the extracts. Among the 24 personal care products, the recoveries in the range of 70-120 % were obtained for 20, 19, and 12 analytes in fish muscle at the spiking concentrations of 10, 5, and 1 ng/g ww, respectively, and for 13, 12, and 11 analytes in liver at the spiking concentrations of 40, 20, and 4 ng/g ww, respectively. Method quantification limits (MQLs) of all analytes were 0.02-2.12 ng/g ww for fish muscle and 0.22-12.2 ng/g ww for fish liver tissues. The method was successfully applied to wild fish samples collected from Dongjiang River, south China. Twenty-one and 17 of the analytes were found in fish muscle and liver samples, respectively, in at least one site of the river with the concentrations between below MQLs and 119 ng/g ww, respectively. Graphical abstract Achieved satisfactory recoveries, high precision, and low method quantification limits (MQLs) for PCPs in wild fish tissues by QuEChERS procedure optimization combined with UPLC-MS/MS and GC-MS analyses.

Surfactant assisted pulsed two-phase electromembrane extraction followed by GC analysis for quantification of basic drugs in biological samples.

PubMed

Zahedi, Pegah; Davarani, Saied Saeed Hosseiny; Moazami, Hamid Reza; Nojavan, Saeed

2016-01-05

In this work, a simple and efficient surfactant assisted pulsed two-phase electromembrane extraction (SA-PEME) procedure combined with gas chromatography (GC) has been developed for the determination of alfentanil, sufentanil and methadone in various samples. It has been found that the addition of anionic surfactant causes the accumulation of the cationic analytes at the SLM/solution interface resulting in an easier transfer of the analytes into the organic phase. The method was accomplished with 1-octanol as the acceptor phase and supported liquid membrane (SLM) by means of an 80 V pulsed electrical driving force and the extraction time of 20 min. The model analytes were extracted from 3.0 mL sample solution (pH 4.0) containing 0.02% w/v surfactant (sodium dodecyl sulfate). The duty cycle of 92% and frequency of 0.357 Hz gave the best performance. Extraction recoveries in the range of 70.5-95.2% and satisfactory repeatability (7.6

Solution of magnetic field and eddy current problem induced by rotating magnetic poles (abstract)

NASA Astrophysics Data System (ADS)

Liu, Z. J.; Low, T. S.

1996-04-01

The magnetic field and eddy current problems induced by rotating permanent magnet poles occur in electromagnetic dampers, magnetic couplings, and many other devices. Whereas numerical techniques, for example, finite element methods can be exploited to study various features of these problems, such as heat generation and drag torque development, etc., the analytical solution is always of interest to the designers since it helps them to gain the insight into the interdependence of the parameters involved and provides an efficient tool for designing. Some of the previous work showed that the solution of the eddy current problem due to the linearly moving magnet poles can give satisfactory approximation for the eddy current problem due to rotating fields. However, in many practical cases, especially when the number of magnet poles is small, there is significant effect of flux focusing due to the geometry. The above approximation can therefore lead to marked errors in the theoretical predictions of the device performance. Bernot et al. recently described an analytical solution in a polar coordinate system where the radial field is excited by a time-varying source. A discussion of an analytical solution of the magnetic field and eddy current problems induced by moving magnet poles in radial field machines will be given in this article. The theoretical predictions obtained from this method is compared with the results obtained from finite element calculations. The validity of the method is also checked by the comparison of the theoretical predictions and the measurements from a test machine. It is shown that the introduced solution leads to a significant improvement in the air gap field prediction as compared with the results obtained from the analytical solution that models the eddy current problems induced by linearly moving magnet poles.

PRSA hydrogen tank thermal acoustic oscillation study

NASA Technical Reports Server (NTRS)

Riemer, D. H.

1979-01-01

The power reactant storage assembly (PRSA) hydrogen tank test data were reviewed. Two hundred and nineteen data points illustrating the effect of flow rate, temperature ratio and configuration were identified. The test data were reduced to produce the thermal acoustic oscillation parameters. Frequency and amplitude were determined for model correlation. A comparison of PRSA hydrogen tank test data with the analytical models indicated satisfactory agreement for the supply and poor agreement for the full line.

Analysis of anti-neoplastic drug in bacterial ghost matrix, w/o/w double nanoemulsion and w/o nanoemulsion by a validated 'green' liquid chromatographic method.

PubMed

Youssof, Abdullah M E; Salem-Bekhit, Mounir M; Shakeel, Faiyaz; Alanazi, Fars K; Haq, Nazrul

2016-07-01

The objective of the present investigation was to develop and validate a 'green' reversed phase high-performance liquid chromatography (RP-HPLC) method for rapid analysis of a cytotoxic drug 5-fluorouracil (5-FU) in bulk drug, marketed injection, water-in-oil (w/o) nanoemulsion, double water-in-oil-in-water (w/o/w) nanoemulsion and bacterial ghost (BG) matrix. The chromatography study was carried out at room temperature (25±1°C) using an HPLC system with the help of ultraviolet (UV)-visible detector. The chromatographic performance was achieved with a Nucleodur 150mm×4.6mm RP C8 column filled with 5µm filler as a static phase. The mobile phase consisted of ethyl acetate: methanol (7:3% v/v) which was delivered at a flow rate of 1.0mLmin(-1) and the drug was detected in UV mode at 254nm. The developed method was validated in terms of linearity (r(2)=0.998), accuracy (98.19-102.09%), precision (% RSD=0.58-1.17), robustness (% RSD=0.12-0.53) and sensitivity with satisfactory results. The efficiency of the method was demonstrated by the assay of the drug in marketed injection, w/o nanoemulsion, w/o/w nanoemulsion and BG with satisfactory results. The successful resolution of the drug along with its degradation products clearly established the stability-indicating nature of the proposed method. Overall, these results suggested that the proposed analytical method could be effectively applied to the routine analysis of 5-FU in bulk drug, various pharmaceutical dosage forms and BG. Copyright © 2016 Elsevier B.V. All rights reserved.

Pell Grants as Performance-Based Aid? An Examination of Satisfactory Academic Progress Requirements in the Nation's Largest Need-Based Aid Program. A CAPSEE Working Paper

ERIC Educational Resources Information Center

Schudde, Lauren; Scott-Clayton, Judith

2014-01-01

The Federal Pell Grant Program is the nation's largest need-based grant program. While students' initial eligibility for the Pell is based on financial need, renewal of the award is contingent on their making satisfactory academic progress (SAP)--meeting minimum academic standards similar to those proposed in models of performance-based…

Simultaneous determination of enalapril and hydrochlorothiazide in pharmaceutical preparations using microemulsion liquid chromatography.

PubMed

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

2015-01-01

A rapid high-performance liquid chromatography procedure for analytical quality control of mixture containing enalapril maleate (ENM) and hydrochlorothiazide (HCT) in their pharmaceutical preparations was developed using a microemulsion as an eluent. The separation was performed on a column packed with cyano-bonded stationary phase adopting UV detection at 210 nm using a flow rate of 1 mL/min. The optimized microemulsion mobile phase consisted of 0.2 M sodium dodecyl sulfate, 1% octanol, 10% n-propanol and 0.3% triethylamine in 0.02 M phosphoric acid, and pH was adjusted at 3.5. The proposed method was found to be linear over the concentration ranges 1-100 and 0.05-5 μg/mL for ENM and HCT, respectively with a correlation coefficient of 0.9999 for both drugs. The developed method was validated in terms of specificity, linearity, lower limit of quantification, lower limit of detection, precision and accuracy. The proposed method is rapid (5 min), reproducible (relative standard deviation <2.0%) and achieves a satisfactory resolution between ENM and HCT (resolution factor = 3.62). The mean recoveries of the analytes in tablets were in agreement with those obtained from a comparison method, as revealed by statistical analysis of the obtained results using Student's t-test and the variance ratio F-test. © The Author [2014]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Ultra-fast LC-ESI-MS/MS method for the simultaneous determination of six highly toxic Aconitum alkaloids from Aconiti kusnezoffii radix in rat plasma and its application to a pharmacokinetic study.

PubMed

Liu, Jingjing; Li, Qing; Yin, Yidi; Liu, Ran; Xu, Huarong; Bi, Kaishun

2014-01-01

A fast, sensitive, and efficient ultra-fast LC-ESI-MS/MS method was developed for the simultaneous quantitation of six highly toxic Aconitum alkaloids, that is, aconitine, mesaconitine, hypaconitine, benzoylaconine, benzoylmesaconine, and benzoylhypaconine, in rat plasma after oral administration of crude ethanol extracts from Aconiti kusnezoffii radix by ultrasonic extraction, reflux extraction for 1 h, and reflux extraction for 3 h, respectively. The separation of six Aconitum alkaloids and aminopyrine (internal standard) was performed on an InertSustain® C18 column, and the quantification of the analytes was performed on a 4000Q ultra-fast LC-MS/MS system with turbo ion spray source in the positive ion and multiple-reaction monitoring mode. Absolute recoveries ranged within 65.06-85.1% for plasma samples. The intra- and interday precision and accuracy of analytes were satisfactory. The methods were validated with sensitivity reaching the lower LOQ for aconitine, mesaconitine, hypaconitine, benzoylaconine, benzoylmesaconine, and benzoylhypaconine, which were 0.025, 0.025, 0.050, 0.025, 0.025, and 0.100 ng/mL, respectively. The method was successfully applied to a pharmacokinetic study of six Aconitum alkaloids in rat plasma after oral administration of crude ethanol extracts from the raw root of Aconitum kusnezoffii Reichb. by three different extraction processes. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ionic liquid as a mobile phase additive in high-performance liquid chromatography for the simultaneous determination of eleven fluorescent whitening agents in paper materials.

PubMed

Wang, Qing; Chen, Xianbo; Qiu, Bin; Zhou, Liang; Zhang, Hui; Xie, Juan; Luo, Yan; Wang, Bin

2016-04-01

In the present study, 11 4,4'-diaminostilbene-2,2'-disulfonic acid based fluorescent whitening agents with different numbers of sulfonic acid groups were separated by using an ionic liquid as a mobile phase additive in high-performance liquid chromatography with fluorescence detection. The effects of ionic liquid concentration, pH of mobile phase B, and composition of mobile phase A on the separation of fluorescent whitening agents were systematically investigated. The ionic liquid tetrabutylammonium tetrafluoroborate is superior to tetrabutylammomnium bromide for the separation of the fluorescent whitening agents. The optimal separation conditions were an ionic liquid concentration at 8 mM and the pH of mobile phase B at 8.5 with methanol as mobile phase A. The established method exhibited low limits of detection (0.04-0.07 ng/mL) and wide linearity ranges (0.30-20 ng/mL) with high linear correlation coefficients from 0.9994 to 0.9998. The optimized procedure was applied to analyze target analytes in paper samples with satisfactory results. Eleven target analytes were quantified, and the recoveries of spiked paper samples were in the range of 85-105% with the relative standard deviations from 2.1 to 5.1%. The obtained results indicated that the method was efficient for detection of 11 fluorescent whitening agents. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous identification and quantification of bisphenol A and 12 bisphenol analogues in environmental samples using precolumn derivatization and ultra high performance liquid chromatography with tandem mass spectrometry.

PubMed

Wang, Zhonghe; Yu, Jing; Yao, Jiaxi; Wu, Linlin; Xiao, Hang; Wang, Jun; Gao, Rong

2018-02-10

A method for the identification and quantification of bisphenol A and 12 bisphenol analogues in river water and sediment samples combining liquid-liquid extraction, precolumn derivatization, and ultra high-performance liquid chromatography coupled with tandem mass spectrometry was developed and validated. Analytes were extracted from the river water sample using a liquid-liquid extraction method. Dansyl chloride was selected as a derivatization reagent. Derivatization reaction conditions affecting production of the dansyl derivatives were tested and optimized. All the derivatized target compounds were well separated and eluted in 10 min. Dansyl chloride labeled compounds were analyzed using a high-resolution mass spectrometer with electrospray ionization in the positive mode, and the results were confirmed and quantified in the parallel reaction monitoring mode. The method validation results showed a satisfactory level of sensitivity. Linearity was assessed using matrix-matched standard calibration, and good correlation coefficients were obtained. The limits of quantification for the analytes ranged from 0.005 to 0.02 ng/mL in river water and from 0.15 to 0.80 ng/g in sediment. Good reproducibility of the method in terms of intra- and interday precision was achieved, yielding relative standard deviations of less than 10.1 and 11.6%, respectively. Finally, this method was successfully applied to the analysis of real samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Pleasure-suffering indicators of nursing work in a hemodialysis nursing service].

PubMed

Prestes, Francine Cassol; Beck, Carmem Lúcia Colomé; Magnago, Tânia Solange Bosi de Souza; Silva, Rosângela Marion da

2015-06-01

To measure the pleasure and suffering indicators at work and relate them to the socio-demographic and employment characteristics of the nursing staff in a hemodialysis center in southern Brazil. Quantitative research, with 46 workers. We used a self-completed form with demographic and labor data and the Pleasure and Suffering Indicators at Work Scale (PSIWS). We conducted a bivariate and correlation descriptive analysis with significance levels of 5% using the Epi-Info® and PredictiveAnalytics Software programs. Freedom of Speech was considered critical; other factors were evaluated as satisfactory. The results revealed a possible association between sociodemographic characteristics and work, and pleasure and suffering indicators. There was a correlation between the factors evaluated. Despite the satisfactory evaluation, suffering is present in the studied context, expressed mainly by a lack of Freedom of Speech, with the need for interventions to prevent injury to the health of workers.

A Micromechanics-Based Elastoplastic Damage Model for Rocks with a Brittle-Ductile Transition in Mechanical Response

NASA Astrophysics Data System (ADS)

Hu, Kun; Zhu, Qi-zhi; Chen, Liang; Shao, Jian-fu; Liu, Jian

2018-06-01

As confining pressure increases, crystalline rocks of moderate porosity usually undergo a transition in failure mode from localized brittle fracture to diffused damage and ductile failure. This transition has been widely reported experimentally for several decades; however, satisfactory modeling is still lacking. The present paper aims at modeling the brittle-ductile transition process of rocks under conventional triaxial compression. Based on quantitative analyses of experimental results, it is found that there is a quite satisfactory linearity between the axial inelastic strain at failure and the confining pressure prescribed. A micromechanics-based frictional damage model is then formulated using an associated plastic flow rule and a strain energy release rate-based damage criterion. The analytical solution to the strong plasticity-damage coupling problem is provided and applied to simulate the nonlinear mechanical behaviors of Tennessee marble, Indiana limestone and Jinping marble, each presenting a brittle-ductile transition in stress-strain curves.

Structural Model Tuning Capability in an Object-Oriented Multidisciplinary Design, Analysis, and Optimization Tool

NASA Technical Reports Server (NTRS)

Lung, Shun-fat; Pak, Chan-gi

2008-01-01

Updating the finite element model using measured data is a challenging problem in the area of structural dynamics. The model updating process requires not only satisfactory correlations between analytical and experimental results, but also the retention of dynamic properties of structures. Accurate rigid body dynamics are important for flight control system design and aeroelastic trim analysis. Minimizing the difference between analytical and experimental results is a type of optimization problem. In this research, a multidisciplinary design, analysis, and optimization (MDAO) tool is introduced to optimize the objective function and constraints such that the mass properties, the natural frequencies, and the mode shapes are matched to the target data as well as the mass matrix being orthogonalized.

Structural Model Tuning Capability in an Object-Oriented Multidisciplinary Design, Analysis, and Optimization Tool

NASA Technical Reports Server (NTRS)

Lung, Shun-fat; Pak, Chan-gi

2008-01-01

Updating the finite element model using measured data is a challenging problem in the area of structural dynamics. The model updating process requires not only satisfactory correlations between analytical and experimental results, but also the retention of dynamic properties of structures. Accurate rigid body dynamics are important for flight control system design and aeroelastic trim analysis. Minimizing the difference between analytical and experimental results is a type of optimization problem. In this research, a multidisciplinary design, analysis, and optimization [MDAO] tool is introduced to optimize the objective function and constraints such that the mass properties, the natural frequencies, and the mode shapes are matched to the target data as well as the mass matrix being orthogonalized.

Collisional evolution - an analytical study for the nonsteady-state mass distribution

NASA Astrophysics Data System (ADS)

Martins, R. Vieira

1999-05-01

To study the collisional evolution of asteroidal groups we can use an analytical solutionfor the self-similar collision cascades. This solution is suitable to study the steady-state massdistribution of the collisional fragmentation. However, out of the steady-state conditions, thissolution is not satisfactory for some values of the collisional parameters. In fact, for some valuesfor the exponent of the mass distribution power law of an asteroidal group and its relation to theexponent of the function which describes how rocks break we arrive at singular points for theequation which describes the collisional evolution. These singularities appear since someapproximations are usually made in the laborious evaluation of many integrals that appear in theanalytical calculations. They concern the cutoff for the smallest and the largest bodies. Thesesingularities set some restrictions to the study of the analytical solution for the collisionalequation. To overcome these singularities we performed an algebraic computationconsidering the smallest and the largest bodies and we obtained the analytical expressions for theintegrals that describe the collisional evolution without restriction on the parameters. However,the new distribution is more sensitive to the values of the collisional parameters. In particular thesteady-state solution for the differential mass distribution has exponents slightly different from11⧸6 for the usual parameters in the Asteroid Belt. The sensitivity of this distribution with respectto the parameters is analyzed for the usual values in the asteroidal groups. With anexpression for the mass distribution without singularities, we can evaluate also its time evolution.We arrive at an analytical expression given by a power series of terms constituted by a smallparameter multiplied by the mass to an exponent, which depends on the initial power lawdistribution. This expression is a formal solution for the equation which describes the collisionalevolution. Furthermore, the first-order term for this solution is the time rate of the distribution atthe initial time. In particular the solution shows the fundamental importance played by theexponent of the power law initial condition in the evolution of the system.

Determination of colistin in animal tissues, egg, milk, and feed by ultra-high performance liquid chromatography-tandem mass spectrometry.

PubMed

Fu, Qin; Li, Xiaowei; Zheng, Kangni; Ke, Yuebin; Wang, Yingyu; Wang, Lina; Yu, Fugen; Xia, Xi

2018-05-15

A confirmatory method for the determination of colistin in animal tissues, egg, milk, and feed was developed and validated. Colistin A and colistin B were extracted from samples with the mixture of 10% trichloroacetic acid-acetonitrile and isolated with mixed-mode weak cation exchange cartridge. Analytes were separated from matrix components using ultra-high performance liquid chromatography, and detected with electrospray ionization on a triple quadrupole mass spectrometer. Mean recoveries ranged from 78.0% to 115.6% with intra-day and inter-day relative standard deviation lower than 8.4% and 12.4%, respectively. The quantitation limits for different matrices were between 5 and 30 μg/kg, which was satisfactory for surveillance monitoring. The developed method was applied to the analysis of real samples collected from different provinces of China, and 19 out of 348 samples were found to be contaminated, with the highest concentration of approximately 12,000 μg/kg colistin A and 10,000 μg/kg colistin B in feed. Copyright © 2017 Elsevier Ltd. All rights reserved.

Optimization of sample preparation by central composite design for multi-class determination of veterinary drugs in bovine muscle, kidney and liver by ultra-high-performance liquid chromatographic-tandem mass spectrometry.

PubMed

Rizzetti, Tiele M; de Souza, Maiara P; Prestes, Osmar D; Adaime, Martha B; Zanella, Renato

2018-04-25

In this study a simple and fast multi-class method for the determination of veterinary drugs in bovine liver, kidney and muscle was developed. The method employed acetonitrile for extraction followed by clean-up with EMR-Lipid® sorbent and trichloracetic acid. Tests indicated that the use of TCA was most effective when added in the final step of the clean-up procedure instead of during extraction. Different sorbents were tested and optimized using central composite design and the analytes determined by ultra-high-performance liquid chromatographic-tandem mass spectrometry (UHPLC-MS/MS). The method was validated according the European Commission Decision 2002/657 presenting satisfactory results for 69 veterinary drugs in bovine liver and 68 compounds in bovine muscle and kidney. The method was applied in real samples and in proficiency tests and proved to be adequate for routine analysis. Residues of abamectin, doramectin, eprinomectin and ivermectin were found in samples of bovine muscle and only ivermectin in bovine liver. Copyright © 2017 Elsevier Ltd. All rights reserved.

Experimental and analytical studies on multiple tuned mass dampers for seismic protection of porcelain electrical equipment

NASA Astrophysics Data System (ADS)

Bai, Wen; Dai, Junwu; Zhou, Huimeng; Yang, Yongqiang; Ning, Xiaoqing

2017-10-01

Porcelain electrical equipment (PEE), such as current transformers, is critical to power supply systems, but its seismic performance during past earthquakes has not been satisfactory. This paper studies the seismic performance of two typical types of PEE and proposes a damping method for PEE based on multiple tuned mass dampers (MTMD). An MTMD damping device involving three mass units, named a triple tuned mass damper (TTMD), is designed and manufactured. Through shake table tests and finite element analysis, the dynamic characteristics of the PEE are studied and the effectiveness of the MTMD damping method is verified. The adverse influence of MTMD redundant mass to damping efficiency is studied and relevant equations are derived. MTMD robustness is verified through adjusting TTMD control frequencies. The damping effectiveness of TTMD, when the peak ground acceleration far exceeds the design value, is studied. Both shake table tests and finite element analysis indicate that MTMD is effective and robust in attenuating PEE seismic responses. TTMD remains effective when the PGA far exceeds the design value and when control deviations are considered.

Numerical study of nonlinear full wave acoustic propagation

NASA Astrophysics Data System (ADS)

Velasco-Segura, Roberto; Rendon, Pablo L.

2013-11-01

With the aim of describing nonlinear acoustic phenomena, a form of the conservation equations for fluid dynamics is presented, deduced using slightly less restrictive hypothesis than those necessary to obtain the well known Westervelt equation. This formulation accounts for full wave diffraction, nonlinearity, and thermoviscous dissipative effects. A CLAWPACK based, 2D finite-volume method using Roe's linearization has been implemented to obtain numerically the solution of the proposed equations. In order to validate the code, two different tests have been performed: one against a special Taylor shock-like analytic solution, the other against published results on a HIFU system, both with satisfactory results. The code is written for parallel execution on a GPU and improves performance by a factor of over 50 when compared to the standard CLAWPACK Fortran code. This code can be used to describe moderate nonlinear phenomena, at low Mach numbers, in domains as large as 100 wave lengths. Applications range from modest models of diagnostic and therapeutic HIFU, parametric acoustic arrays, to acoustic wave guides. A couple of examples will be presented showing shock formation and oblique interaction. DGAPA PAPIIT IN110411, PAEP UNAM 2013.

Trace matrix solid phase dispersion using a molecular sieve as the sorbent for the determination of flavonoids in fruit peels by ultra-performance liquid chromatography.

PubMed

Cao, Wan; Hu, Shuai-Shuai; Ye, Li-Hong; Cao, Jun; Pang, Xiao-Qing; Xu, Jing-Jing

2016-01-01

A simple, rapid, and highly selective trace matrix solid phase dispersion (MSPD) technique, coupled with ultra-performance liquid chromatography-ultraviolet detection, was proposed for extracting flavonoids from orange fruit peel matrices. Molecular sieve SBA-15 was applied for the first time as a solid support in trace MSPD. Parameters, such as the type of dispersant, mass ratio of the sample to the dispersant, grinding time, and elution pH, were optimized in detail. The optimal extraction conditions involved dispersing a powdered fruit peel sample (25 mg) into 25mg of SBA-15 and then eluting the target analytes with 500 μL of methanol. A satisfactory linearity (r(2) > 0.9990) was obtained, and the calculated limits of detection reached 0.02-0.03 μg/mL for the compounds. The results showed that the method developed was successfully applied to determine the content of flavonoids in complex fruit peel matrices. Copyright © 2015 Elsevier Ltd. All rights reserved.

Packed in-tube solid phase microextraction with graphene oxide supported on aminopropyl silica: Determination of target triazines in water samples.

PubMed

De Toffoli, Ana L; Fumes, Bruno H; Lanças, Fernando M

2018-02-22

On-line in-tube solid phase microextraction (in-tube SPME) coupled to high performance liquid chromatography and tandem mass spectrometry (HPLC-MS/MS) was successfully applied to the determination of selected triazines in water samples. The method based on the employment of a packed column containing graphene oxide (GO) supported on aminopropyl silica (Si) showed that the extraction phase has a high potential for triazines extraction aiming to its physical-chemical properties including ultrahigh specific surface area, good mechanical and thermal stability and high fracture strength. Injection volume and loading time were both investigated and optimized. The method validation using Si-GO to extract and concentrate the analytes showed satisfactory results, good sensitivity, good linearity (0.2-4.0 µg L -1 ) and low detection limits (1.1-2.9 ng L -1 ). The high extraction efficiency was determined with enrichment factors ranging from 1.2-2.9 for the lowest level, 1.3-4.9 intermediate level and 1.2-3.0 highest level (n = 3). Although the analytes were not detected in the real samples evaluated, the method has demonstrated to be efficient through its application in the analysis of spiked triazines in ground and mineral water samples.

Fabrication of paper-based analytical devices optimized by central composite design.

PubMed

Hamedpour, Vahid; Leardi, Riccardo; Suzuki, Koji; Citterio, Daniel

2018-04-30

In this work, an application of a design of experiments approach for the optimization of an isoniazid assay on a single-area inkjet-printed paper-based analytical device (PAD) is described. For this purpose, a central composite design was used for evaluation of the effect of device geometry and amount of assay reagents on the efficiency of the proposed device. The factors of interest were printed length, width, and sampling volume as factors related to device geometry, and amounts of the assay reagents polyvinyl alcohol (PVA), NH4OH, and AgNO3. Deposition of the assay reagents was performed by a thermal inkjet printer. The colorimetric assay mechanism of this device is based on the chemical interaction of isoniazid, ammonium hydroxide, and PVA with silver ions to induce the formation of yellow silver nanoparticles (AgNPs). The in situ-formed AgNPs can be easily detected by the naked eye or with a simple flat-bed scanner. Under optimal conditions, the calibration curve was linear in the isoniazid concentration range 0.03-10 mmol L-1 with a relative standard deviation of 3.4% (n = 5 for determination of 1.0 mmol L-1). Finally, the application of the proposed device for isoniazid determination in pharmaceutical preparations produced satisfactory results.

Development of a CZE method for the quantification of pseudoephedrine and cetirizine.

PubMed

Alnajjar, Ahmed O; Idris, Abubakr M

2014-10-01

Pseudoephedrine and cetirizine have been combined in dosage forms with more therapeutic benefits when compared with single-drug treatment. The current manuscript reports the development of the first capillary zone electrophoresis (CZE) assay method for that combination. The effects of pH and buffer concentration on resolution, noise, migration time and peak area were examined employing experimental design approach. The analytes were electropherographed into a 50.2 cm-long and 50 µm i.d. fused-silica capillary column using 10 mmol/L borate at pH 8.3 with a potential of 25 kV at 25°C and UV detection at 214 nm. The method was successfully validated in order to verify its suitability for pharmaceutical analysis for the purposes of quality control. Over previous high-performance liquid chromatographic methods, the current CZE method features the benefits of the use of cost-effective electrolyte, besides high sample throughput (11 samples/h). Furthermore, other analytical results including linear dynamic ranges, recovery (96.9-98.1%), intra- and interday precision (relative standard deviation ≤ 1.70%) as well as the limits of detection and quantification (≤2.65 µg/mL) were all satisfactory for the intended purpose. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Trained nurses can obtain satisfactory bone marrow aspirates and trephine biopsies.

PubMed Central

Lawson, S; Aston, S; Baker, L; Fegan, C D; Milligan, D W

1999-01-01

AIMS: To assess the feasibility of training nurse practitioners to perform bone marrow aspiration and trephine biopsy, and to compare the quality of these samples with those obtained by medical staff. METHODS: A retrospective audit was undertaken of nurse practitioner and medical staff performance in bone marrow procedures in a busy haematology day unit. RESULTS: Nurse practitioners fared favourably in comparison with medical staff in performing bone marrow trephine biopsies, with mean biopsy lengths of 11 mm and 10.7 mm respectively. However, only 78% of the smears obtained by the nurses were judged technically satisfactory, compared with 91% prepared by doctors. This discrepancy was thought to be due largely to the quality of slide spreading. CONCLUSIONS: With motivated staff and a structured educational and training programme it is possible for nurse practitioners to perform the techniques of bone marrow aspiration and biopsy, and obtain specimens of satisfactory quality, thus improving efficiency of the haematology day unit and increasing quality of patient care. Images PMID:10396248

Method validation using weighted linear regression models for quantification of UV filters in water samples.

PubMed

da Silva, Claudia Pereira; Emídio, Elissandro Soares; de Marchi, Mary Rosa Rodrigues

2015-01-01

This paper describes the validation of a method consisting of solid-phase extraction followed by gas chromatography-tandem mass spectrometry for the analysis of the ultraviolet (UV) filters benzophenone-3, ethylhexyl salicylate, ethylhexyl methoxycinnamate and octocrylene. The method validation criteria included evaluation of selectivity, analytical curve, trueness, precision, limits of detection and limits of quantification. The non-weighted linear regression model has traditionally been used for calibration, but it is not necessarily the optimal model in all cases. Because the assumption of homoscedasticity was not met for the analytical data in this work, a weighted least squares linear regression was used for the calibration method. The evaluated analytical parameters were satisfactory for the analytes and showed recoveries at four fortification levels between 62% and 107%, with relative standard deviations less than 14%. The detection limits ranged from 7.6 to 24.1 ng L(-1). The proposed method was used to determine the amount of UV filters in water samples from water treatment plants in Araraquara and Jau in São Paulo, Brazil. Copyright © 2014 Elsevier B.V. All rights reserved.

A micro-flow-batch analyzer with solenoid micro-pumps for the photometric determination of iodate in table salt.

PubMed

Lima, Marcelo B; Barreto, Inakã S; Andrade, Stéfani Iury E; Almeida, Luciano F; Araújo, Mário C U

2012-10-15

In this study, a micro-flow-batch analyzer (μFBA) with solenoid micro-pumps for the photometric determination of iodate in table salt is described. The method is based on the reaction of iodate with iodide to form molecular iodine followed by the reaction with N,N-diethyl-p-phenylenediamine (DPD). The analytical signal was measured at 520 nm using a green LED integrated into the μFBA built in the urethane-acrylate resin. The analytical curve for iodate was linear in the range of 0.01-10.0 mg L(-1) with a correlation coefficient of 0.997. The limit of detection and relative standard deviation were estimated at 0.004 mg L(-1) and<1.5% (n=3), respectively. The accuracy was assessed through recovery test (97.6-103.5%) and independent analysis by a conventional titrimetric method. Comparing this technique with the conventional method, no statistically significant differences were observed when applying the paired t-test at a 95% confidence level. The proposed microsystem using solenoid micro-pumps presented satisfactory robustness and high sampling rate (170 h(-1)), with a low reagents consumption and a low cost to build the device. The proposed microsystem is a new alternative for automatic determination of iodate in table salt, comparing satisfactory to the recently flow system. Copyright © 2012 Elsevier B.V. All rights reserved.

Concepts. The Journal of Defense Systems Acquisition Management. Summer 1981. Volume 4, Number 3.

DTIC Science & Technology

1981-01-01

Performance FREQUENCY POWER OUTPUT GIZMO MODEL 25 0-50 MHZ SATISFACTORY 50-125 MHZ UNSATISFACTORY ASTROMATICS MODEL C 0-50 MHZ SATISFACTORY 50-125 MHZ...MHZ) GIZMO ----- ASTROMATICS- NOTES: 1. Diagrams excellent for portraying precise technical relationships. 2. Diagrams are economical means of

Relationship Between Magnitude of Applied Spin Recovery Moment and Ensuing Number of Recovery Turns

NASA Technical Reports Server (NTRS)

Anglin, Ernie L.

1967-01-01

An analytical study has been made to investigate the relationship between the magnitude of the applied spin recovery moment and the ensuing number of turns made during recovery from a developed spin with a view toward determining how to interpolate or extrapolate spin recovery results with regard to determining the amount of control required for a satisfactory recovery. Five configurations were used which are considered to be representative of modern airplanes: a delta-wing fighter, a stub-wing research vehicle, a boostglide configuration, a supersonic trainer, and a sweptback-wing fighter. The results obtained indicate that there is a direct relationship between the magnitude of the applied spin recovery moments and the ensuing number of recovery turns made and that this relationship can be expressed in either simple multiplicative or exponential form. Either type of relationship was adequate for interpolating or extrapolating to predict turns required for recovery with satisfactory accuracy for configurations having relatively steady recovery motions. Any two recoveries from the same developed spin condition can be used as a basis for the predicted results provided these recoveries are obtained with the same ratio of recovery control deflections. No such predictive method can be expected to give satisfactory results for oscillatory recoveries.

An efficient analytical method for determination of S-phenylmercapturic acid in urine by HPLC fluorimetric detector to assessing benzene exposure.

PubMed

Mendes, Michele P Rocha; Silveira, Josianne Nicácio; Andre, Leiliane Coelho

2017-09-15

Benzene is an important occupational and environmental contaminant, naturally present in petroleum and as by-product in the steel industry. Toxicological studies showed pronounced myelotoxic action, causing leukemic and others blood cells disorders. Assessing of benzene exposure is performed by biomarkers as trans, trans-muconic acid (AttM) and S-phenylmercapturic acid (S-PMA) in urine. Due to specificity of S-PMA, this biomarker has been proposed to asses lower levels of benzene in air. The aim of this study was to validate an analytical method for the quantification of S-PMA by High-Performance Liquid Chromatography with fluorometric detector. The development of an analytical method of S-PMA in urine was carried out by solid phase extraction (SPE) using C-18 phase. The eluated were submitted to water bath at 75°C and nitrogen to analyte concentration, followed by alkaline hydrolysis and derivatization with monobromobimane. The chromatography conditions were reverse phase C-18 column (240mm, 4mm and 5μm) at 35°C; acetonitrile and 0.5% acetic acid (50:50) as mobile phase with a flow of 0.8mL/min. The limits of detection and quantification were 0.22μg/L and 0.68μg/L, respectively. The linearity was verified by simple linear regression, and the method exhibited good linearity in the range of 10-100μg/L. There was no matrix effect for S-PMA using concentrations of 40, 60, 80 and 100μg/L. The intra- and interassay precision showed coefficient of variation of less than 10% and the recovery ranged from 83.4 to 102.8% with an average of 94.4%. The stability of S-PMA in urine stored at -20°C was of seven weeks. The conclusion is that this method presents satisfactory results per their figures of merit. This proposed method for determining urinary S-PMA showed adequate sensitivity for assessment of occupational and environmental exposure to benzene using S-PMA as biomarker of exposure. Copyright © 2017 Elsevier B.V. All rights reserved.

What do you mean by "satisfactory"?

PubMed

Crebbin, W

2005-09-01

One of the difficulties in designing assessment for medical trainees has been defining what is meant by "satisfactory". Whilst a list of "unsatisfactory" and "outstanding" characteristics can be identified with very little difficulty, it is the middle ground that holds the challenge. This is especially true in the non-technical areas of medical practice, which have been brought into greater prominence since the development and publication of CanMEDS 2000. As part of that process, questions about what is meant by "satisfactory", "standards" and/or benchmarks, have been brought into sharper focus. Additional questions are being asked as to whether competencies must necessarily be equated with minimum expectations or if they can be set, in conjunction with standards, to situate required "satisfactory" performance at a level significantly above a minimal level. A search of current literature on competencies and assessment was carried out. From that analysis, it became evident that a definition of "satisfactory" in assessing competence is dependent upon the identification of underlying factors, including the kind of competence, the kind of knowledge, and the level of expertise required to match the standard of assessment. The varying definitions, expectations, and levels of "satisfactory" were mapped to illustrate a way to plot the level of "satisfactory" according to the task, the experience of the trainee, and the stage of training. This map also provides a method for developing shared understandings of the targeted level within the "satisfactory zone".

Overcoming the challenges of conventional dispersive liquid-liquid microextraction: analysis of THMs in chlorinated swimming pools.

PubMed

Faraji, Hakim; Helalizadeh, Masoumeh; Kordi, Mohammad Reza

2018-01-01

A rapid, simple, and sensitive approach to the analysis of trihalomethanes (THMs) in swimming pool water samples has been developed. The main goal of this study was to overcome or to improve the shortcomings of conventional dispersive liquid-liquid microextraction (DLLME) and to maximize the realization of green analytical chemistry principles. The method involves a simple vortex-assisted microextraction step, in the absence of the dispersive solvent, followed by salting-out effect for the elimination of the centrifugation step. A bell-shaped device and a solidifiable solvent were used to simplify the extraction solvent collection after phase separation. Optimization of the independent variables was performed by using chemometric methods in three steps. The method was statistically validated based on authentic guidance documents. The completion time for extraction was less than 8 min, and the limits of detection were in the range between 4 and 72 ng L -1 . Using this method, good linearity and precision were achieved. The results of THMs determination in different real samples showed that in some cases the concentration of total THMs was more than threshold values of THMs determined by accredited healthcare organizations. This method indicated satisfactory analytical figures of merit. Graphical Abstract A novel green microextraction technique for overcoming the challenges of conventional DLLME. The proposed procedure complies with the principles of green/sustainable analytical chemistry, comprising decreasing the sample size, making easy automation of the process, reducing organic waste, diminishing energy consumption, replacing toxic reagents with safer reagents, and enhancing operator safety.

Capillary-wave dynamics and interface structure modulation in binary Bose-Einstein condensate mixtures

NASA Astrophysics Data System (ADS)

Indekeu, Joseph O.; Van Thu, Nguyen; Lin, Chang-You; Phat, Tran Huu

2018-04-01

The localized low-energy interfacial excitations, or interfacial Nambu-Goldstone modes, of phase-segregated binary mixtures of Bose-Einstein condensates are investigated analytically. To this end a double-parabola approximation (DPA) is performed on the Lagrangian density in Gross-Pitaevskii theory for a system in a uniform potential. This DPA entails a model in which analytic expressions are obtained for the excitations underlying capillary waves or ripplons for arbitrary strength K (>1 ) of the phase segregation. The dispersion relation ω (k ) ∝k3 /2 is derived directly from the Bogoliubov-de Gennes equations in the limit that the wavelength 2 π /k is much larger than the interface width. The proportionality constant in the dispersion relation provides the static interfacial tension. A correction term in ω (k ) of order k5 /2 is calculated analytically within the DPA model. The combined result is tested against numerical diagonalization of the exact Bogoliubov-de Gennes equations. Satisfactory agreement is obtained in the range of physically relevant wavelengths. The ripplon dispersion relation is relevant to state-of-the-art experiments using (quasi)uniform optical-box traps. Furthermore, within the DPA model explicit expressions are obtained for the structural deformation of the interface due to the passing of the capillary wave. It is found that the amplitude of the wave is enhanced by an amount that is quadratic in the ratio of the phase velocity ω /k to the sound velocity c . For generic mixtures consisting of condensates with unequal healing lengths, an additional modulation is predicted of the common value of the condensate densities at the interface.

Simultaneous and confirmative detection of multi-residues of β₂-agonists and β-blockers in urine using LC-MS/MS/MS coupled with β-receptor molecular imprinted polymer SPE clean-up.

PubMed

Fan, S; Zou, J H; Miao, H; Zhao, Y F; Chen, H J; Zhao, R; Wu, Y N

2013-01-01

A liquid chromatography-linear ion-trap spectrometry (LC-MS³) method using β-receptor molecular-imprinted polymer (MIP) solid-phase extraction (SPE) as clean-up was developed to determine simultaneously and confirmatively residues of 25 β₂-agonists and 21 β-blockers in urine samples. Urine samples were subjected to enzymatic hydrolysis by β-glucoronidase/arylsulphatase, and then extracted with perchloric acid. Sample clean-up was performed using β-receptor MIP SPE. A Supelco Ascentis® express Rp-Amide column was used to separate the analytes, and MS³ detection used an electrospray ionisation source in positive-ion mode. Recovery studies were carried out using blank urine samples fortified with the 46 analytes at the levels of 0.5, 1.0 and 2.0 μg l⁻¹. Recoveries were obtained ranging from 60.1% to 109.9% with relative standard deviations (RSDs, n = 7) from 0.5% to 19.4%. The limits of detection (LODs) and limits of quantitation (LOQs) of the 46 analytes in urine were 0.02-0.18 and 0.05-0.60 μg l⁻¹, respectively. As a result of the selective clean-up by MIP SPE and MS³ detection of the target drugs, the sensitivity and accuracy of the present method was high enough for monitoring β₂-agonist and β-blocker residues in urine samples. Satisfactory results were obtained in the process of the determination of positive urine samples.

High-throughput multipesticides residue analysis in earthworms by the improvement of purification method: Development and application of magnetic Fe3 O4 -SiO2 nanoparticles based dispersive solid-phase extraction.

PubMed

Sun, Yuhan; Qi, Peipei; Cang, Tao; Wang, Zhiwei; Wang, Xiangyun; Yang, Xuewei; Wang, Lidong; Xu, Xiahong; Wang, Qiang; Wang, Xinquan; Zhao, Changshan

2018-06-01

As a key representative organism, earthworms can directly illustrate the influence of pesticides on environmental organisms in soil ecosystems. The present work aimed to develop a high-throughput multipesticides residue analytical method for earthworms using solid-liquid extraction with acetonitrile as the solvent and magnetic material-based dispersive solid-phase extraction for purification. Magnetic Fe 3 O 4 nanoparticles were modified with a thin silica layer to form Fe 3 O 4 -SiO 2 nanoparticles, which were fully characterized by field-emission scanning electron microscopy, transmission electron microscopy, Fourier-transform infrared spectroscopy, X-ray diffractometry, and vibrating sample magnetometry. The Fe 3 O 4 -SiO 2 nanoparticles were used as the separation media in dispersive solid-phase extraction with primary secondary amine and ZrO 2 as the cleanup adsorbents to eliminate matrix interferences. The amounts of nanoparticles and adsorbents were optimized for the simultaneous determination of 44 pesticides and six metabolites in earthworms by liquid chromatography with tandem mass spectrometry. The method performance was systematically validated with satisfactory results. The limits of quantification were 20 μg/kg for all analytes studied, while the recoveries of the target analytes ranged from 65.1 to 127% with relative standard deviation values lower than 15.0%. The developed method was subsequently utilized to explore the bioaccumulation of bitertanol in earthworms exposed to contaminated soil, verifying its feasibility for real sample analysis. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

On-line coupling of capillary isotachophoresis and zone electrophoresis for the assay of phenolic compounds in plant extracts.

PubMed

Urbánek, Marek; Pospísilová, Marie; Polásek, Miroslav

2002-04-01

The combination of capillary isotachophoresis (ITP) and capillary zone electrophoresis (CZE) in the column coupling configuration was optimized in a mode where the electrolyte for the CZE step is different from the leading and terminating ITP electrolytes. Two colored markers, picric acid and 1-nitroso-2-naphthol, were used for exact timing of the transfer of isotachophoretically stacked analyte zones into the CZE column and for the control of the residual amount of the leading and terminating ITP electrolytes entering the CZE capillary together with the analytes, thus controlling the duration of transient ITP migration in the CZE capillary and ensuring good separation of the analytes and reproducibility of the migration times (relative standard deviations 1%). ITP-CZE was applied to the simultaneous assay of several cinnamic acid derivatives and flavonoids in methanolic extracts of Sambucus flowers and Crataegus leaves and flowers. The preconcentrating and cleansing effect of the ITP step allowed injection of relatively large sample volumes (30 microL). The limits of detection were approximately 20-50 ng x mL(-1) and 100 ng x mL(-1) for the acids and flavonoids, respectively ( thick similar 200-times lower compared to conventional CE) with spectrophotometric detection at 254 nm. The ITP-CZE exhibited satisfactory linearity and precision when using CZE buffer of pseudo "pH" 9.0; 1-nitroso-2-naphthol was employed as the internal standard. The separation took approximately 35 min. The ITP-CZE results for rutin, hyperoside, and vitexin-2-O"-rhamnoside were in good accordance with those obtained previously by high-performance liquid chromatography.

Silicon carbide nanomaterial as a coating for solid-phase microextraction.

PubMed

Tian, Yu; Feng, Juanjuan; Wang, Xiuqin; Sun, Min; Luo, Chuannan

2018-01-26

Silicon carbide has excellent properties, such as corrosion resistance, high strength, oxidation resistance, high temperature, and so on. Based on these properties, silicon carbide was coated on stainless-steel wire and used as a solid-phase microextraction coating, and polycyclic aromatic hydrocarbons were employed as model analytes. Using gas chromatography, some important factors that affect the extraction efficiency were optimized one by one, and an analytical method was established. The analytical method showed wide linear ranges (0.1-30, 0.03-30, and 0.01-30 μg/L) with satisfactory correlation coefficients (0.9922-0.9966) and low detection limits (0.003-0.03 μg/L). To investigate the practical application of the method, rainwater and cigarette ash aqueous solution were collected as real samples for extraction and detection. The results indicate that silicon carbide has excellent application in the field of solid-phase microextraction. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Discrim: a computer program using an interactive approach to dissect a mixture of normal or lognormal distributions

USGS Publications Warehouse

Bridges, N.J.; McCammon, R.B.

1980-01-01

DISCRIM is an interactive computer graphics program that dissects mixtures of normal or lognormal distributions. The program was written in an effort to obtain a more satisfactory solution to the dissection problem than that offered by a graphical or numerical approach alone. It combines graphic and analytic techniques using a Tektronix1 terminal in a time-share computing environment. The main program and subroutines were written in the FORTRAN language. ?? 1980.

Analytical and experimental vibration studies of a 1/8-scale shuttle orbiter

NASA Technical Reports Server (NTRS)

Pinson, L. D.

1975-01-01

Natural frequencies and mode shapes for four symmetric vibration modes and four antisymmetric modes are compared with predictions based on NASTRAN finite-element analyses. Initial predictions gave poor agreement with test data; an extensive investigation revealed that the major factors influencing agreement were out-of-plane imperfections in fuselage panels and a soft fin-fuselage connection. Computations with a more refined analysis indicated satisfactory frequency predictions for all modes studied, within 11 percent of experimental values.

Quality control of the tribological coating PS212

NASA Technical Reports Server (NTRS)

Sliney, Harold E.; Dellacorte, Christopher; Deadmore, Daniel L.

1989-01-01

PS212 is a self-lubricating, composite coating that is applied by the plasma spray process. It is a functional lubricating coating from 25 C (or lower) to 900 C. The coating is prepared from a blend of three different powders with very dissimilar properties. Therefore, the final chemical composition and lubricating effectiveness of the coatings are very sensitive to the process variables used in their preparation. Defined here are the relevant variables. The process and analytical procedures that will result in satisfactory tribological coatings are discussed.

A simulation of streaming flows associated with acoustic levitators

NASA Astrophysics Data System (ADS)

Rednikov, A.; Riley, N.

2002-04-01

Steady-state acoustic streaming flow patterns have been observed by Trinh and Robey [Phys. Fluids 6, 3567 (1994)], during the operation of a variety of single axis ultrasonic levitators in a gaseous environment. Microstreaming around levitated samples is superimposed on the streaming flow which is observed in the levitator even in the absence of any particle therein. In this paper, by physical arguments, numerical and analytical simulations we provide entirely satisfactory interpretations of the observed flow patterns in both isothermal and nonisothermal situations.

Implementation of the qualities of radiodiagnostic: mammography

NASA Astrophysics Data System (ADS)

Pacífico, L. C.; Magalhães, L. A. G.; Peixoto, J. G. P.; Fernandes, E.

2018-03-01

The objective of the present study was to evaluate the expanded uncertainty of the mammographic calibration process and present the result of the internal audit performed at the Laboratory of Radiological Sciences (LCR). The qualities of the mammographic beans that are references in the LCR, comprises two irradiation conditions: no-attenuated beam and attenuated beam. Both had satisfactory results, with an expanded uncertainty equals 2,1%. The internal audit was performed, and the degree of accordance with the ISO/IEC 17025 was evaluated. The result of the internal audit was satisfactory. We conclude that LCR can perform calibrations on mammography qualities for end users.

Development of an integrated, zero-G pneumatic transporter/rotating-paddle incinerator/catalytic afterburner subsystem for processing human waste on board spacecraft

NASA Technical Reports Server (NTRS)

Fields, S. F.; Labak, L. J.; Honegger, R. J.

1974-01-01

A baseline laboratory prototype of an integrated, six man, zero-g subsystem for processing human wastes onboard spacecraft was investigated, and included the development of an operational specification for the baseline subsystem, followed by design and fabrication. The program was concluded by performing a series of six tests over a period of two weeks to evaluate the performance of the subsystem. The results of the tests were satisfactory, however, several changes in the design of the subsystem are required before completely satisfactory performance can be achieved.

Satisfactory visualization rates of standard cardiac views at 18 to 22 weeks' gestation using spatiotemporal image correlation.

PubMed

Cohen, Leeber; Mangers, Kristie; Grobman, William A; Platt, Lawrence D

2009-12-01

The purpose of this study was to determine the frequency with which 3 standard screening views of the fetal heart (4-chamber, left ventricular outflow tract [LVOT], and right ventricular outflow tract [RVOT]) can be obtained satisfactorily with the spatiotemporal image correlation (STIC) technique. A prospective study of 111 patients undergoing anatomic surveys at 18 to 22 weeks was performed. Two ultrasound machines with fetal cardiac settings were used. The best volume set that could be obtained from each patient during a 45-minute examination was graded by 2 sonologists with regard to whether the 4-chamber, LVOT, and RVOT images were satisfactory for screening. All 3 views were judged satisfactory for screening in most patients: 1 sonologist graded the views as satisfactory in 70% of the patients, whereas the other found the views to be satisfactory in 83%. The position of the placenta did not alter the probability of achieving a satisfactory view, but a fetus in the spine anterior position was associated with a significantly lower probability that the views were regarded as satisfactory for screening (odds ratio, 0.28; 95% confidence interval, 0.09-0.70; P < .05). This study suggests that STIC may assist with screening for cardiac anomalies at 18 to 22 weeks' gestation.

Novel analytical model for optimizing the pull-in voltage in a flexured MEMS switch incorporating beam perforation effect

NASA Astrophysics Data System (ADS)

Guha, K.; Laskar, N. M.; Gogoi, H. J.; Borah, A. K.; Baishnab, K. L.; Baishya, S.

2017-11-01

This paper presents a new method for the design, modelling and optimization of a uniform serpentine meander based MEMS shunt capacitive switch with perforation on upper beam. The new approach is proposed to improve the Pull-in Voltage performance in a MEMS switch. First a new analytical model of the Pull-in Voltage is proposed using the modified Mejis-Fokkema capacitance model taking care of the nonlinear electrostatic force, the fringing field effect due to beam thickness and etched holes on the beam simultaneously followed by the validation of same with the simulated results of benchmark full 3D FEM solver CoventorWare in a wide range of structural parameter variations. It shows a good agreement with the simulated results. Secondly, an optimization method is presented to determine the optimum configuration of switch for achieving minimum Pull-in voltage considering the proposed analytical mode as objective function. Some high performance Evolutionary Optimization Algorithms have been utilized to obtain the optimum dimensions with less computational cost and complexity. Upon comparing the applied algorithms between each other, the Dragonfly Algorithm is found to be most suitable in terms of minimum Pull-in voltage and higher convergence speed. Optimized values are validated against the simulated results of CoventorWare which shows a very satisfactory results with a small deviation of 0.223 V. In addition to these, the paper proposes, for the first time, a novel algorithmic approach for uniform arrangement of square holes in a given beam area of RF MEMS switch for perforation. The algorithm dynamically accommodates all the square holes within a given beam area such that the maximum space is utilized. This automated arrangement of perforation holes will further improve the computational complexity and design accuracy of the complex design of perforated MEMS switch.

Simultaneous determination of 12 pharmaceuticals in water samples by ultrasound-assisted dispersive liquid-liquid microextraction coupled with ultra-high performance liquid chromatography with tandem mass spectrometry.

PubMed

Guan, Jin; Zhang, Chi; Wang, Yang; Guo, Yiguang; Huang, Peiting; Zhao, Longshan

2016-11-01

A new analytical method was developed for simultaneous determination of 12 pharmaceuticals using ultrasound-assisted dispersive liquid-liquid microextraction (DLLME) followed by ultra-high performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS). Six nonsteroidal anti-inflammatory drugs (NSAIDs, ketoprofen, mefenamic acid, tolfenamic acid, naproxen, sulindac, and piroxicam) and six antibiotics (tinidazole, cefuroxime axetil, ciprofloxacin, sulfamethoxazole, sulfadiazine, and chloramphenicol) were extracted by ultrasound-assisted DLLME using dichloromethane (800 μL) and methanol/acetonitrile (1:1, v/v, 1200 μL) as the extraction and dispersive solvents, respectively. The factors affecting the extraction efficiency, such as the type and volume of extraction and dispersive solvent, vortex and ultrasonic time, sample pH, and ionic strength, were optimized. The ultrasound-assisted process was applied to accelerate the formation of the fine cloudy solution by using a small volume of dispersive solvent, which increased the extraction efficiency and reduced the equilibrium time. Under the optimal conditions, the calibration curves showed good linearity in the range of 0.04-20 ng mL -1 (ciprofloxacin and sulfadiazine), 0.2-100 ng mL -1 (ketoprofen, tinidazole, cefuroxime axetil, naproxen, sulfamethoxazole, and sulindac), and 1-200 ng mL -1 (mefenamic acid, tolfenamic acid, piroxicam, and chloramphenicol). The LODs and LOQs of the method were in the range of 0.006-0.091 and 0.018-0.281 ng mL -1 , respectively. The relative recoveries of the target analytes were in the range from 76.77 to 99.97 % with RSDs between 1.6 and 8.8 %. The developed method was successfully applied to the extraction and analysis of 12 pharmaceuticals in five kinds of water samples (drinking water, running water, river water, influent and effluent wastewater) with satisfactory results. Graphical Abstract Twelve pharmaceuticals in water samples analyted by UHPLC-MS/MS using ultrasound-assisted DLLME.

Amplitude inversion of the 2D analytic signal of magnetic anomalies through the differential evolution algorithm

NASA Astrophysics Data System (ADS)

Ekinci, Yunus Levent; Özyalın, Şenol; Sındırgı, Petek; Balkaya, Çağlayan; Göktürkler, Gökhan

2017-12-01

In this work, analytic signal amplitude (ASA) inversion of total field magnetic anomalies has been achieved by differential evolution (DE) which is a population-based evolutionary metaheuristic algorithm. Using an elitist strategy, the applicability and effectiveness of the proposed inversion algorithm have been evaluated through the anomalies due to both hypothetical model bodies and real isolated geological structures. Some parameter tuning studies relying mainly on choosing the optimum control parameters of the algorithm have also been performed to enhance the performance of the proposed metaheuristic. Since ASAs of magnetic anomalies are independent of both ambient field direction and the direction of magnetization of the causative sources in a two-dimensional (2D) case, inversions of synthetic noise-free and noisy single model anomalies have produced satisfactory solutions showing the practical applicability of the algorithm. Moreover, hypothetical studies using multiple model bodies have clearly showed that the DE algorithm is able to cope with complicated anomalies and some interferences from neighbouring sources. The proposed algorithm has then been used to invert small- (120 m) and large-scale (40 km) magnetic profile anomalies of an iron deposit (Kesikköprü-Bala, Turkey) and a deep-seated magnetized structure (Sea of Marmara, Turkey), respectively to determine depths, geometries and exact origins of the source bodies. Inversion studies have yielded geologically reasonable solutions which are also in good accordance with the results of normalized full gradient and Euler deconvolution techniques. Thus, we propose the use of DE not only for the amplitude inversion of 2D analytical signals of magnetic profile anomalies having induced or remanent magnetization effects but also the low-dimensional data inversions in geophysics. A part of this paper was presented as an abstract at the 2nd International Conference on Civil and Environmental Engineering, 8-10 May 2017, Cappadocia-Nevşehir (Turkey).

Determination of triazine herbicides in fresh vegetables by dynamic microwave-assisted extraction coupled with homogeneous ionic liquid microextraction high performance liquid chromatography.

PubMed

Wu, Lijie; Hu, Mingzhu; Li, Zhanchao; Song, Ying; Yu, Cui; Zhang, Yupu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

2015-02-01

A novel extraction method, dynamic microwave-assisted extraction coupled with homogeneous ionic liquid microextraction, was developed for the determination of triazine herbicides, including desmetryn, terbumeton, propazine, terbuthylazine, dimethametryn, and dipropetryn in fresh vegetable samples by high performance liquid chromatography (HPLC). In the developed method, 120 μL of 1-butyl-3-methylimidazolium tetrafluoroborate ([C4MIM][BF4]) was added to 10 mL of aqueous solution containing 0.3 g of NaCl to obtained the extraction solvent. Six triazines could be extracted completely within 4 min by the present method. Then, [NH4][PF6] was added into the extract to form a water-insoluble ionic liquid [C4MIM][PF6] via a simple metathesis reaction, and the analytes were enriched into the ionic liquid phase. After centrifugation and dilution with acetonitrile, the resulting solution was analyzed directly by HPLC. The effects of some experimental parameters, including type and volume of ionic liquid, volume of extraction solvent, amount of ion-pairing agent [NH4][PF6], salt concentration, microwave power, and flow rate of extraction solvent on the extraction efficiency were investigated and optimized. Under the optimum experimental conditions, the linearity for determining the analytes was in the range of 2.50-250.00 μg kg(-1), with the correlation coefficients ranging from 0.9989 to 0.9999. When the present method was applied to the analysis of vegetable samples, satisfactory recoveries were obtained in the range of 76.8%-106.9%, and relative standard deviations were lower than 9.8%.

Analysis of multi-class preservatives in leave-on and rinse-off cosmetics by matrix solid-phase dispersion.

PubMed

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

2011-12-01

Matrix solid-phase extraction has been successfully applied for the determination of multi-class preservatives in a wide variety of cosmetic samples including rinse-off and leave-on products. After extraction, derivatization with acetic anhydride, and gas chromatography-mass spectrometry analysis were performed. Optimization studies were done on real non-spiked and spiked leave-on and rinse-off cosmetic samples. The selection of the most suitable extraction conditions was made using statistical tools such as ANOVA, as well as factorial experimental designs. The final optimized conditions were common for both groups of cosmetics and included the dispersion of the sample with Florisil (1:4), and the elution of the MSPD column with 5 mL of hexane/acetone (1:1). After derivatization, the extract was analyzed without any further clean-up or concentration step. Accuracy, precision, linearity and detection limits were evaluated to assess the performance of the proposed method. The recovery studies on leave-on and rinse-off cosmetics gave satisfactory values (>78% for all analytes in all the samples) with an average relative standard deviation value of 4.2%. The quantification limits were well below those set by the international cosmetic regulations, making this multi-component analytical method suitable for routine control. The analysis of a broad range of cosmetics including body milk, moisturizing creams, anti-stretch marks creams, hand creams, deodorant, shampoos, liquid soaps, makeup, sun milk, hand soaps, among others, demonstrated the high use of most of the target preservatives, especially butylated hydroxytoluene, methylparaben, propylparaben, and butylparaben.

A comprehensive and sensitive method for hair analysis in drug-facilitated crimes and incorporation of zolazepam and tiletamine into hair after a single exposure.

PubMed

Kim, Jihyun; Yum, Hyesun; Jang, Moonhee; Shin, Ilchung; Yang, Wonkyung; Baeck, Seungkyung; Suh, Joon Hyuk; Lee, Sooyeun; Han, Sang Beom

2016-01-01

Hair is a highly relevant specimen that is used to verify drug exposure in victims of drug-facilitated crime (DFC) cases. In the present study, a new analytical method involving ultrahigh-performance liquid chromatography-tandem mass spectrometry was developed for determining the presence of model drugs, including zolazepam and tiletamine and their metabolites in hair specimens from DFCs. The incorporation of zolazepam and tiletamine into hair after a single exposure was investigated in Long-Evans rats with the ratio of the hair concentration to the area under the curve. For rapid and simple sample preparation, methanol extraction and protein precipitation were performed for hair and plasma, respectively. No interference was observed in drug-free hair or plasma, except for hair-derived diphenhydramine in blank hair. The coefficients of variance of the matrix effects were below 12%, and the recoveries of the analytes exceeded 70% in all of the matrices. The precision and accuracy results were satisfactory. The limits of quantification ranged from 20 to 50 pg in 10 mg of hair. The drug incorporation rates were 0.03 ± 0.01% for zolazepam and 2.09 ± 0.51% for tiletamine in pigmented hair. We applied the present method to real hair samples in order to determine the drug that was used in seven cases. These results suggest that this comprehensive and sensitive hair analysis method can successfully verify a drug after a single exposure in crimes and can be applied in forensic and clinical toxicology laboratories.

High‐throughput automated scoring of Ki67 in breast cancer tissue microarrays from the Breast Cancer Association Consortium

PubMed Central

Howat, William J; Daley, Frances; Zabaglo, Lila; McDuffus, Leigh‐Anne; Blows, Fiona; Coulson, Penny; Raza Ali, H; Benitez, Javier; Milne, Roger; Brenner, Herman; Stegmaier, Christa; Mannermaa, Arto; Chang‐Claude, Jenny; Rudolph, Anja; Sinn, Peter; Couch, Fergus J; Tollenaar, Rob A.E.M.; Devilee, Peter; Figueroa, Jonine; Sherman, Mark E; Lissowska, Jolanta; Hewitt, Stephen; Eccles, Diana; Hooning, Maartje J; Hollestelle, Antoinette; WM Martens, John; HM van Deurzen, Carolien; Investigators, kConFab; Bolla, Manjeet K; Wang, Qin; Jones, Michael; Schoemaker, Minouk; Broeks, Annegien; van Leeuwen, Flora E; Van't Veer, Laura; Swerdlow, Anthony J; Orr, Nick; Dowsett, Mitch; Easton, Douglas; Schmidt, Marjanka K; Pharoah, Paul D; Garcia‐Closas, Montserrat

2016-01-01

Abstract Automated methods are needed to facilitate high‐throughput and reproducible scoring of Ki67 and other markers in breast cancer tissue microarrays (TMAs) in large‐scale studies. To address this need, we developed an automated protocol for Ki67 scoring and evaluated its performance in studies from the Breast Cancer Association Consortium. We utilized 166 TMAs containing 16,953 tumour cores representing 9,059 breast cancer cases, from 13 studies, with information on other clinical and pathological characteristics. TMAs were stained for Ki67 using standard immunohistochemical procedures, and scanned and digitized using the Ariol system. An automated algorithm was developed for the scoring of Ki67, and scores were compared to computer assisted visual (CAV) scores in a subset of 15 TMAs in a training set. We also assessed the correlation between automated Ki67 scores and other clinical and pathological characteristics. Overall, we observed good discriminatory accuracy (AUC = 85%) and good agreement (kappa = 0.64) between the automated and CAV scoring methods in the training set. The performance of the automated method varied by TMA (kappa range= 0.37–0.87) and study (kappa range = 0.39–0.69). The automated method performed better in satisfactory cores (kappa = 0.68) than suboptimal (kappa = 0.51) cores (p‐value for comparison = 0.005); and among cores with higher total nuclei counted by the machine (4,000–4,500 cells: kappa = 0.78) than those with lower counts (50–500 cells: kappa = 0.41; p‐value = 0.010). Among the 9,059 cases in this study, the correlations between automated Ki67 and clinical and pathological characteristics were found to be in the expected directions. Our findings indicate that automated scoring of Ki67 can be an efficient method to obtain good quality data across large numbers of TMAs from multicentre studies. However, robust algorithm development and rigorous pre‐ and post‐analytical quality control procedures are necessary in order to ensure satisfactory performance. PMID:27499923

Separation of enantiomers of new psychoactive substances by high-performance liquid chromatography.

PubMed

Kadkhodaei, Kian; Forcher, Lisa; Schmid, Martin G

2018-03-01

New psychoactive substances are defined as compounds with consciousness-changing effects and have been developed simultaneously with classical drugs. They arise through structural modifications of illegal substances and are mainly produced to circumvent laws. Availability is simple, since new psychoactive substances can be purchased from the Internet. Among them many chemical drug compound classes are chiral and thus the two resulting enantiomers can differ in their effects. The aim of this study is to develop a suitable chiral high-performance liquid chromatography separation method for a broad spectrum of new psychoactive substances using cellulose tris(3,5-dichlorophenylcarbamate) as a chiral selector. Experiments were performed by high-performance liquid chromatography in normal-phase mode under isocratic conditions using ultraviolet detection. Direct separation was carried out on a high-performance liquid chromatography column (Lux® i-Cellulose-5, 3.5 μm, Phenomenex®), available since 2016. Excellent separation results were obtained for cathinones. After further optimization, even 47 instead of 39 out of 52 cathinones showed baseline separation. For amphetamine derivatives, satisfactory results were not achieved. Further, new psychoactive substances from other compound classes such as benzofuranes, thiophenes, phenidines, phenidates, morpholines, and ketamines were partially resolved, depending on the polarity and degree of substitution. All analytes, which were mainly purchased from the Internet, were proven to be traded as racemates. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Boundary Electron and Beta Dosimetry-Quantification of the Effects of Dissimilar Media on Absorbed Dose

NASA Astrophysics Data System (ADS)

Nunes, Josane C.

1991-02-01

This work quantifies the changes effected in electron absorbed dose to a soft-tissue equivalent medium when part of this medium is replaced by a material that is not soft -tissue equivalent. That is, heterogeneous dosimetry is addressed. Radionuclides which emit beta particles are the electron sources of primary interest. They are used in brachytherapy and in nuclear medicine: for example, beta -ray applicators made with strontium-90 are employed in certain ophthalmic treatments and iodine-131 is used to test thyroid function. More recent medical procedures under development and which involve beta radionuclides include radioimmunotherapy and radiation synovectomy; the first is a cancer modality and the second deals with the treatment of rheumatoid arthritis. In addition, the possibility of skin surface contamination exists whenever there is handling of radioactive material. Determination of absorbed doses in the examples of the preceding paragraph requires considering boundaries of interfaces. Whilst the Monte Carlo method can be applied to boundary calculations, for routine work such as in clinical situations, or in other circumstances where doses need to be determined quickly, analytical dosimetry would be invaluable. Unfortunately, few analytical methods for boundary beta dosimetry exist. Furthermore, the accuracy of results from both Monte Carlo and analytical methods has to be assessed. Although restricted to one radionuclide, phosphorus -32, the experimental data obtained in this work serve several purposes, one of which is to provide standards against which calculated results can be tested. The experimental data also contribute to the relatively sparse set of published boundary dosimetry data. At the same time, they may be useful in developing analytical boundary dosimetry methodology. The first application of the experimental data is demonstrated. Results from two Monte Carlo codes and two analytical methods, which were developed elsewhere, are compared with experimental data. Monte Carlo results compare satisfactory with experimental results for the boundaries considered. The agreement with experimental results for air interfaces is of particular interest because of discrepancies reported previously by another investigator who used data obtained from a different experimental technique. Results from one of the analytical methods differ significantly from the experimental data obtained here. The second analytical method provided data which approximate experimental results to within 30%. This is encouraging but it remains to be determined whether this method performs equally well for other source energies.

Three modified activated carbons by different ligands for the solid phase extraction of copper and lead.

PubMed

Ghaedi, M; Ahmadi, F; Tavakoli, Z; Montazerozohori, M; Khanmohammadi, A; Soylak, M

2008-04-15

In the presented work, 5,5-diphenylimidazolidine-2,4-dione (phenytoin) (DFTD), 5,5-diphenylimidazolidine-2-thione-,4-one (thiophenytoin) (DFID) and 2-(4'-methoxy-benzylidenimine) thiophenole (MBIP) modified activated carbons have been used for the solid phase extraction of copper and lead ions prior to their flame atomic absorption spectrometric determinations. The influences of the various analytical parameters including pH, amounts of reagent, sample volume and eluent type, etc. on the recovery efficiencies of copper and lead ions were investigated. The influences of alkaline, earth alkaline and some transition metals on the adsorption of the analytes were also examined. The detection limits by three sigma for analyte ions were 0.65 and 0.42 microg L(-1) using activated carbon modified with DFID; 0.52 and 0.37 microg L(-1) using activated carbon modified with DFTD and 0.46 and 0.31 microg L(-1) using activated carbon modified with MBIP for Pb(II) and Cu(II), respectively. The procedure was applied to the determination of analytes in natural waters, soil, and blood samples with satisfactory results (recoveries greater than 95%, R.S.D.'s lower than 4%).

Chip-based nanoflow high performance liquid chromatography coupled to mass spectrometry for profiling of soybean flavonoids.

PubMed

Chang, Yuwei; Zhao, Chunxia; Wu, Zeming; Zhou, Jia; Zhao, Sumin; Lu, Xin; Xu, Guowang

2012-08-01

In this work a chip-based nano HPLC coupled MS (HPLC-chip/MS) method with a simple sample preparation procedure was developed for the flavonoid profiling of soybean. The analytical properties of the method including the linearity (R(2) , 0.992-0.995), reproducibility (RSD, 1.50-7.66%), intraday precision (RSD, 1.41-5.14%) and interday precision (RSD, 2.76-16.90%) were satisfactory. Compared with the conventional HPLC/MS method, a fast extraction and analysis procedure was applied and more flavonoids were detected in a single run. Additionally, 13 flavonoids in soybean seed were identified for the first time. The method was then applied to the profiling of six varieties of soybean sowed at the same place. A clear discrimination was observed among different cultivars, three isoflavones, accounting for nearly 80% of total flavonoid contents, were found increased in the spring soybeans compared with the summer cultivars. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Evaluation of a Liquid Amine System for Spacecraft Carbon Dioxide Control

NASA Technical Reports Server (NTRS)

Breaux, D. K.; Friedel, P.; Hwang, K. C.; Probert, G.; Ruder, J. M.; Sawamura, L.

1974-01-01

The analytical and experimental studies are described which were directed toward the acquisition of basic information on utilizing a liquid amine sorbent for in use in a CO2 removal system for manned spacecraft. Liquid amine systems are successfully used on submarines for control of CO2 generated by the crew, but liquid amines were not previously considered for spacecraft applications due to lack of development of satisfactory rotary phase separators. Developments in this area now make consideration of liquid amines practical for spacecraft system CO2 removal. The following major tasks were performed to evaluate liquid amine systems for spacecraft: (1) characterization, through testing, of the basic physical and thermodynamic properties of the amine solution; (2) determination of the dynamic characteristics of a cocurrent flow absorber; and (3) evaluation, synthesis, and selection of a liquid amine system concept oriented toward low power requirements. A low weight, low power system concept was developed. Numerical and graphical data are accompanied by pertinent observations.

HPLC-PDA Combined with Chemometrics for Quantitation of Active Components and Quality Assessment of Raw and Processed Fruits of Xanthium strumarium L.

PubMed

Jiang, Hai; Yang, Liu; Xing, Xudong; Yan, Meiling; Guo, Xinyue; Yang, Bingyou; Wang, Qiuhong; Kuang, Haixue

2018-01-25

As a valuable herbal medicine, the fruits of Xanthium strumarium L. (Xanthii Fructus) have been widely used in raw and processed forms to achieve different therapeutic effects in practice. In this study, a comprehensive strategy was proposed for evaluating the active components in 30 batches of raw and processed Xanthii Fructus (RXF and PXF) samples, based on high-performance liquid chromatography coupled with photodiode array detection (HPLC-PDA). Twelve common peaks were detected and eight compounds of caffeoylquinic acids were simultaneously quantified in RXF and PXF. All the analytes were detected with satisfactory linearity (R² > 0.9991) over wide concentration ranges. Simultaneously, the chemically latent information was revealed by hierarchical cluster analysis (HCA) and principal component analysis (PCA). The results suggest that there were significant differences between RXF and PXF from different regions in terms of the content of eight caffeoylquinic acids. Potential chemical markers for XF were found during processing by chemometrics.

Microwave-assisted Derivatization of Fatty Acids for Its Measurement in Milk Using High-Performance Liquid Chromatography.

PubMed

Shrestha, Rojeet; Miura, Yusuke; Hirano, Ken-Ichi; Chen, Zhen; Okabe, Hiroaki; Chiba, Hitoshi; Hui, Shu-Ping

2018-01-01

Fatty acid (FA) profiling of milk has important applications in human health and nutrition. Conventional methods for the saponification and derivatization of FA are time-consuming and laborious. We aimed to develop a simple, rapid, and economical method for the determination of FA in milk. We applied a beneficial approach of microwave-assisted saponification (MAS) of milk fats and microwave-assisted derivatization (MAD) of FA to its hydrazides, integrated with HPLC-based analysis. The optimal conditions for MAS and MAD were determined. Microwave irradiation significantly reduced the sample preparation time from 80 min in the conventional method to less than 3 min. We used three internal standards for the measurement of short-, medium- and long-chain FA. The proposed method showed satisfactory analytical sensitivity, recovery and reproducibility. There was a significant correlation in the milk FA concentrations between the proposed and conventional methods. Being quick, economic, and convenient, the proposed method for the milk FA measurement can be substitute for the convention method.

Multivariate longitudinal data analysis with censored and intermittent missing responses.

PubMed

Lin, Tsung-I; Lachos, Victor H; Wang, Wan-Lun

2018-05-08

The multivariate linear mixed model (MLMM) has emerged as an important analytical tool for longitudinal data with multiple outcomes. However, the analysis of multivariate longitudinal data could be complicated by the presence of censored measurements because of a detection limit of the assay in combination with unavoidable missing values arising when subjects miss some of their scheduled visits intermittently. This paper presents a generalization of the MLMM approach, called the MLMM-CM, for a joint analysis of the multivariate longitudinal data with censored and intermittent missing responses. A computationally feasible expectation maximization-based procedure is developed to carry out maximum likelihood estimation within the MLMM-CM framework. Moreover, the asymptotic standard errors of fixed effects are explicitly obtained via the information-based method. We illustrate our methodology by using simulated data and a case study from an AIDS clinical trial. Experimental results reveal that the proposed method is able to provide more satisfactory performance as compared with the traditional MLMM approach. Copyright © 2018 John Wiley & Sons, Ltd.

Simultaneous Determination of Isopyrazam and Azoxystrobin in Cucumbers by Liquid Chromatography-Tandem Mass Spectrometry.

PubMed

Hu, Dan; Xu, Xu; Cai, Tian; Wang, Wei-Ying; Wu, Chun-Jie; Ye, Li-Ming

2017-12-01

A rapid and sensitive analytical method based on high-performance liquid chromatography-tandem mass spectrometry was developed and validated for the determination of isopyrazam (IZM) and azoxystrobin (AZT) in cucumbers. A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was used as the pretreatment procedure. The samples were extracted with acetonitrile and cleaned up with octadecylsilyl silica (C18) and graphite carbon black. The proposed method resulted in satisfactory recovery of IZM and AZT (91.48 to 114.62%), and relative standard deviations were less than 13.1% at fortification concentrations of 1, 20, and 500 μg kg -1 (n = 3). The limits of quantification for IZM and AZT were 0.498 and 0.499 μg kg -1 , respectively, which are far below the maximum residue level (0.5 mg kg -1 ) established for this type of sample. Matrix effects were also evaluated. This study established a sensitive and fast method for the detection of IZM and AZT in cucumber samples.

Sol-gel titania-coated needles for solid phase dynamic extraction-GC/MS analysis of desomorphine and desocodeine.

PubMed

Su, Chi-Ju; Srimurugan, Sankarewaran; Chen, Chinpiao; Shu, Hun-Chi

2011-01-01

Novel sol-gel titania film coated needles for solid-phase dynamic extraction (SPDE)-GC/MS analysis of desomorphine and desocodeine are described. The high thermal stability of titania film permits efficient extraction and analysis of poorly volatile opiate drugs. The influences of sol-gel reaction time, coating layer, extraction and desorption time and temperature on the SPDE needle performance were investigated. The deuterium labeled internal standard was introduced either during the extraction of analyte or directly injected to GC after the extraction process. The latter method was shown to be more sensitive for the analysis of water and urine samples containing opiate drugs. The proposed conditions provided a wide linear range (from 5-5000 ppb), and satisfactory linearity, with R(2) values from 0.9958 to 0.9999, and prominent sensitivity, LOQs (1.0-5.0 ng/g). The sol-gel titania film coated needle with SPDE-GC/MS will be a promising technique for desomorphine and desocodeine analysis in urine.

Results achieved by emergency physicians in teaching basic cardiopulmonary resuscitation to secondary school students.

PubMed

Jiménez-Fábrega, Xavier; Escalada-Roig, Xavier; Sánchez, Miquel; Culla, Alexandre; Díaz, Núria; Gómez, Xavier; Villena, Olga; Rodríguez, Esther; Gaspar, Alberto; Molina, José Emilio; Salvador, Jordi; Miró, Oscar

2009-06-01

We investigated the results obtained with a basic cardiopulmonary resuscitation (b-CPR) program (PROCES) specifically designed for secondary school students (14-16 years old) and taught by emergency physicians. We used a multiple-choice test with 20 questions (10 on theory and 10 on skills) answered before and immediately after and 1 year after receiving the b-CPR course. Satisfactory learning was considered when at least 8 out of 10 skill questions were correctly answered. We investigated student variables associated with better immediate and deferred (1 year after) PROCES performance. We compared the results with those obtained using a more standardized program to teach b-CPR to police cadets. We enrolled 600 high school students. PROCES achieved significant improvement in overall, theory and skill marks immediately after the course (P<0.001), with a significant decay in all of them 1 year after the course (P<0.001). Satisfactory learning was achieved by 57% of school students immediately after PROCES and by 37% when assessed 1 year later. Students without pending study subjects (P=0.001) and those from private schools (P<0.01) achieved significantly better performance immediately after PROCES and only female students achieved greater performance 1 year after the course (P<0.05). With respect to police cadets instructed through a standardized course, immediate satisfactory learning of school students was lower (79 vs. 57%, respectively; P<0.001), whereas deferred satisfactory learning was higher (23 vs. 37%, respectively; P<0.05). Emergency physicians can satisfactorily instruct secondary school students in b-CPR using PROCES, and this specific program achieves a reasonable amount of satisfactory learning.

Electrocatalytic oxidation and determination of insulin at nickel oxide nanoparticles-multiwalled carbon nanotube modified screen printed electrode.

PubMed

Rafiee, Banafsheh; Fakhari, Ali Reza

2013-08-15

Nickel oxide nanoparticles modified nafion-multiwalled carbon nanotubes screen printed electrode (NiONPs/Nafion-MWCNTs/SPE) were prepared using pulsed electrodeposition of NiONPs on the MWCNTs/SPE surface. The size, distribution and structure of the NiONPs/Nafion-MWCNTs were characterized by transmission electron microscopy (TEM) and x-ray diffraction (XRD) and also the results show that NiO nanoparticles were homogeneously electrodeposited on the surfaces of MWCNTs. Also, the electrochemical behavior of NiONPs/Nafion-MWCNTs composites in aqueous alkaline solutions of insulin was studied by cyclic voltammetry, chronoamperometry and electrochemical impedance spectroscopy (EIS). It was found that the prepared nanoparticles have excellent electrocatalytic activity towards insulin oxidation due to special properties of NiO nanoparticles. Cyclic voltammetric studies showed that the NiONPs/Nafion-MWCNTs film modified SPE, lowers the overpotentials and improves electrochemical behavior of insulin oxidation, as compared to the bare SPE. Amperometry was also used to evaluate the analytical performance of modified electrode in the quantitation of insulin. Excellent analytical features, including high sensitivity (1.83 μA/μM), low detection limit (6.1 nM) and satisfactory dynamic range (20.0-260.0 nM), were achieved under optimized conditions. Moreover, these sensors show good repeatability and a high stability after a while or successive potential cycling. Copyright © 2013 Elsevier B.V. All rights reserved.

Carbon molecular sieve based micro-matrix-solid-phase dispersion for the extraction of polyphenols in pomegranate peel by UHPLC-Q-TOF/MS.

PubMed

Du, Li-Jing; Huang, Jian-Ping; Wang, Bin; Wang, Chen-Hui; Wang, Qiu-Yan; Hu, Yu-Han; Yi, Ling; Cao, Jun; Peng, Li-Qing; Chen, Yu-Bo; Zhang, Qi-Dong

2018-06-04

A rapid, simple and efficient sample extraction method based on micro-matrix-solid-phase dispersion (micro-MSPD) was applied to the extraction of polyphenols from pomegranate peel. Five target analytes were determined by ultra-high-performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry. Carbon molecular sieve (CMS) was firstly used as dispersant to improve extraction efficiency in micro-MSPD. The major micro-MSPD parameters, such as type of dispersant, amount of dispersant, grinding time and the type and the volume of elution solvents, were studied and optimized. Under optimized conditions, 26 mg of pomegranate peel was dispersed with 32.5 mg of CMS, the grinding time was selected as 90 s, the dispersed sample was eluted with 100 μL of methanol. Results showed that the proposed method was of good linearity for concentrations of analytes against their peak areas (coefficient of determination r 2 >0.990), the limit of the detection was as low as 3.2 ng/mL, and the spiking recoveries were between 88.1% and 106%. Satisfactory results were obtained for the extraction of gallic acid, punicalagin A, punicalagin B, catechin and ellagic acid from pomegranate peel sample, which demonstrated nice reliability and high sensitivity of this approach. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Preparation, characterization and application of a reversed phase liquid chromatography/hydrophilic interaction chromatography mixed-mode C18-DTT stationary phase.

PubMed

Wang, Qing; Long, Yao; Yao, Lin; Xu, Li; Shi, Zhi-Guo; Xu, Lanying

2016-01-01

A mixed-mode chromatographic stationary phase, C18-DTT (dithiothreitol) silica (SiO2) was prepared through "thiol-ene" click chemistry. The obtained material was characterized by fourier transform infrared spectroscope, nitrogen adsorption analysis and contact angle analysis. Chromatographic performance of the C18-DTT was systemically evaluated by studying the effect of acetonitrile content, pH, buffer concentration of the mobile phase and column temperature. It was demonstrated that the novel stationary phase possessed reversed phase liquid chromatography (RPLC)/hydrophilic interaction liquid chromatography (HILIC) mixed-mode property. The stop-flow test revealed that C18-DTT exhibited excellent compatibility with 100% aqueous mobile phase. Additionally, the stability and column-to-column reproducibility of the C18-DTT material were satisfactory, with relative standard deviations of retention factor of the tested analytes (verapamil, fenbufen, guanine, tetrandrine and nicotinic acid) in the range of 1.82-3.72% and 0.85-1.93%, respectively. Finally, the application of C18-DTT column was demonstrated in the separation of non-steroidal anti-inflammatory drugs, aromatic carboxylic acids, alkaloids, nucleo-analytes and polycyclic aromatic hydrocarbons. It had great resolving power in the analysis of various compounds in HILIC and RPLC chromatographic conditions and was a promising RPLC/HILIC mixed-mode stationary phase. Copyright © 2015 Elsevier B.V. All rights reserved.

Development of a quantitative multi-compound method for the detection of 14 nitrogen-rich adulterants by LC-MS/MS in food materials.

PubMed

Frank, Nancy; Bessaire, Thomas; Tarres, Adrienne; Goyon, Alexandre; Delatour, Thierry

2017-11-01

The increasing number of food frauds using exogenous nitrogen-rich adulterants to artificially raise the protein content for economically motivated adulteration has demonstrated the need for a robust analytical methodology. This method should be applicable for quality control in operations covering a wide range of analyte concentrations to be able to analyse high levels as usually found in adulteration, as well as low levels due to contamination. The paper describes a LC-MS/MS method covering 14 nitrogen-rich adulterants using a simple and fast sample preparation based on dilution and clean-up by dispersive SPE. Quantification is carried out by isotopic dilution reaching LOQs of 0.05-0.20 mg/kg in a broad range of food matrices (infant formula, liquid milk, dairy ingredient, high protein meal, cereal, infant cereal, and meat/fish powder). Validation of seven commodity groups was performed according to SANCO 12571/2013, giving satisfactory results demonstrating the method's fitness for purpose at the validated range at contamination level. Method ruggedness was further assessed by transferring the developed method into another laboratory devoted to routine testing for quality control. Next to the method description, emphasis is placed on challenges and problems appearing during method development as well as validation. They are discussed in detail and solutions are provided.

Simultaneous determination of eight active components in Houttuynia cordata injection and its quality control in productive process.

PubMed

Ji, Wei; Bi, Kaishun; Chen, Qianqian; Jiang, Lingyan; Liang, Ke; Li, Qing

2011-11-01

A simple, reliable and effective gas chromatography coupled with flame ionization detection method was developed for the simultaneous determination of eight components (α-pinene, β-pinene, myrcene, limonene, terpinen-4-ol, α-terpineol, bornyl acetate and methyl-n-nonylketone) in Chinese medicine Houttuynia cordata and its injection. The chromatographic separation of all eight components, including undecylene as internal standard was performed on a DB-1 column (30 m×0.25 mm, 0.25 μm). Excellent linear behaviors including herb and injection over the investigated concentration ranges were observed with the values of r(2) higher than 0.9990 for all analytes. Satisfactory intra-day and inter-day precisions were achieved with RSD less than 2% and the average recoveries for all analytes at three different concentrations obtained were in the range of 93.4-104.4%, with RSD ranging from 1.3 to 4.1%. The proposed method was successfully applied in the simultaneous determination of these active components in H. cordata and H. cordata injection (HCI), including the intermediate product of HCI in productive process, from different pharmaceutical factories and different production batches, indicating that the method in this paper was particularly suitable for the routine analysis of HCI and its quality control in productive process. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A Sensitive Dilute-and-Shoot Approach for the Simultaneous Screening of 71 Stimulants and 7 Metabolites in Human Urine by LC-MS-MS with Dynamic MRM.

PubMed

Dong, Ying; Yan, Kuan; Ma, Yanhua; Wang, Shan; He, Genye; Deng, Jing; Yang, Zhiyong

2015-10-01

A novel, reliable and sensitive liquid chromatography-tandem mass spectrometry (LC-MS-MS) method was developed with dynamic multiple reaction monitoring (dMRM) mode for the simultaneous screening of 71 stimulants and 7 metabolites in human urine using unsophisticated MS instruments (Agilent triple-quadruple 6410 B mass spectrometer). With a known retention time of an analyte, dMRM algorithm monitors each MRM transition only around its expected retention time. Therefore, dMRM enables the maximization of dwell times and provides much higher sensitivity and reproducibility than the conventional multiple reaction monitoring mode (cMRM). After precipitation of protein, the urine sample was injected into LC-MS-MS system directly without sample pre-concentration. For comparison, cMRM and dMRM acquisitions were performed under the same chromatographic conditions. The result showed that the signal response and quality of the chromatograms for each stimulant improved significantly with dMRM over cMRM. The method has been fully validated giving limits of detection (0.1-25 ng/mL) satisfactory for its application to anti-doping analysis. The repeatability of the concentrations and the retention times are good both for intra- and for inter-day experiments (%CV of concentrations always <20 and %CV of retention times <0.5). The method also afforded satisfactory results in terms of accuracy, matrix effect and specificity. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Determination of Ochratoxin A in Rye and Rye-Based Products by Fluorescence Polarization Immunoassay

PubMed Central

Lippolis, Vincenzo; Porricelli, Anna C. R.; Cortese, Marina; Zanardi, Sandro; Pascale, Michelangelo

2017-01-01

A rapid fluorescence polarization immunoassay (FPIA) was optimized and validated for the determination of ochratoxin A (OTA) in rye and rye crispbread. Samples were extracted with a mixture of acetonitrile/water (60:40, v/v) and purified by SPE-aminopropyl column clean-up before performing the FPIA. Overall mean recoveries were 86 and 95% for spiked rye and rye crispbread with relative standard deviations lower than 6%. Limits of detection (LOD) of the optimized FPIA was 0.6 μg/kg for rye and rye crispbread, respectively. Good correlations (r > 0.977) were observed between OTA contents in contaminated samples obtained by FPIA and high-performance liquid chromatography (HPLC) with immunoaffinity cleanup used as reference method. Furthermore, single laboratory validation and small-scale collaborative trials were carried out for the determination of OTA in rye according to Regulation 519/2014/EU laying down procedures for the validation of screening methods. The precision profile of the method, cut-off level and rate of false suspect results confirm the satisfactory analytical performances of assay as a screening method. These findings show that the optimized FPIA is suitable for high-throughput screening, and permits reliable quantitative determination of OTA in rye and rye crispbread at levels that fall below the EU regulatory limits. PMID:28954398

Nontargeted Screening Method for Illegal Additives Based on Ultrahigh-Performance Liquid Chromatography-High-Resolution Mass Spectrometry.

PubMed

Fu, Yanqing; Zhou, Zhihui; Kong, Hongwei; Lu, Xin; Zhao, Xinjie; Chen, Yihui; Chen, Jia; Wu, Zeming; Xu, Zhiliang; Zhao, Chunxia; Xu, Guowang

2016-09-06

Identification of illegal additives in complex matrixes is important in the food safety field. In this study a nontargeted screening strategy was developed to find illegal additives based on ultrahigh-performance liquid chromatography-high-resolution mass spectrometry (UHPLC-HRMS). First, an analytical method for possible illegal additives in complex matrixes was established including fast sample pretreatment, accurate UHPLC separation, and HRMS detection. Second, efficient data processing and differential analysis workflow were suggested and applied to find potential risk compounds. Third, structure elucidation of risk compounds was performed by (1) searching online databases [Metlin and the Human Metabolome Database (HMDB)] and an in-house database which was established at the above-defined conditions of UHPLC-HRMS analysis and contains information on retention time, mass spectra (MS), and tandem mass spectra (MS/MS) of 475 illegal additives, (2) analyzing fragment ions, and (3) referring to fragmentation rules. Fish was taken as an example to show the usefulness of the nontargeted screening strategy, and six additives were found in suspected fish samples. Quantitative analysis was further carried out to determine the contents of these compounds. The satisfactory application of this strategy in fish samples means that it can also be used in the screening of illegal additives in other kinds of food samples.

A design of spectrophotometric microfluidic chip sensor for analyzing silicate in seawater

NASA Astrophysics Data System (ADS)

Cao, X.; Zhang, S. W.; Chu, D. Z.; Wu, N.; Ma, H. K.; Liu, Y.

2017-08-01

High quality and continuous in situ silicate data are required to investigate the mechanism of the biogeochemical cycles and the formation of red tide. There is an urgently growing need for autonomous in situ silicate instruments that perform determination on various platforms. However, due to the high reagents and power consumption, as well as high system complexity leading to low reliability and robustness, the performance of the commercially available silicate sensors is not satisfactory. With these problems, here we present a new generation of microfluidic continuous flow analysis silicate sensor with sufficient analytical performance and robustness, for in situ determination of soluble silicate in seawater. The reaction mechanism of this sensor is based on the reaction of silicate with ammonium molybdate to form a yellow silicomolybdate complex and further reduction to silicomoIybdenum blue by ascorbic acid. The minimum limit of detection was 45.1 nmol L-1, and the linear determination range of the sensor is 0-400 μmol L-1. The recovery rate of the actual water is between 98.1%-104.0%, and the analyzing cycle of the sensor is about 5 minutes. This sensor has the advantages of high accuracy, high integration, low water consumption, and strong anti-interference ability. It has been successfully applied to measuring the silicate in seawater in Jiaozhou Bay.

Porous organic polymers with different pore structures for sensitive solid-phase microextraction of environmental organic pollutants.

PubMed

Huang, Zhoubing; Liu, Shuqin; Xu, Jianqiao; Yin, Li; Zheng, Juan; Zhou, Ningbo; Ouyang, Gangfeng

2017-10-09

Adsorption capacity is the major sensitivity-limited factor in solid-phase microextraction. Due to its light-weight properties, large specific surface area and high porosity, especially tunable pore structures, the utilization of porous organic polymers as solid-phase microextraction adsorbents has attracting researchers' attentions. However, these works mostly concentrated on the utilization of specific porous organic polymers for preparing high-performance solid-phase microextraction coatings. The relationship between pore structures and adsorption performance of the porous organic polymers still remain unclear. Herein, three porous organic polymers with similar properties but different pore distributions were prepared by condensation polymerization reaction of phloroglucinol and terephthalaldehyde, which were fabricated as solid-phase microextraction coatings subsequently. The adsorption capacity of the porous organic polymers-coated fibers were evaluated by using benzene and its derivatives (i.e.,benzene, toluene, ethylbenzene and m-xylene) and polycyclic aromatic hydrocarbons as the target analytes. The results showed that the different adsorption performance of these porous organic polymers was mainly caused by their different pore volumes instead of their surface areas or pore sizes. Finally, the proposed method by using the mesoporous organic polymer coating was successfully applied to the determination of benzene and its derivatives in environmental water samples. As for analytical performance, high pre-concentration factors (74-2984), satisfactory relative recoveries (94.5 ± 18.5-116.9 ± 12.5%), intraday precision (2.44-5.34%), inter-day precision (4.62-7.02%), low limit of detections (LODs, 0.10-0.29 ng L -1 ) and limit of quantifications (LOQs, 0.33-0.96 ng L -1 ) were achieved under the optimal conditions. This study provides an important idea in the rational design of porous organic polymers for solid-phase microextraction or other adsorption applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Simultaneous determination of antidementia drugs in human plasma: procedure transfer from HPLC-MS to UPLC-MS/MS.

PubMed

Noetzli, Muriel; Ansermot, Nicolas; Dobrinas, Maria; Eap, Chin B

2012-05-01

A previously developed high performance liquid chromatography mass spectrometry (HPLC-MS) procedure for the simultaneous determination of antidementia drugs, including donepezil, galantamine, memantine, rivastigmine and its metabolite NAP 226-90, was transferred to an ultra performance liquid chromatography system coupled to a tandem mass spectrometer (UPLC-MS/MS). The drugs and their internal standards ([(2)H(7)]-donepezil, [(13)C,(2)H(3)]-galantamine, [(13)C(2),(2)H(6)]-memantine, [(2)H(6)]-rivastigmine) were extracted from 250 μL human plasma by protein precipitation with acetonitrile. Chromatographic separation was achieved on a reverse phase column (BEH C18 2.1 mm × 50 mm; 1.7 μm) with a gradient elution of an ammonium acetate buffer at pH 9.3 and acetonitrile at a flow rate of 0.4 mL/min and an overall run time of 4.5 min. The analytes were detected on a tandem quadrupole mass spectrometer operated in positive electrospray ionization mode, and quantification was performed using multiple reaction monitoring. The method was validated according to the recommendations of international guidelines over a calibration range of 1-300 ng/mL for donepezil, galantamine and memantine, and 0.2-50 ng/mL for rivastimgine and NAP 226-90. The trueness (86-108%), repeatability (0.8-8.3%), intermediate precision (2.3-10.9%) and selectivity of the method were found to be satisfactory. Matrix effects variability was inferior to 15% for the analytes and inferior to 5% after correction by internal standards. A method comparison was performed with patients' samples showing similar results between the HPLC-MS and UPLC-MS/MS procedures. Thus, this validated UPLC-MS/MS method allows to reduce the required amount of plasma, to use a simplified sample preparation, and to obtain a higher sensitivity and specificity with a much shortened run-time. Copyright © 2012 Elsevier B.V. All rights reserved.

Neural Network and Regression Methods Demonstrated in the Design Optimization of a Subsonic Aircraft

NASA Technical Reports Server (NTRS)

Hopkins, Dale A.; Lavelle, Thomas M.; Patnaik, Surya

2003-01-01

The neural network and regression methods of NASA Glenn Research Center s COMETBOARDS design optimization testbed were used to generate approximate analysis and design models for a subsonic aircraft operating at Mach 0.85 cruise speed. The analytical model is defined by nine design variables: wing aspect ratio, engine thrust, wing area, sweep angle, chord-thickness ratio, turbine temperature, pressure ratio, bypass ratio, fan pressure; and eight response parameters: weight, landing velocity, takeoff and landing field lengths, approach thrust, overall efficiency, and compressor pressure and temperature. The variables were adjusted to optimally balance the engines to the airframe. The solution strategy included a sensitivity model and the soft analysis model. Researchers generated the sensitivity model by training the approximators to predict an optimum design. The trained neural network predicted all response variables, within 5-percent error. This was reduced to 1 percent by the regression method. The soft analysis model was developed to replace aircraft analysis as the reanalyzer in design optimization. Soft models have been generated for a neural network method, a regression method, and a hybrid method obtained by combining the approximators. The performance of the models is graphed for aircraft weight versus thrust as well as for wing area and turbine temperature. The regression method followed the analytical solution with little error. The neural network exhibited 5-percent maximum error over all parameters. Performance of the hybrid method was intermediate in comparison to the individual approximators. Error in the response variable is smaller than that shown in the figure because of a distortion scale factor. The overall performance of the approximators was considered to be satisfactory because aircraft analysis with NASA Langley Research Center s FLOPS (Flight Optimization System) code is a synthesis of diverse disciplines: weight estimation, aerodynamic analysis, engine cycle analysis, propulsion data interpolation, mission performance, airfield length for landing and takeoff, noise footprint, and others.

Stir bar sorptive extraction with EG-Silicone coating for bisphenols determination in personal care products by GC-MS.

PubMed

Cacho, Juan Ignacio; Campillo, Natalia; Viñas, Pilar; Hernández-Córdoba, Manuel

2013-05-05

An easy to perform analytical method for the determination of three bisphenol compounds (BPs) in commonly used personal care products (PCPs) is presented. Ethylene glycol-silicone (EG-Silicone) coated stir bars, which have recently become commercially available, are evaluated in this study for the simultaneous determination of bisphenol A (BPA), bisphenol F (BPF) and bisphenol Z (BPZ) by stir bar sorptive extraction (SBSE) in combination with thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). This new sorptive extraction phase allows the analysis of these compounds without any previous derivatization procedure. Different parameters affecting both SBSE extraction and thermal desorption were carefully optimized, using experimental designs based on the Taguchi orthogonal arrays. The procedure was applied to analyzing easily bought PCPs, providing detection limits of about 8 ng g(-1), with precisions lower than 11% in terms of relative standard deviation. Recovery studies performed at two different concentration levels provided satisfactory values for all the compounds. The analyzed personal care samples contained BPA at concentration levels ranging from 30.9 to 88.3 ng g(-1). Copyright © 2013 Elsevier B.V. All rights reserved.

Graphene-sensitized microporous membrane/solvent microextraction for the preconcentration of cinnamic acid derivatives in Rhizoma Typhonii.

PubMed

Xing, Rongrong; Hu, Shuang; Chen, Xuan; Bai, Xiaohong

2014-09-01

A novel graphene-sensitized microporous membrane/solvent microextraction method named microporous membrane/graphene/solvent synergistic microextraction, coupled with high-performance liquid chromatography and UV detection, was developed and introduced for the extraction and determination of three cinnamic acid derivatives in Rhizoma Typhonii. Several factors affecting performance were investigated and optimized, including the types of graphene and extraction solvent, concentration of graphene dispersed in octanol, sample phase pH, ionic strength, stirring rate, extraction time, extraction temperature, and sample volume. Under optimized conditions, the enrichment factors of cinnamic acid derivatives ranged from 75 to 269. Good linearities were obtained from 0.01 to 10 μg/mL for all analytes with regression coefficients between 0.9927 and 0.9994. The limits of quantification were <1 ng/mL, and satisfactory recoveries (99-104%) and precision (1.1-10.8%) were also achieved. The synergistic microextraction mechanism based on graphene sensitization was analyzed and described. The experimental results showed that the method was simple, sensitive, practical, and effective for the preconcentration and determination of cinnamic acid derivatives in Rhizoma Typhonii. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of hexavalent chromium in traditional Chinese medicines by high-performance liquid chromatography with inductively coupled plasma mass spectrometry.

PubMed

Li, Peng; Li, Li-Min; Xia, Jing; Cao, Shuai; Hu, Xin; Lian, Hong-Zhen; Ji, Shen

2015-12-01

An analytical method that combined high-performance liquid chromatography with inductively coupled plasma mass spectrometry has been developed for the determination of hexavalent chromium in traditional Chinese medicines. Hexavalent chromium was extracted using the alkaline solution. The parameters such as the concentration of alkaline and the extraction temperature have been optimized to minimize the interconversion between trivalent chromium and hexavalent chromium. The extracted hexavalent chromium was separated on a weak anion exchange column in isocratic mode, followed by inductively coupled plasma mass spectrometry determination. To obtain a better chromatographic resolution and sensitivity, 75 mM NH4 NO3 at pH 7 was selected as the mobile phase. The linearity of the proposed method was investigated in the range of 0.2-5.0 μg L(-1) (r(2) = 0.9999) for hexavalent chromium. The limits of detection and quantitation are 0.1 and 0.3 μg L(-1) , respectively. The developed method was successfully applied to the determination of hexavalent chromium in Chloriti lapis and Lumbricus with satisfactory recoveries of 95.8-112.8%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Reactive control of subsonic axial fan noise in a duct.

PubMed

Liu, Y; Choy, Y S; Huang, L; Cheng, L

2014-10-01

Suppressing the ducted fan noise at low frequencies without varying the flow capacity is still a technical challenge. This study examines a conceived device consisting of two tensioned membranes backed with cavities housing the axial fan for suppression of the sound radiation from the axial fan directly. The noise suppression is achieved by destructive interference between the sound fields from the axial fan of a dipole nature and sound radiation from the membrane via vibroacoustics coupling. A two-dimensional model with the flow effect is presented which allows the performance of the device to be explored analytically. The air flow influences the symmetrical behavior and excites the odd in vacuo mode response of the membrane due to kinematic coupling. Such an asymmetrical effect can be compromised with off-center alignment of the axial fan. Tension plays an important role to sustain the performance to revoke the deformation of the membrane during the axial fan operation. With the design of four appropriately tensioned membranes covered by a cylindrical cavity, the first and second blade passage frequencies of the axial fan can be reduced by at least 20 dB. The satisfactory agreement between experiment and theory demonstrates that its feasibility is practical.

Two-dimensional preparative liquid chromatography system for preparative separation of minor amount components from complicated natural products.

PubMed

Qiu, Ying-Kun; Chen, Fang-Fang; Zhang, Ling-Ling; Yan, Xia; Chen, Lin; Fang, Mei-Juan; Wu, Zhen

2014-04-11

An on-line comprehensive two-dimensional preparative liquid chromatography system was developed for preparative separation of minor amount components from complicated natural products. Medium-pressure liquid chromatograph (MPLC) was applied as the first dimension and preparative HPLC as the second one, in conjunction with trapping column and makeup pump. The performance of the trapping column was evaluated, in terms of column size, dilution ratio and diameter-height ratio, as well as system pressure from the view of medium pressure liquid chromatograph. Satisfactory trapping efficiency can be achieved using a commercially available 15 mm × 30 mm i.d. ODS pre-column. The instrument operation and the performance of this MPLC×preparative HPLC system were illustrated by gram-scale isolation of crude macro-porous resin enriched water extract of Rheum hotaoense. Automated multi-step preparative separation of 25 compounds, whose structures were identified by MS, (1)H NMR and even by less-sensitive (13)C NMR, could be achieved in a short period of time using this system, exhibiting great advantages in analytical efficiency and sample treatment capacity compared with conventional methods. Copyright © 2014 Elsevier B.V. All rights reserved.

High-performance liquid chromatography of quinoidal imminium compounds derived from triphenylmethanes

USGS Publications Warehouse

Abidi, S.L.

1983-01-01

A series of eleven p-aminotriphenylmethane dyes have been studied by high-performance liquid chromatography (HPLC). The combined use of HPLC and spectrophotometry permits specific detection of these compounds in the visible range around 600 nm. As the high affinity of the imminium cations for the active sites of the hydrocarbonaceous stationary phase has presented difficulties for reversed-phase HPLC with pure solvents, organic electrolytes were added to the mobile phase to facilitate the elution of the components with improved selectivity, sensitivity (minimum detection limit, 0.1 μg/ml), and peak symmetry. The effects of chromatographic variables on the component retentivity were investigated. Retention times of the dye analytes decreased with increasing concentration of the added ionic reagent and with decreasing number of the hydrophobic alkyl substituents on the nitrogen atom. The influence of pH on the retention parameters appears to parallel that observed previously for cationic quaternary ammonium compounds. Among the acidic reagents employed, naphthalenesulfonic acid yielded the most satisfactory results. The use of binary electrolyte systems invariably improved the chromatographic behavior of the imminium solutes analyzed. Results obtained with two different octadecylsilica columns have been compared.

Design of an iterative auto-tuning algorithm for a fuzzy PID controller

NASA Astrophysics Data System (ADS)

Saeed, Bakhtiar I.; Mehrdadi, B.

2012-05-01

Since the first application of fuzzy logic in the field of control engineering, it has been extensively employed in controlling a wide range of applications. The human knowledge on controlling complex and non-linear processes can be incorporated into a controller in the form of linguistic terms. However, with the lack of analytical design study it is becoming more difficult to auto-tune controller parameters. Fuzzy logic controller has several parameters that can be adjusted, such as: membership functions, rule-base and scaling gains. Furthermore, it is not always easy to find the relation between the type of membership functions or rule-base and the controller performance. This study proposes a new systematic auto-tuning algorithm to fine tune fuzzy logic controller gains. A fuzzy PID controller is proposed and applied to several second order systems. The relationship between the closed-loop response and the controller parameters is analysed to devise an auto-tuning method. The results show that the proposed method is highly effective and produces zero overshoot with enhanced transient response. In addition, the robustness of the controller is investigated in the case of parameter changes and the results show a satisfactory performance.

Characteristics of Patients With Satisfactory Functional Gain Following Total Joint Arthroplasty in a Postacute Rehabilitation Setting.

PubMed

Hershkovitz, Avital; Vesilkov, Marina; Beloosesky, Yichayaou; Brill, Shai

2017-01-10

Total joint arthroplasty (TJA) is an effective and successful treatment of osteoarthritis of the hip and knee as quantified by several measures, such as pain relief, improved walking, improved self-care, functions, and increased quality of life. Data are lacking as to the definition of a satisfactory functional gain in a postacute setting and identifying the characteristics of older patients with TJA who may achieve that gain. Our aim was to characterize patients who may achieve a satisfactory functional gain in a postacute rehabilitation setting following TJA. This was a retrospective study of 180 patients with TJA admitted during 2010-2013. The main outcome measures were the Functional Independence Measure (FIM), the Montebello Rehabilitation Factor Score (MRFS) on the motor FIM, and the Timed Get Up and Go Test. Satisfactory functional gain was defined as an mFIM MRFS score above median score. Comparisons of clinical and demographic characteristics between patients who achieved a satisfactory functional gain versus those who did not were performed by the Mann-Whitney U test and the χ test. The proportion of patients who achieved a satisfactory functional gain was similar in the total knee arthroplasty and total hip arthroplasty (THA) groups. The most significant characteristic of patients who achieved a satisfactory functional gain was their admission functional ability. Age negatively impacted the ability to achieve a satisfactory functional gain in patients with THA. Functional level on admission is the best predictive factor for a better rehabilitation outcome for patients with TJA. Age negatively affects functional gain in patients with THA.

Analysis of potential genotoxic impurities in rabeprazole active pharmaceutical ingredient via Liquid Chromatography-tandem Mass Spectrometry, following quality-by-design principles for method development.

PubMed

Iliou, Katerina; Malenović, Anđelija; Loukas, Yannis L; Dotsikas, Yannis

2018-02-05

A novel Liquid Chromatography-tandem mass spectrometry (LC-MS/MS) method is presented for the quantitative determination of two potential genotoxic impurities (PGIs) in rabeprazole active pharmaceutical ingredient (API). In order to overcome the analytical challenges in the trace analysis of PGIs, a development procedure supported by Quality-by-Design (QbD) principles was evaluated. The efficient separation between rabeprazole and the two PGIs in the shortest analysis time was set as the defined analytical target profile (ATP) and to this purpose utilization of a switching valve allowed the flow to be sent to waste when rabeprazole was eluted. The selected critical quality attributes (CQAs) were the separation criterion s between the critical peak pair and the capacity factor k of the last eluted compound. The effect of the following critical process parameters (CPPs) on the CQAs was studied: %ACN content, the pH and the concentration of the buffer salt in the mobile phase, as well as the stationary phase of the analytical column. D-Optimal design was implemented to set the plan of experiments with UV detector. In order to define the design space, Monte Carlo simulations with 5000 iterations were performed. Acceptance criteria were met for C 8 column (50×4mm, 5μm) , and the region having probability π≥95% to achieve satisfactory values of all defined CQAs was computed. The working point was selected with the mobile phase consisting ‎of ACN, ammonium formate 11mM at a ratio 31/69v/v with pH=6,8 for the water phase. The LC protocol was transferred to LC-MS/MS and validated according to ICH guidelines. Copyright © 2017 Elsevier B.V. All rights reserved.

Strength analysis and design of adhesive joints between circular elements made of metal and reinforced polymer materials

NASA Astrophysics Data System (ADS)

Pelekh, B. L.; Marchuk, M. V.; Kogut, I. S.

1992-06-01

The stress-strain state of an adhesive joint between cylindrical components made of a metal (steel) and a cross-reinforced filament-wound composite (glass/polymer or basalt/polymer) was investigated under static axial loading using newly proposed experimental techniques and a refined mathematical model. Analytical expressions are obtained for contact stresses in the adhesive joint. The maximum permissible load and the ultimate shear strength of the joint are determined. The experimental results are found to be in satisfactory agreement with model predictions.

Analytical investigation of the dynamics of tethered constellations in Earth orbit, phase 2

NASA Technical Reports Server (NTRS)

Lorenzini, E. C.; Arnold, D. A.; Grossi, M. D.; Gullahorn, G. E.

1986-01-01

The g-tuning maneuvers of a 3-mass, vertical tethered system are considered. In particular, the case of reaching a zero-g acceleration level on board the middle mass from a non-zero initial condition is analyzed. A control law that provides a satisfactory transient response is derived. The constellation dynamics in the case of the middle mass travelling from one tether tip to the other is also investigated. Instabilities that take place at the end of the maneuver are analyzed and accommodated by devising suitable damping algorithms.

Quantum Kibble-Zurek Mechanism in a Spin-1 Bose-Einstein Condensate

NASA Astrophysics Data System (ADS)

Anquez, M.; Robbins, B. A.; Bharath, H. M.; Boguslawski, M.; Hoang, T. M.; Chapman, M. S.

2016-04-01

The dynamics of a quantum phase transition are explored using slow quenches from the polar to the broken-axisymmetry phases in a small spin-1 ferromagnetic Bose-Einstein condensate. Measurements of the evolution of the spin populations reveal a power-law scaling of the temporal onset of excitations versus quench speed as predicted from quantum extensions of the Kibble-Zurek mechanism. The satisfactory agreement of the measured scaling exponent with the analytical theory and numerical simulations provides experimental confirmation of the quantum Kibble-Zurek model.

Proceedings of the ARO Workshop on Analytical and Computational Issues in Logistics R & D Held at George Washington University, Washington, DC on 7-9 May 1984. Volume 2

DTIC Science & Technology

1984-12-01

with more gene - ral arrival process or service-time distribution, with attention restricted to critical-number policies, have been studied by Adler...points of their respective intervals. This method proved quite satisfactory for df’s that possess no sharp peaks or severe skewness. The method is...then (animal is carnivore))) (rule id6 (if (animal has pointed teeth ) (animal has claws) (animal has forward eyes)) (then (animal is carnivore

Simultaneous LC-MS/MS determination of 40 legal and illegal psychoactive drugs in breast and bovine milk.

PubMed

López-García, Ester; Mastroianni, Nicola; Postigo, Cristina; Valcárcel, Yolanda; González-Alonso, Silvia; Barceló, Damia; López de Alda, Miren

2018-04-15

This work presents a fast, sensitive and reliable multi-residue methodology based on fat and protein precipitation and liquid chromatography-tandem mass spectrometry for the determination of common legal and illegal psychoactive drugs, and major metabolites, in breast milk. One-fourth of the 40 target analytes is investigated for the first time in this biological matrix. The method was validated in breast milk and also in various types of bovine milk, as tranquilizers are occasionally administered to food-producing animals. Absolute recoveries were satisfactory for 75% of the target analytes. The use of isotopically labeled compounds assisted in correcting analyte losses due to ionization suppression matrix effects (higher in whole milk than in the other investigated milk matrices) and ensured the reliability of the results. Average method limits of quantification ranged between 0.4 and 6.8 ng/mL. Application of the developed method showed the presence of caffeine in breast milk samples (12-179 ng/mL). Copyright © 2017 Elsevier Ltd. All rights reserved.

Precise determination of N-acetylcysteine in pharmaceuticals by microchip electrophoresis.

PubMed

Rudašová, Marína; Masár, Marián

2016-01-01

A novel microchip electrophoresis method for the rapid and high-precision determination of N-acetylcysteine, a pharmaceutically active ingredient, in mucolytics has been developed. Isotachophoresis separations were carried out at pH 6.0 on a microchip with conductivity detection. The methods of external calibration and internal standard were used to evaluate the results. The internal standard method effectively eliminated variations in various working parameters, mainly run-to-run fluctuations of an injected volume. The repeatability and accuracy of N-acetylcysteine determination in all mucolytic preparations tested (Solmucol 90 and 200, and ACC Long 600) were more than satisfactory with the relative standard deviation and relative error values <0.7 and <1.9%, respectively. A recovery range of 99-101% of N-acetylcysteine in the analyzed pharmaceuticals predetermines the proposed method for accurate analysis as well. This work, in general, indicates analytical possibilities of microchip isotachophoresis for the quantitative analysis of simplified samples such as pharmaceuticals that contain the analyte(s) at relatively high concentrations. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparison of the acetyl bromide spectrophotometric method with other analytical lignin methods for determining lignin concentration in forage samples.

PubMed

Fukushima, Romualdo S; Hatfield, Ronald D

2004-06-16

Present analytical methods to quantify lignin in herbaceous plants are not totally satisfactory. A spectrophotometric method, acetyl bromide soluble lignin (ABSL), has been employed to determine lignin concentration in a range of plant materials. In this work, lignin extracted with acidic dioxane was used to develop standard curves and to calculate the derived linear regression equation (slope equals absorptivity value or extinction coefficient) for determining the lignin concentration of respective cell wall samples. This procedure yielded lignin values that were different from those obtained with Klason lignin, acid detergent acid insoluble lignin, or permanganate lignin procedures. Correlations with in vitro dry matter or cell wall digestibility of samples were highest with data from the spectrophotometric technique. The ABSL method employing as standard lignin extracted with acidic dioxane has the potential to be employed as an analytical method to determine lignin concentration in a range of forage materials. It may be useful in developing a quick and easy method to predict in vitro digestibility on the basis of the total lignin content of a sample.

Simultaneous determination of multiresidual phenyl acetanilide pesticides in different food commodities by solid-phase cleanup and gas chromatography-mass spectrometry.

PubMed

Li, Yongjun; Wang, Meiling; Yan, Hongfei; Fu, Shanliang; Dai, Hua

2013-03-01

An efficient and sensitive multiresidue method has been developed for quantification and confirmation of 25 phenyl acetanilide pesticides in a wide variety of food commodities including maize, spinach, mushroom, apple, soybean, chestnut, tea, beef, cattle liver, chicken, fish, and milk. Analytes were extracted with acetone-n-hexane (1:2, v/v) followed by cleanup using SPE. Several types of adsorbents were evaluated. Neutral aluminum and graphitized carbon black cartridge showed good cleanup efficiency. The extract was determined by GC-MS in the selected ion monitoring mode using one target and two qualitative ions for each analyte. The limits of detection were 0.01 mg/kg for all analytes. The average recoveries ranged from 66.9 to 110.6% (mean 88.8%) and RSDs were in the range 2.0-19% (mean 10.5%) across three fortification levels. The proposed method was successfully applied to real samples in routine analysis and a satisfactory result was obtained. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development of a hydrophilic interaction liquid chromatography-mass spectrometry method for detection and quantification of urea thermal decomposition by-products in emission from diesel engine employing selective catalytic reduction technology.

PubMed

Yassine, Mahmoud M; Dabek-Zlotorzynska, Ewa; Celo, Valbona

2012-03-16

The use of urea based selective catalytic reduction (SCR) technology for the reduction of NOx from the exhaust of diesel-powered vehicles has the potential to emit at least six thermal decomposition by-products, ammonia, and unreacted urea from the tailpipe. These compounds may include: biuret, dicyandiamine, cyanuric acid, ammelide, ammeline and melamine. In the present study, a simple, sensitive and reliable hydrophilic interaction liquid chromatography (HILIC)-electrospray ionization (ESI)/mass spectrometry (MS) method without complex sample pre-treatment was developed for identification and determination of urea decomposition by-products in diesel exhaust. Gradient separation was performed on a SeQuant ZIC-HILIC column with a highly polar zwitterionic stationary phase, and using a mobile phase consisting of acetonitrile (eluent A) and 15 mM ammonium formate (pH 6; eluent B). Detection and quantification were performed using a quadrupole ESI/MS operated simultaneously in negative and positive mode. With 10 μL injection volume, LODs for all target analytes were in the range of 0.2-3 μg/L. The method showed a good inter-day precision of retention time (RSD<0.5%) and peak area (RSD<3%). Satisfactory extraction recoveries from spiked blanks ranged between 96 and 98%. Analyses of samples collected during transient chassis dynamometer tests of a bus engine equipped with a diesel particulate filter (DPF) and urea based SCR technology showed the presence of five target analytes with cyanuric acid and ammelide the most abundant compounds in the exhaust. Crown Copyright © 2012. Published by Elsevier B.V. All rights reserved.

Improved sample preparation and rapid UHPLC analysis of SO2 binding carbonyls in wine by derivatisation to 2,4-dinitrophenylhydrazine.

PubMed

Jackowetz, J N; Mira de Orduña, R

2013-08-15

Sulphur dioxide (SO2) is essential for the preservation of wines. The presence of SO2 binding compounds in musts and wines may limit sulphite efficacy leading to higher total SO2 additions, which may exceed SO2 limits permitted by law and pose health risks for sensitive individuals. An improved method for the quantification of significant wine SO2 binding compounds is presented that applies a novel sample treatment approach and rapid UHPLC separation. Glucose, galacturonic acid, alpha-ketoglutarate, pyruvate, acetoin and acetaldehyde were derivatised with 2,4-dinitrophenylhydrazine and separated using a solid core C18 phase by ultra high performance liquid chromatography. Addition of EDTA to samples prevented de novo acetaldehyde formation from ethanol oxidation. Optimised derivatisation duration enhanced reproducibility and allowed for glucose and galacturonic acid quantification. High glucose residues were found to interfere with the recovery of other SO2 binders, but practical SO2 concentrations and red wine pigments did not affect derivatisation efficiency. The calibration range, method accuracy, precision and limits of detection were found to be satisfactory for routine analysis of SO2 binders in wines. The current method represents a significant improvement in the comprehensive analysis of SO2 binding wine carbonyls. It allows for the quantification of major SO2 binders at practical analyte concentrations, and uses a simple sample treatment method that prevents treatment artifacts. Equipment utilisation could be reduced by rapid LC separation while maintaining analytical performance parameters. The improved method will be a valuable addition for the analysis of total SO2 binder pools in oenological samples. Published by Elsevier Ltd.

Solid-phase extraction in combination with dispersive liquid-liquid microextraction and ultra-high performance liquid chromatography-tandem mass spectrometry analysis: the ultra-trace determination of 10 antibiotics in water samples.

PubMed

Liang, Ning; Huang, Peiting; Hou, Xiaohong; Li, Zhen; Tao, Lei; Zhao, Longshan

2016-02-01

A novel method, solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME), was developed for ultra-preconcentration of 10 antibiotics in different environmental water samples prior to ultra-high performance liquid chromatography-tandem mass spectrometry detection. The optimized results were obtained as follows: after being adjusted to pH 4.0, the water sample was firstly passed through PEP-2 column at 10 mL min(-1), and then methanol was used to elute the target analytes for the following steps. Dichloromethane was selected as extraction solvent, and methanol/acetonitrile (1:1, v/v) as dispersive solvent. Under optimal conditions, the calibration curves were linear in the range of 1-1000 ng mL(-1) (sulfamethoxazole, cefuroxime axetil), 5-1000 ng mL(-1) (tinidazole), 10-1000 ng mL(-1) (chloramphenicol), 2-1000 ng mL(-1) (levofloxacin oxytetracycline, doxycycline, tetracycline, and ciprofloxacin) and 1-400 ng mL(-1) (sulfadiazine) with a good precision. The LOD and LOQ of the method were at very low levels, below 1.67 and 5.57 ng mL(-1), respectively. The relative recoveries of the target analytes were in the range from 64.16% to 99.80% with relative standard deviations between 0.7 and 8.4%. The matrix effect of this method showed a great decrease compared with solid-phase extraction and a significant value of enrichment factor (EF) compared with dispersive liquid-liquid microextraction. The developed method was successfully applied to the extraction and analysis of antibiotics in different water samples with satisfactory results.

An approach to the determination of aircraft handling qualities using pilot transfer functions

NASA Technical Reports Server (NTRS)

Adams, J. J.; Hatch, H. G., Jr.

1978-01-01

It was shown that a correlation exists between pilot-aircraft system closed-loop characteristics, determined by using analytical expressions for pilot response along with the analytical expression for the aircraft response, and pilot ratings obtained in many previous flight and simulation studies. Two different levels of preferred pilot response were used. These levels were: (1) a static gain and a second-order lag function with a lag time constant of 0.2 second; and (2) a static gain, a lead time constant of 1 second, and a 0.2-second lag time constant. If a system response with a pitch-angle time constant of 2.6 seconds and a stable oscillatory mode of motion with a period of 2.5 seconds could be achieved with the first-level pilot model, it was shown that the pilot rating will be satisfactory for that vehicle.

An analytical probabilistic model of the quality efficiency of a sewer tank

NASA Astrophysics Data System (ADS)

Balistrocchi, Matteo; Grossi, Giovanna; Bacchi, Baldassare

2009-12-01

The assessment of the efficiency of a storm water storage facility devoted to the sewer overflow control in urban areas strictly depends on the ability to model the main features of the rainfall-runoff routing process and the related wet weather pollution delivery. In this paper the possibility of applying the analytical probabilistic approach for developing a tank design method, whose potentials are similar to the continuous simulations, is proved. In the model derivation the quality issues of such devices were implemented. The formulation is based on a Weibull probabilistic model of the main characteristics of the rainfall process and on a power law describing the relationship between the dimensionless storm water cumulative runoff volume and the dimensionless cumulative pollutograph. Following this approach, efficiency indexes were established. The proposed model was verified by comparing its results to those obtained by continuous simulations; satisfactory agreement is shown for the proposed efficiency indexes.

3D-QSAR study and design of 4-hydroxyamino α-pyranone carboxamide analogues as potential anti-HCV agents

NASA Astrophysics Data System (ADS)

Li, Wenlian; Xiao, Faqi; Zhou, Mingming; Jiang, Xuejin; Liu, Jun; Si, Hongzong; Xie, Meng; Ma, Xiuting; Duan, Yunbo; Zhai, Honglin

2016-09-01

The three dimensional-quantitative structure activity relationship (3D-QSAR) study was performed on a series of 4-hydroxyamino α-pyranone carboxamide analogues using comparative molecular similarity indices analysis (COMSIA). The purpose of the present study was to develop a satisfactory model providing a reliable prediction based on 4-hydroxyamino α-pyranone carboxamide analogues as anti-HCV (hepatitis C virus) inhibitors. The statistical results and the results of validation of this optimum COMSIA model were satisfactory. Furthermore, analysis of the contour maps helped to provide guidelines for finding structural requirement. Therefore, the satisfactory results from this study may provide useful guidelines for drug development of anti-HCV inhibitors.

The evaluation of an analytical protocol for the determination of substances in waste for hazard classification

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

Hennebert, Pierre, E-mail: pierre.hennebert@ineris.fr; Papin, Arnaud; Padox, Jean-Marie

Highlights: • Knowledge of wastes in substances will be necessary to assess HP1–HP15 hazard properties. • A new analytical protocol is proposed for this and tested by two service laboratories on 32 samples. • Sixty-three percentage of the samples have a satisfactory analytical balance between 90% and 110%. • Eighty-four percentage of the samples were classified identically (Seveso Directive) for their hazardousness by the two laboratories. • The method, in progress, is being normalized in France and is be proposed to CEN. - Abstract: The classification of waste as hazardous could soon be assessed in Europe using largely the hazardmore » properties of its constituents, according to the the Classification, Labelling and Packaging (CLP) regulation. Comprehensive knowledge of the component constituents of a given waste will therefore be necessary. An analytical protocol for determining waste composition is proposed, which includes using inductively coupled plasma (ICP) screening methods to identify major elements and gas chromatography/mass spectrometry (GC–MS) screening techniques to measure organic compounds. The method includes a gross or indicator measure of ‘pools’ of higher molecular weight organic substances that are taken to be less bioactive and less hazardous, and of unresolved ‘mass’ during the chromatography of volatile and semi-volatile compounds. The concentration of some elements and specific compounds that are linked to specific hazard properties and are subject to specific regulation (examples include: heavy metals, chromium(VI), cyanides, organo-halogens, and PCBs) are determined by classical quantitative analysis. To check the consistency of the analysis, the sum of the concentrations (including unresolved ‘pools’) should give a mass balance between 90% and 110%. Thirty-two laboratory samples comprising different industrial wastes (liquids and solids) were tested by two routine service laboratories, to give circa 7000 parameter results. Despite discrepancies in some parameters, a satisfactory sum of estimated or measured concentrations (analytical balance) of 90% was reached for 20 samples (63% of the overall total) during this first test exercise, with identified reasons for most of the unsatisfactory results. Regular use of this protocol (which is now included in the French legislation) has enabled service laboratories to reach a 90% mass balance for nearly all the solid samples tested, and most of liquid samples (difficulties were caused in some samples from polymers in solution and vegetable oil). The protocol is submitted to French and European normalization bodies (AFNOR and CEN) and further improvements are awaited.« less

Analytical calculation of vibrations of electromagnetic origin in electrical machines

NASA Astrophysics Data System (ADS)

McCloskey, Alex; Arrasate, Xabier; Hernández, Xabier; Gómez, Iratxo; Almandoz, Gaizka

2018-01-01

Electrical motors are widely used and are often required to satisfy comfort specifications. Thus, vibration response estimations are necessary to reach optimum machine designs. This work presents an improved analytical model to calculate vibration response of an electrical machine. The stator and windings are modelled as a double circular cylindrical shell. As the stator is a laminated structure, orthotropic properties are applied to it. The values of those material properties are calculated according to the characteristics of the motor and the known material properties taken from previous works. Therefore, the model proposed takes into account the axial direction, so that length is considered, and also the contribution of windings, which differs from one machine to another. These aspects make the model valuable for a wide range of electrical motor types. In order to validate the analytical calculation, natural frequencies are calculated and compared to those obtained by Finite Element Method (FEM), giving relative errors below 10% for several circumferential and axial mode order combinations. It is also validated the analytical vibration calculation with acceleration measurements in a real machine. The comparison shows good agreement for the proposed model, being the most important frequency components in the same magnitude order. A simplified two dimensional model is also applied and the results obtained are not so satisfactory.

Enantioselective simultaneous analysis of selected pharmaceuticals in environmental samples by ultrahigh performance supercritical fluid based chromatography tandem mass spectrometry.

PubMed

Camacho-Muñoz, Dolores; Kasprzyk-Hordern, Barbara; Thomas, Kevin V

2016-08-31

In order to assess the true impact of each single enantiomer of pharmacologically active compounds (PACs) in the environment, highly efficient, fast and sensitive analytical methods are needed. For the first time this paper focuses on the use of ultrahigh performance supercritical fluid based chromatography coupled to a triple quadrupole mass spectrometer to develop multi-residue enantioselective methods for chiral PACs in environmental matrices. This technique exploits the advantages of supercritical fluid chromatography, ultrahigh performance liquid chromatography and mass spectrometry. Two coated modified 2.5 μm-polysaccharide-based chiral stationary phases were investigated: an amylose tris-3,5-dimethylphenylcarbamate column and a cellulose tris-3-chloro-4-methylphenylcarbamate column. The effect of different chromatographic variables on chiral recognition is highlighted. This novel approach resulted in the baseline resolution of 13 enantiomers PACs (aminorex, carprofen, chloramphenicol, 3-N-dechloroethylifosfamide, flurbiprofen, 2-hydroxyibuprofen, ifosfamide, imazalil, naproxen, ofloxacin, omeprazole, praziquantel and tetramisole) and partial resolution of 2 enantiomers PACs (ibuprofen and indoprofen) under fast-gradient conditions (<10 min analysis time). The overall performance of the methods was satisfactory. The applicability of the methods was tested on influent and effluent wastewater samples. To the best of our knowledge, this is the first feasibility study on the simultaneous separation of chemically diverse chiral PACs in environmental matrices using ultrahigh performance supercritical fluid based chromatography coupled with tandem mass spectrometry. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of type A trichothecenes in coix seed by magnetic solid-phase extraction based on magnetic multi-walled carbon nanotubes coupled with ultra-high performance liquid chromatography-tandem mass spectrometry.

PubMed

Dong, Maofeng; Si, Wenshuai; Wang, Weimin; Bai, Bing; Nie, Dongxia; Song, Weiguo; Zhao, Zhihui; Guo, Yirong; Han, Zheng

2016-09-01

Magnetic solid-phase extraction (m-SPE) is a promising sample preparation approach due to its convenience, speed, and simplicity. For the first time, a rapid and reliable m-SPE approach using magnetic multi-walled carbon nanotubes (m-MWCNTs) as the adsorbent was proposed for purification of type A trichothecenes including T-2 toxins (T2), HT-2 toxins (HT-2), diacetoxyscirpenol (DAS), and neosolaniol (NEO) in coix seed. The m-MWCNTs were synthesized by assembling the magnetic nanoparticles (Fe3O4) with MWCNTs by sonication through an aggregation wrap mechanism, and characterized by transmission electron microscope. Several key parameters affecting the performance of the procedure were extensively investigated including extraction solutions, desorption solvents, and m-MWCNT amounts. Under the optimal sample preparation conditions followed by analysis with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), high sensitivity (limit of quantification in the range of 0.3-1.5 μg kg(-1)), good linearity (R (2) > 0.99), satisfactory recovery (73.6-90.6 %), and acceptable precision (≤2.5 %) were obtained. The analytical performance of the developed method has also been successfully evaluated in real coix seed samples. Graphical Abstract Flow chart of determination of type A trichothecenes in coix seed by magnetic solid-phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry.

Breast cancer screening (breast self-examination, clinical breast exam, and mammography) in women referred to health centers in Tabriz, Iran.

PubMed

Khalili, Azizeh Farshbaf; Shahnazi, Mahnaz

2010-04-01

Breast cancer is the most common cancer and the most common cause of death in Iranian women aged 35-55 years. Breast cancer screening comprises breast self-examination (BSE), clinical breast examination (CBE) and mammography. The study aimed to examine the performance of screening methods among women referring to health centers of Tabriz, Iran. This was a descriptive-analytical research carried out on 400 women aged 20-50 years. The samples were chosen through random multistage sampling among health centers of Tabriz then active records of women. A questionnaire and observational checklist was used to elicit socio-demographic information and performance of women towards breast cancer screening methods. Descriptive and inferential statistics (chi-square and Fisher's exact test) were used to analyze the data. Only 18.8% of women did breast self-examination, 19.1% had clinical breast examination and 3.3% had mammogram. Statistical test showed a significant relationship between performing BSE and educational level, employment, income, number of children, breastfeeding history, breastfeeding quality and family history of breast cancer. There was a significant correlation between performing CBE and history of breast tumor and also, between performing the mammography and family history of breast cancer and history of breast tumor (P < 0.05). The findings showed that the performance of breast cancer screening methods was not satisfactory. Performance in high risk women was very desirable than others. The presentation of imperative education about breast cancer screening methods through health staff especially in pregnancy, post-partum and even in pre marriage counseling periods seems necessary.

A validated method for rapid determination of dibenzo-p-dioxins/furans (PCDD/Fs), polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs) in human milk: focus on utility of tandem solid phase extraction (SPE) cleanup.

PubMed

Lin, Yuanjie; Feng, Chao; Xu, Qian; Lu, Dasheng; Qiu, Xinlei; Jin, Yu'e; Wang, Guoquan; Wang, Dongli; She, Jianwen; Zhou, Zhijun

2016-07-01

An improved method based on tandem solid phase extraction (SPE) cleanup and gas chromatography-high resolution mass spectrometry (GC-HRMS) has been validated for a rapid determination of dibenzo-p-dioxins/furans (PCDD/Fs), dioxin-like polychlorinated biphenyls (PCBs), marker polychlorinated biphenyls (M-PCBs), and polybrominated diphenyl ethers (PBDEs) using a large volume (50 mL) of human milk. This method was well validated for the measurement of these analytes in human milk from the general population with low limits of detection (LODs, 0.004-0.12 ng/g lipid), satisfactory accuracy (75-120 % of recoveries), and precision [less than 10 % of relative standard deviations (RSDs)]. To comprehensively evaluate the performance of this method, a good, presently validated and routinely used method based on an automated sample clean-up system (ASCS, based on the commercial acid multilayer silica, basic alumina, and carbon columns) was used in parallel for comparison. Compared with the ASCS method, this method presented comparable specificity. Additionally, this method, in contrast to ASCS method, highly reduced consumption of solvents (40 mL versus 500 mL), which results in much lower background in the procedural blank, reduced time, and enhanced sample pretreatment throughput. This method was also applied in a pilot study to measure a batch of human milk samples with satisfactory results. Graphical Abstract Characteristics of the application of tandem SPE cleanup for determination of PCDD/Fs, DL-PCBs,M-PCBs and PBDEs in human milk.

36 CFR 223.35 - Performance bond.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 36 Parks, Forests, and Public Property 2 2013-07-01 2013-07-01 false Performance bond. 223.35... Sale Contracts Contract Conditions and Provisions § 223.35 Performance bond. Timber sale contracts may require the purchaser to furnish a performance bond for satisfactory compliance with its terms. ...

36 CFR 223.35 - Performance bond.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 36 Parks, Forests, and Public Property 2 2014-07-01 2014-07-01 false Performance bond. 223.35... Sale Contracts Contract Conditions and Provisions § 223.35 Performance bond. Timber sale contracts may require the purchaser to furnish a performance bond for satisfactory compliance with its terms. ...

Analytical applications of microbial fuel cells. Part II: Toxicity, microbial activity and quantification, single analyte detection and other uses.

PubMed

Abrevaya, Ximena C; Sacco, Natalia J; Bonetto, Maria C; Hilding-Ohlsson, Astrid; Cortón, Eduardo

2015-01-15

Microbial fuel cells were rediscovered twenty years ago and now are a very active research area. The reasons behind this new activity are the relatively recent discovery of electrogenic or electroactive bacteria and the vision of two important practical applications, as wastewater treatment coupled with clean energy production and power supply systems for isolated low-power sensor devices. Although some analytical applications of MFCs were proposed earlier (as biochemical oxygen demand sensing) only lately a myriad of new uses of this technology are being presented by research groups around the world, which combine both biological-microbiological and electroanalytical expertises. This is the second part of a review of MFC applications in the area of analytical sciences. In Part I a general introduction to biological-based analytical methods including bioassays, biosensors, MFCs design, operating principles, as well as, perhaps the main and earlier presented application, the use as a BOD sensor was reviewed. In Part II, other proposed uses are presented and discussed. As other microbially based analytical systems, MFCs are satisfactory systems to measure and integrate complex parameters that are difficult or impossible to measure otherwise, such as water toxicity (where the toxic effect to aquatic organisms needed to be integrated). We explore here the methods proposed to measure toxicity, microbial metabolism, and, being of special interest to space exploration, life sensors. Also, some methods with higher specificity, proposed to detect a single analyte, are presented. Different possibilities to increase selectivity and sensitivity, by using molecular biology or other modern techniques are also discussed here. Copyright © 2014 Elsevier B.V. All rights reserved.

Comprehensive combinatory standard correction: a calibration method for handling instrumental drifts of gas chromatography-mass spectrometry systems.

PubMed

Deport, Coralie; Ratel, Jérémy; Berdagué, Jean-Louis; Engel, Erwan

2006-05-26

The current work describes a new method, the comprehensive combinatory standard correction (CCSC), for the correction of instrumental signal drifts in GC-MS systems. The method consists in analyzing together with the products of interest a mixture of n selected internal standards, and in normalizing the peak area of each analyte by the sum of standard areas and then, select among the summation operator sigma(p = 1)(n)C(n)p possible sums, the sum that enables the best product discrimination. The CCSC method was compared with classical techniques of data pre-processing like internal normalization (IN) or single standard correction (SSC) on their ability to correct raw data from the main drifts occurring in a dynamic headspace-gas chromatography-mass spectrometry system. Three edible oils with closely similar compositions in volatile compounds were analysed using a device which performance was modulated by using new or used dynamic headspace traps and GC-columns, and by modifying the tuning of the mass spectrometer. According to one-way ANOVA, the CCSC method increased the number of analytes discriminating the products (31 after CCSC versus 25 with raw data or after IN and 26 after SSC). Moreover, CCSC enabled a satisfactory discrimination of the products irrespective of the drifts. In a factorial discriminant analysis, 100% of the samples (n = 121) were well-classified after CCSC versus 45% for raw data, 90 and 93%, respectively after IN and SSC.

A bioinspired polydopamine approach toward the preparation of gold-modified magnetic nanoparticles for the magnetic solid-phase extraction of steroids in multiple samples.

PubMed

An, Xuehan; Chai, Weibo; Deng, Xiaojuan; Chen, Hui; Ding, Guosheng

2018-05-02

In this work, a simple, facile, and sensitive magnetic solid-phase extraction method was developed for the extraction and enrichment of three representative steroid hormones before high-performance liquid chromatography analysis. Gold-modified Fe 3 O 4 nanoparticles, as novel magnetic adsorbents, were prepared by a rapid and environmentally friendly procedure in which polydopamine served as the reductant as well as the stabilizer for the gold nanoparticles, thus successfully avoiding the use of some toxic reagents. To obtain maximum extraction efficiency, several significant factors affecting the preconcentration steps, including the amount of adsorbent, extraction time, pH of the sample solution, and the desorption conditions, were optimized, and the enrichment factors for three steroids were all higher than 90. The validity of the established method was evaluated and good analytical characteristics were obtained. A wide linearity range (0.8-500 μg/L for all the analytes) was attained with good correlation (R 2  ≥ 0.991). The low limits of detection were 0.20-0.25 μg/L, and the relative standard deviations ranged from 0.83 to 4.63%, demonstrating a good precision. The proposed method was also successfully applied to the extraction and analysis of steroids in urine, milk, and water samples with satisfactory results, which showed its reliability and feasibility in real sample analysis. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Metal-organic framework based in-syringe solid-phase extraction for the on-site sampling of polycyclic aromatic hydrocarbons from environmental water samples.

PubMed

Zhang, Xiaoqiong; Wang, Peiyi; Han, Qiang; Li, Hengzhen; Wang, Tong; Ding, Mingyu

2018-04-01

In-syringe solid-phase extraction is a promising sample pretreatment method for the on-site sampling of water samples because of its outstanding advantages of portability, simple operation, short extraction time, and low cost. In this work, a novel in-syringe solid-phase extraction device using metal-organic frameworks as the adsorbent was fabricated for the on-site sampling of polycyclic aromatic hydrocarbons from environmental waters. Trace polycyclic aromatic hydrocarbons were effectively extracted through the self-made device followed by gas chromatography with mass spectrometry analysis. Owing to the excellent adsorption performance of metal-organic frameworks, the analytes could be completely adsorbed during one adsorption cycle, thus effectively shortening the extraction time. Moreover, the adsorbed analytes could remain stable on the device for at least 7 days, revealing the potential of the self-made device for on-site sampling of degradable compounds in remote regions. The limit of detection ranged from 0.20 to 1.9 ng/L under the optimum conditions. Satisfactory recoveries varying from 84.4 to 104.5% and relative standard deviations below 9.7% were obtained in real samples analysis. The results of this study promote the application of metal-organic frameworks in sample preparation and demonstrate the great potential of in-syringe solid-phase extraction for the on-site sampling of trace contaminants in environmental waters. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analysis of endocrine disruptor compounds in marine sediments by in cell clean up-pressurized liquid extraction-liquid chromatography tandem mass spectrometry determination.

PubMed

Salgueiro-González, N; Turnes-Carou, I; Muniategui-Lorenzo, S; López-Mahía, P; Prada-Rodríguez, D

2014-12-10

A less time-, solvent- and sorbent-consuming analytical methodology for the determination of bisphenol A and alkylphenols (4-tert-octylphenol, 4-octylphenol, 4-n-nonylphenol, nonylphenol) in marine sediment was developed and validated. The method was based on selective pressurized liquid extraction (SPLE) with a simultaneous in cell clean up combined with liquid chromatography-electrospray ionization tandem mass spectrometry in negative mode (LC-ESI-MS/MS). The SPLE extraction conditions were optimized by a Plackett-Burman design followed by a central composite design. Quantitation was performed by standard addition curves in order to correct matrix effects. The analytical features of the method were satisfactory: relative recoveries varied between 94 and 100% and repeatability and intermediate precision were <6% for all compounds. Uncertainty assessment of measurement was estimated on the basis of an in-house validation according to EURACHEM/CITAC guide. Quantitation limits of the method (MQL) ranged between 0.17 (4-n-nonylphenol) and 4.01 ng g(-1) dry weight (nonylphenol). Sensitivity, selectivity, automaticity and fastness are the main advantages of this green methodology. As an application, marine sediment samples from Galicia coast (NW of Spain) were analysed. Nonylphenol and 4-tert-octylphenol were measured in all samples at concentrations between 20.1 and 1409 ng g(-1) dry weight, respectively. Sediment toxicity was estimated and no risk to aquatic biota was found. Copyright © 2014 Elsevier B.V. All rights reserved.

Magnitude of cyantraniliprole residues in tomato following open field application: pre-harvest interval determination and risk assessment.

PubMed

Malhat, Farag; Kasiotis, Konstantinos M; Shalaby, Shehata

2018-02-05

Cyantraniliprole is an anthranilic diamide insecticide, belonging to the ryanoid class, with a broad range of applications against several pests. In the presented work, a reliable analytical technique employing high-performance liquid chromatography coupled with photodiode array detector (HPLC-DAD) for analyzing cyantraniliprole residues in tomato was developed. The method was then applied to field-incurred tomato samples collected after applications under open field conditions. The latter aimed to ensure the safe application of cyantraniliprole to tomato and contribute the derived residue data to the risk assessment under field conditions. Sample preparation involved a single step extraction with acetonitrile and sodium chloride for partitioning. The extract was purified utilizing florisil as cleanup reagent. The developed method was further evaluated by comparing the analytical results with those obtained using the QuEChERS technique. The novel method outbalanced QuEChERS regarding matrix interferences in the analysis, while it met all guideline criteria. Hence, it showed excellent linearity over the assayed concentration and yielded satisfactory recovery rate in the range of 88.9 to 96.5%. The half-life of degradation of cyantraniliprole was determined at 2.6 days. Based on the Codex MRL, the pre-harvest interval (PHI) for cyantraniliprole on tomato was 3 days, after treatment at the recommended dose. To our knowledge, the present work provides the first record on PHI determination of cyantraniliprole in tomato under open field conditions in Egypt and the broad Mediterranean region.

Fast and selective pressurized liquid extraction with simultaneous in cell clean up for the analysis of alkylphenols and bisphenol A in bivalve molluscs.

PubMed

Salgueiro-González, N; Turnes-Carou, I; Muniategui-Lorenzoa, S; López-Mahía, P; Prada-Rodríguez, D

2012-12-28

A novel and green analytical methodology for the determination of alkylphenols (4-tert-octylphenol, 4-n-octylphenol, 4-n-nonylphenol, nonylphenol technical mixture) and bisphenol A in bivalve mollusc samples was developed and validated. The method was based on selective pressurized liquid extraction (SPLE) with a simultaneous in cell clean up combined with liquid chromatography–electrospray ionization tandem mass spectrometry in negative mode (LC–ESI-MS/MS). Quantitation was performed by standard addition curves in order to correct matrix effects. The analytical features of the method were satisfactory: relative recoveries varied between 80 and 107% and repeatability and intermediate precision were <20% for all compounds. Uncertainty assessment of measurement was estimated on the basis of an in-house validation according to EURACHEM/CITAC guide. Quantitation limits of the method (MQL) ranged between 0.34 (4-n-octylphenol) and 3.6 ng g(−1) dry weight (nonylphenol). The main advantages of the method are sensitivity, selectivity, automaticity, low volumes of solvents required and low sample analysis time (according with the principles of Green Chemistry). The method was applied to the analysis of mussel samples of Galicia coast (NW of Spain). Nonylphenol and 4-tert-octylphenol were measured in all samples at concentrations between 9.3 and 372 ng g(−1) dw. As an approach, the human daily intake of these compounds was estimated and no risk for human health was found.

Synthesis and application of mesoporous molecular sieve for miniaturized matrix solid-phase dispersion extraction of bioactive flavonoids from toothpaste, plant, and saliva.

PubMed

Cao, Wan; Cao, Jun; Ye, Li-Hong; Xu, Jing-Jing; Hu, Shuai-Shuai; Peng, Li-Qing

2015-12-01

This article describes the use of the mesoporous molecular sieve KIT-6 as a sorbent in miniaturized matrix solid-phase dispersion (MSPD) in combination with ultra-performance LC for the determination of bioactive flavonoids in toothpaste, Scutellariae Radix, and saliva. In this study, for the first time, KIT-6 was used as a sorbent material for this mode of extraction. Compared with common silica-based sorbents (C18 and activated silica gel), the proposed KIT-6 dispersant with a three-dimensional cubic Ia3d structure and highly ordered arrays of mesoporous channels exhibits excellent adsorption capability of the tested compounds. In addition, several experimental variables, such as the mass ratio of sample to dispersant, grinding time, and elution solvent, were optimized to maximize the extraction efficiency. The proposed analytical method is simple, fast, and entails low consumption of samples, dispersants and elution solvents, thereby meeting "green chemistry" requirements. Under the optimized conditions, the recoveries of three bioactive flavonoids obtained by analyzing the spiked samples were from 89.22 to 101.17%. Also, the LODs and LOQs for determining the analytes were in the range of 0.02-0.04 μg/mL and 0.07-0.13 μg/mL, respectively. Finally, the miniaturized matrix solid-phase dispersion method was successfully applied to the analysis of target solutes in real samples, and satisfactory results were obtained. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A Method of Calibrating Airspeed Installations on Airplanes at Transonic and Supersonic Speeds by the Use of Accelerometer and Attitude-Angle Measurements

NASA Technical Reports Server (NTRS)

Zalovick, John A; Lina, Lindsay J; Trant, James P , Jr

1953-01-01

A method is described for calibrating airspeed installation on airplanes at transonic and supersonic speeds in vertical-plane maneuvers in which use is made of measurements of normal and longitudinal accelerations and attitude angle. In this method all the required instrumentation is carried within the airplane. An analytical study of the effects of various sources of error on the accuracy of an airspeed calibration by the accelerometer method indicated that the required measurements can be made accurately enough to insure a satisfactory calibration.

Rapid amino acid quantitation with pre-column derivatization; ultra-performance reverse phase liquid chromatography and single quadrupole mass spectrometry.

PubMed

Pretorius, Carel J; McWhinney, Brett C; Sipinkoski, Bilyana; Wilce, Alice; Cox, David; McWhinney, Avis; Ungerer, Jacobus P J

2018-03-01

We optimized a quantitative amino acid method with pre-column derivatization, norvaline (nva) internal standard and reverse phase ultra-performance liquid chromatography by replacing the ultraviolet detector with a single quadrupole mass spectrometer (MS nva ). We used 13 C 15 N isotopically labeled amino acid internal standards and a C18 column with 1.6μm particles to optimize the chromatography and to confirm separation of isobaric compounds (MS lis ). We compared the analytical performance of MS nva with MS lis and the original method (UV nva ) with clinical samples. The chromatography time per sample of MS nva was 8min, detection capabilities were <1μmol/L for most components, intermediate imprecisions at low concentrations were <10% and there was negligible carryover. MS nva was linear up to a total amino acid concentration in a sample of approximately 9500μmol/L. The agreements between most individual amino acids were satisfactory compared to UV nva with the latter prone to outliers and suboptimal quantitation of urinary arginine, aspartate, glutamate and methionine. MS nva reliably detected argnininosuccinate, β-alanine, citrulline and cysteine-s-sulfate. MS nva resulted in a more than fivefold increase in operational efficiency with accurate detection of amino acids and metabolic intermediates in clinical samples. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.

Integrating an artificial intelligence approach with k-means clustering to model groundwater salinity: the case of Gaza coastal aquifer (Palestine)

NASA Astrophysics Data System (ADS)

Alagha, Jawad S.; Seyam, Mohammed; Md Said, Md Azlin; Mogheir, Yunes

2017-12-01

Artificial intelligence (AI) techniques have increasingly become efficient alternative modeling tools in the water resources field, particularly when the modeled process is influenced by complex and interrelated variables. In this study, two AI techniques—artificial neural networks (ANNs) and support vector machine (SVM)—were employed to achieve deeper understanding of the salinization process (represented by chloride concentration) in complex coastal aquifers influenced by various salinity sources. Both models were trained using 11 years of groundwater quality data from 22 municipal wells in Khan Younis Governorate, Gaza, Palestine. Both techniques showed satisfactory prediction performance, where the mean absolute percentage error (MAPE) and correlation coefficient ( R) for the test data set were, respectively, about 4.5 and 99.8% for the ANNs model, and 4.6 and 99.7% for SVM model. The performances of the developed models were further noticeably improved through preprocessing the wells data set using a k-means clustering method, then conducting AI techniques separately for each cluster. The developed models with clustered data were associated with higher performance, easiness and simplicity. They can be employed as an analytical tool to investigate the influence of input variables on coastal aquifer salinity, which is of great importance for understanding salinization processes, leading to more effective water-resources-related planning and decision making.

Multi-mode application of graphene quantum dots bonded silica stationary phase for high performance liquid chromatography.

PubMed

Wu, Qi; Sun, Yaming; Zhang, Xiaoli; Zhang, Xia; Dong, Shuqing; Qiu, Hongdeng; Wang, Litao; Zhao, Liang

2017-04-07

Graphene quantum dots (GQDs), which possess hydrophobic, hydrophilic, π-π stacking and hydrogen bonding properties, have great prospect in HPLC. In this study, a novel GQDs bonded silica stationary phase was prepared and applied in multiple separation modes including normal phase, reversed phase and hydrophilic chromatography mode. Alkaloids, nucleosides and nucleobases were chosen as test compounds to evaluate the separation performance of this column in hydrophilic chromatographic mode. The tested polar compounds achieved baseline separation and the resolutions reached 2.32, 4.62, 7.79, 1.68 for thymidine, uridine, adenosine, cytidine and guanosine. This new column showed satisfactory chromatographic performance for anilines, phenols and polycyclic aromatic hydrocarbons in normal and reversed phase mode. Five anilines were completely separated within 10min under the condition of mobile phase containing only 10% methanol. The effect of water content, buffer concentration and pH on chromatographic separation was further investigated, founding that this new stationary phase showed a complex retention mechanism of partitioning, adsorption and electrostatic interaction in hydrophilic chromatography mode, and the multiple retention interactions such as π-π stacking and π-π electron-donor-acceptor interaction played an important role during the separation process. This GQDs bonded column, which allows us to adjust appropriate chromatography mode according to the properties of analytes, has possibility in actual application after further research. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of a simple and rapid solid phase microextraction-gas chromatography-triple quadrupole mass spectrometry method for the analysis of dopamine, serotonin and norepinephrine in human urine.

PubMed

Naccarato, Attilio; Gionfriddo, Emanuela; Sindona, Giovanni; Tagarelli, Antonio

2014-01-31

The work aims at developing a simple and rapid method for the quantification of dopamine (DA), serotonin (5-HT) and norepinephrine (NE) in human urine. The urinary levels of these biogenic amines can be correlated with several pathological conditions concerning heart disease, stress, neurological disorders and cancerous tumors. The proposed analytical approach is based on the use of solid phase microextraction (SPME) combined with gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS) after a fast derivatization of both aliphatic amino and phenolic moieties by propyl chloroformate. The variables influencing the derivatization reaction were reliably optimized by the multivariate approach of "Experimental design". The optimal conditions were obtained by performing derivatization with 100μL of propyl chloroformate and 100μL of pyridine. The extraction ability of five commercially available SPME fibers was evaluated in univariate mode and the best results were obtained using the polyacrylate fiber. The variables affecting the efficiency of SPME analysis were again optimized by the multivariate approach of "Experimental design" and, in particular, a central composite design (CCD) was applied. The optimal values were extraction in 45min at room temperature, desorption temperature at 300°C, no addition of NaCl. Assay of derivatized analytes was performed by using a gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS) system in selected reaction monitoring (SRM) acquisition. An evaluation of all analytical parameters demonstrates that the developed method provides satisfactory results. Indeed, very good linearities were achieved in the tested calibration range with correlation coefficient values of 0.9995, 0.9999 and 0.9997 for DA, 5-HT and NE, respectively. Accuracies and RSDs calculated for between-run and tested at concentrations of 30, 200, and 800μg L(-1) were in the range from 92.8% to 103.0%, and from 0.67 to 4.5%, respectively. Finally, the LOD values obtained can be considered very good (0.587, 0.381 and 1.23μg L(-1) for DA, 5-HT and NE, respectively). Copyright © 2013 Elsevier B.V. All rights reserved.

Structural damage detection based on stochastic subspace identification and statistical pattern recognition: II. Experimental validation under varying temperature

NASA Astrophysics Data System (ADS)

Lin, Y. Q.; Ren, W. X.; Fang, S. E.

2011-11-01

Although most vibration-based damage detection methods can acquire satisfactory verification on analytical or numerical structures, most of them may encounter problems when applied to real-world structures under varying environments. The damage detection methods that directly extract damage features from the periodically sampled dynamic time history response measurements are desirable but relevant research and field application verification are still lacking. In this second part of a two-part paper, the robustness and performance of the statistics-based damage index using the forward innovation model by stochastic subspace identification of a vibrating structure proposed in the first part have been investigated against two prestressed reinforced concrete (RC) beams tested in the laboratory and a full-scale RC arch bridge tested in the field under varying environments. Experimental verification is focused on temperature effects. It is demonstrated that the proposed statistics-based damage index is insensitive to temperature variations but sensitive to the structural deterioration or state alteration. This makes it possible to detect the structural damage for the real-scale structures experiencing ambient excitations and varying environmental conditions.

Disposable pipette extraction for gas chromatographic determination of codeine, morphine, and 6-monoacetylmorphine in vitreous humor.

PubMed

Kovatsi, Leda; Rentifis, Konstantinos; Giannakis, Dimitrios; Njau, Samuel; Samanidou, Victoria

2011-07-01

The availability of a sensitive and rapid analytical method for the determination of opiates, and other substances of forensic interest, in a variety of biological specimens is of utmost importance to forensic laboratories. Solid-phase extraction is very popular in the pre-treatment of forensic samples. Nevertheless, a new approach, disposable pipette extraction (DPX), is gaining increasing interest in sample preparation. DPX has already been applied to the analysis of drugs of abuse in common biological matrices, such as urine and blood, but has not yet been evaluated on alternative biological samples, such as vitreous humor. The objective of this study was to evaluate the applicability of DPX on the analysis of opiates in vitreous humor. The currently developed method is fast, reliable, and easy to perform. The sensitivity, precision, and accuracy are satisfactory. Recoveries obtained are within the range of 72-91%, whereas the sample volume of vitreous humor required is only 100 μL. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Non-enzymatic detection of glucose using poly(azure A)-nickel modified glassy carbon electrode.

PubMed

Liu, Tong; Luo, Yiqun; Zhu, Jiaming; Kong, Liyan; Wang, Wen; Tan, Liang

2016-08-15

A simple, sensitive and selective non-enzymatic glucose sensor was constructed in this paper. The poly(azure A)-nickel modified glassy carbon electrode was successfully fabricated by the electropolymerization of azure A and the adsorption of Ni(2+). The Ni modified electrode, which was characterized by scanning electron microscope, cyclic voltammetry, electrochemical impedance spectra and X-ray photoelectron spectroscopy measurements, respectively, displayed well-defined current responses of the Ni(III)/Ni(II) couple and showed a good activity for electrocatalytic oxidation of glucose in alkaline medium. Under the optimized conditions, the developed sensor exhibited a broad linear calibration range of 5 μM-12mM for quantification of glucose and a low detection limit of 0.64μM (3σ). The excellent analytical performance including simple structure, fast response time, good anti-interference ability, satisfying stability and reliable reproducibility were also found from the proposed amperometric sensor. The results were satisfactory for the determination of glucose in human serum samples as comparison to those from a local hospital. Copyright © 2016 Elsevier B.V. All rights reserved.

A Simple Method for Deriving the Confidence Regions for the Penalized Cox’s Model via the Minimand Perturbation†

PubMed Central

Lin, Chen-Yen; Halabi, Susan

2017-01-01

We propose a minimand perturbation method to derive the confidence regions for the regularized estimators for the Cox’s proportional hazards model. Although the regularized estimation procedure produces a more stable point estimate, it remains challenging to provide an interval estimator or an analytic variance estimator for the associated point estimate. Based on the sandwich formula, the current variance estimator provides a simple approximation, but its finite sample performance is not entirely satisfactory. Besides, the sandwich formula can only provide variance estimates for the non-zero coefficients. In this article, we present a generic description for the perturbation method and then introduce a computation algorithm using the adaptive least absolute shrinkage and selection operator (LASSO) penalty. Through simulation studies, we demonstrate that our method can better approximate the limiting distribution of the adaptive LASSO estimator and produces more accurate inference compared with the sandwich formula. The simulation results also indicate the possibility of extending the applications to the adaptive elastic-net penalty. We further demonstrate our method using data from a phase III clinical trial in prostate cancer. PMID:29326496

A Simple Method for Deriving the Confidence Regions for the Penalized Cox's Model via the Minimand Perturbation.

PubMed

Lin, Chen-Yen; Halabi, Susan

2017-01-01

We propose a minimand perturbation method to derive the confidence regions for the regularized estimators for the Cox's proportional hazards model. Although the regularized estimation procedure produces a more stable point estimate, it remains challenging to provide an interval estimator or an analytic variance estimator for the associated point estimate. Based on the sandwich formula, the current variance estimator provides a simple approximation, but its finite sample performance is not entirely satisfactory. Besides, the sandwich formula can only provide variance estimates for the non-zero coefficients. In this article, we present a generic description for the perturbation method and then introduce a computation algorithm using the adaptive least absolute shrinkage and selection operator (LASSO) penalty. Through simulation studies, we demonstrate that our method can better approximate the limiting distribution of the adaptive LASSO estimator and produces more accurate inference compared with the sandwich formula. The simulation results also indicate the possibility of extending the applications to the adaptive elastic-net penalty. We further demonstrate our method using data from a phase III clinical trial in prostate cancer.

Identification and quantification of 5,6,7,8-tetrahydro-2-(2-phenylethyl)chromones in Chinese eaglewood by HPLC with diode array detection and MS.

PubMed

Li, Jun; Chen, Dong; Jiang, Yong; Zhang, Qian; Zhang, Liang; Tu, Peng-Fei

2013-12-01

A sensitive and reliable HPLC coupled with diode array detection and MS method was developed and validated for the first time to simultaneously identify and quantify eight characteristic 5,6,7,8-tetrahydro-2-(2-phenylethyl)chromones (THPECs) in Chinese eaglewood. Chromatographic separation was performed on a Zorbax SB C18 column with a gradient of acetonitrile/0.1% formic acid/water as the mobile phase. The MS fragmentation behavior of THPECs was characterized as the successive neutral loss of two molecules of H2 O ([M+H-18-18](+) ) and then two molecules of CO ([M+H-18-18-28-28](+) ), which could be used to differentiate Chinese eaglewood from counterfeits. Validation of the developed analytical method showed good linearity, satisfactory precision, and good recovery. The established method was successfully applied to the simultaneous determination of eight THPECs in ten batches of Chinese eaglewood, which could be used as a tool for the quality control of Chinese eaglewood. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

An enhanced electrochemical platform based on graphene oxide and multi-walled carbon nanotubes nanocomposite for sensitive determination of Sunset Yellow and Tartrazine.

PubMed

Qiu, Xinlan; Lu, Limin; Leng, Jing; Yu, Yongfang; Wang, Wenmin; Jiang, Min; Bai, Ling

2016-01-01

A novel electrochemical platform was designed for the simultaneous determination of Sunset Yellow (SY) and Tartrazine (TT), synthetic food dyes, by combining the signal amplification properties of graphene oxide (GO) and the excellent electronic and antifouling properties of multi-walled carbon nanotubes (MWCNTs). Stable dispersion of GO/MWCNTs composite was produced by sonication mixing. Compared with glassy carbon, MWCNTs and GO electrodes, GO/MWCNTs electrode exhibited strong enhancement effect and greatly increased the oxidation signal of SY and TT. Under optimized conditions, the enhanced anodic peak currents represented the excellent analytical performance of simultaneous detection of SY and TT in the range of 0.09-8.0 μM, with a low limit of detection of 0.025 μM for SY and 0.01 μM for TT (S/N = 3), respectively. To further validate its possible application, the proposed method was successfully used for the determination of SY and TT in orange juice with satisfactory results. Copyright © 2015 Elsevier Ltd. All rights reserved.

Determination of Inorganic Arsenic in a Wide Range of Food Matrices using Hydride Generation - Atomic Absorption Spectrometry.

PubMed

de la Calle, Maria B; Devesa, Vicenta; Fiamegos, Yiannis; Vélez, Dinoraz

2017-09-01

The European Food Safety Authority (EFSA) underlined in its Scientific Opinion on Arsenic in Food that in order to support a sound exposure assessment to inorganic arsenic through diet, information about distribution of arsenic species in various food types must be generated. A method, previously validated in a collaborative trial, has been applied to determine inorganic arsenic in a wide variety of food matrices, covering grains, mushrooms and food of marine origin (31 samples in total). The method is based on detection by flow injection-hydride generation-atomic absorption spectrometry of the iAs selectively extracted into chloroform after digestion of the proteins with concentrated HCl. The method is characterized by a limit of quantification of 10 µg/kg dry weight, which allowed quantification of inorganic arsenic in a large amount of food matrices. Information is provided about performance scores given to results obtained with this method and which were reported by different laboratories in several proficiency tests. The percentage of satisfactory results obtained with the discussed method is higher than that of the results obtained with other analytical approaches.

Pharmacokinetics and Tissue Distribution Study of Chlorogenic Acid from Lonicerae Japonicae Flos Following Oral Administrations in Rats

PubMed Central

Zhou, Yulu; Zhou, Ting; Pei, Qi; Liu, Shikun; Yuan, Hong

2014-01-01

Chlorogenic acid (ChA) is proposed as the major bioactive compounds of Lonicerae Japonicae Flos (LJF). Forty-two Wistar rats were randomly divided into seven groups to investigate the pharmacokinetics and tissue distribution of ChA, via oral administration of LJF extract, using ibuprofen as internal standard, employing a high performance liquid chromatography in conjunction with tandem mass spectrometry. Analytes were extracted from plasma samples and tissue homogenate by liquid–liquid extraction with acetonitrile, separated on a C 18 column by linear gradient elution, and detected by electrospray ionization mass spectrometry in negative selected multiple reaction monitoring mode. Our results successfully demonstrate that the method has satisfactory selectivity, linearity, extraction recovery, matrix effect, precision, accuracy, and stability. Using noncompartment model to study pharmacokinetics, profile revealed that ChA was rapidly absorbed and eliminated. Tissue study indicated that the highest level was observed in liver, followed by kidney, lung, heart, and spleen. In conclusion, this method was suitable for the study on pharmacokinetics and tissue distribution of ChA after oral administration. PMID:25140190

Sensor fault detection and isolation via high-gain observers: application to a double-pipe heat exchanger.

PubMed

Escobar, R F; Astorga-Zaragoza, C M; Téllez-Anguiano, A C; Juárez-Romero, D; Hernández, J A; Guerrero-Ramírez, G V

2011-07-01

This paper deals with fault detection and isolation (FDI) in sensors applied to a concentric-pipe counter-flow heat exchanger. The proposed FDI is based on the analytical redundancy implementing nonlinear high-gain observers which are used to generate residuals when a sensor fault is presented (as software sensors). By evaluating the generated residual, it is possible to switch between the sensor and the observer when a failure is detected. Experiments in a heat exchanger pilot validate the effectiveness of the approach. The FDI technique is easy to implement allowing the industries to have an excellent alternative tool to keep their heat transfer process under supervision. The main contribution of this work is based on a dynamic model with heat transfer coefficients which depend on temperature and flow used to estimate the output temperatures of a heat exchanger. This model provides a satisfactory approximation of the states of the heat exchanger in order to allow its implementation in a FDI system used to perform supervision tasks. Copyright © 2011 ISA. Published by Elsevier Ltd. All rights reserved.

A novel voltammetric sensor for ascorbic acid based on molecularly imprinted poly(o-phenylenediamine-co-o-aminophenol).

PubMed

Kong, Yong; Shan, Xueling; Ma, Jianfeng; Chen, Meilan; Chen, Zhidong

2014-01-27

A molecularly imprinted copolymer, poly(o-phenylenediamine-co-o-aminophenol) (PoPDoAP), was prepared as a new ascorbic acid (AA) sensor. The copolymer was synthesized by incorporation of AA as template molecules during the electrochemical copolymerization of o-phenylenediamine and o-aminophenol, and complementary sites were formed after the copolymer was electrochemically reduced in ammonium aqueous solution. The molecularly imprinted copolymer sensor exhibited a high sensitivity and selectivity toward AA. Differential pulse voltammograms (DPVs) showed a linear concentration range of AA from 0.1 to 10 mM, and the detection limit was calculated to be 36.4 μM. Compared to conventional polyaniline-based AA sensors, the analytical performance of the imprinted copolymer sensor was improved due to the broadened usable pH range of PoPDoAP (from pH 1.0 to pH 8.0). The sensor also exhibited a good reproducibility and stability. And it has been successfully applied in the determination of AA in real samples, including vitamin C tablet and orange juices, with satisfactory results. Copyright © 2013 Elsevier B.V. All rights reserved.

Analytical methods for multiresidue determination of sulfonamides and trimethoprim in meat and ground water samples by CE-MS and CE-MS/MS.

PubMed

Soto-Chinchilla, Jorge J; García-Campaña, Ana M; Gámiz-Gracia, Laura

2007-11-01

This paper presents two methods based on CZE-MS detection and CZE-MS/MS detection developed for the multiresidue determination of ten sulfonamides (sulfapyridine, sulfadoxin, sulfamethazine, sulfadimethoxine, sulfameter, sulfamerazine, sulfachlorpyridazine, sulfadiazine, sulfamethoxazole, and sulfamethizole) and a potentiator, trimethoprim (TMP), whose contents are regulated by the EU Council Regulation no. 2377/90 in animal edible tissues. Experimental designs were employed to optimize the electrospray conditions. MS/MS experiments using an IT as analyzer operating in multiple reaction monitoring (MRM) mode were carried out to achieve the minimum number of points according to the 2002/657/EC European Decision for unambiguous identification. The proposed procedures have been compared in terms of the performance characteristics and trueness. The limits of detection and quantification were in all cases lower than the maximum residue limits legislated for these compounds and the recoveries were satisfactory, being possible the application for their monitoring in foodstuff of animal origin and in environmental samples, allowing the determination of sulfonamides and TMP residues in meat and in superficial water in the low microg/L range.

Fabrication of a novel metal chromite - Carbon nanotube composite for the highly efficient electrocatalytic reduction of hydrogen peroxide

NASA Astrophysics Data System (ADS)

Shahnavaz, Zohreh; Abd Hamid, Sharifah Bee

2017-06-01

The new electrocatalyst, ZnCr2O4/MWCNTs composite was successfully synthesized by hydrothermal method followed by calcination at 500 °C. A potential application of ZnCr2O4/MWCNTs composite modified electrode as enzyme-free sensor to monitor H2O2 has been studied. The sensor exhibited a high sensitivity of 1717.14 μA mM-1 cm-2 and a low detection limit down to 0.11 μM with a linear wide range from 50 μM to 34.8 mM with a fast response time of 2 s. In addition, modified electrode performance was investigated by measuring current responses of the sensor for three weeks to confirm the great stability of the proposed sensor. Along with these considerable analytical advantages, the as-prepared composite showed very high specificity to H2O2 with complete elimination of interference from uric acid, ascorbic acid, dopamine and glucose. The sensor gave satisfactory results in a real sample, when employed for determination of H2O2 in lens cleaning solution.

One-step construction of a molybdenum disulfide/multi-walled carbon nanotubes/polypyrrole nanocomposite biosensor for the ex-vivo detection of dopamine in mouse brain tissue.

PubMed

Vijayaraj, Kathiresan; Dinakaran, Thirumalai; Lee, Yujeong; Kim, Suhkmann; Kim, Hyung Sik; Lee, Jaewon; Chang, Seung-Cheol

2017-12-09

We developed a new strategy for construction of a biosensor for the neurotransmitter dopamine. The biosensor was constructed by one-step electrochemical deposition of a nanocomposite in aqueous solution at pH 7.0, consisting of molybdenum disulfide, multi-walled carbon nanotubes, and polypyrrole. A series of analytical methods was performed to investigate the surface characteristics and the improved electrocatalytic effect of the nanocomposite, including cyclic voltammetry, electrochemical impedance spectroscopy, field-emission scanning electron microscopy, atomic force microscopy, and Raman spectroscopy. The constructed biosensor showed high sensitivity (1.130 μAμM -1 cm -2 ) with a dynamic linearity range of 25-1000 nM and a detection limit of 10 nM. Additionally, the designed sensor exhibited strong anti-interference ability and satisfactory reproducibility. The practical application of the sensor was manifested for the ex vivo determination of dopamine neurotransmitters using brain tissue samples of a mouse Parkinson's disease model. Copyright © 2017 Elsevier Inc. All rights reserved.

Extraction and Determination of Cyproheptadine in Human Urine by DLLME-HPLC Method.

PubMed

Maham, Mehdi; Kiarostami, Vahid; Waqif-Husain, Syed; Abroomand-Azar, Parviz; Tehrani, Mohammad Saber; Khoeini Sharifabadi, Malihe; Afrouzi, Hossein; Shapouri, Mahmoudreza; Karami-Osboo, Rouhollah

2013-01-01

Novel dispersive liquid-liquid microextraction (DLLME), coupled with high performance liquid chromatography with photodiode array detection (HPLC-DAD) has been applied for the extraction and determination of cyproheptadine (CPH), an antihistamine, in human urine samples. In this method, 0.6 mL of acetonitrile (disperser solvent) containing 30 μL of carbon tetrachloride (extraction solvent) was rapidly injected by a syringe into 5 mL urine sample. After centrifugation, the sedimented phase containing enriched analyte was dissolved in acetonitrile and an aliquot of this solution injected into the HPLC system for analysis. Development of DLLME procedure includes optimization of some important parameters such as kind and volume of extraction and disperser solvent, pH and salt addition. The proposed method has good linearity in the range of 0.02-4.5 μg mL(-1) and low detection limit (13.1 ng mL(-1)). The repeatability of the method, expressed as relative standard deviation was 4.9% (n = 3). This method has also been applied to the analysis of real urine samples with satisfactory relative recoveries in the range of 91.6-101.0%.

A Wide Linearity Range Method for the Determination of Lenalidomide in Plasma by High-Performance Liquid Chromatography: Application to Pharmacokinetic Studies.

PubMed

Guglieri-López, Beatriz; Pérez-Pitarch, Alejandro; Martinez-Gómez, Maria Amparo; Porta-Oltra, Begoña; Climente-Martí, Mónica; Merino-Sanjuán, Matilde

2016-12-01

A wide linearity range analytical method for the determination of lenalidomide in patients with multiple myeloma for pharmacokinetic studies is required. Plasma samples were ultrasonicated for protein precipitation. A solid-phase extraction was performed. The eluted samples were evaporated to dryness under vacuum, and the solid obtained was diluted and injected into the high-performance liquid chromatography (HPLC) system. Separation of lenalidomide was performed on an Xterra RP C18 (250 mm length × 4.6 mm i.d., 5 µm) using a mobile phase consisting of phosphate buffer/acetonitrile (85:15, v/v, pH 3.2) at a flow rate of 0.5 mL · min -1 The samples were monitored at a wavelength of 311 nm. A linear relationship with good correlation coefficient (r = 0.997, n = 9) was found between the peak area and lenalidomide concentrations in the range of 100 to 950 ng · mL -1 The limits of detection and quantitation were 28 and 100 ng · mL -1 , respectively. The intra- and interassay precisions were satisfactory, and the accuracy of the method was proved. In conclusion, the proposed method is suitable for the accurate quantification of lenalidomide in human plasma with a wide linear range, from 100 to 950 ng · mL -1 This is a valuable method for pharmacokinetic studies of lenalidomide in human subjects. © 2016 Society for Laboratory Automation and Screening.

Capillary electrophoresis for rapid identification of monoclonal antibodies for routine application in hospital.

PubMed

Jaccoulet, Emmanuel; Smadja, Claire; Prognon, Patrice; Taverna, Myriam

2015-09-01

mAbs are widely used in cancer therapy. Their compounding, performed just before their administration to patients, is executed in a production unit of the hospital. Identification of these drugs, individually prepared in bags for infusion before patient administration, is of paramount importance to detect potential mistakes during compounding stage. A fast and reliable analytical method based on CZE combined to a cationic capillary coating (hexadimethrine bromide) was developed for identification of the most widely used compounded therapeutic for cancer therapy (bevacizumab, cetuximab, rituximab, and trastuzumab). Considering the high structural and physico-chemical similarities of these mAbs, an extensive optimization of the BGE composition has been performed. The addition of perchlorate ions and polysorbate in the BGE greatly increased the resolution. To validate the method, an internal standard was used and the relative migration times (RTm) were estimated. Very satisfactory RSDs of the RTm for rituximab (0.76%), cetuximab (0.46%), bevacizumab (0.31%), and trastuzumab (0.60%) were obtained. The intraday and interday RSD of the method were less than 0.32 and 1.3%, respectively for RTm. Significant differences between theses RTms have been demonstrated allowing mAbs identification. Finally, accurate mAbs identification has been demonstrated by a blind test. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development and Application of an HPLC–UV Procedure to Determine Multiple Flavonoids and Phenolics in Acanthopanax Leaf Extracts

PubMed Central

Zhang, Xiaodan; Zhou, Xinqi; Liu, Xiangqian; Li, Xiaolong; Whang, Wankyunn

2016-01-01

Acanthopanax species are used in traditional medicine to treat numerous diseases. A simultaneous high-performance liquid chromatography (HPLC) method was developed and validated for the determination of the flavonoid and phenolic content of Acanthopanax leaves. HPLC analysis was performed on an AKZO NOBEL Kromasil 100-5C18 column (250 × 4.6 mm, 5 µm) using a gradient elution of acetonitrile–water containing 0.2% formic acid with a flow rate of 1.0 mL/min, monitored at 320 nm. The method was linear over the range 1–500 µg/mL (determination coefficients R2 > 0.999). Satisfactory intraday and interday precision was achieved, with the relative standard deviation (RSD) <2.99%. The mean recoveries measured at the three concentrations were in the range of 90.11–104.83%, with RSD <2.91% for the targets. Twenty-four samples of Acanthopanax leaves from different species and locations were examined using this analytical method, and their chemical profiles provided information for the chemotaxonomic investigation. The established method is simple, rapid and reliable for the quality control of Acanthopanax leaves of various species from different collections. The complete phenolic and flavonoid profiles of Acanthopanax leaves of various species have been established. PMID:26711585

Analytical evaluation of the impact of broad specification fuels on high bypass turbofan engine combustors

NASA Technical Reports Server (NTRS)

Lohmann, R. P.; Szetela, E. J.; Vranos, A.

1978-01-01

The impact of the use of broad specification fuels on the design, performance durability, emissions and operational characteristics of combustors for commercial aircraft gas turbine engines was assessed. Single stage, vorbix and lean premixed prevaporized combustors, in the JT9D and an advanced energy efficient engine cycle were evaluated when operating on Jet A and ERBS (Experimental Referee Broad Specification) fuels. Design modifications, based on criteria evolved from a literature survey, were introduced and their effectiveness at offsetting projected deficiencies resulting from the use of ERBS was estimated. The results indicate that the use of a broad specification fuel such as ERBS, will necessitate significant technology improvements and redesign if deteriorated performance, durability and emissions are to be avoided. Higher radiant heat loads are projected to seriously compromise liner life while the reduced thermal stability of ERBS will require revisions to the engine-airframe fuel system to reduce the thermal stress on the fuel. Smoke and emissions output are projected to increase with the use of broad specification fuels. While the basic geometry of the single stage and vorbix combustors are compatible with the use of ERBS, extensive redesign of the front end of the lean premixed prevaporized burner will be required to achieve satisfactory operation and optimum emissions.

Headspace and direct immersion solid phase microextraction procedures for selenite determination in urine, saliva and milk by gas chromatography mass spectrometry.

PubMed

Kapsimali, D C; Zachariadis, G A

2009-10-01

Two solid phase microextraction modes were investigated and compared for their performance on the determination of selenites in various biological liquids like human urine and saliva and various types of milk. Using sodium tetraethylborate (NaBEt(4)) as ethylating reagent, selenites are converted in situ to volatile diethylselenides (DESe) in aqueous medium. The derivative is collected in situ by solid phase microextraction (SPME) using a silica fiber coated with poly(dimethylsiloxane) (PDMS) either from the headspace (HS-SPME) or directly from the liquid phase (LP-SPME) and finally determined by capillary GC/MS. Under optimum conditions of SPME, the GC separation was also optimized. Between the two examined microextraction techniques, direct immersion of the PDMS fiber in the liquid phase was proved less satisfactory. In contrast, the headspace procedure appears to be more efficient. The quantification of selenites was achieved in SIM mode with good analytical performance. A non-fat milk powder certified reference material was analyzed to evaluate the accuracy of the method. The overall precision of the method was ranged between 6.2% and 9.7%. Detection limits achieved were 0.05microgL(-1) for human urine, 0.08microgL(-1) for saliva and 0.03-0.06microgL(-1) in various milk matrices.

Monitoring leachables from single-use bioreactor bags for mammalian cell culture by dispersive liquid-liquid microextraction followed by ultra high performance liquid chromatography quadrupole time of flight mass spectrometry.

PubMed

Dorival-García, N; Bones, J

2017-08-25

A method for the identification of leachables in chemically defined media for CHO cell culture using dispersive liquid-liquid microextraction (DLLME) and UHPLC-MS is described. A Box-Behnken design of experiments (DoE) approach was applied to obtain the optimum extraction conditions of the target analytes. Performance of DLLME as extraction technique was studied by comparison of two commercial chemically defined media for CHO cell culture. General extraction conditions for any group of leachables, regardless of their specific chemical functionalities can be applied and similar optimum conditions were obtained with the two media. Extraction efficiency and matrix effects were determined. The method was validated using matrix-matched standard calibration followed by recovery assays with spiked samples. Finally, cell culture media was incubated in 7 single use bioreactors (SUBs) from different vendors and analysed. TBPP was not detected in any of the samples, whereas DtBP and TBPP-ox were found in all samples, with bDtBPP detected in six SUBs. This method can be used for early identification of non-satisfactory SUB films for cultivation of CHO cell lines for biopharmaceutical production. Copyright © 2017 Elsevier B.V. All rights reserved.

Enhanced direct electrochemistry of glucose oxidase and biosensing for glucose via synergy effect of graphene and CdS nanocrystals.

PubMed

Wang, Kun; Liu, Qian; Guan, Qing-Meng; Wu, Jun; Li, He-Nan; Yan, Jia-Jia

2011-01-15

Integrating graphene-based composites with enzyme provides a potent strategy to enhance biosensor performance due to their unique physicochemical properties. Herein we report on the utilization of graphene-CdS (G-CdS) nanocomposite as a novel immobilization matrix for the enzymes, which glucose oxidase (GOD) was chosen as model enzyme. In comparison with the graphene sheet and CdS nanocrystal, G-CdS nanocomposite exhibited excellent electron transfer properties for GOD with the rate constant (k(s)) of 5.9 s(-1) due to the synergy effect of graphene sheet and CdS nanocrystals. Further, based on the decrease of the electrocatalytic response of the reduced form of GOD to dissolved oxygen, the obtained glucose biosensor displays satisfactory analytical performance over an acceptable linear range from 2.0 to 16 mM with a detection limit of 0.7 mM, and also prevents the effects of interfering species, which is suitable for glucose determination by real samples. These results mean that this immobilization matrix not only can be used for immobilizing GOD, but also can be extended to other enzymes and bioactive molecules, thus providing a promising platform for the development of biosensors. Copyright © 2010 Elsevier B.V. All rights reserved.

Determination of benzimidazole anthelmintics in milk and honey by monolithic fiber-based solid-phase microextraction combined with high-performance liquid chromatography-diode array detection.

PubMed

Zhang, Yong; Huang, Xiaojia; Yuan, Dongxing

2015-01-01

A porous poly(methacrylic acid-co-ethylene dimethacrylate) monolithic fiber (MEMF) for solid-phase microextraction (SPME) of five benzimidazole anthelmintics was prepared by in-situ polymerization. The effect of polymerization conditions on SPME of the target analytes was studied thoroughly. The physicochemical properties of the monolith were characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy, and mercury intrusion porosimetry. Several conditions affecting the extraction efficiency were investigated and, under the optimized conditions, a simple and sensitive method for the determination of trace benzimidazoles residues in milk and honey was established by coupling MEMF-SPME with high-performance liquid chromatography-diode array detection (MEMF-SPME-HPLC-DAD). Under the optimum experimental conditions, the limits of detection (S/N = 3) of the method were 0.11-0.30 μg L(-1) for milk and 0.086-0.28 μg L(-1) for honey. Evaluation of intra-day and inter-day precision showed reproducibility was satisfactory-relative standard deviations (RSD) for both were <10 %. Finally, the method was successfully used for determination of benzimidazole residues in milk and honey. Recoveries obtained for determination of benzimidazole anthelmintics in spiked samples ranged from 72.3 to 121 %, with RSD always <11 %.

13 CFR 120.434 - What are SBA's requirements for loan pledges?

Code of Federal Regulations, 2012 CFR

2012-01-01

... factors, will be considered in determining satisfactory SBA performance. Other factors may include, but... default rate, purchase rate and loss rate), loan volume to the extent that it impacts performance measures...

36 CFR 9.13 - Performance bond.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 36 Parks, Forests, and Public Property 1 2011-07-01 2011-07-01 false Performance bond. 9.13... MINERALS MANAGEMENT Mining and Mining Claims § 9.13 Performance bond. (a) Upon approval of a plan of operations the operator shall be required to file a suitable performance bond with satisfactory surety...

36 CFR 9.48 - Performance bond.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 36 Parks, Forests, and Public Property 1 2011-07-01 2011-07-01 false Performance bond. 9.48... MINERALS MANAGEMENT Non-Federal Oil and Gas Rights § 9.48 Performance bond. (a) Prior to approval of a plan of operations, the operator shall be required to file a suitable performance bond with satisfactory...

36 CFR 9.13 - Performance bond.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 36 Parks, Forests, and Public Property 1 2013-07-01 2013-07-01 false Performance bond. 9.13... MINERALS MANAGEMENT Mining and Mining Claims § 9.13 Performance bond. (a) Upon approval of a plan of operations the operator shall be required to file a suitable performance bond with satisfactory surety...

36 CFR 9.48 - Performance bond.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 36 Parks, Forests, and Public Property 1 2013-07-01 2013-07-01 false Performance bond. 9.48... MINERALS MANAGEMENT Non-Federal Oil and Gas Rights § 9.48 Performance bond. (a) Prior to approval of a plan of operations, the operator shall be required to file a suitable performance bond with satisfactory...

36 CFR 9.13 - Performance bond.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 36 Parks, Forests, and Public Property 1 2010-07-01 2010-07-01 false Performance bond. 9.13... MINERALS MANAGEMENT Mining and Mining Claims § 9.13 Performance bond. (a) Upon approval of a plan of operations the operator shall be required to file a suitable performance bond with satisfactory surety...

Determination of low-molecular-weight amines and ammonium in saline waters by ion chromatography after their extraction by steam distillation.

PubMed

Ferreira, Fernanda Nunes; Afonso, Julio Carlos; Pontes, Fernanda Veronesi Marinho; Carneiro, Manuel Castro; Neto, Arnaldo Alcover; Tristão, Maria Luiza Bragança; Monteiro, Maria Inês Couto

2016-04-01

A new method was developed for the determination of ammonium ion, monomethylamine and monoethylamine in saline waters by ion chromatography. Steam distillation was used to eliminate matrix interferences. Variables such as distillation time, concentration of sodium hydroxide solution and analyte mass were optimized by using a full two-level factorial (2(3) ) design. The influence of steam distillation on the analytical curves prepared in different matrices was also investigated. Limits of detection of 0.03, 0.05 and 0.05 mg/L were obtained for ammoniumion, monomethylamine and monoethylamine, respectively. Saline water samples from the Brazilian oil industry, containing sodium and potassium concentrations between 2.0-5.2% w/v and 96-928 mg/L, respectively, were analyzed. Satisfactory recoveries (90-105%) of the analytes were obtained for all spiked samples, and the precision was ≤ 7% (n = 3). The proposed method is adequate for analyzing saline waters containing sodium to ammoniumion, monomethylamine and monoethylamine concentration ratios up to 28 000:1 and potassium to ammonium, monomethylamine and monoethylamine concentration ratios up to 12 000:1. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Spontaneous imbibition of water and determination of effective contact angles in the Eagle Ford Shale Formation using neutron imaging

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

DiStefano, Victoria H.; Cheshire, Michael C.; McFarlane, Joanna

Understanding of fundamental processes and prediction of optimal parameters during the horizontal drilling and hydraulic fracturing process results in economically effective improvement of oil and natural gas extraction. Although, the modern analytical and computational models can capture fracture growth, there is a lack of experimental data on spontaneous imbibition and wettability in oil and gas reservoirs for the validation of further model development. In this work, we used neutron imaging to measure the spontaneous imbibition of water into fractures of Eagle Ford Shale with known geometries and fracture orientations. An analytical solution for a set of nonlinear second-order differential equationsmore » was applied to the measured imbibition data to determine effective contact angles. The analytical solution fit the measured imbibition data reasonably well and determined effective contact angles were slightly higher than static contact angles due to effects of in-situ changes in velocity, surface roughness, and heterogeneity of mineral surfaces on the fracture surface. Additionally, small fracture widths may have retarded imbibition and affected model fits, which suggests that average fracture widths are not satisfactory for modeling imbibition in natural systems.« less

Integration of electrochemistry in micro-total analysis systems for biochemical assays: recent developments.

PubMed

Xu, Xiaoli; Zhang, Song; Chen, Hui; Kong, Jilie

2009-11-15

Micro-total analysis systems (microTAS) integrate different analytical operations like sample preparation, separation and detection into a single microfabricated device. With the outstanding advantages of low cost, satisfactory analytical efficiency and flexibility in design, highly integrated and miniaturized devices from the concept of microTAS have gained widespread applications, especially in biochemical assays. Electrochemistry is shown to be quite compatible with microanalytical systems for biochemical assays, because of its attractive merits such as simplicity, rapidity, high sensitivity, reduced power consumption, and sample/reagent economy. This review presents recent developments in the integration of electrochemistry in microdevices for biochemical assays. Ingenious microelectrode design and fabrication methods, and versatility of electrochemical techniques are involved. Practical applications of such integrated microsystem in biochemical assays are focused on in situ analysis, point-of-care testing and portable devices. Electrochemical techniques are apparently suited to microsystems, since easy microfabrication of electrochemical elements and a high degree of integration with multi-analytical functions can be achieved at low cost. Such integrated microsystems will play an increasingly important role for analysis of small volume biochemical samples. Work is in progress toward new microdevice design and applications.

Separation, preconcentration and inductively coupled plasma-mass spectrometric (ICP-MS) determination of thorium(IV), titanium(IV), iron(III), lead(II) and chromium(III) on 2-nitroso-1-naphthol impregnated MCI GEL CHP20P resin.

PubMed

Aydin, Funda Armagan; Soylak, Mustafa

2010-01-15

A simple and effective method is presented for the separation and preconcentration of Th(IV), Ti(IV), Fe(III), Pb(II) and Cr(III) by solid phase extraction on 2-nitroso-1-naphthol impregnated MCI GEL CHP20P resin prior to their inductively coupled plasma-mass spectrometric determinations. The influence of analytical parameters including pH of the aqueous solution, flow rates of sample and eluent solutions and sample volume on the quantitative recoveries of analyte ions was investigated. Matrix effects caused by the presence of alkali, earth alkali and some metal ions in the analyzed solutions were investigated. The presented solid phase extraction method was applied to BCR-144R Sewage Sludge (domestic origin), BCR-141R Calcareous Loam Soil, NIST 1568a Rice Flour and NIST 1577b Bovine Liver certified reference materials (CRMs) for the determination of analyte ions and the results were in good agreement with the certified values. The separation procedure presented was also applied to the various natural water samples collected from Turkey with satisfactory results.

Simultaneous gas chromatographic determination of chlorpyrifos and its impurity sulfotep in liquid pesticide formulations.

PubMed

Płonka, Marlena; Walorczyk, Stanisław; Miszczyk, Marek; Kronenbach-Dylong, Dorota

2016-11-01

An analytical method for simultaneous determination of the active substance (chlorpyrifos) and its relevant impurity (sulfotep) in commercial pesticide formulations has been developed and validated. The proposed method entails extraction of the analytes from samples by sonication with acetone and analysis by gas chromatography-flame ionization detection (GC-FID). The proposed method was characterized by satisfactory accuracy and precision. The repeatability expressed as relative standard deviation (RSD) was lower than the acceptable values calculated from the modified Horwitz equation whereas individual recoveries were in the range of 98-102% and 80-120% for chlorpyrifos and sulfotep, respectively. The limit of quantification (LOQ) for the impurity (sulfotep) was 0.003 mg mL(-1) corresponding to the maximum permitted level according to Food and Agricultural Organization of the United Nations (FAO) specifications for the active substance (chlorpyrifos) being 3 g kg(-1) of the chlorpyrifos content found. The main advantage of the proposed method was a considerable reduction in the analysis time since both analytes were determined based on a single injection into the GC-FID. Analysis of real samples of commercial pesticide formulations confirmed fitness-for-purpose of the proposed method.

Integrated atomic layer deposition and chemical vapor reaction for the preparation of metal organic framework coatings for solid-phase microextraction Arrow.

PubMed

Lan, Hangzhen; Salmi, Leo D; Rönkkö, Tuukka; Parshintsev, Jevgeni; Jussila, Matti; Hartonen, Kari; Kemell, Marianna; Riekkola, Marja-Liisa

2018-09-18

New chemical vapor reaction (CVR) and atomic layer deposition (ALD)-conversion methods were utilized for preparation of metal organic frameworks (MOFs) coatings of solid phase microextraction (SPME) Arrow for the first time. With simple, easy and convenient one-step reaction or conversion, four MOF coatings were made by suspend ALD iron oxide (Fe 2 O 3 ) film or aluminum oxide (Al 2 O 3 ) film above terephthalic acid (H 2 BDC) or trimesic acid (H 3 BTC) vapor. UIO-66 coating was made by zirconium (Zr)-BDC film in acetic acid vapor. As the first documented instance of all-gas phase synthesis of SPME Arrow coatings, preparation parameters including CVR/conversion time and temperature, acetic acid volume, and metal oxide film/metal-ligand films thickness were investigated. The optimal coatings exhibited crystalline structures, excellent uniformity, satisfactory thickness (2-7.5 μm), and high robustness (>80 times usage). To study the practical usefulness of the coatings for the extraction, several analytes with different chemical properties were tested. The Fe-BDC coating was found to be the most selective and sensitive for the determination of benzene ring contained compounds due to its highly hydrophobic surface and unsaturated metal site. UIO-66 coating was best for small polar, aromatic, and long chain polar compounds owing to its high porosity. The usefulness of new coatings were evaluated for gas chromatography-mass spectrometer (GC-MS) determination of several analytes, present in wastewater samples at three levels of concentration, and satisfactory results were achieved. Copyright © 2018 Elsevier B.V. All rights reserved.

VIS-NIR spectroscopy as a process analytical technology for compositional characterization of film biopolymers and correlation with their mechanical properties.

PubMed

Barbin, Douglas Fernandes; Valous, Nektarios A; Dias, Adriana Passos; Camisa, Jaqueline; Hirooka, Elisa Yoko; Yamashita, Fabio

2015-11-01

There is an increasing interest in the use of polysaccharides and proteins for the production of biodegradable films. Visible and near-infrared (VIS-NIR) spectroscopy is a reliable analytical tool for objective analyses of biological sample attributes. The objective is to investigate the potential of VIS-NIR spectroscopy as a process analytical technology for compositional characterization of biodegradable materials and correlation to their mechanical properties. Biofilms were produced by single-screw extrusion with different combinations of polybutylene adipate-co-terephthalate, whole oat flour, glycerol, magnesium stearate, and citric acid. Spectral data were recorded in the range of 400-2498nm at 2nm intervals. Partial least square regression was used to investigate the correlation between spectral information and mechanical properties. Results show that spectral information is influenced by the major constituent components, as they are clustered according to polybutylene adipate-co-terephthalate content. Results for regression models using the spectral information as predictor of tensile properties achieved satisfactory results, with coefficients of prediction (R(2)C) of 0.83, 0.88 and 0.92 (calibration models) for elongation, tensile strength, and Young's modulus, respectively. Results corroborate the correlation of NIR spectra with tensile properties, showing that NIR spectroscopy has potential as a rapid analytical technology for non-destructive assessment of the mechanical properties of the films. Copyright © 2015 Elsevier B.V. All rights reserved.

A solid phase extraction procedure for the determination of Cd(II) and Pb(II) ions in food and water samples by flame atomic absorption spectrometry.

PubMed

Daşbaşı, Teslima; Saçmacı, Şerife; Ülgen, Ahmet; Kartal, Şenol

2015-05-01

A relatively rapid, accurate and precise solid phase extraction method is presented for the determination of cadmium(II) and lead(II) in various food and water samples. Quantitation is carried out by flame atomic absorption spectrometry (FAAS). The method is based on the retention of the trace metal ions on Dowex Marathon C, a strong acid cation exchange resin. Some important parameters affecting the analytical performance of the method such as pH, flow rate and volume of the sample solution; type, concentration, volume, flow rate of the eluent; and matrix effects on the retention of the metal ions were investigated. Common coexisting ions did not interfere on the separation and determination of the analytes. The detection limits (3 σb) for Cd(II) and Pb(II) were found as 0.13 and 0.18 μg L(-1), respectively, while the limit of quantification values (10 σb) were computed as 0.43 and 0.60 μg L(-1) for the same sequence of the analytes. The precision (as relative standard deviation was lower than 4% at 5 μg L(-1) Cd(II) and 10 μg L(-1) Pb(II) levels, and the preconcentration factor was found to be 250. The accuracy of the proposed procedure was verified by analysing the certified reference materials, SPS-WW2 Batch 108 wastewater level 2 and INCT-TL-1 tea leaves, with the satisfactory results. In addition, for the accuracy of the method the recovery studies (⩾ 95%) were carried out. The method was applied to the determination of the analytes in the various natural waters (lake water, tap water, waste water with boric acid, waste water with H2SO4) and food samples (pomegranate flower, organic pear, radish leaf, lamb meat, etc.), and good results were obtained. While the food samples almost do not contain cadmium, they have included lead at low levels of 0.13-1.12 μg g(-1). Copyright © 2014 Elsevier Ltd. All rights reserved.

Paper-based assay of antioxidant activity using analyte-mediated on-paper nucleation of gold nanoparticles as colorimetric probes.

PubMed

Choleva, Tatiana G; Kappi, Foteini A; Giokas, Dimosthenis L; Vlessidis, Athanasios G

2015-02-20

With the increasing interest in the health benefits arising from the consumption of dietary products rich in antioxidants, there exists a clear demand for easy-to-use and cost-effective tests that can be used for the identification of the antioxidant power of food products. Paper-based analytical devices constitute a remarkable platform for such expedient and low-cost assays with minimal external resources but efforts in this direction are still scarce. In this work we introduce a new paper-based device in the form of a sensor patch that enables the determination of antioxidant activity through analyte-driven on-paper formation of gold nanoparticles. The principle of detection capitalizes, for the first time, on the on-paper nucleation of gold ions to its respective nanoparticles, upon reduction by antioxidant compounds present in an aqueous sample. The ensuing chromatic transitions, induced on the paper surface, are used as an optical "signature" of the antioxidant strength of the solution. The response of the paper-based sensor was evaluated against a large variety of antioxidant species and the respective dose response curves were constructed. On the basis of these data, the contribution of each species according to its chemical structure was elucidated. For the analysis of real samples, a concentration-dependent colorimetric response was established against Gallic acid equivalents over a linear range of 10 μM-1.0 mM, with detection limits at the low and ultra-low μM levels (i.e. <1.0 μM) and satisfactory precision (RSD=3.6-12.6%). The sensor has been tested for the assessment of antioxidant activity in real samples (teas and wines) and the results correlated well with commonly used antioxidant detection methods. Importantly, the sensor performed favorably for long periods of time when stored at moisture-free and low temperature conditions without losing its activity thus posing as an attractive alternative to the assessment of antioxidant activity without specialized equipment. The use of the sensor by non-experts for a rapid assessment of natural products in field testing is envisioned. Importantly, we demonstrate for the first time that analyte-mediated growth of nanomaterials directly on the paper surface could open new opportunities in paper-based analytical devices. Copyright © 2014 Elsevier B.V. All rights reserved.

Adrenal venous sampling: the learning curve of a single interventionalist with 282 consecutive procedures.

PubMed

Jakobsson, Hugo; Farmaki, Katerina; Sakinis, Augustinas; Ehn, Olof; Johannsson, Gudmundur; Ragnarsson, Oskar

2018-01-01

Primary aldosteronism (PA) is a common cause of secondary hypertension. Adrenal venous sampling (AVS) is the gold standard for assessing laterality of PA, which is of paramount importance to decide adequate treatment. AVS is a technically complicated procedure with success rates ranging between 30% and 96%. The aim of this study was to investigate the success rate of AVS over time, performed by a single interventionalist. This was a retrospective study based on consecutive AVS procedures performed by a single operator between September 2005 and June 2016. Data on serum concentrations of aldosterone and cortisol from right and left adrenal vein, inferior vena cava, and peripheral vein were collected and selectivity index (SI) calculated. Successful AVS was defined as SI > 5. In total, 282 AVS procedures were performed on 269 patients, 168 men (62%) and 101 women (38%), with a mean age of 55±11 years (range, 26-78 years). Out of 282 AVS procedures, 259 were successful, giving an overall success rate of 92%. The most common reason for failure was inability to localize the right adrenal vein (n=16; 76%). The success rates were 63%, 82%, and 94% during the first, second, and third years, respectively. During the last 8 years the success rate was 95%, and on average 27 procedures were performed annually. Satisfactory AVS success rate was achieved after approximately 36 procedures and satisfactory success rate was maintained by performing approximately 27 procedures annually. AVS should be limited to few operators that perform sufficiently large number of procedures to achieve, and maintain, satisfactory AVS success rate.

Multi-residue determination of seventeen sulfonamides and five tetracyclines in fish tissue using a multi-stage LC-ESI-MS/MS approach based on advanced mass spectrometric techniques.

PubMed

Dasenaki, Marilena E; Thomaidis, Nikolaos S

2010-07-05

A strategy was newly developed to rapidly screen seventeen sulfonamides and five tetracyclines in a single run from fish tissues using ultra-high performance liquid chromatography (UHPLC) coupled with comprehensive mass spectrometric approaches, including precursor-ion scan and data dependent scan. The product ions for precursor-ion scanning were selected by studying the MS/MS fragmentation of the analytes. All sulfonamides share the same diagnostic product ion at m/z 156 in positive MS/MS scan, while for tetracycline antibiotics the diagnostic product ion was proved to be at m/z 153.8. Further characterization of each compound was performed using a data dependent scan. Separation was performed on a Zorbax Eclipse Plus C18 column with a gradient elution using acetonitrile - 0.1% formic acid mobile phase at a flow rate of 0.1 mL min(-1). This approach has proven to be a powerful, highly selective, and sensitive tool for rapid screening and detection of non-targeted components in fish tissue and requires a minimum sample preparation such as one generic extraction step with MeOH:ACN 50:50 (v/v) acidified with 0.05% formic acid. The method has also been applied successfully to porcine and poultry meat. The validation of such a screening method was performed for the first time according to Commission Decision 2002/657/EC and satisfactory method performance characteristics were achieved. Copyright 2010 Elsevier B.V. All rights reserved.

20 CFR 627.422 - Selection of service providers.

Code of Federal Regulations, 2010 CFR

2010-04-01

... which provide training, such performance measures as retention in training, training completion, job... listed in paragraph (d) of this section; and may, if appropriate, be documented and described in the Job... ability to meet performance goals; (3) A satisfactory record of past performance (in job training, basic...

12 CFR 345.28 - Assigned ratings.

Code of Federal Regulations, 2010 CFR

2010-01-01

...,” “satisfactory,” “needs to improve,” or “substantial noncompliance” based on the bank's performance under the lending, investment and service tests, the community development test, the small bank performance... evaluation of a bank's CRA performance is adversely affected by evidence of discriminatory or other illegal...

Need assessment of staffs' welfare services at tehran university of medical sciences: a cross-sectional study.

PubMed

Dehghan, Reza; Mafimoradi, Shiva; Hadi, Mohammad

2015-01-01

Reviewing the human resources management literature shows an absence of attention given to the employee's benefits. Taking a look at functions of the Tehran University of Medical Sciences' wellbeing services system, it uncovers a gap between employees' real needs and what is delivered to meet their needs. So it requires an improved comprehensive system for delivering wellbeing services (financial, insurance, health care services, educational and training services, etc). Wellbeing need assessment can helps planners to identify vital needs of employee and response to them effectively. Moreover it can be used to evaluate the effectiveness of the current services which are delivered. Thus, the aim of this study is to assess wellbeing services of staffs working in TUMS to (1) evaluate the satisfactory rate of services which are delivered, and (2) exploring those wellbeing needs which were not fulfilled by the organization. Being a cross-sectional and analytic-descriptive survey including 98 responding participants, it is conducted by a questionnaire collecting employees' demographic information, their satisfactory rate of the implemented services, and determines unfulfilled wellbeing needs which were not already covered. Results indicated that services related to financial, educational, non-financial, insurance, occupational health and tourism/recreational services were the most satisfactory services successively. 'Staff's unwillingness to receive services' and 'poor announcement' (unawareness on the wellbeing services),' were found to be the most frequent reasons for not receiving the existing wellbeing services. To increase the satisfaction rate and responsiveness to the real needs of the staff, the current delivery system of wellbeing services in the TUMS should be redesigned by defining new wellbeing packages.

13 CFR 120.433 - What are SBA's other requirements for sales and sales of participating interests?

Code of Federal Regulations, 2012 CFR

2012-01-01

..., among other factors, will be considered in determining satisfactory SBA performance. Other factors may... (like default rate, purchase rate and loss rate), loan volume to the extent that it impacts performance...

Transformational, Transactional Leadership Styles and Job Performance of Academic Leaders

ERIC Educational Resources Information Center

Mahdinezhad, Maryam; Bin Suandi, Turiman; bin Silong, Abu Daud; Omar, Zoharah Binti

2013-01-01

In higher learning education, the performance is influenced by many factors. Effective leadership has an imperative role in the better performance and growth of the organization. Yet, several performance efforts were unsuccessful as a result of factors such as satisfactory leadership style of leaders. This study was carried out to identify the…

49 CFR 179.400-4 - Insulation system and performance standard.

Code of Federal Regulations, 2012 CFR

2012-10-01

... of heat transfer used for determining the satisfactory performance of the insulation system of a... 49 Transportation 3 2012-10-01 2012-10-01 false Insulation system and performance standard. 179... DOT-113 and 107A) § 179.400-4 Insulation system and performance standard. (a) For the purposes of this...

49 CFR 179.400-4 - Insulation system and performance standard.

Code of Federal Regulations, 2010 CFR

2010-10-01

... of heat transfer used for determining the satisfactory performance of the insulation system of a... 49 Transportation 2 2010-10-01 2010-10-01 false Insulation system and performance standard. 179... DOT-113 and 107A) § 179.400-4 Insulation system and performance standard. (a) For the purposes of this...

49 CFR 179.400-4 - Insulation system and performance standard.

Code of Federal Regulations, 2013 CFR

2013-10-01

... of heat transfer used for determining the satisfactory performance of the insulation system of a... 49 Transportation 3 2013-10-01 2013-10-01 false Insulation system and performance standard. 179... DOT-113 and 107A) § 179.400-4 Insulation system and performance standard. (a) For the purposes of this...

49 CFR 179.400-4 - Insulation system and performance standard.

Code of Federal Regulations, 2011 CFR

2011-10-01

... of heat transfer used for determining the satisfactory performance of the insulation system of a... 49 Transportation 3 2011-10-01 2011-10-01 false Insulation system and performance standard. 179... DOT-113 and 107A) § 179.400-4 Insulation system and performance standard. (a) For the purposes of this...

49 CFR 179.400-4 - Insulation system and performance standard.

Code of Federal Regulations, 2014 CFR

2014-10-01

... of heat transfer used for determining the satisfactory performance of the insulation system of a... 49 Transportation 3 2014-10-01 2014-10-01 false Insulation system and performance standard. 179... DOT-113 and 107A) § 179.400-4 Insulation system and performance standard. (a) For the purposes of this...

43 CFR 23.9 - Performance bond.

Code of Federal Regulations, 2013 CFR

2013-10-01

... 43 Public Lands: Interior 1 2013-10-01 2013-10-01 false Performance bond. 23.9 Section 23.9 Public... LANDS § 23.9 Performance bond. (a)(1) Upon approval of an exploration plan or mining plan, the operator shall be required to file a suitable performance bond of not less than $2,000 with satisfactory surety...

43 CFR 23.9 - Performance bond.

Code of Federal Regulations, 2012 CFR

2012-10-01

... 43 Public Lands: Interior 1 2012-10-01 2011-10-01 true Performance bond. 23.9 Section 23.9 Public... LANDS § 23.9 Performance bond. (a)(1) Upon approval of an exploration plan or mining plan, the operator shall be required to file a suitable performance bond of not less than $2,000 with satisfactory surety...

43 CFR 23.9 - Performance bond.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 43 Public Lands: Interior 1 2010-10-01 2010-10-01 false Performance bond. 23.9 Section 23.9 Public... LANDS § 23.9 Performance bond. (a)(1) Upon approval of an exploration plan or mining plan, the operator shall be required to file a suitable performance bond of not less than $2,000 with satisfactory surety...

43 CFR 23.9 - Performance bond.

Code of Federal Regulations, 2014 CFR

2014-10-01

... 43 Public Lands: Interior 1 2014-10-01 2014-10-01 false Performance bond. 23.9 Section 23.9 Public... LANDS § 23.9 Performance bond. (a)(1) Upon approval of an exploration plan or mining plan, the operator shall be required to file a suitable performance bond of not less than $2,000 with satisfactory surety...

Quality-Assurance Data for Routine Water Analyses by the U.S. Geological Survey Laboratory in Troy, New York-July 1997 through June 1999

USGS Publications Warehouse

Lincoln, Tricia A.; Horan-Ross, Debra A.; McHale, Michael R.; Lawrence, Gregory B.

2006-01-01

The laboratory for analysis of low-ionic-strength water at the U.S. Geological Survey (USGS) Water Science Center in Troy, N.Y., analyzes samples collected by USGS projects throughout the Northeast. The laboratory's quality-assurance program is based on internal and interlaboratory quality-assurance samples and quality-control procedures that were developed to ensure proper sample collection, processing, and analysis. The quality-assurance/quality-control data for the time period addressed in this report were stored in the laboratory's SAS data-management system, which provides efficient review, compilation, and plotting of data. This report presents and discusses results of quality-assurance and quality- control samples analyzed from July 1997 through June 1999. Results for the quality-control samples for 18 analytical procedures were evaluated for bias and precision. Control charts indicate that data for eight of the analytical procedures were occasionally biased for either high-concentration and (or) low-concentration samples but were within control limits; these procedures were: acid-neutralizing capacity, total monomeric aluminum, total aluminum, ammonium, calcium, chloride, specific conductance, and sulfate. The data from the potassium and sodium analytical procedures are insufficient for evaluation. Results from the filter-blank and analytical-blank analyses indicate that the procedures for 11 of 13 analytes were within control limits, although the concentrations for blanks were occasionally outside the control limits. Blank analysis results for chloride showed that 22 percent of blanks did not meet data-quality objectives and results for dissolved organic carbon showed that 31 percent of the blanks did not meet data-quality objectives. Sampling and analysis precision are evaluated herein in terms of the coefficient of variation obtained for triplicate samples in the procedures for 14 of the 18 analytes. At least 90 percent of the samples met data-quality objectives for all analytes except total aluminum (70 percent of samples met objectives) and potassium (83 percent of samples met objectives). Results of the USGS interlaboratory Standard Reference Sample (SRS) Project indicated good data quality for most constituents over the time period. The P-sample (low-ionic-strength constituents) analysis had good ratings in two of these studies and a satisfactory rating in the third. The results of the T-sample (trace constituents) analysis indicated high data quality with good ratings in all three studies. The N-sample (nutrient constituents) studies had one each of excellent, good, and satisfactory ratings. Results of Environment Canada's National Water Research Institute (NWRI) program indicated that at least 80 percent of the samples met data-quality objectives for 9 of the 13 analytes; the exceptions were dissolved organic carbon, ammonium, chloride, and specific conductance. Data-quality objectives were not met for dissolved organic carbon in two NWRI studies, but all of the samples were within control limits for the last study. Data-quality objectives were not met in 41 percent of samples analyzed for ammonium, 25 percent of samples analyzed for chloride, and 30 percent of samples analyzed for specific conductance. Results from blind reference-sample analyses indicated that data-quality objectives were met by at least 84 percent of the samples analyzed for calcium, chloride, magnesium, pH, and potassium. Data-quality objectives were met by 73 percent of those analyzed for sulfate. The data-quality objective was not met for sodium. The data are insufficient for evaluation of the specific conductance results.

Experimental and Analytical Seismic Studies of a Four-Span Bridge System with Innovative Materials

NASA Astrophysics Data System (ADS)

Cruz Noguez, Carlos Alonso

As part of a multi-university project utilizing the NSF Network for Earthquake Engineering Simulation (NEES), a quarter-scale model of a four-span bridge incorporating plastic hinges with different advanced materials was tested to failure on the three shake table system at the University of Nevada, Reno (UNR). The bridge was the second test model in a series of three 4-span bridges, with the first model being a conventional reinforced-concrete (RC) structure. The purpose of incorporating advanced materials was to improve the seismic performance of the bridge with respect to two damage indicators: (1) column damage and (2) permanent deformations. The goals of the study presented in this document were to (1) evaluate the seismic performance of a 4-span bridge system incorporating SMA/ECC and built-in rubber pad plastic hinges as well as post-tensioned piers, (2) quantify the relative merit of these advanced materials and details compared to each other and to conventional reinforced concrete plastic hinges, (3) determine the influence of abutment-superstructure interaction on the response, (4) examine the ability of available elaborate analytical modeling techniques to model the performance of advanced materials and details, and (5) conduct an extensive parametric study of different variations of the bridge model to study several important issues in bridge earthquake engineering. The bridge model included six columns, each pair of which utilized a different advanced detail at bottom plastic hinges: shape memory alloys (SMA), special engineered cementitious composites (ECC), elastomeric pads embedded into columns, and post-tensioning tendons. The design of the columns, location of the bents, and selection of the loading protocol were based on pre-test analyses conducted using computer program OpenSees. The bridge model was subjected to two-horizontal components of simulated earthquake records of the 1994 Northridge earthquake. Over 340 channels of data were collected. The test results showed the effectiveness of the advanced materials in reducing damage and permanent displacements. The damage was minimal in plastic hinges with SMA/ECC and those with built-in elastomeric pads. Conventional RC plastic hinges were severely damaged due to spalling of concrete and rupture of the longitudinal and transverse reinforcement. Extensive post-test analytical studies were conducted and it was determined that a computational model of the bridge that included bridge-abutment interaction using OpenSees was able to provide satisfactory estimations of key structural parameters such as superstructure displacements and base shears. The analytical model was also used to conduct parametric studies on single-column and bridge-system response under near-fault ground motions. The effects of vertical excitations and transverse shear-keys at the bridge abutments on the superstructure displacement and column drifts were also explored.

Development of a SPME-GC-MS method for the determination of volatile compounds in Shanxi aged vinegar and its analytical characterization by aroma wheel.

PubMed

Zhu, Hong; Zhu, Jie; Wang, Lili; Li, Zaigui

2016-01-01

A solid-phase microextraction followed by gas chromatography-mass spectrometry method was developed to determine the volatile compounds in Shanxi aged vinegar. The optimal extraction conditions were: 50 °C for 20 min with a PDMS/DVB fiber. This analytical method was validated and showed satisfactory repeatability (0.5 %

Evaluation of the Technicon Axon analyser.

PubMed

Martínez, C; Márquez, M; Cortés, M; Mercé, J; Rodriguez, J; González, F

1990-01-01

An evaluation of the Technicon Axon analyser was carried out following the guidelines of the 'Sociedad Española de Química Clínica' and the European Committee for Clinical Laboratory Standards.A photometric study revealed acceptable results at both 340 nm and 404 nm. Inaccuracy and imprecision were lower at 404 nm than at 340 nm, although poor dispersion was found at both wavelengths, even at low absorbances. Drift was negligible, the imprecision of the sample pipette delivery system was greater for small sample volumes, the reagent pipette delivery system imprecision was acceptable and the sample diluting system study showed good precision and accuracy.Twelve analytes were studied for evaluation of the analyser under routine working conditions. Satisfactory results were obtained for within-run imprecision, while coefficients of variation for betweenrun imprecision were much greater than expected. Neither specimenrelated nor specimen-independent contamination was found in the carry-over study. For all analytes assayed, when comparing patient sample results with those obtained in a Hitachi 737 analyser, acceptable relative inaccuracy was observed.

Sequential Injection Chromatography with an Ultra-short Monolithic Column for the Low-Pressure Separation of α-Tocopherol and γ-Oryzanol in Vegetable Oils and Nutrition Supplements.

PubMed

Thaithet, Sujitra; Kradtap Hartwell, Supaporn; Lapanantnoppakhun, Somchai

2017-01-01

A low-pressure separation procedure of α-tocopherol and γ-oryzanol was developed based on a sequential injection chromatography (SIC) system coupled with an ultra-short (5 mm) C-18 monolithic column, as a lower cost and more compact alternative to the HPLC system. A green sample preparation, dilution with a small amount of hexane followed by liquid-liquid extraction with 80% ethanol, was proposed. Very good separation resolution (R s = 3.26), a satisfactory separation time (10 min) and a total run time including column equilibration (16 min) were achieved. The linear working range was found to be 0.4 - 40 μg with R 2 being more than 0.99. The detection limits of both analytes were 0.28 μg with the repeatability within 5% RSD (n = 7). Quantitative analyses of the two analytes in vegetable oil and nutrition supplement samples, using the proposed SIC method, agree well with the results from HPLC.

Two-dimensional fracture analysis of piezoelectric material based on the scaled boundary node method

NASA Astrophysics Data System (ADS)

Shen-Shen, Chen; Juan, Wang; Qing-Hua, Li

2016-04-01

A scaled boundary node method (SBNM) is developed for two-dimensional fracture analysis of piezoelectric material, which allows the stress and electric displacement intensity factors to be calculated directly and accurately. As a boundary-type meshless method, the SBNM employs the moving Kriging (MK) interpolation technique to an approximate unknown field in the circumferential direction and therefore only a set of scattered nodes are required to discretize the boundary. As the shape functions satisfy Kronecker delta property, no special techniques are required to impose the essential boundary conditions. In the radial direction, the SBNM seeks analytical solutions by making use of analytical techniques available to solve ordinary differential equations. Numerical examples are investigated and satisfactory solutions are obtained, which validates the accuracy and simplicity of the proposed approach. Project supported by the National Natural Science Foundation of China (Grant Nos. 11462006 and 21466012), the Foundation of Jiangxi Provincial Educational Committee, China (Grant No. KJLD14041), and the Foundation of East China Jiaotong University, China (Grant No. 09130020).

Comparison of theoretical and experimental boundary-layer development in a Mach 2.5 mixed-compression inlet

NASA Technical Reports Server (NTRS)

Hingst, W. R.; Towne, C. E.

1974-01-01

An analytical investigation was made of the boundary layer flow in an axisymmetric Mach 2.5 mixed compression inlet, and the results were compared with experimental measurements. The inlet tests were conducted in the Lewis 10- by 10-foot supersonic wind tunnel at a unit Reynolds number of 8.2 million/m. The inlet incorporated porous bleed regions for boundary layer control, and the effect of this bleed was taken into account in the analysis. The experimental boundary layer data were analyzed by using similarity laws from which the skin friction coefficient was obtained. The boundary layer analysis included predictions of laminar and turbulent boundary layer growth, transition, and the effects of the shock boundary layer interactions. In addition, the surface static pressures were compared with those obtained from an inviscid characteristics program. The results of investigation showed that the analytical techniques gave satisfactory predictions of the boundary layer flow except in regions that were badly distorted by the terminal shock.

The National energy modeling system

NASA Astrophysics Data System (ADS)

The DOE uses a variety of energy and economic models to forecast energy supply and demand. It also uses a variety of more narrowly focussed analytical tools to examine energy policy options. For the purpose of the scope of this work, this set of models and analytical tools is called the National Energy Modeling System (NEMS). The NEMS is the result of many years of development of energy modeling and analysis tools, many of which were developed for different applications and under different assumptions. As such, NEMS is believed to be less than satisfactory in certain areas. For example, NEMS is difficult to keep updated and expensive to use. Various outputs are often difficult to reconcile. Products were not required to interface, but were designed to stand alone. Because different developers were involved, the inner workings of the NEMS are often not easily or fully understood. Even with these difficulties, however, NEMS comprises the best tools currently identified to deal with our global, national and regional energy modeling, and energy analysis needs.

The detection of problem analytes in a single proficiency test challenge in the absence of the Health Care Financing Administration rule violations.

PubMed

Cembrowski, G S; Hackney, J R; Carey, N

1993-04-01

The Clinical Laboratory Improvement Act of 1988 (CLIA 88) has dramatically changed proficiency testing (PT) practices having mandated (1) satisfactory PT for certain analytes as a condition of laboratory operation, (2) fixed PT limits for many of these "regulated" analytes, and (3) an increased number of PT specimens (n = 5) for each testing cycle. For many of these analytes, the fixed limits are much broader than the previously employed Standard Deviation Index (SDI) criteria. Paradoxically, there may be less incentive to identify and evaluate analytically significant outliers to improve the analytical process. Previously described "control rules" to evaluate these PT results are unworkable as they consider only two or three results. We used Monte Carlo simulations of Kodak Ektachem analyzers participating in PT to determine optimal control rules for the identification of PT results that are inconsistent with those from other laboratories using the same methods. The analysis of three representative analytes, potassium, creatine kinase, and iron was simulated with varying intrainstrument and interinstrument standard deviations (si and sg, respectively) obtained from the College of American Pathologists (Northfield, Ill) Quality Assurance Services data and Proficiency Test data, respectively. Analytical errors were simulated in each of the analytes and evaluated in terms of multiples of the interlaboratory SDI. Simple control rules for detecting systematic and random error were evaluated with power function graphs, graphs of probability of error detected vs magnitude of error. Based on the simulation results, we recommend screening all analytes for the occurrence of two or more observations exceeding the same +/- 1 SDI limit. For any analyte satisfying this condition, the mean of the observations should be calculated. For analytes with sg/si ratios between 1.0 and 1.5, a significant systematic error is signaled by the mean exceeding 1.0 SDI. Significant random error is signaled by one observation exceeding the +/- 3-SDI limit or the range of the observations exceeding 4 SDIs. For analytes with higher sg/si, significant systematic or random error is signaled by violation of the screening rule (having at least two observations exceeding the same +/- 1 SDI limit). Random error can also be signaled by one observation exceeding the +/- 1.5-SDI limit or the range of the observations exceeding 3 SDIs. We present a practical approach to the workup of apparent PT errors.

USE OF FAST GC/TOFMS AS REFERENCE STANDARD FOR FIELD COMPARISON STUDIES WITH ON-SITE INSTRUMENTS

EPA Science Inventory

A faster reference standard for field comparison studies of portable gas chromatographs (PGC) is needed. A performance evaluation of a high-speed GCMS (FGC/MS) system conducted during 1998 demonstrated generally satisfactory performance, but it was evident that performance of b...

Effect of duct shape, Mach number, and lining construction on measured suppressor attenuation and comparison with theory

NASA Technical Reports Server (NTRS)

Olsen, W. A.; Krejsa, E. A.; Coats, J. W.

1972-01-01

Noise attenuation was measured for several types of cylindrical suppressors that use a duct lining composed of honeycomb cells covered with a perforated plate. The experimental technique used gave attenuation data that were repeatable and free of noise floors and other sources of error. The suppressor length, the effective acoustic diameter, suppressor shape and flow velocity were varied. The agreement among the attenuation data and two widely used analytical models was generally satisfactory. Changes were also made in the construction of the acoustic lining to measure their effect on attenuation. One of these produced a very broadband muffler.

Solution of non-steady-state substrate concentration in the action of biosensor response at mixed enzyme kinetics

NASA Astrophysics Data System (ADS)

Senthamarai, R.; Jana Ranjani, R.

2018-04-01

In this paper, a mathematical model of an amperometric biosensor at mixed enzyme kinetics and diffusion limitation in the case of substrate inhibition has been developed. The model is based on time dependent reaction diffusion equation containing a non -linear term related to non -Michaelis - Menten kinetics of the enzymatic reaction. Solution for the concentration of the substrate has been derived for all values of parameters using the homotopy perturbation method. All the approximate analytic expressions of substrate concentration are compared with simulation results using Scilab/Matlab program. Finally, we have given a satisfactory agreement between them.

Evaluation of Superparamagnetic Silica Nanoparticles for Extraction of Triazines in Magnetic in-Tube Solid Phase Microextraction Coupled to Capillary Liquid Chromatography

PubMed Central

González-Fuenzalida, R. A.; Moliner-Martínez, Y.; Prima-Garcia, Helena; Ribera, Antonio; Campins-Falcó, P.; Zaragozá, Ramon J.

2014-01-01

The use of magnetic nanomaterials for analytical applications has increased in the recent years. In particular, magnetic nanomaterials have shown great potential as adsorbent phase in several extraction procedures due to the significant advantages over the conventional methods. In the present work, the influence of magnetic forces over the extraction efficiency of triazines using superparamagnetic silica nanoparticles (NPs) in magnetic in tube solid phase microextraction (Magnetic-IT-SPME) coupled to CapLC has been evaluated. Atrazine, terbutylazine and simazine has been selected as target analytes. The superparamagnetic silica nanomaterial (SiO2-Fe3O4) deposited onto the surface of a capillary column gave rise to a magnetic extraction phase for IT-SPME that provided a enhancemment of the extraction efficiency for triazines. This improvement is based on two phenomena, the superparamegnetic behavior of Fe3O4 NPs and the diamagnetic repulsions that take place in a microfluidic device such a capillary column. A systematic study of analytes adsorption and desorption was conducted as function of the magnetic field and the relationship with triazines magnetic susceptibility. The positive influence of magnetism on the extraction procedure was demonstrated. The analytical characteristics of the optimized procedure were established and the method was applied to the determination of the target analytes in water samples with satisfactory results. When coupling Magnetic-IT-SPME with CapLC, improved adsorption efficiencies (60%–63%) were achieved compared with conventional adsorption materials (0.8%–3%). PMID:28344221

Determination of endocrine-disrupting compounds in drinking waters by fast liquid chromatography-tandem mass spectrometry.

PubMed

Magi, Emanuele; Scapolla, Carlo; Di Carro, Marina; Liscio, Camilla

2010-09-01

Growing attention has been recently paid to safety of food and drinking water, making necessary the adoption of policies for water sources protection and the development of sensitive and rapid analytical methods to identify micropollutants. Endocrine-disrupting compounds (EDCs) have emerged as a major issue as they alter the functioning of the endocrine system. Since ingestion of EDCs via food is considered the major exposure route, there is a growing interest in understanding EDC fate during drinking water treatment and in monitoring potential contamination of surface waters and groundwaters. In this work, a fast liquid chromatography-electrospray ionization-tandem mass spectrometry method was developed for the determination of 4-n-nonylphenol (NP), bisphenol A (BPA), estrone (E1), 17β-estradiol (E2) and 17α-ethinylestradiol (EE2) in drinking waters. In the literature analytical articles seldom provide details regarding fragmentation pathways. In this paper spectra of the five EDCs in negative ESI were interpreted with the support of accurate mass spectra acquired by a quadrupole time-of-flight instrument; fragmentation pathways were also proposed. The chromatographic separation of EDCs was optimized on a Pinnacle DB Biphenylic column with a water-acetonitrile gradient. Quantitative analysis was performed in multiple reaction monitoring (MRM) mode using bisphenol A-d(16) (BPA-d(16)) as internal standard; calibration curves showed good correlation coefficients (0.9989-0.9997). All figures of merit of the method were satisfactory; limits of detection were in the range 0.2-0.4 ng/ml. The method was applied to the determination of the analytes in waters sampled by polar organic chemical integrative samplers in a drinking water treatment plant. Rather low concentration of BPA, NP and E1 were measured in the inlet, while none of the considered EDCs was detected in the outlet. 2010 John Wiley & Sons, Ltd.

Trace analysis and occurrence of anhydroerythromycin and tylosin in influent and effluent wastewater by liquid chromatography combined with electrospray tandem mass spectrometry.

PubMed

Yang, Shinwoo; Cha, Jongmun; Carlson, Kenneth

2006-06-01

Two wastewater treatment plants (WWTPs) of northern Colorado were monitored for anhydroerythromycin and tylosin. An analytical method has been developed and validated for the trace determination and confirmation of these compounds in the raw influent and final effluent water matrices. This method was used to evaluate the occurrence and fate of these compounds in WWTPs. The method uses solid-phase extraction and liquid chromatography-tandem mass spectrometry with positive electrospray ionization. Detection and quantification was performed using selected reaction monitoring, and a method detection limit of between 0.01 and 0.06 microg/L was obtained. Unequivocal confirmation analysis of analyte identity according to the criteria (based on the use of identification points) of the 2002/657/EC European Commission Decision was possible with satisfactory results. Average recoveries for the two compounds ranged from 89.2+/-9.7% for raw influent to 93.7+/-6.9% for effluent wastewaters. The within-run precision of the assay was found to be always less than 14.1% for the two analytes. The overall precision was always less than 13.7%. The relative uncertainty of the present assay was also evaluated and the combined relative uncertainty ranged from 6.4 to 15.5% over three days of the validation study. These compounds were partially removed in the WWTPs with a removal efficiency of >50%. The measured concentrations in raw influents and effluents ranged from 0.09-0.35 and 0.04-0.12 microg/L for anhydroerythromycin to 0.06-0.18 and ND-0.06 microg/L for tylosin, respectively. The results indicate that WWTP effluents are relevant point sources for residues of these compounds in the aquatic environment. These occurrence results were compared with those in WWTP wastewaters of other countries.

Using PAT to accelerate the transition to continuous API manufacturing.

PubMed

Gouveia, Francisca F; Rahbek, Jesper P; Mortensen, Asmus R; Pedersen, Mette T; Felizardo, Pedro M; Bro, Rasmus; Mealy, Michael J

2017-01-01

Significant improvements can be realized by converting conventional batch processes into continuous ones. The main drivers include reduction of cost and waste, increased safety, and simpler scale-up and tech transfer activities. Re-designing the process layout offers the opportunity to incorporate a set of process analytical technologies (PAT) embraced in the Quality-by-Design (QbD) framework. These tools are used for process state estimation, providing enhanced understanding of the underlying variability in the process impacting quality and yield. This work describes a road map for identifying the best technology to speed-up the development of continuous processes while providing the basis for developing analytical methods for monitoring and controlling the continuous full-scale reaction. The suitability of in-line Raman, FT-infrared (FT-IR), and near-infrared (NIR) spectroscopy for real-time process monitoring was investigated in the production of 1-bromo-2-iodobenzene. The synthesis consists of three consecutive reaction steps including the formation of an unstable diazonium salt intermediate, which is critical to secure high yield and avoid formation of by-products. All spectroscopic methods were able to capture critical information related to the accumulation of the intermediate with very similar accuracy. NIR spectroscopy proved to be satisfactory in terms of performance, ease of installation, full-scale transferability, and stability to very adverse process conditions. As such, in-line NIR was selected to monitor the continuous full-scale production. The quantitative method was developed against theoretical concentration values of the intermediate since representative sampling for off-line reference analysis cannot be achieved. The rapid and reliable analytical system allowed the following: speeding up the design of the continuous process and a better understanding of the manufacturing requirements to ensure optimal yield and avoid unreacted raw materials and by-products in the continuous reactor effluent. Graphical Abstract Using PAT to accelerate the transition to continuous API manufacturing.

Automated Mini-Column Solid-Phase Extraction Cleanup for High-Throughput Analysis of Chemical Contaminants in Foods by Low-Pressure Gas Chromatography-Tandem Mass Spectrometry.

PubMed

Lehotay, Steven J; Han, Lijun; Sapozhnikova, Yelena

2016-01-01

This study demonstrated the application of an automated high-throughput mini-cartridge solid-phase extraction (mini-SPE) cleanup for the rapid low-pressure gas chromatography-tandem mass spectrometry (LPGC-MS/MS) analysis of pesticides and environmental contaminants in QuEChERS extracts of foods. Cleanup efficiencies and breakthrough volumes using different mini-SPE sorbents were compared using avocado, salmon, pork loin, and kale as representative matrices. Optimum extract load volume was 300 µL for the 45 mg mini-cartridges containing 20/12/12/1 (w/w/w/w) anh. MgSO 4 /PSA (primary secondary amine)/C 18 /CarbonX sorbents used in the final method. In method validation to demonstrate high-throughput capabilities and performance results, 230 spiked extracts of 10 different foods (apple, kiwi, carrot, kale, orange, black olive, wheat grain, dried basil, pork, and salmon) underwent automated mini-SPE cleanup and analysis over the course of 5 days. In all, 325 analyses for 54 pesticides and 43 environmental contaminants (3 analyzed together) were conducted using the 10 min LPGC-MS/MS method without changing the liner or retuning the instrument. Merely, 1 mg equivalent sample injected achieved <5 ng g -1 limits of quantification. With the use of internal standards, method validation results showed that 91 of the 94 analytes including pairs achieved satisfactory results (70-120 % recovery and RSD ≤ 25 %) in the 10 tested food matrices ( n  = 160). Matrix effects were typically less than ±20 %, mainly due to the use of analyte protectants, and minimal human review of software data processing was needed due to summation function integration of analyte peaks. This study demonstrated that the automated mini-SPE + LPGC-MS/MS method yielded accurate results in rugged, high-throughput operations with minimal labor and data review.

Multi-class multi-residue analysis of veterinary drugs in meat using enhanced matrix removal lipid cleanup and liquid chromatography-tandem mass spectrometry.

PubMed

Zhao, Limian; Lucas, Derick; Long, David; Richter, Bruce; Stevens, Joan

2018-05-11

This study presents the development and validation of a quantitation method for the analysis of multi-class, multi-residue veterinary drugs using lipid removal cleanup cartridges, enhanced matrix removal lipid (EMR-Lipid), for different meat matrices by liquid chromatography tandem mass spectrometry detection. Meat samples were extracted using a two-step solid-liquid extraction followed by pass-through sample cleanup. The method was optimized based on the buffer and solvent composition, solvent additive additions, and EMR-Lipid cartridge cleanup. The developed method was then validated in five meat matrices, porcine muscle, bovine muscle, bovine liver, bovine kidney and chicken liver to evaluate the method performance characteristics, such as absolute recoveries and precision at three spiking levels, calibration curve linearity, limit of quantitation (LOQ) and matrix effect. The results showed that >90% of veterinary drug analytes achieved satisfactory recovery results of 60-120%. Over 97% analytes achieved excellent reproducibility results (relative standard deviation (RSD) < 20%), and the LOQs were 1-5 μg/kg in the evaluated meat matrices. The matrix co-extractive removal efficiency by weight provided by EMR-lipid cartridge cleanup was 42-58% in samples. The post column infusion study showed that the matrix ion suppression was reduced for samples with the EMR-Lipid cartridge cleanup. The reduced matrix ion suppression effect was also confirmed with <15% frequency of compounds with significant quantitative ion suppression (>30%) for all tested veterinary drugs in all of meat matrices. The results showed that the two-step solid-liquid extraction provides efficient extraction for the entire spectrum of veterinary drugs, including the difficult classes such as tetracyclines, beta-lactams etc. EMR-Lipid cartridges after extraction provided efficient sample cleanup with easy streamlined protocol and minimal impacts on analytes recovery, improving method reliability and consistency. Copyright © 2018 Elsevier B.V. All rights reserved.

Simultaneous determination of organophosphorus pesticides in fruits and vegetables using atmospheric pressure gas chromatography quadrupole-time-of-flight mass spectrometry.

PubMed

Cheng, Zhipeng; Dong, Fengshou; Xu, Jun; Liu, Xingang; Wu, Xiaohu; Chen, Zenglong; Pan, Xinglu; Gan, Jay; Zheng, Yongquan

2017-09-15

This paper describes the application of atmospheric pressure gas chromatography quadrupole-time-of-flight mass spectrometry for the simultaneous determination of organophosphorus pesticides in apple, pear, tomato, cucumber and cabbage. Soft ionization with atmospheric pressure ionization source was compared with traditional electron impact ionization (EI). The sensitivity of GC coupled to atmospheric pressure ionization (APGC) for all the analytes was enhanced by 1.0-8.2 times. The ionization modes with atmospheric pressure ionization source was studied by comparing the charge-transfer and proton-transfer conditions. The optimized QuEChERs method was used to pretreat the samples. The calibration curves were found linear from 10 to 1000μg/L, obtaining correlation coefficients higher than 0.9845. Satisfactory mean recovery values, in the range of 70.0-115.9%, and satisfactory precision, with all RSD r <19.7% and all RSD R values <19.5% at the three fortified concentration levels for all the fifteen OPPs. The results demonstrate the potential of APGC-QTOF-MS for routine quantitative analysis of organophosphorus pesticide in fruits and vegetables. Copyright © 2017 Elsevier Ltd. All rights reserved.

A paper-based nanomodified electrochemical biosensor for ethanol detection in beers.

PubMed

Cinti, Stefano; Basso, Mattia; Moscone, Danila; Arduini, Fabiana

2017-04-01

Herein, we report the first example of a paper-based screen-printed biosensor for the detection of ethanol in beer samples. Common office paper was adopted to fabricate the analytical device. The properties of this paper-based screen-printed electrode (SPE) were investigated by cyclic voltammetry, electrochemical impedance spectroscopy, and scanning electron microscopy, and they were compared with the well-established polyester-based SPEs as well. Paper demonstrated similar properties when compared with polyester, highlighting suitability towards its utilization in sensor development, with the advantages of low cost and simple disposal by incineration. A nanocomposite formed by Carbon Black (CB) and Prussian Blue nanoparticles (PBNPs), namely CB/PBNPs, was utilized as an electrocatalyst to detect the hydrogen peroxide generated by the enzymatic reaction between alcohol oxidase (AOx) and ethanol. After optimizing the analytical parameters, such as pH, enzyme, concentration, and working potential, the developed biosensor allowed a facile quantification of ethanol up to 10 mM (0.058 % vol ), with a sensitivity of 9.13 μA/mM cm 2 (1574 μA/% vol cm 2 ) and a detection limit equal to 0.52 mM (0.003% vol ). These satisfactory performances rendered the realized paper-based biosensor reliable over the analysis of ethanol contained in four different types of beers, including Pilsner, Weiss, Lager, and alcohol-free. The proposed manufacturing approach offers an affordable and sustainable tool for food quality control and for the realization of different electrochemical sensors and biosensors as well. Copyright © 2017 Elsevier B.V. All rights reserved.

RP-HPLC×HILIC chromatography for quantifying ertapenem sodium with a look at green chemistry.

PubMed

Pedroso, Tahisa M; Medeiros, Ana C D; Salgado, Herida R N

2016-11-01

Ertapenem sodium is a polar and ionizable compound; therefore, it has little retention on traditional C18 columns in reverse-phase high-performance liquid chromatography, even using a highly-aqueous mobile phase that can result in dewetting in the stationary phase. Thus, the most coherent process for ERTM is to develop a method for Hydrophilic Interaction Chromatography. However, for the traditional methods in HILIC, the use of a highly organic mobile phase is necessary; usually an amount exceeding 80% acetonitrile is necessary. On the other hand, the RP-HPLC mode is considered for the analysis technique, which is more often used for quantification of substances, and new columns are often introduced to analyze different groups of compounds. Two new analytical methods have been developed for routine analysis. The proposed chromatographic method was adequate and advantageous by presenting simplicity, linearity, precision, accuracy, robustness, detection limits, and satisfactory quantification. Analytical methods are constantly undergoing changes and improvements. Researchers worldwide are rapidly adopting Green Chemistry. The development of new pharmaceutical methods based in Green chemistry has been encouraged by universities and the pharmaceutical industry. Issues related to green chemistry are in evidence and they have been featured in international journals of high impact. The methods described here have economic advantages and they feature an eco-friendly focus, which is discussed in this work. This work was developed with an environmental conscience, always looking to minimize the possible generated organic waste. Therefore, discussion on this aspect is included. Copyright © 2016 Elsevier B.V. All rights reserved.

Simultaneous determination of 24 polycyclic aromatic hydrocarbons in edible oil by tandem solid-phase extraction and gas chromatography coupled/tandem mass spectrometry.

PubMed

Xu, Ting; Tang, Hua; Chen, Dazhou; Dong, Haifeng; Li, Lei

2015-01-01

An efficient and fast tandem SPE method followed by GC/MS/MS has been developed for the determination and the quantification of 24 polycyclic aromatic hydrocarbons (PAHs) in edible oil. This method includes the monitoring of 15 + 1 PAHs designated as a priority by the European Union in their 2005/108/EC recommendation and 16 PAHs listed by the U. S. Environmental Protection Agency. The sample preparation procedures were based on SPE in which PAH-dedicated cartridges with molecularly imprinted polymers and graphitized carbon black were used in series. The novel tandem SPE combination of selective extraction and purification of light and heavy PAHs provided highly purified analytes. Identification and quantification of 24 target PAHs were performed using GC/MS/MS with the isotope dilution approaches using D-labeled and (13)C-labeled PAHs. The advantages of GC/MS/MS as compared to other detection methods include high sensitivity, selectivity, and interpretation ability. The method showed satisfactory linearity (R(2) > 0.998) over the range assayed (0.5-200 μg/kg); the LODs ranged from 0.03 to 0.6 μg/kg, and LOQs from 0.1 to 2.0 μg/kg. The recoveries using this method at three spiked concentration levels (2, 10, and 50 μg/kg) ranged from 56.8 to 117.7%. The RSD was lower than 12.7% in all cases. The proposed analytical method has been successfully applied for the analysis of the 24 PAHs in edible oil.

Micellar and analytical implications of a new potentiometric PVC sensor based on neutral ion-pair complexes of dodecylmethylimidazolium bromide-sodium dodecylsulfate.

PubMed

Sanan, Reshu; Mahajan, Rakesh Kumar

2013-03-15

With an aim to characterize the micellar aggregates of imidazolium based ionic liquids, a new potentiometric PVC sensor based on neutral ion-pair complexes of dodecylmethylimidazolium bromide-sodium dodecylsulfate (C12MeIm(+)DS(-)) has been developed. The electrode exhibited a linear response for the concentration range of 7.9×10(-5)-9.8×10(-3) M with a super-Nernstian slope of 92.94 mV/decade, a response time of 5 s and critical micellar concentration (cmc) of 10.09 mM for C12MeImBr. The performance of the electrode in investigating the cmc of C12MeImBr in the presence of two drugs [promazine hydrochloride (PMZ) and promethazine hydrochloride (PMT)] and three triblock copolymers (P123, L64 and F68) has been found to be satisfactory on comparison with conductivity measurements. Various micellar parameters have been evaluated for the binary mixtures of C12MeImBr with drugs and triblock copolymers using Clint's, Rubingh's, and Motomura's approach. Thus the electrode offers a simple, straightforward and relatively fast technique for the characterization of micellar aggregates of C12MeImBr, complementing existing conventional techniques. Further, the analytical importance of proposed C12MeIm(+)-ISE as end point indicator in potentiometric titrations and for direct determination of cationic surfactants [cetylpyridinium chloride (CPC), tetradecyltrimethylammonium bromide (TTAB), benzalkonium chloride (BC)] in some commercial products was judged by comparing statistically with classical two-phase titration methods. Copyright © 2013 Elsevier Inc. All rights reserved.

Modeling of the dispersion of depleted uranium aerosol.

PubMed

Mitsakou, C; Eleftheriadis, K; Housiadas, C; Lazaridis, M

2003-04-01

Depleted uranium is a low-cost radioactive material that, in addition to other applications, is used by the military in kinetic energy weapons against armored vehicles. During the Gulf and Balkan conflicts concern has been raised about the potential health hazards arising from the toxic and radioactive material released. The aerosol produced during impact and combustion of depleted uranium munitions can potentially contaminate wide areas around the impact sites or can be inhaled by civilians and military personnel. Attempts to estimate the extent and magnitude of the dispersion were until now performed by complex modeling tools employing unclear assumptions and input parameters of high uncertainty. An analytical puff model accommodating diffusion with simultaneous deposition is developed, which can provide a reasonable estimation of the dispersion of the released depleted uranium aerosol. Furthermore, the period of the exposure for a given point downwind from the release can be estimated (as opposed to when using a plume model). The main result is that the depleted uranium mass is deposited very close to the release point. The deposition flux at a couple of kilometers from the release point is more than one order of magnitude lower than the one a few meters near the release point. The effects due to uncertainties in the key input variables are addressed. The most influential parameters are found to be atmospheric stability, height of release, and wind speed, whereas aerosol size distribution is less significant. The output from the analytical model developed was tested against the numerical model RPM-AERO. Results display satisfactory agreement between the two models.

Nondestructive atomic compositional analysis of BeMgZnO quaternary alloys using ion beam analytical techniques

NASA Astrophysics Data System (ADS)

Zolnai, Z.; Toporkov, M.; Volk, J.; Demchenko, D. O.; Okur, S.; Szabó, Z.; Özgür, Ü.; Morkoç, H.; Avrutin, V.; Kótai, E.

2015-02-01

The atomic composition with less than 1-2 atom% uncertainty was measured in ternary BeZnO and quaternary BeMgZnO alloys using a combination of nondestructive Rutherford backscattering spectrometry with 1 MeV He+ analyzing ion beam and non-Rutherford elastic backscattering experiments with 2.53 MeV energy protons. An enhancement factor of 60 in the cross-section of Be for protons has been achieved to monitor Be atomic concentrations. Usually the quantitative analysis of BeZnO and BeMgZnO systems is challenging due to difficulties with appropriate experimental tools for the detection of the light Be element with satisfactory accuracy. As it is shown, our applied ion beam technique, supported with the detailed simulation of ion stopping, backscattering, and detection processes allows of quantitative depth profiling and compositional analysis of wurtzite BeZnO/ZnO/sapphire and BeMgZnO/ZnO/sapphire layer structures with low uncertainty for both Be and Mg. In addition, the excitonic bandgaps of the layers were deduced from optical transmittance measurements. To augment the measured compositions and bandgaps of BeO and MgO co-alloyed ZnO layers, hybrid density functional bandgap calculations were performed with varying the Be and Mg contents. The theoretical vs. experimental bandgaps show linear correlation in the entire bandgap range studied from 3.26 eV to 4.62 eV. The analytical method employed should help facilitate bandgap engineering for potential applications, such as solar blind UV photodetectors and heterostructures for UV emitters and intersubband devices.

Surfactant-enhanced spectrofluorimetric determination of total aflatoxins from wheat samples after magnetic solid-phase extraction using modified Fe3O4 nanoparticles

NASA Astrophysics Data System (ADS)

Manafi, Mohammad Hanif; Allahyari, Mehdi; Pourghazi, Kamyar; Amoli-Diva, Mitra; Taherimaslak, Zohreh

2015-07-01

The extraction and preconcentration of total aflatoxins (including aflatoxin B1, B2, G1, and G2) using magnetic nanoparticles based solid phase extraction (MSPE) followed by surfactant-enhanced spectrofluorimetric detection was proposed. Ethylene glycol bis-mercaptoacetate modified silica coated Fe3O4 nanoparticles as an efficient antibody-free adsorbent was successfully applied to extract aflatoxins from wheat samples. High surface area and strong magnetization properties of magnetic nanoparticles were utilized to achieve high enrichment factor (97), and satisfactory recoveries (92-105%) using only 100 mg of the adsorbent. Furthermore, the fast separation time (less than 10 min) avoids many time-consuming cartridge loading or column-passing procedures accompany with the conventional SPE. In determination step, signal enhancement was performed by formation of Triton X-100 micelles around the analytes in 15% (v/v) acetonitrile-water which dramatically increase the sensitivity of the method. Main factors affecting the extraction efficiency and signal enhancement of the analytes including pH of sample solution, desorption conditions, extraction time, sample volume, adsorbent amount, surfactant concentration and volume and time of micelle formation were evaluated and optimized. Under the optimum conditions, wide linear range of 0.1-50 ng mL-1 with low detection limit of 0.03 ng mL-1 were obtained. The developed method was successfully applied to the extraction and preconcentration of aflatoxins in three commercially available wheat samples and the results were compared with the official AOAC method.

Immunosuppressant therapeutic drug monitoring by LC-MS/MS: workflow optimization through automated processing of whole blood samples.

PubMed

Marinova, Mariela; Artusi, Carlo; Brugnolo, Laura; Antonelli, Giorgia; Zaninotto, Martina; Plebani, Mario

2013-11-01

Although, due to its high specificity and sensitivity, LC-MS/MS is an efficient technique for the routine determination of immunosuppressants in whole blood, it involves time-consuming manual sample preparation. The aim of the present study was therefore to develop an automated sample-preparation protocol for the quantification of sirolimus, everolimus and tacrolimus by LC-MS/MS using a liquid handling platform. Six-level commercially available blood calibrators were used for assay development, while four quality control materials and three blood samples from patients under immunosuppressant treatment were employed for the evaluation of imprecision. Barcode reading, sample re-suspension, transfer of whole blood samples into 96-well plates, addition of internal standard solution, mixing, and protein precipitation were performed with a liquid handling platform. After plate filtration, the deproteinised supernatants were submitted for SPE on-line. The only manual steps in the entire process were de-capping of the tubes, and transfer of the well plates to the HPLC autosampler. Calibration curves were linear throughout the selected ranges. The imprecision and accuracy data for all analytes were highly satisfactory. The agreement between the results obtained with manual and those obtained with automated sample preparation was optimal (n=390, r=0.96). In daily routine (100 patient samples) the typical overall total turnaround time was less than 6h. Our findings indicate that the proposed analytical system is suitable for routine analysis, since it is straightforward and precise. Furthermore, it incurs less manual workload and less risk of error in the quantification of whole blood immunosuppressant concentrations than conventional methods. © 2013.

13 CFR 120.424 - What are the basic conditions a Lender must meet to securitize?

Code of Federal Regulations, 2012 CFR

2012-01-01

... performance, as determined by SBA in its discretion. The Lender's Risk Rating, among other factors, will be considered in determining satisfactory SBA performance. Other factors may include, but are not limited to, on... and loss rate), loan volume to the extent that it impacts performance measures, and other performance...

Efficacy Evaluation of a non-contact automatic articulating paper dispenser in controlling articulating paper microbial contamination

PubMed Central

Li, Yajin; Chen, Litong; Yuan, Fusong; Li, Yugui; Zhou, Yongsheng; Sun, Yuchun

2017-01-01

This study is to quantitatively evaluate the efficacy of using a non-contact automatic articulating paper dispenser for reducing microbial articulating paper contamination. Articulating papers in four-handed mode, non-four-handed mode, and via an automatic articulating paper dispenser were evaluated. An adenosine triphosphate bioluminescence assay was used to quantitatively measure the relative light unit (RLU) values of the rest unused articulating papers in the same package to detect contamination at 4 time points, and triplicate examinations were performed for all three methods. The RLUs were recorded, compared, and evaluated. For four-handed mode (n = 36), the RLUs at the four time points were 2.44, 32.89, 37.89, and 27.22, with a satisfactory rate of 94%. The RLUs for non-four-handed mode (n = 36) were 2.22, 286.44, 299.44, and 493.56, with a satisfactory rate of 36%. The RLUs for using the automatic dispenser (n = 36) were all 0 with a satisfactory rate of 100%. The satisfactory rates were significantly different among three methods. No significant differences were observed in the satisfactory rates for the four time points samples. Contact by gloved hands can cause severe biological contamination of articulating paper. However, by using standard four-handed mode or a non-contact automatic articulating paper dispenser, contamination can be controlled. PMID:28466846

Dual-cloud point extraction coupled to high performance liquid chromatography for simultaneous determination of trace sulfonamide antimicrobials in urine and water samples.

PubMed

Nong, Chunyan; Niu, Zongliang; Li, Pengyao; Wang, Chunping; Li, Wanyu; Wen, Yingying

2017-04-15

Dual-cloud point extraction (dCPE) was successfully developed for simultaneous extraction of trace sulfonamides (SAs) including sulfamerazine (SMZ), sulfadoxin (SDX), sulfathiazole (STZ) in urine and water samples. Several parameters affecting the extraction were optimized, such as sample pH, concentration of Triton X-114, extraction temperature and time, centrifugation rate and time, back-extraction solution pH, back-extraction temperature and time, back-extraction centrifugation rate and time. High performance liquid chromatography (HPLC) was applied for the SAs analysis. Under the optimum extraction and detection conditions, successful separation of the SAs was achieved within 9min, and excellent analytical performances were attained. Good linear relationships (R 2 ≥0.9990) between peak area and concentration for SMZ and STZ were optimized from 0.02 to 10μg/mL, for SDX from 0.01 to 10μg/mL. Detection limits of 3.0-6.2ng/mL were achieved. Satisfactory recoveries ranging from 85 to 108% were determined with urine, lake and tap water spiked at 0.2, 0.5 and 1μg/mL, respectively, with relative standard deviations (RSDs, n=6) of 1.5-7.7%. This method was demonstrated to be convenient, rapid, cost-effective and environmentally benign, and could be used as an alternative tool to existing methods for analysing trace residues of SAs in urine and water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Adrenal venous sampling: the learning curve of a single interventionalist with 282 consecutive procedures

PubMed Central

Jakobsson, Hugo; Farmaki, Katerina; Sakinis, Augustinas; Ehn, Olof; Johannsson, Gudmundur; Ragnarsson, Oskar

2018-01-01

PURPOSE Primary aldosteronism (PA) is a common cause of secondary hypertension. Adrenal venous sampling (AVS) is the gold standard for assessing laterality of PA, which is of paramount importance to decide adequate treatment. AVS is a technically complicated procedure with success rates ranging between 30% and 96%. The aim of this study was to investigate the success rate of AVS over time, performed by a single interventionalist. METHODS This was a retrospective study based on consecutive AVS procedures performed by a single operator between September 2005 and June 2016. Data on serum concentrations of aldosterone and cortisol from right and left adrenal vein, inferior vena cava, and peripheral vein were collected and selectivity index (SI) calculated. Successful AVS was defined as SI >5. RESULTS In total, 282 AVS procedures were performed on 269 patients, 168 men (62%) and 101 women (38%), with a mean age of 55±11 years (range, 26–78 years). Out of 282 AVS procedures, 259 were successful, giving an overall success rate of 92%. The most common reason for failure was inability to localize the right adrenal vein (n=16; 76%). The success rates were 63%, 82%, and 94% during the first, second, and third years, respectively. During the last 8 years the success rate was 95%, and on average 27 procedures were performed annually. CONCLUSION Satisfactory AVS success rate was achieved after approximately 36 procedures and satisfactory success rate was maintained by performing approximately 27 procedures annually. AVS should be limited to few operators that perform sufficiently large number of procedures to achieve, and maintain, satisfactory AVS success rate. PMID:29467114

Knox's Cube Imitation Test: A Historical Review and an Experimental Analysis

ERIC Educational Resources Information Center

Richardson, John T. E.

2005-01-01

The cube imitation test was developed by Knox (1913) as a nonverbal test of intelligence. Many variants show satisfactory reliability, but performance is correlated both with Verbal IQ and with Performance IQ. Performance is impaired by cerebral lesions but unrelated to the side of lesion. Examinees describe both verbal and visuospatial…

Estimation and optimization of thermal performance of evacuated tube solar collector system

NASA Astrophysics Data System (ADS)

Dikmen, Erkan; Ayaz, Mahir; Ezen, H. Hüseyin; Küçüksille, Ecir U.; Şahin, Arzu Şencan

2014-05-01

In this study, artificial neural networks (ANNs) and adaptive neuro-fuzzy (ANFIS) in order to predict the thermal performance of evacuated tube solar collector system have been used. The experimental data for the training and testing of the networks were used. The results of ANN are compared with ANFIS in which the same data sets are used. The R2-value for the thermal performance values of collector is 0.811914 which can be considered as satisfactory. The results obtained when unknown data were presented to the networks are satisfactory and indicate that the proposed method can successfully be used for the prediction of the thermal performance of evacuated tube solar collectors. In addition, new formulations obtained from ANN are presented for the calculation of the thermal performance. The advantages of this approaches compared to the conventional methods are speed, simplicity, and the capacity of the network to learn from examples. In addition, genetic algorithm (GA) was used to maximize the thermal performance of the system. The optimum working conditions of the system were determined by the GA.

Novel control modes to improve the performance of rectilinear ion trap mass spectrometer with dual pressure chambers

NASA Astrophysics Data System (ADS)

Huo, Xinming; Tang, Fei; Zhang, Xiaohua; Chen, Jin; Zhang, Yan; Guo, Cheng'an; Wang, Xiaohao

2016-10-01

The rectilinear ion trap (RIT) has gradually become one of the preferred mass analyzers for portable mass spectrometers because of its simple configuration. In order to enhance the performance, including sensitivity, quantitation capability, throughput, and resolution, a novel RIT mass spectrometer with dual pressure chambers was designed and characterized. The studied system constituted a quadrupole linear ion trap (QLIT) in the first chamber and a RIT in the second chamber. Two control modes are hereby proposed: Storage Quadrupole Linear Ion Trap-Rectilinear Ion Trap (SQLIT-RIT) mode, in which the QLIT was used at high pressure for ion storage and isolation, and the RIT was used for analysis; and Analysis Quadrupole Linear Ion Trap-Rectilinear Ion Trap (AQLIT-RIT) mode, in which the QLIT was used for ion storage and cooling. Subsequently, synchronous scanning and analysis were carried out by QLIT and RIT. In SQLIT-RIT mode, signal intensity was improved by a factor of 30; the limit of quantitation was reduced more than tenfold to 50 ng mL-1, and an optimal duty cycle of 96.4% was achieved. In AQLIT-RIT mode, the number of ions coexisting in the RIT was reduced, which weakened the space-charge effect and reduced the mass shift. Furthermore, the mass resolution was enhanced by a factor of 3. The results indicate that the novel control modes achieve satisfactory performance without adding any system complexity, which provides a viable pathway to guarantee good analytical performance in miniaturization of the mass spectrometer.

Residential Saudi load forecasting using analytical model and Artificial Neural Networks

NASA Astrophysics Data System (ADS)

Al-Harbi, Ahmad Abdulaziz

In recent years, load forecasting has become one of the main fields of study and research. Short Term Load Forecasting (STLF) is an important part of electrical power system operation and planning. This work investigates the applicability of different approaches; Artificial Neural Networks (ANNs) and hybrid analytical models to forecast residential load in Kingdom of Saudi Arabia (KSA). These two techniques are based on model human modes behavior formulation. These human modes represent social, religious, official occasions and environmental parameters impact. The analysis is carried out on residential areas for three regions in two countries exposed to distinct people activities and weather conditions. The collected data are for Al-Khubar and Yanbu industrial city in KSA, in addition to Seattle, USA to show the validity of the proposed models applied on residential load. For each region, two models are proposed. First model is next hour load forecasting while second model is next day load forecasting. Both models are analyzed using the two techniques. The obtained results for ANN next hour models yield very accurate results for all areas while relatively reasonable results are achieved when using hybrid analytical model. For next day load forecasting, the two approaches yield satisfactory results. Comparative studies were conducted to prove the effectiveness of the models proposed.

Monitoring of Cr, Cu, Pb, V and Zn in polluted soils by laser induced breakdown spectroscopy (LIBS).

PubMed

Dell'Aglio, Marcella; Gaudiuso, Rosalba; Senesi, Giorgio S; De Giacomo, Alessandro; Zaccone, Claudio; Miano, Teodoro M; De Pascale, Olga

2011-05-01

Laser Induced Breakdown Spectroscopy (LIBS) is a fast and multi-elemental analytical technique particularly suitable for the qualitative and quantitative analysis of heavy metals in solid samples, including environmental ones. Although LIBS is often recognised in the literature as a well-established analytical technique, results about quantitative analysis of elements in chemically complex matrices such as soils are quite contrasting. In this work, soil samples of various origins have been analyzed by LIBS and data compared to those obtained by Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES). The emission intensities of one selected line for each of the five analytes (i.e., Cr, Cu, Pb, V, and Zn) were normalized to the background signal, and plotted as a function of the concentration values previously determined by ICP-OES. Data showed a good linearity for all calibration lines drawn, and the correlation between ICP-OES and LIBS was confirmed by the satisfactory agreement obtained between the corresponding values. Consequently, LIBS method can be used at least for metal monitoring in soils. In this respect, a simple method for the estimation of the soil pollution degree by heavy metals, based on the determination of an anthropogenic index, was proposed and determined for Cr and Zn.

Anisotropies in the cosmic microwave background: an analytic approach

NASA Astrophysics Data System (ADS)

Hu, Wayne; Sugiyama, Naoshi

1995-05-01

We introduce a conceptually simple yet powerful analytic method which traces the structure of cosmic microwave background anisotropies to better than 5%-10% in temperature fluctuations on all scales. It is applicable to any model in which the gravitational potential is known and last scattering is sufficiently early. Moreover, it recovers and explains the presence of the 'Doppler peaks' at degree scales as driven acoustic oscillations of the photon-baryon fluid. We treat in detail such subtleties as the time dependence of the gravitational driving force, anisotropic stress from the neutrino quadrupole, and damping during the recombination process, again all from an analytic standpoint. We apply this formalism to the standard cold dark matter model to gain physical insight into the anisotropies, including the dependence of the peak locations and heights on cosmological parameters such as Omegab and h. Furthermore, the ionization history controls damping due to the finite thickness of the last scattering surface, which is in fact mianly caused by photon diffusion. In addition to being a powerful probe into the nature of anisotropies, this treatment can be used in place of the standard Boltzmann code where 5%-10% accuracy in temperature fluctuations is satisfactory and/or speed is essential. Equally importantly, it can be used as a portable standard by which numerical codes can be tested and compared.

Electrochemosensor for trace analysis of perfluorooctane sulfonate in water based on a molecularly imprinted poly o-phenylenediamine polymer.

PubMed

Karimian, Najmeh; Stortini, Angela Maria; Moretto, Ligia Maria; Costantino, Claudio; Bogialli, Sara; Ugo, Paolo

2018-06-18

This work is aimed at developing an electrochemical sensor for the sensitive and selective detection of trace levels of perfluorooctane sulfonate (PFOS) in water. Contamination of waters by perfluorinated alkyl substances (PFAS) is a problem of global concern due to their suspected toxicity and ability to bioaccumulate. PFOS is the perfluorinated compound of major concern, as it has the lowest suggested control concentrations. The sensor reported here is based on a gold electrode modified with a thin coating of a molecularly imprinted polymer (MIP), prepared by anodic electropolymerization of o-phenylenediamine (o-PD) in the presence of PFOS as the template. Activation of the sensor is achieved by template removal with suitable a solvent mixture. Voltammetry, a quartz crystal microbalance, scanning electron microscopy and elemental analysis were used to monitor the electropolymerization process, template removal and binding of the analyte. Ferrocenecarboxylic acid (FcCOOH) has been exploited as an electrochemical probe able to generate analytically useful voltammetric signals by competing for the binding sites with PFOS, as the latter is not electroactive. The sensor has a low detection limit (0.04 nM), a satisfactory selectivity, and is reproducible and repeatable, giving analytical results in good agreement with those obtained by HPLC-MS/MS analyses.

Development of a fast and simple gas chromatographic protocol based on the combined use of alkyl chloroformate and solid phase microextraction for the assay of polyamines in human urine.

PubMed

Naccarato, Attilio; Elliani, Rosangela; Cavaliere, Brunella; Sindona, Giovanni; Tagarelli, Antonio

2018-05-11

Polyamines are aliphatic amines with low molecular weight that are widely recognized as one of the most important cancer biomarkers for early diagnosis and treatment. The goal of the work herein presented is the development of a rapid and simple method for the quantification of free polyamines (i.e., putrescine, cadaverine, spermidine, spermine) and N-monoacetylated polyamines (i.e., N 1 -Acetylspermidine, N 8 -Acetylspermidine, and N 1 -Acetylspermine) in human urine. A preliminary derivatization with propyl chloroformate combined with the use of solid phase microextraction (SPME) allowed for an easy and automatable protocol involving minimal sample handling and no consumption of organic solvents. The affinity of the analytes toward five commercial SPME coatings was evaluated in univariate mode, and the best result in terms of analyte extraction was achieved using the divinylbenzene/carboxen/polydimethylsiloxane fiber. The variables affecting the performance of SPME analysis were optimized by the multivariate approach of experimental design and, in particular, using a central composite design (CCD). The optimal working conditions in terms of response values are the following: extraction temperature 40 °C, extraction time of 15 min and no addition of NaCl. Analyses were carried out by gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS) in selected reaction monitoring (SRM) acquisition mode. The developed method was validated according to the guidelines issued by the Food and Drug Administration (FDA). The satisfactory performances reached in terms of linearity, sensitivity (LOQs between 0.01 and 0.1 μg/mL), matrix effect (68-121%), accuracy, and precision (inter-day values between -24% and +16% and in the range 3.3-28.4%, respectively) make the proposed protocol suitable to be adopted for quantification of these important biomarkers in urine samples. Copyright © 2018 Elsevier B.V. All rights reserved.

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.

Comparative evaluation of liquid-liquid extraction, solid-phase extraction and solid-phase microextraction for the gas chromatography-mass spectrometry determination of multiclass priority organic contaminants in wastewater.

PubMed

Robles-Molina, José; Gilbert-López, Bienvenida; García-Reyes, Juan F; Molina-Díaz, Antonio

2013-12-15

The European Water Framework Directive (WFD) 2000/60/EC establishes guidelines to control the pollution of surface water by sorting out a list of priority substances that involves a significant risk to or via the aquatic systems. In this article, the analytical performance of three different sample preparation methodologies for the GC-MS/MS determination of multiclass organic contaminants-including priority comprounds from the WFD-in wastewater samples using gas chromatography-mass spectrometry was evaluated. The methodologies tested were: (a) liquid-liquid extraction (LLE) with n-hexane; (b) solid-phase extraction (SPE) with C18 cartridges and elution with ethyl acetate:dichloromethane (1:1 (v/v)), and (c) headspace solid-phase microextraction (HS-SPME) using two different fibers: polyacrylate and polydimethylsiloxane/carboxen/divinilbenzene. Identification and confirmation of the selected 57 compounds included in the study (comprising polycyclic aromatic hydrocarbons (PAHs), pesticides and other contaminants) were accomplished using gas chromatography tandem mass spectrometry (GC-MS/MS) with a triple quadrupole instrument operated in the multiple reaction monitoring (MRM) mode. Three MS/MS transitions were selected for unambiguous confirmation of the target chemicals. The different advantages and pitfalls of each method were discussed. In the case of both LLE and SPE procedures, the method was validated at two different concentration levels (15 and 150 ng L(-1)) obtaining recovery rates in the range 70-120% for most of the target compounds. In terms of analyte coverage, results with HS-SPME were not satisfactory, since 14 of the compounds tested were not properly recovered and the overall performance was worse than the other two methods tested. LLE, SPE and HS-SPME (using polyacrylate fiber) procedures also showed good linearity and precision. Using any of the three methodologies tested, limits of quantitation obtained for most of the detected compounds were in the low nanogram per liter range. © 2013 Elsevier B.V. All rights reserved.

Enzyme-labeled Pt@BSA nanocomposite as a facile electrochemical biosensing interface for sensitive glucose determination.

PubMed

Hu, Chenyi; Yang, Da-Peng; Zhu, Fengjuan; Jiang, Fengjing; Shen, Shuiyun; Zhang, Junliang

2014-03-26

Electrocatalytic reactions of glucose oxidation based on enzyme-labeled electrochemical biosensors demand a high enzymatic activity and fast electron transfer property to produce the amplified signal response. Through a "green" synthesis method, Pt@BSA nanocomposite was prepared as a biosensing interface for the first time. Herein we presented a convenient and effective glucose sensing matrix based on Pt@BSA nanocomposite along with the covalent adsorption of glucose oxidase (GOD). The electrocatalytic activity toward oxygen reduction was significantly enhanced due to the excellent bioactivity of anchored GOD and superior catalytic performance of interior platinum nanoparticles, which was gradually restrained with the addition of glucose. A sensitive glucose biosensor was then successfully developed upon the restrained oxygen reduction peak current. Differential pulse voltammetry (DPV) was employed to investigate the determination performance of the enzyme biosensor, resulting in a linear response range from 0.05 to 12.05 mM with an optimal detection limit of 0.015 mM. The as-proposed sensing technique revealed high selectivity against endogenous interfering species, satisfactory storage stability, acceptable durability, and favorable fabrication reproducibility with the RSD of 3.8%. During the practical application in human blood serum samples, this glucose biosensor obtained a good detection accuracy of analytical recoveries within 97.5 to 104.0%, providing an alternative scheme for glucose level assay in clinical application.

Solution for blank and matrix difficulties encountered during phthalate analysis of edible oils by high performance liquid chromatography coupled with tandem mass spectrometry.

PubMed

Vavrouš, Adam; Pavloušková, Jana; Ševčík, Václav; Vrbík, Karel; Čabala, Radomír

2016-07-22

Worldwide production of phthalates has led to their undesirable presence in the food chain. Particularly edible oils have become an area of growing concern owing to numerous reported occurrences of phthalates. The analytical methods used in this field face difficulties associated mainly with matrix complexity or phthalate contamination which this study has aimed to describe and resolve. The proposed procedure consisting of liquid-liquid extraction, solid phase extraction and high performance liquid chromatography coupled with tandem mass spectrometry allowed us to analyze simultaneously 6 individual phthalates and 2 phthalate isomeric mixtures. DSC-18 SPE phase was selected for cleanup owing to the most efficient co-extract removal (assessed using high resolution mass spectrometry). Several sources of phthalate contamination were identified, however, the mobile phase was the most serious. The key improvement was achieved by equipping a contamination trap, a 50-mm reverse phase HPLC column, generating a delay between target and mobile phase peaks of the same compounds. RSDs ranging between 2.4 and 16 % confirm good precision and LOQs between 5.5 and 110μgkg(-1) reflect satisfactory blank management. With up to 19 occurrences in 25 analyzed edible oil samples and levels up to 33mgkg(-1), bis(2-ethylhexyl), diisononyl and diisodecyl phthalates were the most important contaminants. Copyright © 2016 Elsevier B.V. All rights reserved.

Rapid determination of letrozole, citalopram and their metabolites by high performance liquid chromatography-fluorescence detection in urine: Method validation and application to real samples.

PubMed

Rodríguez, J; Castañeda, G; Muñoz, L

2013-01-15

This work reports the validation of a high precision and accuracy method for the simultaneous determination of letrozole, citalopram and their metabolites in urine by high performance liquid chromatography with fluorescence detection. Dilution (urine:mobile phase, 1:2, v/v) was the only sample preparation step. The separation was carried out in a Kromasil C(18) (150mm×4.6mm) column, and the mobile phase was phosphate buffer 80mM (pH 3.0) and acetonitrile (65:35, v/v) at a flow rate of 1.0mL/min. The analytes were detected at 295nm after excitation at 230nm. Linearity was observed in the range of 1.0-1000ng/mL for letrozole and its metabolite and 2.5-1000ng/mL for citalopram and their metabolites, with limits of detection and quantification between 0.09-1.0 and 0.27-1.65ng/mL, respectively. The precisions were satisfactory with RSDs between 0.17 and 5.71%. The accuracy was studied by spiking three urines from healthy female volunteers, and the recoveries were from 85 to 103%. The method was applied to urine samples from women under treatment for breast cancer and depression diseases. Copyright © 2012 Elsevier B.V. All rights reserved.

Solid-phase microextraction-gas chromatography-mass spectrometry for the analysis of selective serotonin reuptake inhibitors in environmental water.

PubMed

Lamas, J Pablo; Salgado-Petinal, Carmen; García-Jares, Carmen; Llompart, María; Cela, Rafael; Gómez, Mariano

2004-08-13

The continuous contamination of surface waters by pharmaceuticals is of most environmental concern. Selective serotonin reuptake inhibitors (SSRIs) are drugs currently prescribed for the treatment of depressions and other psychiatric disorders and then, they are among the pharmaceuticals that can occur in environmental waters. Solid-phase microextraction (SPME) coupled to gas chromatography-mass spectrometry has been applied to the extraction of five SSRIs--venlafaxine, fluvoxamine, fluoxetine, citalopram and sertraline--from water samples. Some of the analytes were not efficiently extracted as underivatized compounds and so, an in situ acetylation step was introduced in the sample preparation procedure. Different parameters affecting extraction efficiency such as extraction mode, fiber coating and temperature were studied. A mixed-level fractional factorial design was also performed to simultaneously study the influence of other five experimental factors. Finally, a method based on direct SPME at 100 degrees C using polydimethylsiloxane-divinylbenzene fibers is proposed. The performance of the method was evaluated, showing good linearity and precision. The detection limits were in the sub-ng/mL level. Practical applicability was demonstrated through the analysis of real samples. Recoveries obtained for river water and wastewater samples were satisfactory in all cases. An important aspect of the proposed method is that no matrix effects were observed. Two of the target compounds, venlafaxine and citalopram, were detected and quantified in a sewage water sample.

Open-Source Assisted Laboratory Automation through Graphical User Interfaces and 3D Printers: Application to Equipment Hyphenation for Higher-Order Data Generation.

PubMed

Siano, Gabriel G; Montemurro, Milagros; Alcaráz, Mirta R; Goicoechea, Héctor C

2017-10-17

Higher-order data generation implies some automation challenges, which are mainly related to the hidden programming languages and electronic details of the equipment. When techniques and/or equipment hyphenation are the key to obtaining higher-order data, the required simultaneous control of them demands funds for new hardware, software, and licenses, in addition to very skilled operators. In this work, we present Design of Inputs-Outputs with Sikuli (DIOS), a free and open-source code program that provides a general framework for the design of automated experimental procedures without prior knowledge of programming or electronics. Basically, instruments and devices are considered as nodes in a network, and every node is associated both with physical and virtual inputs and outputs. Virtual components, such as graphical user interfaces (GUIs) of equipment, are handled by means of image recognition tools provided by Sikuli scripting language, while handling of their physical counterparts is achieved using an adapted open-source three-dimensional (3D) printer. Two previously reported experiments of our research group, related to fluorescence matrices derived from kinetics and high-performance liquid chromatography, were adapted to be carried out in a more automated fashion. Satisfactory results, in terms of analytical performance, were obtained. Similarly, advantages derived from open-source tools assistance could be appreciated, mainly in terms of lesser intervention of operators and cost savings.

Construction of novel xanthine biosensor by using polymeric mediator/MWCNT nanocomposite layer for fish freshness detection.

PubMed

Dervisevic, Muamer; Custiuc, Esma; Çevik, Emre; Şenel, Mehmet

2015-08-15

A novel nanocomposite host matrix for enzyme immobilization of xanthine oxidase was developed by incorporating MWCNT in poly(GMA-co-VFc) copolymer film. In the food industry fish is a product with a very low commercial life, and a high variability as well elevated level of xanthine is an important biomarker as a sign of spoilage. The fabricated process was characterized by scanning electron microscopy (SEM), and the electrochemical behaviors of the biosensor were characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The prepared enzyme electrodes exhibited maximum response at pH 7.0 and 45°C +0.35 V and reached 95% of steady-state current in about ∼ 4 s and its sensitivity was 16 mAM(-1). Linear ranges (2-28 μM, 28-46 and 46-86 μM), analytical performance and a low detection limit 0.12 μM obtained from the xanthine biosensor gives reliable results in measuring xanthine concentration in the fish meat. All the results indicating that the resulting biosensor exhibited a good response to xanthine that was related to the addition of MWCNT in the polymeric mediator film which played an important role in the biosensor performance. In addition, the biosensor exhibited high good storage stability and satisfactory anti-interference ability. Copyright © 2015 Elsevier Ltd. All rights reserved.

Comparison of the Automated cobas u 701 Urine Microscopy and UF-1000i Flow Cytometry Systems and Manual Microscopy in the Examination of Urine Sediments.

PubMed

Lee, Wonmok; Ha, Jung-Sook; Ryoo, Nam-Hee

2016-09-01

The cobas u 701, a new automated image-based urine sediment analyzer, was introduced recently. In this study, we compared its performance with that of UF-1000i flow cytometry and manual microscopy in the examination of urine sediments. Precision, linearity, and carry-over were determined for the two urine sediment analyzers. For a comparison of the method, 300 urine samples were examined by the automated analyzers and by manual microscopy using a KOVA chamber. Within-run coefficients of variation (CVs) for the control materials were 7.0-8.8% and 1.7-5.7% for the cobas u 701 and UF-1000i systems, respectively. Between-run CVs were 8.5-9.8% and 2.7-5.4%, respectively. Both instruments showed good linearity and negligible carry-over. For red blood cells (RBC), white blood cells (WBC), and epithelial cells (EPI), the overall concordance rates within one grade of difference among the three methods were good (78.6-86.0%, 88.7-93.8%, and 81.3-90.7%, respectively). The concordance rate for casts was poor (66.5-68.9%). Compared with manual microscopy, the two automated sediment analyzers tested in this study showed satisfactory analytical performances for RBC, WBC, and EPI. However, for other urine sediment particles confirmation by visual microscopy is still required. © 2016 Wiley Periodicals, Inc.

Hasse diagram as a green analytical metrics tool: ranking of methods for benzo[a]pyrene determination in sediments.

PubMed

Bigus, Paulina; Tsakovski, Stefan; Simeonov, Vasil; Namieśnik, Jacek; Tobiszewski, Marek

2016-05-01

This study presents an application of the Hasse diagram technique (HDT) as the assessment tool to select the most appropriate analytical procedures according to their greenness or the best analytical performance. The dataset consists of analytical procedures for benzo[a]pyrene determination in sediment samples, which were described by 11 variables concerning their greenness and analytical performance. Two analyses with the HDT were performed-the first one with metrological variables and the second one with "green" variables as input data. Both HDT analyses ranked different analytical procedures as the most valuable, suggesting that green analytical chemistry is not in accordance with metrology when benzo[a]pyrene in sediment samples is determined. The HDT can be used as a good decision support tool to choose the proper analytical procedure concerning green analytical chemistry principles and analytical performance merits.

Need Assessment of Staffs’ Welfare Services at Tehran University of Medical Sciences: A Cross-Sectional Study

PubMed Central

Dehghan, Reza; Mafimoradi, Shiva; Hadi, Mohammad

2015-01-01

Background: Reviewing the human resources management literature shows an absence of attention given to the employee's benefits. Taking a look at functions of the Tehran University of Medical Sciences’ wellbeing services system, it uncovers a gap between employees’ real needs and what is delivered to meet their needs. So it requires an improved comprehensive system for delivering wellbeing services (financial, insurance, health care services, educational and training services, etc). Wellbeing need assessment can helps planners to identify vital needs of employee and response to them effectively. Moreover it can be used to evaluate the effectiveness of the current services which are delivered. Thus, the aim of this study is to assess wellbeing services of staffs working in TUMS to (1) evaluate the satisfactory rate of services which are delivered, and (2) exploring those wellbeing needs which were not fulfilled by the organization. Material and Methods: Being a cross-sectional and analytic-descriptive survey including 98 responding participants, it is conducted by a questionnaire collecting employees’ demographic information, their satisfactory rate of the implemented services, and determines unfulfilled wellbeing needs which were not already covered. Result: Results indicated that services related to financial, educational, non-financial, insurance, occupational health and tourism/recreational services were the most satisfactory services successively. ‘Staff's unwillingness to receive services’ and ‘poor announcement’ (unawareness on the wellbeing services),’ were found to be the most frequent reasons for not receiving the existing wellbeing services. Conclusion: To increase the satisfaction rate and responsiveness to the real needs of the staff, the current delivery system of wellbeing services in the TUMS should be redesigned by defining new wellbeing packages. PMID:25767818

Showerheads

EPA Pesticide Factsheets

WaterSense labeled showerheads provide a satisfactory shower that is equal to or better than conventional showerheads on the market. WaterSense labeled showerheads are independently certified to meet EPA water efficiency and performance criteria.

Quality-Assurance Data for Routine Water Analyses by the U.S. Geological Survey Laboratory in Troy, New York--July 1999 through June 2001

USGS Publications Warehouse

Lincoln, Tricia A.; Horan-Ross, Debra A.; McHale, Michael R.; Lawrence, Gregory B.

2006-01-01

The laboratory for analysis of low-ionic-strength water at the U.S. Geological Survey (USGS) Water Science Center in Troy, N.Y., analyzes samples collected by USGS projects throughout the Northeast. The laboratory's quality-assurance program is based on internal and interlaboratory quality-assurance samples and quality-control procedures that were developed to ensure proper sample collection, processing, and analysis. The quality-assurance and quality-control data were stored in the laboratory's LabMaster data-management system, which provides efficient review, compilation, and plotting of data. This report presents and discusses results of quality-assurance and quality-control samples analyzed from July 1999 through June 2001. Results for the quality-control samples for 18 analytical procedures were evaluated for bias and precision. Control charts indicate that data for eight of the analytical procedures were occasionally biased for either high-concentration or low-concentration samples but were within control limits; these procedures were: acid-neutralizing capacity, total monomeric aluminum, total aluminum, calcium, chloride and nitrate (ion chromatography and colormetric method) and sulfate. The total aluminum and dissolved organic carbon procedures were biased throughout the analysis period for the high-concentration sample, but were within control limits. The calcium and specific conductance procedures were biased throughout the analysis period for the low-concentration sample, but were within control limits. The magnesium procedure was biased for the high-concentration and low concentration samples, but was within control limits. Results from the filter-blank and analytical-blank analyses indicate that the procedures for 14 of 15 analytes were within control limits, although the concentrations for blanks were occasionally outside the control limits. The data-quality objective was not met for dissolved organic carbon. Sampling and analysis precision are evaluated herein in terms of the coefficient of variation obtained for triplicate samples in the procedures for 17 of the 18 analytes. At least 90 percent of the samples met data-quality objectives for all analytes except ammonium (81 percent of samples met objectives), chloride (75 percent of samples met objectives), and sodium (86 percent of samples met objectives). Results of the USGS interlaboratory Standard Reference Sample (SRS) Project indicated good data quality over the time period, with most ratings for each sample in the good to excellent range. The P-sample (low-ionic-strength constituents) analysis had one satisfactory rating for the specific conductance procedure in one study. The T-sample (trace constituents) analysis had one satisfactory rating for the aluminum procedure in one study and one unsatisfactory rating for the sodium procedure in another. The remainder of the samples had good or excellent ratings for each study. Results of Environment Canada's National Water Research Institute (NWRI) program indicated that at least 89 percent of the samples met data-quality objectives for 10 of the 14 analytes; the exceptions were ammonium, total aluminum, dissolved organic carbon, and sodium. Results indicate a positive bias for the ammonium procedure in all studies. Data-quality objectives were not met in 50 percent of samples analyzed for total aluminum, 38 percent of samples analyzed for dissolved organic carbon, and 27 percent of samples analyzed for sodium. Results from blind reference-sample analyses indicated that data-quality objectives were met by at least 91 percent of the samples analyzed for calcium, chloride, fluoride, magnesium, pH, potassium, and sulfate. Data-quality objectives were met by 75 percent of the samples analyzed for sodium and 58 percent of the samples analyzed for specific conductance.

Determination of arbutin and bergenin in Bergeniae Rhizoma by capillary electrophoresis with a carbon nanotube-epoxy composite electrode.

PubMed

Zhang, Luyan; Zhang, Wei; Chen, Gang

2015-11-10

This report describes the fabrication and the application of a novel carbon nanotube (CNT)-epoxy composite electrode as a sensitive amperometric detector for the capillary electrophoresis (CE). The composite electrode was fabricated on the basis of the in situ polycondensation of a mixture of CNTs and 1,2-ethanediamine-containing bisphenol A epoxy resin in the inner bore of a piece of fused silica capillary under heat. It was coupled with CE for the separation and detection of arbutin and bergenin in Bergeniae Rhizoma, a traditional Chinese medicine, to demonstrate its feasibility and performance. The two phenolic constituents were well separated within 10min in a 45cm capillary length at a separation voltage of 12kV using a 50mM borate buffer (pH 9.2). The CNT-based detector offered higher sensitivity, significantly lower operating potential, satisfactory resistance to surface fouling, and lower expense of operation, indicating great promise for a wide range of analytical applications. It showed long-term stability and reproducibility with relative standard deviations of less than 5% for the peak current (n=15). Copyright © 2015 Elsevier B.V. All rights reserved.

The Self-Stigma of Depression Scale (SSDS): development and psychometric evaluation of a new instrument.

PubMed

Barney, Lisa J; Griffiths, Kathleen M; Christensen, Helen; Jorm, Anthony F

2010-12-01

Self-stigma may feature strongly and be detrimental for people with depression, but the understanding of its nature and prevalence is limited by the lack of psychometrically-validated measures. This study aimed to develop and validate a measure of self-stigma about depression. Items assessing self-stigma were developed from focus group discussions, and were tested and refined over three studies using surveys of 408 university students, 330 members of a depression Internet network, and 1312 members of the general Australian public. Evaluation involved item-level and bivariate analyses, and factor analytic procedures. Items performed consistently across the three surveys. The resulting Self-Stigma of Depression Scale (SSDS) comprised 16 items representing subscales of Shame, Self-Blame, Social Inadequacy, and Help-Seeking Inhibition. Construct validity, internal consistency and test-retest reliability were satisfactory. The SSDS distinguishes self-stigma from perceptions of stigma by others, yields in-depth information about self-stigma of depression, and possesses good psychometric properties. It is a promising tool for the measurement of self-stigma and is likely to be useful in further understanding self-stigma and evaluating stigma interventions. Copyright © 2010 John Wiley & Sons, Ltd.

Synergetic signal amplification of multi-walled carbon nanotubes-Fe3O4 hybrid and trimethyloctadecylammonium bromide as a highly sensitive detection platform for tetrabromobisphenol A

PubMed Central

Zhou, Feng; Wang, Yue; Wu, Wei; Jing, Tao; Mei, Surong; Zhou, Yikai

2016-01-01

In this work, we fabricated an electrochemical sensor based on trimethyloctadecylammonium bromide and multi-walled carbon nanotubes-Fe3O4 hybrid (TOAB/MWCNTs-Fe3O4) for sensitive detection of tetrabromobisphenol A (TBBPA). The nanocomposite was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FT-IR) techniques. The electrochemical behaviors of TBBPA on TOAB/MWCNTs-Fe3O4 composite film modified glassy carbon electrode (GCE) were investigated by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and electrochemical impedance spectroscopy (EIS) method. The experimental results indicated that the incorporation of MWCNTs-Fe3O4 with TOAB greatly enhanced the electrochemical response of TBBPA. This fabricated sensor displayed excellent analytical performance for TBBPA detection over a range from 3.0 nM to 1000.0 nM with a detection limit of 0.73 nM (S/N = 3). Moreover, the proposed electrochemical sensor exhibited good reproducibility and stability, and could be successfully applied to detect TBBPA in water samples with satisfactory results. PMID:27897238

A reliable and rapid tool for plasma quantification of 18 psychotropic drugs by ESI tandem mass spectrometry.

PubMed

Vecchione, Gennaro; Casetta, Bruno; Chiapparino, Antonella; Bertolino, Alessandro; Tomaiuolo, Michela; Cappucci, Filomena; Gatta, Raffaella; Margaglione, Maurizio; Grandone, Elvira

2012-01-01

A simple liquid chromatographic tandem mass spectrometry (LC-MS/MS) method has been developed for simultaneous analysis of 17 basic and one acid psychotropic drugs in human plasma. The method relies on a protein precipitation step for sample preparation and offers high sensitivity, wide linearity without interferences from endogenous matrix components. Chromatography was run on a reversed-phase column with an acetonitrile-H₂O mixture. The quantification of target compounds was performed in multiple reaction monitoring (MRM) and by switching the ionization polarity within the analytical run. A further sensitivity increase was obtained by implementing the functionality "scheduled multiple reaction monitoring" (sMRM) offered by the recent version of the software package managing the instrument. The overall injection interval was less than 5.5 min. Regression coefficients of the calibration curves and limits of quantification (LOQ) showed a good coverage of over-therapeutic, therapeutic and sub-therapeutic ranges. Recovery rates, measured as percentage of recovery of spiked plasma samples, were ≥ 94%. Precision and accuracy data have been satisfactory for a therapeutic drug monitoring (TDM) service as for managing plasma samples from patients receiving psycho-pharmacological treatment. Copyright © 2012 Elsevier B.V. All rights reserved.

Objective assessment of MPEG-2 video quality

NASA Astrophysics Data System (ADS)

Gastaldo, Paolo; Zunino, Rodolfo; Rovetta, Stefano

2002-07-01

The increasing use of video compression standards in broadcasting television systems has required, in recent years, the development of video quality measurements that take into account artifacts specifically caused by digital compression techniques. In this paper we present a methodology for the objective quality assessment of MPEG video streams by using circular back-propagation feedforward neural networks. Mapping neural networks can render nonlinear relationships between objective features and subjective judgments, thus avoiding any simplifying assumption on the complexity of the model. The neural network processes an instantaneous set of input values, and yields an associated estimate of perceived quality. Therefore, the neural-network approach turns objective quality assessment into adaptive modeling of subjective perception. The objective features used for the estimate are chosen according to the assessed relevance to perceived quality and are continuously extracted in real time from compressed video streams. The overall system mimics perception but does not require any analytical model of the underlying physical phenomenon. The capability to process compressed video streams represents an important advantage over existing approaches, like avoiding the stream-decoding process greatly enhances real-time performance. Experimental results confirm that the system provides satisfactory, continuous-time approximations for actual scoring curves concerning real test videos.

A Semiempirical Model for Sigma-Phase Precipitation in Duplex and Superduplex Stainless Steels

NASA Astrophysics Data System (ADS)

Ferro, P.; Bonollo, F.

2012-04-01

Sigma phase is known to reduce the mechanical properties and corrosion resistance of duplex and superduplex stainless steels. Therefore, heat treatments and welding must be carefully performed so as to avoid the appearance of such a detrimental phase, and clearly, models suitable to faithfully predict σ-phase precipitation are very useful tools. Most fully analytical models are based on thermodynamic calculations whose agreement with experimental results is not always good, so that such models should be used for qualitative purposes only. Alternatively, it is possible to exploit semiempirical models, where time-temperature-transformation (TTT) diagrams are empirically determined for a given alloy and the continuous-cooling-transformation (CCT) diagram is calculated from the TTT diagram. In this work, a semiempirical model for σ-phase precipitation in duplex and superduplex stainless steels, under both isothermal and unisothermal conditions, is proposed. Model parameters are calculated from empirical data and CCT diagrams are obtained by means of the additivity rule, whereas experimental measurements for model validation are taken from the literature. This model gives a satisfactory estimation of σ-phase precipitates during both isothermal aging and the continuous cooling process.

Effervescence-assisted dispersive solid-phase extraction using ionic-liquid-modified magnetic β-cyclodextrin/attapulgite coupled with high-performance liquid chromatography for fungicide detection in honey and juice.

PubMed

Wu, Xiaoling; Yang, Miyi; Zeng, Haozhe; Xi, Xuefei; Zhang, Sanbing; Lu, Runhua; Gao, Haixiang; Zhou, Wenfeng

2016-11-01

In this study, a simple effervescence-assisted dispersive solid-phase extraction method was developed to detect fungicides in honey and juice. Most significantly, an innovative ionic-liquid-modified magnetic β-cyclodextrin/attapulgite sorbent was used because its large specific surface area enhanced the extraction capacity and also led to facile separation. A one-factor-at-a-time approach and orthogonal design were employed to optimize the experimental parameters. Under the optimized conditions, the entire extraction procedure was completed within 3 min. In addition, the calibration curves exhibited good linearity, and high enrichment factors were achieved for pure water and honey samples. For the honey samples, the extraction efficiencies for the target fungicides ranged from 77.0 to 94.3% with relative standard deviations of 2.3-5.44%. The detection and quantitation limits were in the ranges of 0.07-0.38 and 0.23-1.27 μg/L, respectively. Finally, the developed technique was successfully applied to real samples, and satisfactory results were achieved. This analytical technique is cost-effective, environmentally friendly, and time-saving. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Merits and limitations of optimality criteria method for structural optimization

NASA Technical Reports Server (NTRS)

Patnaik, Surya N.; Guptill, James D.; Berke, Laszlo

1993-01-01

The merits and limitations of the optimality criteria (OC) method for the minimum weight design of structures subjected to multiple load conditions under stress, displacement, and frequency constraints were investigated by examining several numerical examples. The examples were solved utilizing the Optimality Criteria Design Code that was developed for this purpose at NASA Lewis Research Center. This OC code incorporates OC methods available in the literature with generalizations for stress constraints, fully utilized design concepts, and hybrid methods that combine both techniques. Salient features of the code include multiple choices for Lagrange multiplier and design variable update methods, design strategies for several constraint types, variable linking, displacement and integrated force method analyzers, and analytical and numerical sensitivities. The performance of the OC method, on the basis of the examples solved, was found to be satisfactory for problems with few active constraints or with small numbers of design variables. For problems with large numbers of behavior constraints and design variables, the OC method appears to follow a subset of active constraints that can result in a heavier design. The computational efficiency of OC methods appears to be similar to some mathematical programming techniques.

Multivariate Optimization for Extraction of Pyrethroids in Milk and Validation for GC-ECD and CG-MS/MS Analysis

PubMed Central

Zanchetti Meneghini, Leonardo; Rübensam, Gabriel; Claudino Bica, Vinicius; Ceccon, Amanda; Barreto, Fabiano; Flores Ferrão, Marco; Bergold, Ana Maria

2014-01-01

A simple and inexpensive method based on solvent extraction followed by low temperature clean-up was applied for determination of seven pyrethroids residues in bovine raw milk using gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) and gas chromatography with electron-capture detector (GC-ECD). Sample extraction procedure was established through the evaluation of seven different extraction protocols, evaluated in terms of analyte recovery and cleanup efficiency. Sample preparation optimization was based on Doehlert design using fifteen runs with three different variables. Response surface methodologies and polynomial analysis were used to define the best extraction conditions. Method validation was carried out based on SANCO guide parameters and assessed by multivariate analysis. Method performance was considered satisfactory since mean recoveries were between 87% and 101% for three distinct concentrations. Accuracy and precision were lower than ±20%, and led to no significant differences (p < 0.05) between results obtained by GC-ECD and GC-MS/MS techniques. The method has been applied to routine analysis for determination of pyrethroid residues in bovine raw milk in the Brazilian National Residue Control Plan since 2013, in which a total of 50 samples were analyzed. PMID:25380457

Simultaneous determination of quinolones in fish by liquid chromatography coupled with fluorescence detection: comparison of sub-2 microm particles and conventional C18 columns.

PubMed

Zhang, Hong; Chen, Si; Lu, Yanbin; Dai, Zhiyuan

2010-07-01

A simple and effective multi-residue analysis method is presented for the extraction and determination of eleven quinolones (pipemidic acid, enoxacin, norfloxacin, ciprofloxacin, lomefloxacin, enrofloxacin, gatifloxacin, difloxacin, oxolinic acid, nalidixic acid and flumequine) in fish tissues. In this study, multi-residue separations on four columns packed with 5 microm or sub-2 microm particles were simultaneously developed for the purpose of comparison. Various gradients were optimized and best resolutions were achieved on each column. A short and sub-2 microm particle-sized HPLC column was chosen for its advantages in analysis time and column performance. Additionally, considering the matrix effect of the complex crude fish tissue, an effective extraction protocol was also established for sample pre-treatment procedure. Good recoveries (71-98%) were obtained from samples fortified with a mix of eleven quinolones at three levels, with satisfactory relative standard deviations and limits of detection. As a result, the sub-2 microm HPLC column and proposed analytical procedures have been evaluated and applied to the analysis of different fish tissues. Detectable residues were observed in 8 of 30 samples, at concentrations ranging from 4.74 to 23.27 microg/kg.

[Determination of LF-VD refining furnace slag by X ray fluorescence spectrometry].

PubMed

Kan, Bin; Cheng, Jian-ping; Song, Zu-feng

2004-10-01

Eight components, i.e. TFe, CaO, MgO, Al2O3, SiO2, TiO2, MnO and P2O5 in refining furnace slag were determined by X ray fluorescence spectrometer. Because the content of CaO was high, the authors selected 12 national and departmental grade slag standard samples and prepared a series of synthetic standard samples by adding spectrally pure reagents to them. The calibration curve is suitable to the sample analysis of CaO, MgO and SiO2 with widely varying range. Meanwhile, the points on the curve are even. The samples were prepared at high temperature by adding Li2B4O7 as flux. The experiments for the selection of the sample preparation conditions about strip reagents, melting temperature and dulition ratio were carried out. The matrix effects on absorption and enhancement were corrected by means of PH model and theoretical alpha coefficient. Moreover, the precision and accuracy experiments were performed. In comparison with chemical analysis method, the quantitative analytical results for each component are satisfactory. The method has proven rapid, precise and simple.

[Method of fused sample preparation after nitrify-determination of primary and minor elements in manganese ore by X-ray fluorescence spectrometry].

PubMed

Song, Yi; Guo, Fen; Gu, Song-hai

2007-02-01

Eight components, i. e. Mn, SiO2, Fe, P, Al2O3, CaO, MgO and S, in manganese ore were determined by X-ray fluorescence spectrometer. Because manganese ore sample releases a lot of air bubbles during fusion which effect accuracy and reproducibility of determination, nitric acid was added to the sample to destroy organic matter before fusion by the mixture flux at 1000 degrees C. This method solved the problem that the flux splashed during fusion because organic matter volatilized brought out a lot of air bubbles, eliminated particle size effects and mineral effect, while solved the problem of volatilization of sulfur during fusion. The experiments for the selection of the sample preparation conditions, i. e. fusion flux, fusion time and volume of HNO3, were carried out. The matrix effects on absorption and enhancement were corrected by variable theoretical alpha coefficient to expand the range of determination. Moreover, the precision and accuracy experiments were performed. In comparison with chemical analysis method, the quantitative analytical results for each component are satisfactory. The method has proven rapid, precise and simple.

Quantitative analysis of flavonoids and phenolic acid in Coreopsis tinctoria Nutt. by capillary zone electrophoresis.

PubMed

Deng, Yong; Lam, Shing-Chung; Zhao, Jing; Li, Shao-Ping

2017-10-01

Capillary zone electrophoresis was developed for the simultaneous determination of five flavonoids and one phenolic acid, including taxifolin-7-O-glucoside, flavanomarein, quercetagetin-7-O-glucoside, okanin 4'-O-glucoside, okanin, and chlorogenic acid, in different parts and origins of Coreopsis tinctoria and its related species. Effects of acidity, running-buffer concentration, and modifier concentration were investigated to determine the optimum conditions for analyte determination. Analysis was performed within 18 min by using 50 mM borax buffer containing 15% acetonitrile as a modifier (pH 9.0) at 25 kV and 25°C. Hyperoside was used as internal standard for quantification. The method was accurate, simple, and repeatable, and was successfully applied to the analysis in 13 samples with satisfactory assay results. Results showed that C. tinctoria obviously differed from the related flower tea materials, "Hangju" and "Gongju". The parts (flowers, buds, seeds, stems, and leaves) of C. tinctoria also varied among one another. This study can serve as a foundation for the quality control and pharmacological evaluation of different parts of C. tinctoria and its related species. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Extraction and Determination of Cyproheptadine in Human Urine by DLLME-HPLC Method

PubMed Central

Maham, Mehdi; Kiarostami, Vahid; Waqif-Husain, Syed; Abroomand-Azar, Parviz; Tehrani, Mohammad Saber; Khoeini Sharifabadi, Malihe; Afrouzi, Hossein; Shapouri, MahmoudReza; Karami-Osboo, Rouhollah

2013-01-01

Novel dispersive liquid-liquid microextraction (DLLME), coupled with high performance liquid chromatography with photodiode array detection (HPLC-DAD) has been applied for the extraction and determination of cyproheptadine (CPH), an antihistamine, in human urine samples. In this method, 0.6 mL of acetonitrile (disperser solvent) containing 30 μL of carbon tetrachloride (extraction solvent) was rapidly injected by a syringe into 5 mL urine sample. After centrifugation, the sedimented phase containing enriched analyte was dissolved in acetonitrile and an aliquot of this solution injected into the HPLC system for analysis. Development of DLLME procedure includes optimization of some important parameters such as kind and volume of extraction and disperser solvent, pH and salt addition. The proposed method has good linearity in the range of 0.02-4.5 μg mL-1 and low detection limit (13.1 ng mL-1). The repeatability of the method, expressed as relative standard deviation was 4.9% (n = 3). This method has also been applied to the analysis of real urine samples with satisfactory relative recoveries in the range of 91.6-101.0%. PMID:24250605

75 FR 63419 - Surety Bond Guarantee Program; Timber Sales

Federal Register 2010, 2011, 2012, 2013, 2014

2010-10-15

... timber sale contracts may require the purchaser to furnish a performance bond for satisfactory compliance.... With respect to a Performance Bond involving the sale of timber on land managed by USDA, the Federal... Sales AGENCY: Small Business Administration. ACTION: Proposed rule. SUMMARY: The Small Business...

A simple and highly selective molecular imprinting polymer-based methodology for propylparaben monitoring in personal care products and industrial waste waters.

PubMed

Vicario, Ana; Aragón, Leslie; Wang, Chien C; Bertolino, Franco; Gomez, María R

2018-02-05

In this work, a novel molecularly imprinted polymer (MIP) proposed as solid phase extraction sorbent was developed for the determination of propylparaben (PP) in diverse cosmetic samples. The use of parabens (PAs) is authorized by regulatory agencies as microbiological preservative; however, recently several studies claim that large-scale use of these preservatives can be a potential health risk and harmful to the environment. Diverse factors that influence on polymer synthesis were studied, including template, functional monomer, porogen and crosslinker used. Morphological characterization of the MIP was performed using SEM and BET analysis. Parameters affecting the molecularly imprinted solid phase extraction (MISPE) and elution efficiency of PP were evaluated. After sample clean-up, the analyte was analyzed by high performance liquid chromatography (HPLC). The whole procedure was validated, showing satisfactory analytical parameters. After applying the MISPE methodology, the extraction recoveries were always better than 86.15%; the obtained precision expressed as RSD% was always lower than 2.19 for the corrected peak areas. Good linear relationship was obtained within the range 8-500ngmL -1 of PP, r 2 =0.99985. Lower limits of detection and quantification after MISPE procedure of 2.4 and 8ngmL -1 , respectively were reached, in comparison with previously reported methodologies. The development of MISPE-HPLC methodology provided a simple an economic way for accomplishing a clean-up/preconcentration step and the subsequent determination of PP in a complex matrix. The performance of the proposed method was compared against C-18 and silica solid phase extraction (SPE) cartridges. The recovery factors obtained after applying extraction methods were 96.6, 64.8 and 0.79 for MISPE, C18-SPE and silica-SPE procedures, respectively. The proposed methodology improves the retention capability of SPE material plus robustness and possibility of reutilization, enabling it to be used for PP routine monitoring in diverse personal care products (PCP) and environmental samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Validated high-performance anion-exchange chromatography with pulsed amperometric detection method for the determination of residual keratan sulfate and other glucosamine impurities in sodium chondroitin sulfate.

PubMed

Bottelli, Susanna; Grillo, Gianluca; Barindelli, Edoardo; Nencioni, Alessandro; Di Maria, Alessandro; Fossati, Tiziano

2017-07-07

An efficient and sensitive analytical method based on high-performance anion exchange chromatography with pulsed amperometric detection (HPAEC-PAD) was devised for the determination of glucosamine (GlcN) in sodium chondroitin sulfate (CS). Glucosamine (GlcN) is intended as marker of residual keratan sulfate (KS) and other impurities generating glucosamine by acidic hydrolyzation. The latter brings CS and KS to their respective monomers. Since GlcN is present only in KS we developed a method that separates GlcN from GalN, the principal hydrolytic product of CS, and then we validated it in order to quantify GlcN. Method validation was performed by spiking CS raw material with known amounts of KS. Detection limit was 0.5% of KS in CS (corresponding to 0.1μg/ml), and the linear range was 0.5-5% of KS in CS (corresponding to 0.1-1μg/ml). The optimized analysis was carried out on an ICS-5000 system (Dionex, Sunnyvale, CA, USA) equipped with a Dionex Amino Trap guard column (3mm×30mm), Dionex CarboPac-PA20 (3mm×30mm) and a Dionex CarboPac-PA20 analytical column (3mm×150mm) using gradient elution at a 0.5ml/min flow rate. Regression equations revealed good linear relationship (R 2 =0.99, n=5) within the test ranges. Quality parameters, including precision and accuracy, were fully validated and found to be satisfactory. The fully validated HPAEC-PAD method was readily applied for the quantification of residual KS in CS in several raw materials and USP/EP reference substance. Results confirmed that the HPAEC-PAD method is more specific than the electrophoretic method for related substance reported in EP and provides sensitive determination of KS in acid-hydrolyzed CS samples, enabling the quantitation of KS and other impurities (generating glucosamine) in CS. Copyright © 2017 Elsevier B.V. All rights reserved.

Inner workings of aerodynamic sweep

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

Wadia, A.R.; Szucs, P.N.; Crall, D.W.

1998-10-01

The recent trend in using aerodynamic sweep to improve the performance of transonic blading has been one of the more significant technological evolutions for compression components in turbomachinery. This paper reports on the experimental and analytical assessment of the pay-off derived from both aft and forward sweep technology with respect to aerodynamic performance and stability. The single-stage experimental investigation includes two aft-swept rotors with varying degree and type of aerodynamic sweep and one swept forward rotor. On a back-to-back test basis, the results are compared with an unswept rotor with excellent performance and adequate stall margin. Although designed to satisfymore » identical design speed requirements as the unswept rotor, the experimental results reveal significant variations in efficiency and stall margin with the swept rotors. At design speed, all the swept rotors demonstrated a peak stage efficiency level that was equal to that of the unswept rotor. However, the forward-swept rotor achieved the highest rotor-alone peak efficiency. At the same time, the forward-swept rotor demonstrated a significant improvement in stall margin relative to the already satisfactory level achieved by the unswept rotor. Increasing the level of aft sweep adversely affected the stall margin. A three-dimensional viscous flow analysis was used to assist in the interpretation of the data. The reduced shock/boundary layer interaction, resulting from reduced axial flow diffusion and less accumulation of centrifuged blade surface boundary layer at the tip, was identified as the prime contributor to the enhanced performance with forward sweep. The impact of tip clearance on the performance and stability for one of the aft-swept rotors was also assessed.« less

36 CFR 51.46 - May the Director determine that a concessioner has not operated satisfactorily after a prospectus...

Code of Federal Regulations, 2010 CFR

2010-07-01

... of an annual evaluation of a concessioner's performance may not occur until after the selection of the best proposal submitted in response to a prospectus, the Director will make an annual performance... performance evaluation. In the event the concessioner receives a second less than satisfactory annual...

Correlations among Jamaican 12th-Graders' Five Variables and Performance in Genetics

ERIC Educational Resources Information Center

Bloomfield, Deen-Paul; Soyibo, Kola

2008-01-01

This study was aimed at finding out if the level of performance of selected Jamaican Grade 12 students on an achievement test on the concept of genetics was satisfactory; if there were statistically significant differences in their performance on the concept linked to their gender, self-esteem, cognitive abilities in biology, school-type and…

[Pregnancy in systemic autoimmune diseases: Myths, certainties and doubts].

PubMed

Danza, Álvaro; Ruiz-Irastorza, Guillermo; Khamashta, Munther

2016-10-07

Systemic autoimmune diseases especially affect young women during childbearing age. The aim of this review is to update systemic lupus erythematosus, antiphospholipid syndrome and systemic sclerosis management during pregnancy. These diseases present variable maternal and fetal risks. Studies show that an appropriate disease control and a reasonable remission period prior to pregnancy are associated with satisfactory obstetric outcomes. Antiphospholipid autoantibodies profile, anti-Ro/anti-La antibodies, pulmonary pressure and activity evaluation are crucial to assess the pregnancy risk. Monitoring requires a multidisciplinary team, serial analytic controls and Doppler ultrasound of maternal and fetal circulation. Evaluation of the activity of the disease is essential. Copyright © 2016 Elsevier España, S.L.U. All rights reserved.

Agricultural soil moisture experiment, Colby, Kansas 1978: Measured and predicted hydrological properties of the soil

NASA Technical Reports Server (NTRS)

Arya, L. M. (Principal Investigator)

1980-01-01

Predictive procedures for developing soil hydrologic properties (i.e., relationships of soil water pressure and hydraulic conductivity to soil water content) are presented. Three models of the soil water pressure-water content relationship and one model of the hydraulic conductivity-water content relationship are discussed. Input requirements for the models are indicated, and computational procedures are outlined. Computed hydrologic properties for Keith silt loam, a soil typer near Colby, Kansas, on which the 1978 Agricultural Soil Moisture Experiment was conducted, are presented. A comparison of computed results with experimental data in the dry range shows that analytical models utilizing a few basic hydrophysical parameters can produce satisfactory data for large-scale applications.

Study of Effects of Sweep on the Flutter of Cantilever Wings

NASA Technical Reports Server (NTRS)

Barmby, J G; Cunningham, H J; Garrick, I E

1951-01-01

An experimental and analytical investigation of the flutter of sweptback cantilever wings is reported. The experiments employed groups of wings swept back by rotating and by shearing. The angle of sweep range from 0 degree to 60 degrees and Mach numbers extended to approximately 0.85. A theoretical analysis of the air forces on an oscillating swept wing of high length-chord ratio is developed, and the approximations inherent in the assumptions are discussed. Comparison with experiment indicates that the analysis developed in the present report is satisfactory for giving the main effects of sweep, at least for nearly uniform cantilever wings of high and moderate length-chord ratios.

Theory for solubility in static systems

NASA Astrophysics Data System (ADS)

Gusev, Andrei A.; Suter, Ulrich W.

1991-06-01

A theory for the solubility of small particles in static structures has been developed. The distribution function of the solute in a frozen solid has been derived in analytical form for the quantum and the quasiclassical cases. The solubility at infinitesimal gas pressure (Henry's constant) as well as the pressure dependence of the solute concentration at elevated pressures has been found from the statistical equilibrium between the solute in the static matrix and the ideal-gas phase. The distribution function of a solute containing different particles has been evaluated in closed form. An application of the theory to the sorption of methane in the computed structures of glassy polycarbonate has resulted in a satisfactory agreement with experimental data.

Influence of dipolar interactions on the superparamagnetic relaxation time of γ-Fe2O3

NASA Astrophysics Data System (ADS)

Labzour, A.; Housni, A.; Limame, K.; Essahlaoui, A.; Sayouri, S.

2017-03-01

Influence of dipolar interactions on the Néel superparamagnetic relaxation time, τ , of an assembly of ultrafine ferromagnetic particles (γ-Fe2O3 ) with uniaxial anisotropy and of different sizes has been widely studied using Mössbauer technique. These studies, based on different analytical approaches, have shown that τ decreases with increasing interactions between particles. To interpret these results, we propose a model where interaction effects are considered as being due to a constant and external randomly oriented magnetic field B(Ψ, ϕ). The model is based on the resolution of the Fokker-Planck equation (FPE), generalizes previous calculations and gives satisfactory interpretation of the relaxation phenomenon in such systems.

Field assessment of balance in 10 to 14 year old children, reproducibility and validity of the Nintendo Wii board.

PubMed

Larsen, Lisbeth Runge; Jørgensen, Martin Grønbech; Junge, Tina; Juul-Kristensen, Birgit; Wedderkopp, Niels

2014-06-10

Because body proportions in childhood are different to those in adulthood, children have a relatively higher centre of mass location. This biomechanical difference and the fact that children's movements have not yet fully matured result in different sway performances in children and adults. When assessing static balance, it is essential to use objective, sensitive tools, and these types of measurement have previously been performed in laboratory settings. However, the emergence of technologies like the Nintendo Wii Board (NWB) might allow balance assessment in field settings. As the NWB has only been validated and tested for reproducibility in adults, the purpose of this study was to examine reproducibility and validity of the NWB in a field setting, in a population of children. Fifty-four 10-14 year-olds from the CHAMPS-Study DK performed four different balance tests: bilateral stance with eyes open (1), unilateral stance on dominant (2) and non-dominant leg (3) with eyes open, and bilateral stance with eyes closed (4). Three rounds of the four tests were completed with the NWB and with a force platform (AMTI). To assess reproducibility, an intra-day test-retest design was applied with a two-hour break between sessions. Bland-Altman plots supplemented by Minimum Detectable Change (MDC) and concordance correlation coefficient (CCC) demonstrated satisfactory reproducibility for the NWB and the AMTI (MDC: 26.3-28.2%, CCC: 0.76-0.86) using Centre Of Pressure path Length as measurement parameter. Bland-Altman plots demonstrated satisfactory concurrent validity between the NWB and the AMTI, supplemented by satisfactory CCC in all tests (CCC: 0.74-0.87). The ranges of the limits of agreement in the validity study were comparable to the limits of agreement of the reproducibility study. Both NWB and AMTI have satisfactory reproducibility for testing static balance in a population of children. Concurrent validity of NWB compared with AMTI was satisfactory. Furthermore, the results from the concurrent validity study were comparable to the reproducibility results of the NWB and the AMTI. Thus, NWB has the potential to replace the AMTI in field settings in studies including children. Future studies are needed to examine intra-subject variability and to test the predictive validity of NWB.

Field assessment of balance in 10 to 14 year old children, reproducibility and validity of the Nintendo Wii board

PubMed Central

2014-01-01

Background Because body proportions in childhood are different to those in adulthood, children have a relatively higher centre of mass location. This biomechanical difference and the fact that children’s movements have not yet fully matured result in different sway performances in children and adults. When assessing static balance, it is essential to use objective, sensitive tools, and these types of measurement have previously been performed in laboratory settings. However, the emergence of technologies like the Nintendo Wii Board (NWB) might allow balance assessment in field settings. As the NWB has only been validated and tested for reproducibility in adults, the purpose of this study was to examine reproducibility and validity of the NWB in a field setting, in a population of children. Methods Fifty-four 10–14 year-olds from the CHAMPS-Study DK performed four different balance tests: bilateral stance with eyes open (1), unilateral stance on dominant (2) and non-dominant leg (3) with eyes open, and bilateral stance with eyes closed (4). Three rounds of the four tests were completed with the NWB and with a force platform (AMTI). To assess reproducibility, an intra-day test-retest design was applied with a two-hour break between sessions. Results Bland-Altman plots supplemented by Minimum Detectable Change (MDC) and concordance correlation coefficient (CCC) demonstrated satisfactory reproducibility for the NWB and the AMTI (MDC: 26.3-28.2%, CCC: 0.76-0.86) using Centre Of Pressure path Length as measurement parameter. Bland-Altman plots demonstrated satisfactory concurrent validity between the NWB and the AMTI, supplemented by satisfactory CCC in all tests (CCC: 0.74-0.87). The ranges of the limits of agreement in the validity study were comparable to the limits of agreement of the reproducibility study. Conclusion Both NWB and AMTI have satisfactory reproducibility for testing static balance in a population of children. Concurrent validity of NWB compared with AMTI was satisfactory. Furthermore, the results from the concurrent validity study were comparable to the reproducibility results of the NWB and the AMTI. Thus, NWB has the potential to replace the AMTI in field settings in studies including children. Future studies are needed to examine intra-subject variability and to test the predictive validity of NWB. PMID:24913461

Do instability markers predict satisfactory reduction and requirement for later surgery in emergency department patients with wrist fracture?

PubMed

Winayak, Amar; Gossat, Alyza; Cooper, Jenny; Ritchie, Peter; Lim, Wei; Klim, Sharon; Kelly, Anne-Maree

2018-02-01

Research suggests that the presence of instability markers in patients with displaced distal radial fractures is associated with poorer outcome. Our aims were to determine whether the presence of previously defined instability markers could predict the likelihood of successful ED reduction and requirement for a secondary procedure after ED reduction. Retrospective cohort study performed by medical record review. Adult ED patients coded as having an isolated wrist fracture and having fracture reduction in ED were eligible for inclusion. Data collected included demographics, history of osteoporosis, mechanism of injury, radiological features on X-rays and performance of a secondary procedure. Outcomes of interest were the rate of successful fracture reduction in ED (against defined radiological criteria), the rate of secondary procedures and the association between the number of defined instability risk factors and successful reduction and performance of a secondary surgical procedure. Analysis was by χ 2 test, receiver operating characteristic curve, logistic regression analyses. Three hundred and nineteen patients were studied; median age 62 years, 77% female. Sixty-five per cent of patients had satisfactory fracture reduction in ED (95% CI 59%-70%). Eighty-six patients underwent a secondary procedure to reduce/stabilise their fracture (28%, 95% CI 23%-33%). Younger age, lack of satisfactory ED reduction and increased number of instability factors were independently predictive of the performance of a secondary procedure. Instability risk factors are common in patients with wrist fractures requiring reduction in ED. The number of instability factors is not a strong predictor of the performance of secondary procedures. © 2017 Australasian College for Emergency Medicine and Australasian Society for Emergency Medicine.

STOL ride control feasibility study

NASA Technical Reports Server (NTRS)

Gordon, C. K.; Dodson, R. O.

1973-01-01

The feasibility of developing a ride-smoothing control system for a 20-passenger turboprop STOL transport was assessed. Five different ride-control system configurations with varying degrees of complexity, performance, and cost were investigated. Results indicate that a satisfactory ride-control system can be practically implemented on the aircraft with minimum flight performance degradation.

[Evaluation of the analyzer of hematology Beckman Coulter® HmX™ in the university hospital of Oran].

PubMed

Zmouli, N; Moulasserdoun, K; Seghier, F

2013-11-01

The choice of an automaton of haematology is a determining stage, which has to take into account at the same time the quality of the results and the economic imperatives: workload, structure and organization of the laboratory. [corrected] It is in this spirit that we estimated during a period of 3 months the analyzer of haematology: the HmX™ Coulter with boatman of samples of the company Beckman. This automaton realizes the blood numeration, the formula leukocytic and the reticulocyte count. At first, we estimated the appropriate characteristics of device. Secondly, we estimated the relevance, the sensibility and the specificity of the alarms by comparing with the reference method, which is the optical microscopy. For that purpose, 125 blood smears resulting from service of haematology and from resuscitation were examined in optical microscopy. The technical tests were realized according to the recommendations of the International committee for evaluation of automatons of haematology. The analytical performances were satisfactory in particular the big interval of linearity and the absence of contamination. As regards the evaluation of the alarms system: rate of rejection is 63%, the sensibility 86%, the specificity 70%, the positive predictive value 80%, the negative predictive value 78% and the efficiency 80%. The alarms myelaemia and atypical lymphocytes were never sources of false negatives. The alarms erythroblasts and platelet aggregates did not engendered positive forgery. The blast cell alarm was responsible for a single case of false negative. The faithfulness of automaton is satisfactory: the absence of contamination, the big interval of linearity for the leukocytes, the red blood cells and the platelets as well as a good relevance of the alarms with regard to the anomalies found on the peripheral blood smear. From the user-friendliness and practicability point of view, the HmX™ Coulter was deeply appreciated. Copyright © 2013 Elsevier Masson SAS. All rights reserved.

Comparison of midwifery students' satisfaction with direct observation of procedural skills and current methods in evaluation of procedural skills in Mashhad Nursing and Midwifery School.

PubMed

Hoseini, Bibi Leila; Mazloum, Seyed Reza; Jafarnejad, Farzaneh; Foroughipour, Mohsen

2013-03-01

The clinical evaluation, as one of the most important elements in medical education, must measure students' competencies and abilities. The implementation of any assessment tool is basically dependent on the acceptance of students. This study tried to assess midwifery students' satisfaction with Direct Observation of Procedural Skills (DOPS) and current clinical evaluation methods. This quasi-experimental study was conducted in the university hospitals affiliated to Mashhad University of Medical Sciences. The subjects comprised 67 undergraduate midwifery students selected by convenience sampling and allocated to control and intervention groups according to the training transposition. Current method was performed in the control group, and DOPS was conducted in the intervention group. The applied tools included DOPS rating scales, logbook, and satisfaction questionnaires with clinical evaluation methods. Validity and reliability of these tools were approved. At the end of training, students' satisfaction with the evaluation methods was assessed by the mentioned tools. The data were analyzed by descriptive and analytical statistics. Satisfaction mean scores of midwifery students with DOPS and current methods were 76.7 ± 12.9 and 62.6 ± 14.7 (out of 100), respectively. DOPS students' satisfaction mean score was significantly higher than the score obtained in current method (P < 0.000). The most satisfactory domains in the current method were "consistence with learning objectives" (71.2 ± 14.9) and "objectiveness" in DOPS (87.9 ± 15.0). In contrast, the least satisfactory domains in the current method were "interested in applying the method" (57.8 ± 26.5) and "number of assessments for each skill" (58.8 ± 25.9) in DOPS method. This study showed that DOPS method is associated with greater students' satisfaction. Since the students' satisfaction with the current method was also acceptable, we recommend combining this new clinical evaluation method with the current method, which covers its weaknesses, to promote the students' satisfaction with clinical evaluation methods in a perfect manner.

34 CFR 361.89 - Enforcement procedures.

Code of Federal Regulations, 2011 CFR

2011-07-01

... Standards and Performance Indicators § 361.89 Enforcement procedures. (a) If a DSU fails to meet the... satisfactory level on the compliance indicators. (Approved by the Office of Management and Budget under control...

Fast UPLC/PDA determination of squalene in Sicilian P.D.O. pistachio from Bronte: Optimization of oil extraction method and analytical characterization.

PubMed

Salvo, Andrea; La Torre, Giovanna Loredana; Di Stefano, Vita; Capocchiano, Valentina; Mangano, Valentina; Saija, Emanuele; Pellizzeri, Vito; Casale, Katia Erminia; Dugo, Giacomo

2017-04-15

A fast reversed-phase UPLC method was developed for squalene determination in Sicilian pistachio samples that entry in the European register of the products with P.D.O. In the present study the SPE procedure was optimized for the squalene extraction prior to the UPLC/PDA analysis. The precision of the full analytical procedure was satisfactory and the mean recoveries were 92.8±0.3% and 96.6±0.1% for 25 and 50mgL -1 level of addition, respectively. Selected chromatographic conditions allowed a very fast squalene determination; in fact it was well separated in ∼0.54min with good resolution. Squalene was detected in all the pistachio samples analyzed and the levels ranged from 55.45-226.34mgkg -1 . Comparing our results with those of other studies it emerges that squalene contents in P.D.O. Sicilian pistachio samples, generally, were higher than those measured for other samples of different geographic origins. Copyright © 2016 Elsevier Ltd. All rights reserved.

Graphene oxide-based dispersive solid-phase extraction combined with in situ derivatization and gas chromatography-mass spectrometry for the determination of acidic pharmaceuticals in water.

PubMed

Naing, Nyi Nyi; Li, Sam Fong Yau; Lee, Hian Kee

2015-12-24

A fast and low-cost sample preparation method of graphene based dispersive solid-phase extraction combined with gas chromatography-mass spectrometric (GC-MS) analysis, was developed. The procedure involves an initial extraction with water-immiscible organic solvent, followed by a rapid clean-up using amine functionalized reduced graphene oxide as sorbent. Simple and fast one-step in situ derivatization using trimethylphenylammonium hydroxide was subsequently applied on acidic pharmaceuticals serving as model analytes, ibuprofen, gemfibrozil, naproxen, ketoprofen and diclofenac, before GC-MS analysis. Extraction parameters affecting the derivatization and extraction efficiency such as volume of derivatization agent, effect of desorption solvent, effect of pH and effect of ionic strength were investigated. Under the optimum conditions, the method demonstrated good limits of detection ranging from 1 to 16ngL(-1), linearity (from 0.01 to 50 and 0.05 to 50μgL(-1), depending on the analytes) and satisfactory repeatability of extractions (relative standard deviations, below 13%, n=3). Copyright © 2015 Elsevier B.V. All rights reserved.

Method validation for simultaneous determination of chromium, molybdenum and selenium in infant formulas by ICP-OES and ICP-MS.

PubMed

Khan, Naeem; Jeong, In Seon; Hwang, In Min; Kim, Jae Sung; Choi, Sung Hwa; Nho, Eun Yeong; Choi, Ji Yeon; Kwak, Byung-Man; Ahn, Jang-Hyuk; Yoon, Taehyung; Kim, Kyong Su

2013-12-15

This study aimed to validate the analytical method for simultaneous determination of chromium (Cr), molybdenum (Mo), and selenium (Se) in infant formulas available in South Korea. Various digestion methods of dry-ashing, wet-digestion and microwave were evaluated for samples preparation and both inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS) were compared for analysis. The analytical techniques were validated by detection limits, precision, accuracy and recovery experiments. Results showed that wet-digestion and microwave methods were giving satisfactory results for sample preparation, while ICP-MS was found more sensitive and effective technique than ICP-OES. The recovery (%) of Se, Mo and Cr by ICP-OES were 40.9, 109.4 and 0, compared to 99.1, 98.7 and 98.4, respectively by ICP-MS. The contents of Cr, Mo and Se in infant formulas by ICP-MS were found in good nutritional values in accordance to nutrient standards for infant formulas CODEX values. Copyright © 2013 Elsevier Ltd. All rights reserved.

Assessment of crack opening area for leak rates

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

Sharples, J.K.; Bouchard, P.J.

1997-04-01

This paper outlines the background to recommended crack opening area solutions given in a proposed revision to leak before break guidance for the R6 procedure. Comparisons with experimental and analytical results are given for some selected cases of circumferential cracks in cylinders. It is shown that elastic models can provide satisfactory estimations of crack opening displacement (and area) but they become increasingly conservative for values of L{sub r} greater than approximately 0.4. The Dugdale small scale yielding model gives conservative estimates of crack opening displacement with increasing enhancement for L{sub r} values greater than 0.4. Further validation of the elastic-plasticmore » reference stress method for up to L{sub r} values of about 1.0 is presented by experimental and analytical comparisons. Although a more detailed method, its application gives a best estimate of crack opening displacement which may be substantially greater than small scale plasticity models. It is also shown that the local boundary conditions in pipework need to be carefully considered when evaluating crack opening area for through-wall bending stresses resulting from welding residual stresses or geometry discontinuities.« less

Can matrix solid phase dispersion (MSPD) be more simplified? Application of solventless MSPD sample preparation method for GC-MS and GC-FID analysis of plant essential oil components.

PubMed

Wianowska, Dorota; Dawidowicz, Andrzej L

2016-05-01

This paper proposes and shows the analytical capabilities of a new variant of matrix solid phase dispersion (MSPD) with the solventless blending step in the chromatographic analysis of plant volatiles. The obtained results prove that the use of a solvent is redundant as the sorption ability of the octadecyl brush is sufficient for quantitative retention of volatiles from 9 plants differing in their essential oil composition. The extraction efficiency of the proposed simplified MSPD method is equivalent to the efficiency of the commonly applied variant of MSPD with the organic dispersing liquid and pressurized liquid extraction, which is a much more complex, technically advanced and highly efficient technique of plant extraction. The equivalency of these methods is confirmed by the variance analysis. The proposed solventless MSPD method is precise, accurate, and reproducible. The recovery of essential oil components estimated by the MSPD method exceeds 98%, which is satisfactory for analytical purposes. Copyright © 2016 Elsevier B.V. All rights reserved.

Correlations among Five Demographic Variables and the Performance of Selected Jamaican 11th-Graders on Some Numerical Problems on Energy

ERIC Educational Resources Information Center

Emepue, Nicholas; Soyibo, Kola

2009-01-01

This study was designed to assess whether the level of performance of selected Jamaican 11th-grade physics students on some numerical problems on the energy concept was satisfactory and if there were significant differences in their performance linked to their gender, socioeconomic background (SEB), school location, English language and…

76 FR 5431 - Publication of FY 2010 Service Contract Inventory

Federal Register 2010, 2011, 2012, 2013, 2014

2011-01-31

... available to the public at http://www.treasury.gov/about/organizational-structure/offices/Pages/Office-of... employees and contractors in the Department is effectively balanced, if contract performance is satisfactory...

24 CFR 570.411 - Joint Community Development Program.

Code of Federal Regulations, 2011 CFR

2011-04-01

... legislative body of each such unit of general local government. (h) NOFA contents. The NOFA will describe any... activities in a timely fashion, including satisfactory performance in carrying out any previous HUD-assisted...

46 CFR 160.037-3 - Materials, workmanship, construction, and performance requirements.

Code of Federal Regulations, 2010 CFR

2010-10-01

... preclude variations of density which may adversely affect uniformity of its smoke emitting characteristics... the signal plus packaging in a sealed plastic waterproof bag satisfactory to the Commandant. (d...

Modified Grice-Green subtalar arthrodesis performed using a partial fibular graft yields satisfactory results in patients with cerebral palsy.

PubMed

Güven, Melih; Tokyay, Abbas; Akman, Budak; Encan, Mehmet E; Altintaş, Faik

2016-03-01

The aim of this study was to report the experience with the use of a modified Grice-Green technique, which was performed using a partial subperiosteal fibular bone graft because of valgus unstable foot in children with cerebral palsy. Fifteen feet of 11 patients were evaluated on the basis of the appearance of the feet, clinical symptoms, and radiographic measurements. After an average follow-up duration of 24 (9-39) months, all feet showed satisfactory clinical and radiological results. Solid fusion and sustained correction took place in all feet. The gap at the donor site was bridged with new bone in all cases. No donor-site morbidity was detected. This modification of the Grice-Green technique can be used effectively in the correction of planovalgus foot in cerebral palsy.

A solid-phase microextraction fiber with carbon nanoparticles as sorbent material prepared by a simple flame-based preparation process.

PubMed

Sun, Min; Feng, Juanjuan; Qiu, Huamin; Fan, Lulu; Li, Leilei; Luo, Chuannan

2013-07-26

A novel carbon nanoparticles-coated solid-phase microextraction (SPME) fiber was prepared via a simple and low-cost flame-based preparation process, with stainless steel wire as support. Surface characteristic of the fiber was studied with scanning electron microscope. A nano-scaled brushy structure was observed. Coupled to gas chromatography (GC), the fiber was used to extract phthalate esters (PAEs) and polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. Analytical performances of the proposed method were investigated under the optimum extraction conditions (extraction temperature, 40°C; content of KCl, 30% (w/v); extraction time, 50min for PAEs and 40min for PAHs) and compared with other reports for the same analytes. Calibration ranges were 0.06-500μgL(-1) for di-n-butyl phthalate (DBP), and 0.1-300μgL(-1) for di-cyclohexyl phthalate (DCHP) and di-(2-ethyl-hexyl) phthalate (DEHP). For the eight PAHs, good linearity was obtained ranging from 0.01 to 150μgL(-1). Limits of detection were 0.005μgL(-1) for three PAEs and 0.001-0.003μgL(-1) for eight PAHs. The fiber exhibited excellent stability. It can be used for 100 times with RSDs of extraction efficiency less than 22.4%. The as-established SPME-GC method was applied to determine PAEs in food-wrap and PAHs in cigarette ash and snow water, and satisfactory results were obtained. The carbon nanoparticles-coated SPME fiber was efficient for sampling of organic compounds from aqueous samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Characterization and validation of sampling and analytical methods for mycotoxins in workplace air.

PubMed

Jargot, Danièle; Melin, Sandrine

2013-03-01

Mycotoxins are produced by certain plant or foodstuff moulds under growing, transport or storage conditions. They are toxic for humans and animals, some are carcinogenic. Methods to monitor occupational exposure to seven of the most frequently occurring airborne mycotoxins have been characterized and validated. Experimental aerosols have been generated from naturally contaminated particles for sampler evaluation. Air samples were collected on foam pads, using the CIP 10 personal aerosol sampler with its inhalable health-related aerosol fraction selector. The samples were subsequently solvent extracted from the sampling media, cleaned using immunoaffinity (IA) columns and analyzed by liquid chromatography with fluorescence detection. Ochratoxin A (OTA) or fumonisin and aflatoxin derivatives were detected and quantified. The quantification limits were 0.015 ng m(-3) OTA, 1 ng m(-3) fumonisins or 0.5 pg m(-3) aflatoxins, with a minimum dust concentration level of 1 mg m(-3) and a 4800 L air volume sampling. The methods were successfully applied to field measurements, which confirmed that workers could be exposed when handling contaminated materials. It was observed that airborne particles may be more contaminated than the bulk material itself. The validated methods have measuring ranges fully adapted to the concentrations found in the workplace. Their performance meets the general requirements laid down for chemical agent measurement procedures, with an expanded uncertainty less than 50% for most mycotoxins. The analytical uncertainty, comprised between 14 and 24%, was quite satisfactory given the low mycotoxin amounts, when compared to the food benchmarks. The methods are now user-friendly enough to be adopted for personal workplace sampling. They will later allow for mycotoxin occupational risk assessment, as only very few quantitative data have been available till now.

Comparatively evaluating the pharmacokinetic of fifteen constituents in normal and blood deficiency rats after oral administration of Xin-Sheng-Hua Granule by UPLC-MS/MS.

PubMed

Pang, Han-Qing; Tang, Yu-Ping; Cao, Yu-Jie; Tan, Ya-Jie; Jin, Yi; Shi, Xu-Qin; Huang, Sheng-Liang; Sun, Da-Zheng; Sun, Jin; Tang, Zhi-Shu; Duan, Jin-Ao

2017-09-01

Xin-Sheng-Hua Granule (XSHG), a famous traditional Chinese medicine prescription, are clinically applied for the treatment of postpartum disease through nourishing blood and promoting blood circulation. In this investigation, a multi-constituents (trigonelline, stachydrine hydrochloride, hydroxysafflor yellow A, chlorogenic acid, amygdalin, leonurine, liquiritin, ferulic acid, senkyunolide I, senkyunolide H, glycyrrhizic acid, senkyunolide A, ligustilide, butylidenephthalide and glycyrrhetinic acid) pharmacokinetic study of XSHG was conducted for the first time. These fifteen constituents in both normal and blood deficiency rat plasma were monitored by using the established and validated ultra-high-performance liquid chromatography coupled with a triple quadrupole electrospray tandem mass spectrometry (UPLC-TQ-MS/MS) method. The samples were prepared through removing protein from plasma with three volumes of methanol. Sufficient separation of target constituents and internal standards (chloramphenicol and clarithromycin) was obtained on a Thermo Scientific Hypersil GOLD column (100mm×3mm, 1.9μm) within a 20min gradient elution (0.1% formic acid aqueous - acetonitrile). Multiple reaction monitoring (MRM) mode was applied to monitor target analytes in both positive and negative electrospray ionization. For the fifteen selected target analytes, this method was fully validated with excellent linearity (r≥0.9925), satisfactory intra- and inter-day precisions (RSD≤11.87%), as well as good accuracies (RE, between -12.84 and 11.69). And the stabilities, matrix effects and extraction recoveries of the rat plasma samples were also within acceptable limits (RSD<15%). Compared to normal group, the pharmacokinetics of major active constituents (except liquiritin and glycyrrhetinic acid) had significant differences (P<0.05) in the model rats, indicated that several metabolite enzymes activities could be altered at disease condition. Copyright © 2017 Elsevier B.V. All rights reserved.

Simple and ultra-fast recognition and quantitation of compounded monoclonal antibodies: Application to flow injection analysis combined to UV spectroscopy and matching method.

PubMed

Jaccoulet, E; Schweitzer-Chaput, A; Toussaint, B; Prognon, P; Caudron, E

2018-09-01

Compounding of monoclonal antibody (mAbs) constantly increases in hospital. Quality control (QC) of the compounded mAbs based on quantification and identification is required to prevent potential errors and fast method is needed to manage outpatient chemotherapy administration. A simple and ultra-fast (less than 30 s) method using flow injection analysis associated to least square matching method issued from the analyzer software was performed and evaluated for the routine hospital QC of three compounded mAbs: bevacizumab, infliximab and rituximab. The method was evaluated through qualitative and quantitative parameters. Preliminary analysis of the UV absorption and second derivative spectra of the mAbs allowed us to adapt analytical conditions according to the therapeutic range of the mAbs. In terms of quantitative QC, linearity, accuracy and precision were assessed as specified in ICH guidelines. Very satisfactory recovery was achieved and the RSD (%) of the intermediate precision were less than 1.1%. Qualitative analytical parameters were also evaluated in terms of specificity, sensitivity and global precision through a matrix of confusion. Results showed to be concentration and mAbs dependant and excellent (100%) specificity and sensitivity were reached within specific concentration range. Finally, routine application on "real life" samples (n = 209) from different batch of the three mAbs complied with the specifications of the quality control i.e. excellent identification (100%) and ± 15% of targeting concentration belonging to the calibration range. The successful use of the combination of second derivative spectroscopy and partial least square matching method demonstrated the interest of FIA for the ultra-fast QC of mAbs after compounding using matching method. Copyright © 2018 Elsevier B.V. All rights reserved.

Commercial lateral flow devices for rapid detection of peanut (Arachis hypogaea) and hazelnut (Corylus avellana) cross-contamination in the industrial production of cookies.

PubMed

Röder, Martin; Vieths, Stefan; Holzhauser, Thomas

2009-09-01

Lateral flow devices (LFDs) are qualitative immunochromatographic tests for the rapid and specific detection of target analytes. We investigated commercially available LFDs for their ability to detect potentially allergenic peanut and hazelnut in raw cookie dough and chocolate, two important food matrices in the industrial production of cookies. Each three commercial LFDs for the detection of hazelnut and peanut were performed according to the manufacturers' instructions. All LFDs had comparably satisfactory specificity that was investigated with a variety of characteristic foods and food ingredients used in the production of cookies. In concordance with hazelnut-specific enzyme-linked immunosorbent assays (ELISAs), walnut was the most cross-reactive food for hazelnut-specific LFD. The sensitivity was verified in raw cookie doughs and chocolates that were either spiked with peanut or hazelnut between 1 and 25 mg/kg, respectively. Two hazelnut-specific LFDs detected hazelnut at a level of 3.5 mg/kg in both matrices, whereas the third LFD detected hazelnut at a level of 3.9 mg/kg in dough and 12.5 mg/kg in chocolate. Two peanut-specific LFDs detected peanut at a level of 1 mg/kg in both matrices. The third LFD detected peanut at a level of 14.2 mg/kg in chocolate and 4 mg/kg in dough. In conclusion, specific and sensitive LFD were identified for each hazelnut and peanut, having a level of sensitivity that is comparable to commercial ELISA for the investigated matrices. Such sensitive, specific, and rapid tests are useful analytical tools for allergen screening and sanitation in the industrial manufacture of foods.

Development of a gas chromatography-mass spectrometry method for the determination of pesticides in gaseous and particulate phases in the atmosphere.

PubMed

Borrás, E; Sánchez, P; Muñoz, A; Tortajada-Genaro, L A

2011-08-05

A reliable multi-residue method for determining gaseous and particulate phase pesticides in atmospheric samples has been developed. This method, based on full scan gas chromatography-mass spectrometry (GC-MS), allowed the proper determination of sixteen relevant pesticides, in a wide range of concentrations and without the influence of interferences. The pesticides were benfluralin, bitertanol, buprofezin, chlorfenvinphos, chlorpyrifos, chlorpyrifos-methyl, ethalfluralin, fenthion, lindane, malathion, methidathion, propachlor, propanil, pyriproxifen, tebuconazol and trifluralin. Comparisons of two types of sampling filters (quartz and glass fibre) and four types of solid-phase cartridges (XAD-2, XAD-4, Florisil and Orbo-49P) showed that the most suitable supports were glass fibre filter for particulate pesticides and XAD-2 and XAD-4 cartridges for gaseous pesticides (>95% recovery). Evaluations of elution solvents for ultrasonic-assisted extraction demonstrated that isooctane is better than ethylacetate, dichloromethane, methanol or a mixture of acetone:hexane (1:1). Recovery assays and the standard addition method were performed to validate the proposed methodology. Moreover, large simulator chamber experiments allowed the best study of the gas-particle partitioning of pesticides for testing the sampling efficiency for the validation of an analytical multiresidue method for pesticides in air. Satisfactory analytical parameters were obtained, with a repeatability of 5±1%, a reproducibility of 13±3% and detection limits of 0.05-0.18 pg m(-3) for the particulate phase and 26-88 pg m(-3) for the gaseous phase. Finally, the methodology was successfully applied to rural and agricultural samples in the Mediterranean area. Copyright © 2011 Elsevier B.V. All rights reserved.

Analysis of pulsating spray flames propagating in lean two-phase mixtures with unity Lewis number

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

Nicoli, C.; Haldenwang, P.; Suard, S.

2005-11-01

Pulsating (or oscillatory) spray flames have recently been observed in experiments on two-phase combustion. Numerical studies have pointed out that such front oscillations can be obtained even with very simple models of homogeneous two-phase mixtures, including elementary vaporization schemes. The paper presents an analytical approach within the simple framework of the thermal-diffusive model, which is complemented by a vaporization rate independent of gas temperature, as soon as the latter reaches a certain thermal threshold ({theta}{sub v} in reduced form). The study involves the Damkoehler number (Da), the ratio of chemical reaction rate to vaporization rate, and the Zeldovich number (Ze)more » as essential parameters. We use the standard asymptotic method based on matched expansions in terms of 1/Ze. Linear analysis of two-phase flame stability is performed by studying, in the absence of differential diffusive effects (unity Lewis number), the linear growth rate of 2-D perturbations added to steady plane solutions and characterized by wavenumber k in the direction transverse to spreading. A domain of existence is found for the pulsating regime. It corresponds to mixture characteristics often met in air-fuel two-phase systems: low boiling temperature ({theta}{sub v} << 1), reaction rate not higher than vaporization rate (Da < 1, i.e., small droplets), and activation temperature assumed to be high compared with flame temperature (Ze {>=} 10). Satisfactory comparison with numerical simulations confirms the validity of the analytical approach; in particular, positive growth rates have been found for planar perturbations (k = 0) and for wrinkled fronts (k {ne} 0). Finally, comparison between predicted frequencies and experimental measurements is discussed.« less

A simple and fast method based on mixed hemimicelles coated magnetite nanoparticles for simultaneous extraction of acidic and basic pollutants.

PubMed

Asgharinezhad, Ali Akbar; Ebrahimzadeh, Homeira

2016-01-01

One of the considerable and disputable areas in analytical chemistry is a single-step simultaneous extraction of acidic and basic pollutants. In this research, a simple and fast coextraction of acidic and basic pollutants (with different polarities) with the aid of magnetic dispersive micro-solid phase extraction based on mixed hemimicelles assembly was introduced for the first time. Cetyltrimethylammonium bromide (CTAB)-coated Fe3O4 nanoparticles as an efficient sorbent was successfully applied to adsorb 4-nitrophenol and 4-chlorophenol as two acidic and chlorinated aromatic amines as basic model compounds. Using a central composite design methodology combined with desirability function approach, the optimal experimental conditions were evaluated. The opted conditions were pH = 10; concentration of CTAB = 0.86 mmol L(-1); sorbent amount = 55.5 mg; sorption time = 11.0 min; no salt addition to the sample, type, and volume of the eluent = 120 μL methanol containing 5% acetic acid and 0.01 mol L(-1) HCl; and elution time = 1.0 min. Under the optimum conditions, detection limits and linear dynamic ranges were achieved in the range of 0.05-0.1 and 0.25-500 μg L(-1), respectively. The percent of extraction recoveries and relative standard deviations (n = 5) were in the range of 71.4-98.0 and 4.5-6.5, respectively. The performance of the optimized method was certified by coextraction of other acidic and basic compounds. Ultimately, the applicability of the method was successfully confirmed by the extraction and determination of the target analytes in various water samples, and satisfactory results were obtained.

Validation of the analysis of respirable crystalline silica (quartz) in foams used with CIP 10-R samplers.

PubMed

Eypert-Blaison, Céline; Moulut, Jean-Claude; Lecaque, Thierry; Marc, Florian; Kauffer, Edmond

2011-05-01

Sampling the respirable fraction to measure exposure to crystalline silica is most often carried out using cyclones. However, low flow rates (<4 l min(-1)) and continuing improvement in workplace hygiene means less and less material is sampled for analysis, resulting in increased analytical uncertainty. Use of the CIP 10-R sampler, working at a flow rate of 10 l min(-1), is one attempt to solve current analytical difficulties. To check the ability of the analysis of quartz sampled on foams, known amounts of quartz associated with a matrix have been injected into foams. The results obtained show that the proposed protocol, with prior acid attack and ashing of the foams, satisfies the recommendations of EN 482 Standard [CEN. (2006) Workplace atmospheres-general requirements for the performance of procedures for the measurements of chemical agents. Brussels, Belgium: EN 482 Comité Européen de normalization (CEN).], namely an expanded uncertainty of <50% for quartz weights between 0.1 and 0.5 times the 8-h exposure limit value and <30% for quartz weights between 0.5 and 2 times the 8-h exposure limit value, assuming an exposure limit value equal to 0.1 mg m(-3). Results obtained show that the 101 reflection line allows a quartz quantity of the order of 25 μg to be satisfactorily measured, which corresponds to a 10th of the exposure limit value, assuming an exposure limit value of 0.05 mg m(-3). In this case, the 100 and 112 reflection lines with expanded uncertainties of ~50% would also probably lead to satisfactory quantification. Particular recommendations are also proposed for the preparation of calibration curves to improve the method.

Green and simple analytical method to determine benzimidazoles in milk samples by using salting-out assisted liquid-liquid extraction and capillary liquid chromatography.

PubMed

Tejada-Casado, Carmen; Del Olmo-Iruela, Monsalud; García-Campaña, Ana M; Lara, Francisco J

2018-08-01

A green and simple multiresidue method using capillary liquid chromatography (CLC) with UV-diode array detection (DAD) has been developed for the determination of sixteen benzimidazoles (BZs) and its metabolites in milk samples. The separation was achieved in <32 min, using a Zorbax XDB-C18 column (150 mm × 0.5 mm I.D, 5 μm), with a mobile phase consisting of 50 mM ammonium acetate (solvent A) and a mixture of acetonitrile/methanol (1:1 v/v) (solvent B), at a flow rate of 9 μL min -1 . The temperature of the column was 20 °C and 6 μL of sample were injected. In spite of the complexity of milk samples, an effective, simple and fast sample preparation method called salting out-assisted liquid-liquid extraction (SALLE) was developed for the analysis of these compounds in cow milk samples. To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized including the amount of sample, type and volume of the extraction solvent, and the nature and amount of the salt. Good linearity was obtained (R 2  > 0.9985 for all BZs) with limits of detection (LOD) between 1.0 and 2.8 μg kg -1 . Relative standard deviations of repeatability and intermediate precision were below 1.6 and 14.2%, respectively. Satisfactory recoveries between 79.1 and 99.6% were also obtained for three types of milk samples (cow, sheep and goat). The advantages of a miniaturized technique such as CLC in terms of better efficiencies and reduced solvent consumption, combined with the simplicity of the SALLE procedure, make this method a useful alternative for the monitoring of these residues at trace level. Copyright © 2018 Elsevier B.V. All rights reserved.

Kinetic-spectrophotometric determination of trace amounts of vanadium(V) based on its catalytic effect on the reaction of DBM-arsenazo and potassium bromate

NASA Astrophysics Data System (ADS)

Zhai, Qing-zhou; Zhang, Xiao-xia; Huang, Chong

2008-03-01

A simple and sensitive kinetic-spectrophotometric method is developed for the determination of trace vanadium(V), based on the catalytic effect of vanadium(V) on the oxidation of DBM-arsenazo by potassium bromate in 0.0138 mol l -1 phosphoric acid medium and at 100 °C in the presence of citric acid as activator. The absorbance is measured at 528 nm with the fixed-time method. The optimization of the operating conditions regarding concentrations of the reagents, temperature and interferences are also investigated. The working curve is linear over the concentration range 0-20 ng ml -1 of vanadium(V) with good precision and accuracy and the detection limit was down to 3.44 ng l -1. The relative standard deviation for a standard solution of 14 ng ml -1 is 0.28% ( n = 11). The apparent activity energies of the catalytic reaction and the non-catalytic reaction are 73.48, 113.5 kJ/mol, respectively. The proposed method proved highly sensitive, selective and relatively rapid for the assay of vanadium at low-level range of 0-20 ng ml -1 without any pre-concentration step. Thw method was applied to the determination of vanadium(V) in steels, rice, flour, cabbage, potato, fish, shrimp and tea samples with satisfactory results. The obtained results for the steel samples were excellent agreement with the standard reference values. The analytical results of the rice, flour, cabbage, potato, fish, shrimp and tea samples were excellent agreement with those of atomic absorption spectrometry. The recovery experiments have been made for the rice, flour, cabbage, potato, fish, shrimp and tea samples except the steels; excellent results were obtained. The relative standard deviations were over the range of 0.18-2.60% and the recoveries were over the range of 98.00-102.4%, respectively. The analytical results obtained were satisfactory.

A normal incidence X-ray telescope

NASA Technical Reports Server (NTRS)

Golub, Leon

1987-01-01

The postflight performance evaluation of the X-ray telescope was summarized. All payload systems and subsystems performed well within acceptable limits, with the sole exception of the light-blocking prefilters. Launch, flight and recovery were performed in a fully satisfactory manner. The payload was recovered in a timely manner and in excellent condition. The prefilter performance analysis showed that no X-ray images were detected on the processed flight film. Recommendations for improved performance are listed.

Holistic rubric vs. analytic rubric for measuring clinical performance levels in medical students.

PubMed

Yune, So Jung; Lee, Sang Yeoup; Im, Sun Ju; Kam, Bee Sung; Baek, Sun Yong

2018-06-05

Task-specific checklists, holistic rubrics, and analytic rubrics are often used for performance assessments. We examined what factors evaluators consider important in holistic scoring of clinical performance assessment, and compared the usefulness of applying holistic and analytic rubrics respectively, and analytic rubrics in addition to task-specific checklists based on traditional standards. We compared the usefulness of a holistic rubric versus an analytic rubric in effectively measuring the clinical skill performances of 126 third-year medical students who participated in a clinical performance assessment conducted by Pusan National University School of Medicine. We conducted a questionnaire survey of 37 evaluators who used all three evaluation methods-holistic rubric, analytic rubric, and task-specific checklist-for each student. The relationship between the scores on the three evaluation methods was analyzed using Pearson's correlation. Inter-rater agreement was analyzed by Kappa index. The effect of holistic and analytic rubric scores on the task-specific checklist score was analyzed using multiple regression analysis. Evaluators perceived accuracy and proficiency to be major factors in objective structured clinical examinations evaluation, and history taking and physical examination to be major factors in clinical performance examinations evaluation. Holistic rubric scores were highly related to the scores of the task-specific checklist and analytic rubric. Relatively low agreement was found in clinical performance examinations compared to objective structured clinical examinations. Meanwhile, the holistic and analytic rubric scores explained 59.1% of the task-specific checklist score in objective structured clinical examinations and 51.6% in clinical performance examinations. The results show the usefulness of holistic and analytic rubrics in clinical performance assessment, which can be used in conjunction with task-specific checklists for more efficient evaluation.

Development of an in Silico Model of DPPH• Free Radical Scavenging Capacity: Prediction of Antioxidant Activity of Coumarin Type Compounds.

PubMed

Goya Jorge, Elizabeth; Rayar, Anita Maria; Barigye, Stephen J; Jorge Rodríguez, María Elisa; Sylla-Iyarreta Veitía, Maité

2016-06-07

A quantitative structure-activity relationship (QSAR) study of the 2,2-diphenyl-l-picrylhydrazyl (DPPH•) radical scavenging ability of 1373 chemical compounds, using DRAGON molecular descriptors (MD) and the neural network technique, a technique based on the multilayer multilayer perceptron (MLP), was developed. The built model demonstrated a satisfactory performance for the training ( R 2 = 0.713 ) and test set ( Q ext 2 = 0.654 ) , respectively. To gain greater insight on the relevance of the MD contained in the MLP model, sensitivity and principal component analyses were performed. Moreover, structural and mechanistic interpretation was carried out to comprehend the relationship of the variables in the model with the modeled property. The constructed MLP model was employed to predict the radical scavenging ability for a group of coumarin-type compounds. Finally, in order to validate the model's predictions, an in vitro assay for one of the compounds (4-hydroxycoumarin) was performed, showing a satisfactory proximity between the experimental and predicted pIC50 values.

[ASSOCIATION BETWEEN FITNESS, NUTRITIONAL STATUS AND ACADEMIC PERFORMANCE IN PHYSICAL EDUCATION STUDENTS].

PubMed

Godoy Cumillaf, Andrés; Valdés Badilla, Pablo; Fariña Herrera, Custodio; Cárcamo Mora, Francisco; Medina Herrera, Bernice; Meneses Sandoval, Elías; Gedda Muñoz, Relmu; Durán Agüero, Samuel

2015-10-01

several studies demonstrated that regular physical exercise would impact positively on the academic performance of students. to determine the association between physical fitness, nutritional status and academic performance of students of Pedagogy in Physical Education from Temuco, Chile. the sample was selected on a non-probabilistic approach, which included 208 subjects (n = 153 women and n = 55 women). The variables studied were physical fitness (short Abs, long jump with feet together, forward trunk flexion, elbow flexion and extension and "course navette" test), nutritional status (BMI) and academic performance (classified as up and down the academic average). 87.5% of students have a satisfactory fitness and a BMI of 23.8 ± 2.9 kg/m2. The students with the best academic performance were those with the higher proportion of satisfactory physical condition (92.5 %). No association between academic performance and nutritional status was determined, but it was observed between low fitness and a great risk of low academic performance (OR = 2.8, 95% CI 1.0 to 8 1; p < 0.05). a relationship between academic achievement and physical fitness among students is observed, but no for the nutritional status and the academic performance. Copyright AULA MEDICA EDICIONES 2014. Published by AULA MEDICA. All rights reserved.

Self-reported academic performance in relation to health behaviours among Bahria University students.

PubMed

Rehman, Rehana; Zafar, Amara; Mohib, Aleena; Hussain, Mehwish; Ali, Rabiya

2018-02-01

To find an association between self-reported academic performance with different socio-demographic factors, health behaviours and mental health amongst university students. This cross-sectional study was conducted at Bahria University, Karachi, from January 2012 to December 2013, and comprised university students of different disciplines. An anonymous, self-reported questionnaire was distributed among the subjects. Convenient sampling technique was used. Demographic information, including age, gender and field of study, were obtained. Depresion was evaluated via Centre for Epidemiological Studies Depression Scale. SPSS 22 was used to analyse data. Of the 813 respondents, 334(41.1%) were males and 479(58.9%) females. The mean age was 19.9±1.8 years. Overall, 126(15.5%) subjects reported excellent, 242(29.8%) very good, 310(38.1%) good, 100(12.3%) satisfactory and 35(4.3%) not satisfactory academic performance. Residential status of students played a significant role on their academic performance (p=0.011). Breakfast eating behaviour depicted a significant association with the academic performance (p=0.04).The proportion of unsatisfactory academic performances among students having severe sleep disorder was the highest, followed by mild/moderate (p=0.01). The depression scale's item 'troubling in mind' was highly associated with academic performance (p<0.05). A constructive association existed among healthy behaviours and academic performance. .

U.S. Geological Survey Standard Reference Sample Project: Performance Evaluation of Analytical Laboratories

USGS Publications Warehouse

Long, H. Keith; Daddow, Richard L.; Farrar, Jerry W.

1998-01-01

Since 1962, the U.S. Geological Survey (USGS) has operated the Standard Reference Sample Project to evaluate the performance of USGS, cooperator, and contractor analytical laboratories that analyze chemical constituents of environmental samples. The laboratories are evaluated by using performance evaluation samples, called Standard Reference Samples (SRSs). SRSs are submitted to laboratories semi-annually for round-robin laboratory performance comparison purposes. Currently, approximately 100 laboratories are evaluated for their analytical performance on six SRSs for inorganic and nutrient constituents. As part of the SRS Project, a surplus of homogeneous, stable SRSs is maintained for purchase by USGS offices and participating laboratories for use in continuing quality-assurance and quality-control activities. Statistical evaluation of the laboratories results provides information to compare the analytical performance of the laboratories and to determine possible analytical deficiences and problems. SRS results also provide information on the bias and variability of different analytical methods used in the SRS analyses.

Course Evaluation in Sweden--When, How, What and Why

ERIC Educational Resources Information Center

Cronholm, Stefan

2010-01-01

This study is about course evaluation in Swedish higher education. Performing course evaluation is regulated in Swedish law. Despite this, only half of the courses are evaluated. The aim of this study is to understand why satisfactory course evaluations not are performed. Problems are identified from a student perspective and the paper provides…

The Academic Progress Rate: Good PR, Bad Policy

ERIC Educational Resources Information Center

Cusack, Michael J.

2007-01-01

This fall the Academic Progress Rate, a formula that the National Collegiate Athletic Association developed to measure the academic performance of its member teams, will go into full effect. Known as the APR, the formula consists of two variables: academic performance (which requires satisfactory grades and timely progress to a degree) and student…

32 CFR 1656.4 - Alternative Service Office: jurisdiction and authority.

Code of Federal Regulations, 2010 CFR

2010-07-01

... for job placement; (5) Monitor the ASW's job performance; (6) Issue a certificate of satisfactory... assigned to perform alternative service. (b) The ASO shall: (1) Evaluate and approve jobs and employers for Alternative Service; (2) Order the ASW to report for alternative service work; (3) Issue such orders as are...

Generalized Hill-stability criteria for hierarchical three-body systems at arbitrary inclinations

NASA Astrophysics Data System (ADS)

Grishin, Evgeni; Perets, Hagai B.; Zenati, Yossef; Michaely, Erez

2017-04-01

A fundamental aspect of the three-body problem is its stability. Most stability studies have focused on the co-planar three-body problem, deriving analytic criteria for the dynamical stability of such pro/retrograde systems. Numerical studies of inclined systems phenomenologically mapped their stability regions, but neither complement it by theoretical framework, nor provided satisfactory fit for their dependence on mutual inclinations. Here we present a novel approach to study the stability of hierarchical three-body systems at arbitrary inclinations, which accounts not only for the instantaneous stability of such systems, but also for the secular stability and evolution through Lidov-Kozai cycles and evection. We generalize the Hill-stability criteria to arbitrarily inclined triple systems, explain the existence of quasi-stable regimes and characterize the inclination dependence of their stability. We complement the analytic treatment with an extensive numerical study, to test our analytic results. We find excellent correspondence up to high inclinations (˜120°), beyond which the agreement is marginal. At such high inclinations, the stability radius is larger, the ratio between the outer and inner periods becomes comparable and our secular averaging approach is no longer strictly valid. We therefore combine our analytic results with polynomial fits to the numerical results to obtain a generalized stability formula for triple systems at arbitrary inclinations. Besides providing a generalized secular-based physical explanation for the stability of non-co-planar systems, our results have direct implications for any triple systems and, in particular, binary planets and moon/satellite systems; we briefly discuss the latter as a test case for our models.

Microchip electrophoresis with background electrolyte containing polyacrylic acid and high content organic solvent in cyclic olefin copolymer microchips for easily adsorbed dyes.

PubMed

Wei, Xuan; Sun, Ping; Yang, Shenghong; Zhao, Lei; Wu, Jing; Li, Fengyun; Pu, Qiaosheng

2016-07-29

Plastic microchips can significantly reduce the fabrication cost but the adsorption of some analytes limits their application. In this work, background electrolyte containing ionic polymer and high content of organic solvent was adopted to eliminate the analyte adsorption and achieve highly efficient separation in microchip electrophoresis. Two dyes, rhodamine 6G (Rh6G) and rhodamine B (RhB) were used as the model analytes. By using methanol as the organic solvent and polyacrylic acid (PAA) as a multifunctional additive, successful separation of the two dyes within 75μm id. microchannels was realized. The role of PAA is multiple, including viscosity regulator, selectivity modifier and active additive for counteracting analyte adsorption on the microchannel surface. The number of theoretical plate of 7.0×10(5)/m was attained within an effective separation distance of 2cm using background electrolyte consisting 80% methanol, 0.36% PAA and 30mmol/L phosphate at pH 5.0. Under optimized conditions, relative standard deviations of Rh6G and RhB detection (n=5) were no more than 1.5% for migration time and 2.0% for peak area, respectively. The limit of detection (S/N=3) was 0.1nmol/L for Rh6G. The proposed technique was applied in the determination of both Rh6G and RhB in chilli powder and lipstick samples with satisfactory recoveries of 81.3-103.7%. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of multiple pesticides in fruits and vegetables using a modified quick, easy, cheap, effective, rugged and safe method with magnetic nanoparticles and gas chromatography tandem mass spectrometry.

PubMed

Li, Yan-Fei; Qiao, Lu-Qin; Li, Fang-Wei; Ding, Yi; Yang, Zi-Jun; Wang, Ming-Lin

2014-09-26

Based on a modified quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation method with Fe3O4 magnetic nanoparticles (MNPs) as the adsorbing material and gas chromatography-tandem mass spectrometry (GC-MS/MS) determination in multiple reaction monitoring (MRM) mode, we established a new method for the determination of multiple pesticides in vegetables and fruits. It was determined that bare MNPs have excellent function as adsorbent when purified, and it is better to be separated from the extract. The amount of MNPs influenced the clean-up performance and recoveries. To achieve the optimum performance of modified QuEChERS towards the target analytes, several parameters including the amount of the adsorbents and purification time were investigated. Under the optimum conditions, recoveries were evaluated in four representative matrices (tomato, cucumber, orange and apple) with the spiked concentrations of 10 μg kg(-1), 50 μg kg(-1)and 200 μg kg(-1) in all cases. The results showed that the recovery of 101 pesticides ranged between 71.5 and 111.7%, and the relative standard deviation was less than 10.5%. The optimum clean-up system improved the purification efficiency and simultaneously obtained satisfactory recoveries of multiple pesticides, including planar-ring pesticides. In short, the modified QuEChERS method in addition to MNPs used for removing impurities improved the speed of sample pre-treatment and exhibited an enhanced performance and purifying effect. Copyright © 2014 Elsevier B.V. All rights reserved.

A comparison of the analytical performance of five commercially available assays for neutrophil gelatinase-associated lipocalin using urine.

PubMed

Kift, Rebecca L; Messenger, Michael P; Wind, Tobias C; Hepburn, Sophie; Wilson, Michelle; Thompson, Douglas; Smith, Matthew Welberry; Sturgeon, Catharine; Lewington, Andrew J; Selby, Peter J; Banks, Rosamonde E

2013-05-01

Neutrophil gelatinase-associated lipocalin (NGAL) is a promising biomarker for acute kidney injury that is beginning to be used in clinical practice in addition to research studies. The current study describes an independent validation and comparison of five commercially available NGAL assays, focusing on urine samples. This is an essential step in the translation of this marker to clinical use in terms of allowing valid inter-study comparison and generation of robust results. Two CE (Conformité Européenne)-marked assays, the NGAL Test (BioPorto) on Siemens ADVIA(®) 1800 and the ARCHITECT Urine NGAL assay on i2000SR (Abbott Laboratories), and three research-use-only (RUO) ELISAs (R&D Systems, Hycult and BioPorto) were evaluated. Imprecision, parallelism, recovery, selectivity, limit of quantitation (LOQ), vulnerability to interference and hook effect were assessed and inter-assay agreement was determined using 68 urine samples from patients with various renal diseases and healthy controls. The Abbott and R&D Systems assays demonstrated satisfactory performance for all parameters tested. However for the other three assays evaluated, problems were identified with LOQ (BioPorto/ADVIA(®)), parallelism (BioPorto ELISA) or several parameters (Hycult). Between-method agreement varied with the Hycult assay in particular being markedly different and highlighting issues with standardization and form of NGAL measured. Variability exists between the five NGAL assays in terms of their performance and this should be taken into account when interpreting results from the various clinical or research studies measuring urinary NGAL.

34 CFR 668.34 - Satisfactory academic progress.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 34 Education 3 2013-07-01 2013-07-01 false Satisfactory academic progress. 668.34 Section 668.34... Satisfactory academic progress. (a) Satisfactory academic progress policy. An institution must establish a reasonable satisfactory academic progress policy for determining whether an otherwise eligible student is...

34 CFR 668.34 - Satisfactory academic progress.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 34 Education 3 2014-07-01 2014-07-01 false Satisfactory academic progress. 668.34 Section 668.34... Satisfactory academic progress. (a) Satisfactory academic progress policy. An institution must establish a reasonable satisfactory academic progress policy for determining whether an otherwise eligible student is...

34 CFR 668.34 - Satisfactory academic progress.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 34 Education 3 2012-07-01 2012-07-01 false Satisfactory academic progress. 668.34 Section 668.34... Satisfactory academic progress. (a) Satisfactory academic progress policy. An institution must establish a reasonable satisfactory academic progress policy for determining whether an otherwise eligible student is...

34 CFR 668.34 - Satisfactory academic progress.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 34 Education 3 2011-07-01 2011-07-01 false Satisfactory academic progress. 668.34 Section 668.34... Satisfactory academic progress. (a) Satisfactory academic progress policy. An institution must establish a reasonable satisfactory academic progress policy for determining whether an otherwise eligible student is...

38 CFR 21.8360 - Satisfactory conduct and cooperation.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 38 Pensions, Bonuses, and Veterans' Relief 2 2010-07-01 2010-07-01 false Satisfactory conduct and... Children of Vietnam Veterans-Spina Bifida and Covered Birth Defects Satisfactory Conduct and Cooperation § 21.8360 Satisfactory conduct and cooperation. The provisions for satisfactory conduct and cooperation...

A rapid and sensitive analytical method for the determination of 14 pyrethroids in water samples.

PubMed

Feo, M L; Eljarrat, E; Barceló, D

2010-04-09

A simple, efficient and environmentally friendly analytical methodology is proposed for extracting and preconcentrating pyrethroids from water samples prior to gas chromatography-negative ion chemical ionization mass spectrometry (GC-NCI-MS) analysis. Fourteen pyrethroids were selected for this work: bifenthrin, cyfluthrin, lambda-cyhalothrin, cypermethrin, deltamethrin, esfenvalerate, fenvalerate, fenpropathrin, tau-fluvalinate, permethrin, phenothrin, resmethrin, tetramethrin and tralomethrin. The method is based on ultrasound-assisted emulsification-extraction (UAEE) of a water-immiscible solvent in an aqueous medium. Chloroform was used as extraction solvent in the UAEE technique. Target analytes were quantitatively extracted achieving an enrichment factor of 200 when 20 mL aliquot of pure water spiked with pyrethroid standards was extracted. The method was also evaluated with tap water and river water samples. Method detection limits (MDLs) ranged from 0.03 to 35.8 ng L(-1) with RSDs values < or =3-25% (n=5). The coefficients of estimation of the calibration curves obtained following the proposed methodology were > or =0.998. Recovery values were in the range of 45-106%, showing satisfactory robustness of the method for analyzing pyrethroids in water samples. The proposed methodology was applied for the analysis of river water samples. Cypermethrin was detected at concentration levels ranging from 4.94 to 30.5 ng L(-1). Copyright 2010 Elsevier B.V. All rights reserved.

Digital filtering implementations for the detection of broad spectral features by direct analysis of passive Fourier transform infrared interferograms.

PubMed

Tarumi, Toshiyasu; Small, Gary W; Combs, Roger J; Kroutil, Robert T

2004-04-01

Finite impulse response (FIR) filters and finite impulse response matrix (FIRM) filters are evaluated for use in the detection of volatile organic compounds with wide spectral bands by direct analysis of interferogram data obtained from passive Fourier transform infrared (FT-IR) measurements. Short segments of filtered interferogram points are classified by support vector machines (SVMs) to implement the automated detection of heated plumes of the target analyte, ethanol. The interferograms employed in this study were acquired with a downward-looking passive FT-IR spectrometer mounted on a fixed-wing aircraft. Classifiers are trained with data collected on the ground and subsequently used for the airborne detection. The success of the automated detection depends on the effective removal of background contributions from the interferogram segments. Removing the background signature is complicated when the analyte spectral bands are broad because there is significant overlap between the interferogram representations of the analyte and background. Methods to implement the FIR and FIRM filters while excluding background contributions are explored in this work. When properly optimized, both filtering procedures provide satisfactory classification results for the airborne data. Missed detection rates of 8% or smaller for ethanol and false positive rates of at most 0.8% are realized. The optimization of filter design parameters, the starting interferogram point for filtering, and the length of the interferogram segments used in the pattern recognition is discussed.

An analytic performance model of disk arrays and its application

NASA Technical Reports Server (NTRS)

Lee, Edward K.; Katz, Randy H.

1991-01-01

As disk arrays become widely used, tools for understanding and analyzing their performance become increasingly important. In particular, performance models can be invaluable in both configuring and designing disk arrays. Accurate analytic performance models are desirable over other types of models because they can be quickly evaluated, are applicable under a wide range of system and workload parameters, and can be manipulated by a range of mathematical techniques. Unfortunately, analytical performance models of disk arrays are difficult to formulate due to the presence of queuing and fork-join synchronization; a disk array request is broken up into independent disk requests which must all complete to satisfy the original request. We develop, validate, and apply an analytic performance model for disk arrays. We derive simple equations for approximating their utilization, response time, and throughput. We then validate the analytic model via simulation and investigate the accuracy of each approximation used in deriving the analytical model. Finally, we apply the analytical model to derive an equation for the optimal unit of data striping in disk arrays.

Studies of the Lateral-Directional Flying Qualities of a Tandem Helicopter in Forward Flight

NASA Technical Reports Server (NTRS)

Amer, Kenneth B; Tapscott, Robert J

1954-01-01

An investigation of the lateral-directional flying qualities of a tandem-rotor helicopter in forward flight was undertaken to determine desirable goals for helicopter lateral-directional flying qualities and possible methods of achieving these goals in the tandem-rotor helicopter. Comparison between directional stability as measured in flight and rotor-off model tests in a wind tunnel shows qualitative agreement and, hence, indicates such wind-tunnel test, despite the absence of the rotors, to be one effective method of studying means of improving the directional stability of the tandem helicopter. Flight-test measurements of turns and oscillations, in conjunction with analytical studies, suggest possible practical methods of achieving the goals of satisfactory turn and oscillatory characteristics in the tandem helicopter.

NOTE: Solving the ECG forward problem by means of a meshless finite element method

NASA Astrophysics Data System (ADS)

Li, Z. S.; Zhu, S. A.; He, Bin

2007-07-01

The conventional numerical computational techniques such as the finite element method (FEM) and the boundary element method (BEM) require laborious and time-consuming model meshing. The new meshless FEM only uses the boundary description and the node distribution and no meshing of the model is required. This paper presents the fundamentals and implementation of meshless FEM and the meshless FEM method is adapted to solve the electrocardiography (ECG) forward problem. The method is evaluated on a single-layer torso model, in which the analytical solution exists, and tested in a realistic geometry homogeneous torso model, with satisfactory results being obtained. The present results suggest that the meshless FEM may provide an alternative for ECG forward solutions.

On the dielectric conductivity of molecular ionic liquids.

PubMed

Schröder, Christian; Steinhauser, Othmar

2009-09-21

The contribution of the conductivity to the spectrum of the generalized dielectric constant or susceptibility of molecular ionic liquids is analyzed, both in theoretical terms and computationally by means of molecular dynamics simulation of the concrete system 1-ethyl-3-methyl-imidazolium dicyanoamide at 300 K. As a central quantity the simulated current autocorrelation function is modeled by a carefully designed fit function. This not only gives a satisfactory numerical representation but yields the correct conductivity upon integration. In addition the fit function can be Fourier-Laplace transformed analytically. Both, the real and imaginary parts of the transform show expected behavior, in particular, the right limits for zero frequency. This altogether demonstrates that the components of the fit function are of physical relevance.

Porous matrix structures for alkaline electrolyte fuel cells

NASA Technical Reports Server (NTRS)

Vine, R. W.; Narsavage, S. T.

1975-01-01

A number of advancements have been realized by a continuing research program to develop higher chemically stable porous matrix structures with high bubble pressure (crossover resistance) for use as separators in potassium hydroxide electrolyte fuel cells. More uniform, higher-bubble-pressure asbestos matrices were produced by reconstituting Johns-Manville asbestos paper; Fybex potassium titanate which was found compatible with 42% KOH at 250 F for up to 3000 hr; good agreement was found between bubble pressures predicted by an analytical study and those measured with filtered structures; Teflon-bonded Fybex matrices with bubble pressures greater than 30 psi were obtained by filtering a water slurry of the mixture directly onto fuel cell electrodes; and PBI fibers have satisfactory compatibility with 42% KOH at 250 F.

[Studies on the interaction between RNA with neutral red and determination of RNA by spectrophotometry].

PubMed

Si, Wen-Hui

2007-06-01

An analytical method for the determination of ribonucleic acid by spectrophotometry was established. At the maximum absorption wavelength for neutral red in B-R buffer solution, and under the best conditions, the decrease in the absorbance was linear with the amount of ribonucleic acid. The linearity range was 0.0-9.0 microg x mL(-1), the detection limit was 0.52 microg x mL(-1), and the correlation coeffient was 0.999 8. This method was simple, rapid, and selective. So its application to the determination of ribonucleic acid was satisfactory. The reaction mechanism was that the electrostatic interaction leads to molecular association of RNA with neutral red, resulting in anti-ion permutation and bonding reaction.

Size-dependent resonance frequencies of cantilevered and bridged nanosensors

NASA Astrophysics Data System (ADS)

Shi, W.; Zou, J.; Lee, K. Y.; Li, X. F.

2018-03-01

This paper studies transverse vibration of nanoscale cantilevered and bridged sensors carrying a nanoparticle. The nanoscale sensors are modelled as Euler-Bernoulli beams with surface effect and nanoparticle as a concentrated mass. Frequency equations of cantilevered and bridged beam-mass system are derived and exact resonance frequencies are calculated. An alternative Fredholm integral equation method is used to obtain an approximate explicit expression for the fundamental frequency for both cases. A comparison between the approximate and analytical results is made and the approximation accuracy is satisfactory. The influences of the residual surface stress, surface elasticity, and attached mass on the resonance frequencies and mode shapes are discussed. These results are useful to illustrate the surface phenomena and are helpful to design micro-/nano-mechanical sensors.

Portal scatter to primary dose ratio of 4 to 18 MV photon spectra incident on heterogeneous phantoms

NASA Astrophysics Data System (ADS)

Ozard, Siobhan R.

Electronic portal imagers designed and used to verify the positioning of a cancer patient undergoing radiation treatment can also be employed to measure the in vivo dose received by the patient. This thesis investigates the ratio of the dose from patient-scattered particles to the dose from primary (unscattered) photons at the imaging plane, called the scatter to primary dose ratio (SPR). The composition of the SPR according to the origin of scatter is analyzed more thoroughly than in previous studies. A new analytical method for calculating the SPR is developed and experimentally verified for heterogeneous phantoms. A novel technique that applies the analytical SPR method for in vivo dosimetry with a portal imager is evaluated. Monte Carlo simulation was used to determine the imager dose from patient-generated electrons and photons that scatter one or more times within the object. The database of SPRs reported from this investigation is new since the contribution from patient-generated electrons was neglected by previous Monte Carlo studies. The SPR from patient-generated electrons was found here to be as large as 0.03. The analytical SPR method relies on the established result that the scatter dose is uniform for an air gap between the patient and the imager that is greater than 50 cm. This method also applies the hypothesis that first-order Compton scatter only, is sufficient for scatter estimation. A comparison of analytical and measured SPRs for neck, thorax, and pelvis phantoms showed that the maximum difference was within +/-0.03, and the mean difference was less than +/-0.01 for most cases. This accuracy was comparable to similar analytical approaches that are limited to homogeneous phantoms. The analytical SPR method could replace lookup tables of measured scatter doses that can require significant time to measure. In vivo doses were calculated by combining our analytical SPR method and the convolution/superposition algorithm. Our calculated in vivo doses agreed within +/-3% with the doses measured in the phantom. The present in vivo method was faster compared to other techniques that use convolution/superposition. Our method is a feasible and satisfactory approach that contributes to on-line patient dose monitoring.

Analytical techniques and instrumentation: A compilation. [analytical instrumentation, materials performance, and systems analysis

NASA Technical Reports Server (NTRS)

1974-01-01

Technical information is presented covering the areas of: (1) analytical instrumentation useful in the analysis of physical phenomena; (2) analytical techniques used to determine the performance of materials; and (3) systems and component analyses for design and quality control.

42 CFR 493.845 - Standard; Toxicology.

Code of Federal Regulations, 2012 CFR

2012-10-01

... acceptable responses for each analyte in each testing event is unsatisfactory analyte performance for the... testing event. (e)(1) For any unsatisfactory analyte or test performance or testing event for reasons... any unacceptable analyte or testing event score, remedial action must be taken and documented, and the...

42 CFR 493.851 - Standard; Hematology.

Code of Federal Regulations, 2014 CFR

2014-10-01

... acceptable responses for each analyte in each testing event is unsatisfactory analyte performance for the... testing event. (e)(1) For any unsatisfactory analyte or test performance or testing event for reasons... any unacceptable analyte or testing event score, remedial action must be taken and documented, and the...

42 CFR 493.843 - Standard; Endocrinology.

Code of Federal Regulations, 2013 CFR

2013-10-01

... acceptable responses for each analyte in each testing event is unsatisfactory analyte performance for the... testing event. (e)(1) For any unsatisfactory analyte or test performance or testing event for reasons... any unacceptable analyte or testing event score, remedial action must be taken and documented, and the...

42 CFR 493.845 - Standard; Toxicology.

Code of Federal Regulations, 2014 CFR

2014-10-01

... acceptable responses for each analyte in each testing event is unsatisfactory analyte performance for the... testing event. (e)(1) For any unsatisfactory analyte or test performance or testing event for reasons... any unacceptable analyte or testing event score, remedial action must be taken and documented, and the...

42 CFR 493.845 - Standard; Toxicology.

Code of Federal Regulations, 2013 CFR

2013-10-01

... acceptable responses for each analyte in each testing event is unsatisfactory analyte performance for the... testing event. (e)(1) For any unsatisfactory analyte or test performance or testing event for reasons... any unacceptable analyte or testing event score, remedial action must be taken and documented, and the...

42 CFR 493.851 - Standard; Hematology.

Code of Federal Regulations, 2013 CFR

2013-10-01

... acceptable responses for each analyte in each testing event is unsatisfactory analyte performance for the... testing event. (e)(1) For any unsatisfactory analyte or test performance or testing event for reasons... any unacceptable analyte or testing event score, remedial action must be taken and documented, and the...

42 CFR 493.843 - Standard; Endocrinology.

Code of Federal Regulations, 2012 CFR

2012-10-01

... acceptable responses for each analyte in each testing event is unsatisfactory analyte performance for the... testing event. (e)(1) For any unsatisfactory analyte or test performance or testing event for reasons... any unacceptable analyte or testing event score, remedial action must be taken and documented, and the...

42 CFR 493.843 - Standard; Endocrinology.

Code of Federal Regulations, 2014 CFR

2014-10-01

... acceptable responses for each analyte in each testing event is unsatisfactory analyte performance for the... testing event. (e)(1) For any unsatisfactory analyte or test performance or testing event for reasons... any unacceptable analyte or testing event score, remedial action must be taken and documented, and the...

42 CFR 493.851 - Standard; Hematology.

Code of Federal Regulations, 2012 CFR

2012-10-01

... acceptable responses for each analyte in each testing event is unsatisfactory analyte performance for the... testing event. (e)(1) For any unsatisfactory analyte or test performance or testing event for reasons... any unacceptable analyte or testing event score, remedial action must be taken and documented, and the...

High-Pressure Hot-Gas Self-Acting Floating Ring Shaft Seal for Liquid Rocket Turbopumps. [tapered bore seals

NASA Technical Reports Server (NTRS)

Burcham, R. E.; Diamond, W. A.

1980-01-01

Design analysis, detail design, fabrication, and experimental evaluation was performed on two self acting floating ring shaft seals for a rocket engine turbopump high pressure 24132500 n/sq m (3500 psig) hot gas 533 K 9500 F) high speed 3142 rad/sec (30000 rmp) turbine. The initial design used Rayleigh step hydrodynamic lift pads to assist in centering the seal ring with minimum rubbing contact. The final design used a convergent tapered bore to provide hydrostatic centering force. The Rayleigh step design was tested for 107 starts and 4.52 hours total. The leakage was satisfactory; however, the design was not acceptable due to excessive wear caused by inadequate centering force and failure of the sealing dam caused by erosion damage. The tapered bore design was tested for 370 starts and 15.93 hours total. Satisfactory performance for the required life of 7.5 hours per seal was successfully demonstrated.

A short-term clinical evaluation of IPS Empress 2 crowns.

PubMed

Toksavul, Suna; Toman, Muhittin

2007-01-01

The aim of this study was to evaluate the clinical performance of all-ceramic crowns made with the IPS Empress 2 system after an observation period of 12 to 60 months. Seventy-nine IPS Empress 2 crowns were placed in 21 patients. The all-ceramic crowns were evaluated clinically, radiographically, and using clinical photographs. The evaluations took place at baseline (2 days after cementation) and at 6-month intervals for 12 to 60 months. Survival rate of the crowns was determined using Kaplan-Meier statistical analysis. Based on the US Public Health Service criteria, 95.24% of the crowns were rated satisfactory after a mean follow-up period of 58 months. Fracture was registered in only 1 crown. One endodontically treated tooth failed as a result of fracture at the cervical margin area. In this in vivo study, IPS Empress 2 crowns exhibited a satisfactory clinical performance during an observation period ranging from 12 to 60 months.

High performance UV and thermal cure hybrid epoxy adhesive

NASA Astrophysics Data System (ADS)

Chen, C. F.; Iwasaki, S.; Kanari, M.; Li, B.; Wang, C.; Lu, D. Q.

2017-06-01

New type one component UV and thermal curable hybrid epoxy adhesive was successfully developed. The hybrid epoxy adhesive is complete initiator free composition. Neither photo-initiator nor thermal initiator is contained. The hybrid adhesive is mainly composed of special designed liquid bismaleimide, partially acrylated epoxy resin, acrylic monomer, epoxy resin and latent curing agent. Its UV light and thermal cure behavior was studied by FT-IR spectroscopy and FT-Raman spectroscopy. Adhesive samples cured at UV only, thermal only and UV + thermal cure conditions were investigated. By calculated conversion rate of double bond in both acrylic component and maleimide compound, satisfactory light curability of the hybrid epoxy adhesive was confirmed quantitatively. The investigation results also showed that its UV cure components, acrylic and bismalimide, possess good thermal curability too. The initiator free hybrid epoxy adhesive showed satisfactory UV curability, good thermal curability and high adhesion performance.

Ionic liquid-salt aqueous two-phase extraction based on salting-out coupled with high-performance liquid chromatography for the determination of sulfonamides in water and food.

PubMed

Han, Juan; Wang, Yun; Liu, Yan; Li, Yanfang; Lu, Yang; Yan, Yongsheng; Ni, Liang

2013-02-01

Ionic liquid-salt aqueous two-phase extraction coupled with high-performance liquid chromatography with ultraviolet detection was developed for the determination of sulfonamides in water and food samples. In the procedure, the analytes were extracted from the aqueous samples into the ionic liquid top phase in one step. Three sulfonamides, sulfamerazine, sulfamethoxazole, and sulfamethizole were selected here as model compounds for developing and evaluating the method. The effects of various experimental parameters in extraction step were studied using two optimization methods, one variable at a time and Box-Behnken design. The results showed that the amount of sulfonamides did not have effect on the extraction efficiency. Therefore, a three-level Box-Behnken experimental design with three factors, which combined the response surface modeling, was used to optimize sulfonamides extraction. Under the most favorable extraction parameters, the detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target compounds were achieved within the range of 0.15-0.3 ng/mL and 0.5-1.0 ng/mL from spiked samples, respectively, which are lower than or comparable with other reported approaches applied to the determination of the same compounds. Finally, the proposed method was successfully applied to the determination of sulfonamide compounds in different water and food samples and satisfactory recoveries of spiked target compounds in real samples were obtained.

Novel combined stir bar sorptive extraction coupled with ultrasonic assisted extraction for the determination of brominated flame retardants in environmental samples using high performance liquid chromatography.

PubMed

Yu, Chunhe; Hu, Bin

2007-08-10

A combined stir bar coated with poly (dimethysiloxane)-beta-cyclodextrin (PDMS-beta-CD) on single side has been prepared for the first time by sol-gel method and was coupled with ultrasonic assisted extraction (UAE) for the determination of some brominated flame-retardant compounds (BFRs) in soil and dust samples by high performance liquid chromatography (HPLC). Four different kinds of coatings including PDMS-beta-CD, PDMS, carbowax (CW)-PDMS-poly (vinyl alcohol) (PVA) and PDMS-PVA were evaluated for stir bar sorptive extraction of BFRs by orthogonal experiment design. The experimental results reveal that the PDMS-beta-CD combined stir bar exhibited the best extraction efficiency for the target analytes. The reproducibility for the preparation of PDMS-beta-CD combined stir bar ranged from 1.3% to 15.7% in one batch, and 7.2% to 15.1% among batches. Extraction time, desorption solvent, concentration of methanol and NaCl in the matrix, pH, temperature and stirring speed were optimized. The combined stir bar can avoid direct friction of the coating with the bottom of the vessel, and could be used for more than 100 times. Linearity (>0.993), repeatability (<10.5%), reproducibility (<16.5%), recovery (56-118%) and detection limits (2.9-4.2 microg L(-1)) were proper to determine the seven BFRs. The developed method was applied to the determination of BFRs in soil and dust with satisfactory results.

A rapid and simple pretreatment method for benzoylurea insecticides in honey samples using in-syringe dispersive liquid-liquid microextraction based on the direct solidification of ionic liquids.

PubMed

Wang, Huazi; Hu, Lu; Li, Wanzhen; Lu, Runhua; Zhang, Sanbing; Zhou, Wenfeng; Gao, Haixiang

2016-11-04

A pretreatment method using in-syringe dispersive liquid-liquid microextraction based on the direct solidification of ionic liquids before high performance liquid chromatography analysis was developed for the determination of benzoylurea insecticides (BUs) in honey samples. The hydrophobic ionic liquid [N 4444 ][PF 6 ], formed in situ by the hydrophilic ionic liquid [N 4444 ]Cl and the ion exchange reagent KPF 6 , was used to extract the target analytes. The entire extraction procedure was performed in a syringe. The extractant was solidified at room temperature and collected using a nylon membrane filter. This technique did not require a dispersive solvent, vortex mixer, ultrasound bath, or centrifugation. The parameters affecting the extraction efficiency were investigated through an experimental design. Under the optimal conditions, the limits of detection for the four BUs varied from 0.21 to 0.42μgL -1 in solution (2.1-4.2μgkg -1 in honey). Good linearities were obtained in the range of 2-300μgL -1 , with coefficients of determination greater than 0.999. The recoveries of the four BUs ranged from 80.94% to 84.59%. The intra-day (n=3) and inter-day (n=3) relative standard deviations were less than 5.08%. Finally, the proposed method was applied to the determination of BUs in commercial honey samples with satisfactory results. Copyright © 2016 Elsevier B.V. All rights reserved.

Data-analysis driven comparison of analytic and numerical coalescing binary waveforms: Nonspinning case

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

Pan Yi; Buonanno, Alessandra; McWilliams, Sean T.

2008-01-15

We compare waveforms obtained by numerically evolving nonspinning binary black holes to post-Newtonian (PN) template families currently used in the search for gravitational waves by ground-based detectors. We find that the time-domain 3.5PN template family, which includes the inspiral phase, has fitting factors (FFs) {>=}0.96 for binary systems with total mass M=10-20M{sub {center_dot}}. The time-domain 3.5PN effective-one-body template family, which includes the inspiral, merger, and ring-down phases, gives satisfactory signal-matching performance with FFs {>=}0.96 for binary systems with total mass M=10-120M{sub {center_dot}}. If we introduce a cutoff frequency properly adjusted to the final black-hole ring-down frequency, we find that themore » frequency-domain stationary-phase-approximated template family at 3.5PN order has FFs {>=}0.96 for binary systems with total mass M=10-20M{sub {center_dot}}. However, to obtain high matching performances for larger binary masses, we need to either extend this family to unphysical regions of the parameter space or introduce a 4PN order coefficient in the frequency-domain gravitational wave (GW) phase. Finally, we find that the phenomenological Buonanno-Chen-Vallisneri family has FFs {>=}0.97 with total mass M=10-120M{sub {center_dot}}. The main analyses use the noise-spectral density of LIGO, but several tests are extended to VIRGO and advanced LIGO noise-spectral densities.« less

Electromembrane extraction of biogenic amines in food samples by a microfluidic-chip system followed by dabsyl derivatization prior to high performance liquid chromatography analysis.

PubMed

Zarghampour, Fereshteh; Yamini, Yadollah; Baharfar, Mahroo; Faraji, Mohammad

2018-06-29

In the present research, an on-chip electromembrane extraction coupled with high performance liquid chromatography was developed for monitoring the trace levels of biogenic amines (BAs), including histamine, tryptamine, putrescine, cadaverine and spermidine in food samples. A porous polypropylene sheet membrane impregnated with an organic solvent was placed between the two parts of the chip device to separate the channels. Two platinum electrodes were mounted at the bottom of these channels, which were connected to a power supply, providing the electrical driving force for migration of ionized analytes from the sample solution through the porous sheet membrane into the acceptor phase. BAs were extracted from 2 mL aqueous sample solutions at neutral pH into 50 μL of acidified (HCl 90 mM) acceptor solution. Supported liquid membrane including NPOE containing 10% DEHP was used to ensure efficient extraction. Low voltage of 40 V was applied over the SLMs during extraction time. The influences of fundamental parameters affecting the transport of BAs were optimized. Under the optimized conditions, the relative standard deviations based on four replicate measurements were less than 8.0% and limit of detections were in range of 3.0-8.0 μg L -1 . Finally, the method was successfully applied to determinate BAs in the food samples and satisfactory results (recovery > 95.6) were obtained. Copyright © 2018 Elsevier B.V. All rights reserved.

High-performance liquid chromatography determination of ketone bodies in human plasma by precolumn derivatization with p-nitrobenzene diazonium fluoroborate.

PubMed

Yamato, Susumu; Shinohara, Kumiko; Nakagawa, Saori; Kubota, Ai; Inamura, Katsushi; Watanabe, Gen; Hirayama, Satoshi; Miida, Takashi; Ohta, Shin

2009-01-01

We developed and validated a sensitive and convenient high-performance liquid chromatography (HPLC) method for the specific determination of ketone bodies (acetoacetate and D-3-hydroxybutyrate) in human plasma. p-Nitrobenzene diazonium fluoroborate (diazo reagent) was used as a precolumn derivatization agent, and 3-(2-hydroxyphenyl) propionic acid was used as an internal standard. After the reaction, excess diazo reagent and plasma proteins were removed by passing through a solid-phase cartridge (C(18)). The derivatives retained on the cartridge were eluted with methanol, introduced into the HPLC system, and then detected with UV at 380 nm. A calibration curve for acetoacetate standard solution with a 20-microl injection volume showed good linearity in the range of 1 to 400 microM with a 0.9997 correlation coefficient. For the determination of D-3-hydroxybutyrate, it was converted to acetoacetate before reaction with the diazo reagent by an enzymatic coupling method using D-3-hydroxybutyrate dehydrogenase and lactate dehydrogenase. A calibration curve for D-3-hydroxybutyrate standard solution also showed good linearity in the range of 1.5 to 2000 microM with a 0.9988 correlation coefficient. Analytical recoveries of acetoacetate and D-3-hydroxybutyrate in human plasma were satisfactory. The method was successfully applied to samples from diabetic patients, and results were consistent with those obtained using the thio-NAD enzymatic cycling method used in clinical laboratories.

The Link between Higher Order Thinking Skills, Representation and Concepts in Enhancing TIMSS Tasks

ERIC Educational Resources Information Center

Tajudin, Nor'ain Mohd.; Chinnappan, Mohan

2016-01-01

Students' performances in TIMSS have featured strongly in recent discussions and debates about the quality of mathematical learning outcomes both from teachers and policy makers. Findings of TIMSS trends showed that most high school students in Malaysia continue to perform at less than satisfactory levels, particularly, in tasks that are…

Analytical method validation to evaluate dithiocarbamates degradation in biobeds in South of Brazil.

PubMed

Vareli, Catiucia S; Pizzutti, Ionara R; Gebler, Luciano; Cardoso, Carmem D; Gai, Daniela S H; Fontana, Marlos E Z

2018-07-01

In order to evaluate the efficiency of biobeds on DTC degradation, the aim of this study was to apply, optimize and validate a method to determine dithiocarbamate (mancozeb) in biobeds using gas chromatography-tandem mass spectrometry (GC-MS). The DTC pesticide mancozeb was hydrolysed in a tin (II) chloride solution at 1.5% in HCl (4 mol L -1 ), during 1 h in a water bath at 80 °C, and the CS 2 formed was extracted in isooctane. After cooling, 1 mL of the organic layer was transferred to an auto sampler vial and analyzed by GC-MS. A complete validation study was performed and the following parameters were assessed: linearity of the analytical curve (r 2 ), estimated method and instrument limits of detection and limits of quantification (LODm, LODi, LOQm and LOQi, respectively), accuracy (recovery%), precision (RSD%) and matrix effects. Recovery experiments were carried out with a standard spiking solution of the DTC pesticide thiram. Blank biobed (biomixture) samples were spiked at the three levels corresponding to the CS 2 concentrations of 1, 3 and 5 mg kg -1 , with seven replicates each (n = 7). The method presented satisfactory accuracy, with recoveries within the range of 89-96% and RSD ≤ 11%. The analytical curves were linear in the concentration range of 0.05-10 µg CS 2 mL -1 (r 2 > 0.9946). LODm and LOQm were 0.1 and 0.5 mg CS 2 kg -1 , respectively, and the calculated matrix effects were not significant (≤ 20%). The validated method was applied to 80 samples (biomixture), from sixteen different biobeds (collected at five sampling times) during fourteen months. Ten percent of samples presented CS 2 concentration below the LOD (0.1 mg CS 2 kg -1 ) and 49% of them showed results below the LOQ (0.5 mg CS 2 kg -1 ), which demonstrates the biobeds capability to degrade DTC. Copyright © 2018 Elsevier B.V. All rights reserved.

Quality assurance and quality control in light stable isotope laboratories: A case study of Rio Grande, Texas, water samples

USGS Publications Warehouse

Coplen, T.B.; Qi, H.

2009-01-01

New isotope laboratories can achieve the goal of reporting the same isotopic composition within analytical uncertainty for the same material analysed decades apart by (1) writing their own acceptance testing procedures and putting them into their mass spectrometric or laser-based isotope-ratio equipment procurement contract, (2) requiring a manufacturer to demonstrate acceptable performance using all sample ports provided with the instrumentation, (3) for each medium to be analysed, prepare two local reference materials substantially different in isotopic composition to encompass the range in isotopic composition expected in the laboratory and calibrated them with isotopic reference materials available from the International Atomic Energy Agency (IAEA) or the US National Institute of Standards and Technology (NIST), (4) using the optimum storage containers (for water samples, sealing in glass ampoules that are sterilised after sealing is satisfactory), (5) interspersing among sample unknowns local laboratory isotopic reference materials daily (internationally distributed isotopic reference materials can be ordered at three-year intervals, and can be used for elemental analyser analyses and other analyses that consume less than 1 mg of material) - this process applies to H, C, N, O, and S isotope ratios, (6) calculating isotopic compositions of unknowns by normalising isotopic data to that of local reference materials, which have been calibrated to internationally distributed isotopic reference materials, (7) reporting results on scales normalised to internationally distributed isotopic reference materials (where they are available) and providing to sample submitters the isotopic compositions of internationally distributed isotopic reference materials of the same substance had they been analysed with unknowns, (8) providing an audit trail in the laboratory for analytical results - this trail commonly will be in electronic format and might include a laboratory information management system, (9) making at regular intervals a complete backup of laboratory analytical data (both of samples logged into the laboratory and of mass spectrometric analyses), being sure to store one copy of this backup offsite, and (10) participating in interlaboratory comparison exercises sponsored by the IAEA and other agencies at regular intervals. ?? Taylor & Francis.

Smart Water Conservation System for Irrigated Landscape. ESTCP Cost and Performance Report

DTIC Science & Technology

2016-10-01

water use by as much as 70% in support of meeting EO 13693. Additional performance objectives were to validate energy reduction, cost effectiveness ...Additional performance objectives were to validate energy reduction, cost effectiveness , and system reliability while maintaining satisfactory plant health...developments. The demonstration was conducted for two different climatic regions in the southwestern part of the United States (U.S.), where a typical

Correlations among Six Learner Variables and the Performance of a Sample of Jamaican Eleventh-Graders on an Achievement Test on Respiration

ERIC Educational Resources Information Center

Soyibo, Kola; Pinnock, Jacqueline

2005-01-01

This study aimed at establishing if the level of performance of 500 Jamaican Grade 11 students on an achievement test on the concept of respiration was satisfactory (mean = 28 or 70% and above) or not (less than 70%); if there were statistically significant differences in their performance on the concept linked to their gender, cognitive abilities…

Influenza detection and prediction algorithms: comparative accuracy trial in Östergötland county, Sweden, 2008-2012.

PubMed

Spreco, A; Eriksson, O; Dahlström, Ö; Timpka, T

2017-07-01

Methods for the detection of influenza epidemics and prediction of their progress have seldom been comparatively evaluated using prospective designs. This study aimed to perform a prospective comparative trial of algorithms for the detection and prediction of increased local influenza activity. Data on clinical influenza diagnoses recorded by physicians and syndromic data from a telenursing service were used. Five detection and three prediction algorithms previously evaluated in public health settings were calibrated and then evaluated over 3 years. When applied on diagnostic data, only detection using the Serfling regression method and prediction using the non-adaptive log-linear regression method showed acceptable performances during winter influenza seasons. For the syndromic data, none of the detection algorithms displayed a satisfactory performance, while non-adaptive log-linear regression was the best performing prediction method. We conclude that evidence was found for that available algorithms for influenza detection and prediction display satisfactory performance when applied on local diagnostic data during winter influenza seasons. When applied on local syndromic data, the evaluated algorithms did not display consistent performance. Further evaluations and research on combination of methods of these types in public health information infrastructures for 'nowcasting' (integrated detection and prediction) of influenza activity are warranted.

Evaluating resistance of hot mix asphalt to reflective cracking using geocomposites.

DOT National Transportation Integrated Search

2013-01-01

The Pennsylvania Department of Transportation has sponsored a project with Penn State to evaluate new or : existing products to ensure satisfactory application and performance of these products. PennDOT Publication : 447 contains those products that ...

0-6687 : minimize premature distresses in continuously reinforced concrete pavement : [project summary].

DOT National Transportation Integrated Search

2013-08-01

The performance of continuously reinforced concrete : pavement (CRCP) has been quite satisfactory in Texas, : providing one of the most cost-effective pavement systems : for the Texas Department of Transportation (TxDOT). : However, distresses do occ...

Performance of ultra-thin whitetopping (UTW) in Oklahoma.

DOT National Transportation Integrated Search

2010-12-01

With the current level of deterioration of pavements in Oklahoma and the United States a satisfactory repai : technique that is economical and can be applied rapidly while resisting a significant volume of traffic is becomin : important. Thin concret...

Double half-cone flap umbilicoplasty for proboscoid umbilical hernia in a 2 years old child with satisfactory results 2 years later.

PubMed

Ashu, Eseme Ebai; Leroy, Guifo Marc; Aristide, Bang Guy; Joss, Bitang Mafok Louis; Bonaventure, Jemea; Patrick, Savom Eric; Myriam, Fotso Guegne

2015-01-01

Surgical repair of large umbilical hernias may present a challenging surgical problem; standard surgical techniques have proven to be inadequate for both closing the fascial defect of the umbilicus and providing a satisfactory cosmetic result. We describe here a case of double half-cone flap umbilicoplasty that was performed in a 2 years old boy. The case of a 2 years old child with proboscoid umbilical hernia. The protruding umbilical skin was excised sharply by two V-shaped cuts leaving two half cones, a short cephalic (0.5cm) and a long caudal (1cm). A classic herniotomy was carried out, with repair of the facial defect. The caudal half cone was sutured from its apex till half it's length upon itself with interrupted sutures and it was anchored deeply to the fascia. Then we inverted the cephalic half cone which was sutured to the caudal cone to form the new umbilicus. The early result was excellent with no complications and the result after 2years revealed a cosmetically satisfactory shape of the umbilicus. this technique provides a good solution for reconstruction of the protruding umbilical skin and it is easy to learn, easy to be taught and perform in surgical environments and may be applicable for any kind of umbilical reconstruction.

Double half-cone flap umbilicoplasty for proboscoid umbilical hernia in a 2 years old child with satisfactory results 2 years later

PubMed Central

Ashu, Eseme Ebai; Leroy, Guifo Marc; Aristide, Bang Guy; Joss, Bitang Mafok Louis; Bonaventure, Jemea; Patrick, Savom Eric; Myriam, Fotso Guegne

2015-01-01

Surgical repair of large umbilical hernias may present a challenging surgical problem; standard surgical techniques have proven to be inadequate for both closing the fascial defect of the umbilicus and providing a satisfactory cosmetic result. We describe here a case of double half-cone flap umbilicoplasty that was performed in a 2 years old boy. The case of a 2 years old child with proboscoid umbilical hernia. The protruding umbilical skin was excised sharply by two V-shaped cuts leaving two half cones, a short cephalic (0.5cm) and a long caudal (1cm). A classic herniotomy was carried out, with repair of the facial defect. The caudal half cone was sutured from its apex till half it's length upon itself with interrupted sutures and it was anchored deeply to the fascia. Then we inverted the cephalic half cone which was sutured to the caudal cone to form the new umbilicus. The early result was excellent with no complications and the result after 2years revealed a cosmetically satisfactory shape of the umbilicus. this technique provides a good solution for reconstruction of the protruding umbilical skin and it is easy to learn, easy to be taught and perform in surgical environments and may be applicable for any kind of umbilical reconstruction. PMID:26664545

Haematological validation of a computer-based bone marrow reporting system.

PubMed Central

Nguyen, D T; Diamond, L W; Cavenagh, J D; Parameswaran, R; Amess, J A

1997-01-01

AIMS: To prove the safety and effectiveness of "Professor Belmonte", a knowledge-based system for bone marrow reporting, a formal evaluation of the reports generated by the system was performed. METHODS: Three haematologists (a consultant, a senior registrar, and a junior registrar), none of whom were involved in the development of the software, compared the unedited reports generated by Professor Belmonte with the original bone marrow reports in 785 unselected cases. Each haematologist independently graded the quality of Belmonte's reports using one of four categories: (a) better than the original report (more informative, containing useful information missing in the original report); (b) equivalent to the original report; (c) satisfactory, but missing information that should have been included; and (d) unsatisfactory. RESULTS: The consultant graded 64 reports as more informative than the original, 687 as equivalent to the original, 32 as satisfactory, and two as unsatisfactory. The senior registrar considered 29 reports to be better than the original, 739 to be equivalent to the original, 15 to be satisfactory, and two to be unsatisfactory. The junior registrar found that 88 reports were better than the original, 681 were equivalent to the original, 14 were satisfactory, and two were unsatisfactory. Each judge found two different reports to be unsatisfactory according to their criteria. All 785 reports generated by the computer system received at least two scores of satisfactory or better. CONCLUSIONS: In this representative study, Professor Belmonte generated bone marrow reports that proved to be as accurate as the original reports in a large university hospital. The haematology knowledge contained within the system, the reasoning process, and the function of the software are safe and effective for assisting haematologists in generating high quality bone marrow reports. PMID:9215118

Equine sperm-bound antisperm antibodies are associated with poor semen quality.

PubMed

Ferrer, M S; Miller, L M J

2018-06-01

Antisperm antibodies (ASAs) have been associated with infertility in stallions. The objectives of this study were to investigate the frequency of ASA-positive semen samples in satisfactory and non-satisfactory breeder stallions, the association between ASA binding and semen quality, and factors that may affect the diagnosis. Breeding soundness examinations were performed in 21 stallions and the percentage of IgG- and IgA-bound spermatozoa was evaluated using flow cytometry. Median IgG and IgA binding did not differ between the first and second ejaculates. The percentage of IgA-bound spermatozoa was higher in non-satisfactory (n = 10) than satisfactory breeder stallions (n = 11). However, IgG binding or frequency of IgG-positive ejaculates did not differ with stallion classification. The IgG-positive stallions had significantly lower total sperm motility, concentration and total numbers than IgG-negative stallions in the first ejaculate, and lower sperm concentration in the second ejaculate. The IgA-positive stallions had lower total sperm motility, normal spermatozoa and total numbers than IgA-negative stallions in the first ejaculate, and lower total sperm motility, normal spermatozoa and total numbers in the second ejaculate. While IgG binding did not differ with season, IgA binding was higher in the non-breeding season (n = 6 stallions) than the breeding season (n = 15 stallions) in the first ejaculate. Stallion age did not differ with ASA classification. In conclusion, IgG binding was highly prevalent in both groups of stallions, while IgA binding was higher and more prevalent in non-satisfactory breeders. Both isotypes were associated with poor semen quality. Season and sexual rest had an effect on IgA but not IgG binding. Copyright © 2018 Elsevier Inc. All rights reserved.

Combining oxytocin administration and positive emotion inductions: Examining social perception and analytical performance.

PubMed

Human, Lauren J; Thorson, Katherine R; Woolley, Joshua D; Mendes, Wendy Berry

2017-04-01

Intranasal administration of the hypothalamic neuropeptide oxytocin (OT) has, in some studies, been associated with positive effects on social perception and cognition. Similarly, positive emotion inductions can improve a range of perceptual and performance-based behaviors. In this exploratory study, we examined how OT administration and positive emotion inductions interact in their associations with social and analytical performance. Participants (N=124) were randomly assigned to receive an intranasal spray of OT (40IU) or placebo and then viewed one of three videos designed to engender one of the following emotion states: social warmth, pride, or an affectively neutral state. Following the emotion induction, participants completed social perception and analytical tasks. There were no significant main effects of OT condition on social perception tasks, failing to replicate prior research, or on analytical performance. Further, OT condition and positive emotion inductions did not interact with each other in their associations with social perception performance. However, OT condition and positive emotion manipulations did significantly interact in their associations with analytical performance. Specifically, combining positive emotion inductions with OT administration was associated with worse analytical performance, with the pride induction no longer benefiting performance and the warmth induction resulting in worse performance. In sum, we found little evidence for main or interactive effects of OT on social perception but preliminary evidence that OT administration may impair analytical performance when paired with positive emotion inductions. Copyright © 2017 Elsevier Inc. All rights reserved.

Evaluation of analytical performance based on partial order methodology.

PubMed

Carlsen, Lars; Bruggemann, Rainer; Kenessova, Olga; Erzhigitov, Erkin

2015-01-01

Classical measurements of performances are typically based on linear scales. However, in analytical chemistry a simple scale may be not sufficient to analyze the analytical performance appropriately. Here partial order methodology can be helpful. Within the context described here, partial order analysis can be seen as an ordinal analysis of data matrices, especially to simplify the relative comparisons of objects due to their data profile (the ordered set of values an object have). Hence, partial order methodology offers a unique possibility to evaluate analytical performance. In the present data as, e.g., provided by the laboratories through interlaboratory comparisons or proficiency testings is used as an illustrative example. However, the presented scheme is likewise applicable for comparison of analytical methods or simply as a tool for optimization of an analytical method. The methodology can be applied without presumptions or pretreatment of the analytical data provided in order to evaluate the analytical performance taking into account all indicators simultaneously and thus elucidating a "distance" from the true value. In the present illustrative example it is assumed that the laboratories analyze a given sample several times and subsequently report the mean value, the standard deviation and the skewness, which simultaneously are used for the evaluation of the analytical performance. The analyses lead to information concerning (1) a partial ordering of the laboratories, subsequently, (2) a "distance" to the Reference laboratory and (3) a classification due to the concept of "peculiar points". Copyright © 2014 Elsevier B.V. All rights reserved.

Simultaneous determination of four trace level endocrine disrupting compounds in environmental samples by solid-phase microextraction coupled with HPLC.

PubMed

Wang, Lingling; Zhang, Zhenzhen; Xu, Xu; Zhang, Danfeng; Wang, Fang; Zhang, Lei

2015-09-01

A simple, rapid, sensitive and effective method for the simultaneous determination of four endocrine disrupting compounds (EDCs) (bisphenol A (BPA), bisphenol F (BPF), bisphenol AF (BPAF) and bisphenol AP (BPAP)) in environment water samples based on solid-phase microextraction (SPME) coupled with high performance liquid chromatography (HPLC) was developed. Multi-wall carbon nanotubes (MWCNTs) adsorbents showed a good affinity to the target analytes. These compounds were rapidly extracted within 10 min. Various experimental parameters that could affect the extraction efficiencies had been investigated in detail. Under the optimum conditions, the enrichment factors of the method for the target EDCs were found to be 500. Satisfactory precision and accuracy of the method were obtained in a low concentration range of 2.0-500.0 ng mL(-1). The method detection limits were in the range of 0.10-0.30 ng mL(-1). The high pre-concentration rate and efficiency of the method ensure its successful application in extraction of trace EDCs from large volumes of environmental water samples. The extraction recoveries in real samples ranged from 85.3% to 102.5% with the relative standard deviations (n=5) less than 3.74%. Copyright © 2015 Elsevier B.V. All rights reserved.

A glucose biosensor based on partially unzipped carbon nanotubes.

PubMed

Hu, Huifang; Feng, Miao; Zhan, Hongbing

2015-08-15

An amperometric glucose biosensor based on direct electron transfer of glucose oxidase (GOD) self-assembled on the surface of partially unzipped carbon nanotubes (PUCNTs) modified glassy carbon electrode (GCE) has been successfully fabricated. PUCNTs were synthesized via a facile chemical oxidative etching CNTs and used as a novel immobilization matrix for GOD. The cyclic voltammetric result of the PUCNT/GOD/GCE showed a pair of well-defined and quasi-reversible redox peaks with a formal potential of -0.470V and a peak to peak separation of 37mV, revealing that the fast direct electron transfer between GOD and the electrode has been achieved. It is notable that the glucose determination has been achieved in mediator-free condition. The developed biosensor displayed satisfactory analytical performance toward glucose including high sensitivity (19.50μA mM(-1)cm(-2)), low apparent Michaelis-Menten (5.09mM), a wide linear range of 0-17mM, and also preventing the interference from ascorbic acid, uric acid and dopamine usually coexisting with glucose in human blood. In addition, the biosensor acquired excellent storage stabilities. This facile, fast, environment-friendly and economical preparation strategy of PUCNT-GOD may provide a new platform for the fabrication of biocompatible glucose biosensors and other types of biosensors. Copyright © 2015 Elsevier B.V. All rights reserved.

Silver nanoparticles deposited on graphene oxide for ultrasensitive surface-enhanced Raman scattering immunoassay of cancer biomarker.

PubMed

Yang, Lin; Zhen, Shu Jun; Li, Yuan Fang; Huang, Cheng Zhi

2018-06-14

Graphene oxide (GO) exhibits distinctive Raman scattering features for its high frequency D (disordered) and tangential modes (G-band), which are characteristically sharp at 1580 cm-1 and 1350 cm-1, respectively, but are too weak for sensitive quantitation purposes. By depositing silver nanoparticles on the surface of GO in this contribution, both D and G bands of GO become enhanced. The enzyme label of this method controls the dissolution of silver nanoparticles on the surface of GO through hydrogen peroxide which is produced by the oxidation of the enzyme substrate. With the dissolution of the silver nanoparticles a greatly decreased SERS signal of GO was obtained. This strategy involves dual signal amplification of the enzyme and nanocomposites to improve the detection sensitivity. As a proof of concept, prostate specific antigen (PSA), a biomarker for prostate cancer, is successfully detected as a target by forming a sandwich structure in immunoassay. The SERS immunoassay possesses excellent analytical performance in the range 0.5 pg mL-1 to 500 pg mL-1 with a limit of detection of 0.23 pg mL-1, making the detection of PSA serum samples from prostate cancer patients satisfactory, demonstrating that the sensitive enzyme-assisted dissolved AgNPs SERS immunoassay of PSA has potential applications in clinical diagnosis.

An HPLC method for the determination of selected amino acids in human embryo culture medium.

PubMed

Drábková, Petra; Andrlová, Lenka; Kanďár, Roman

2017-02-01

A method for the determination of selected amino acids in culture medium using HPLC with fluorescence detection is described. Twenty hours after intra-cytoplasmic sperm injection, one randomly selected zygote was transferred to the culture medium. After incubation (72 h after fertilization), the culture medium in which the embryo was incubated and blank medium was immediately stored at -80°C. Filtered medium samples were derivatized with ortho-phthalaldehyde (naphthalene-2,3-dicarboxaldehyde), forming highly fluorescent amino acids derivatives. Reverse-phase columns (LichroCART, Purospher STAR RP 18e or Ascentis Express C 18 ) were used for the separation. The derivatives were analyzed by gradient elution with a mobile phase containing ethanol and sodium dihydrogen phosphate. The analytical performance of this method is satisfactory for all amino acids; the intra-assay coefficients of variation were <10% and quantitative recoveries were between 95.5 and 104.4%. Changes in the levels of selected amino acids before and after human embryo cultivation were observed. After embryo incubation, the levels of all amino acids in the medium were increased, apart from aspartate and asparagine. After the cultivation of some embryos, amino acids which were not part of the medium were detected. Low amino acids turnover was observed in some embryos. Copyright © 2016 John Wiley & Sons, Ltd.

Simultaneous determination of main reaction components in the reaction mixture during biodiesel production.

PubMed

Sánek, Lubomír; Pecha, Jiří; Kolomazník, Karel

2013-03-01

The proposed analytical method allows for simultaneous determination by GC using a programed temperature vaporization injector and a flame ionization detector of the main reaction components (i.e. glycerol, methyl esters, mono-, di-, and triacylglycerols) in the reaction mixture during biodiesel production. The suggested method is convenient for the rapid and simple evaluation of the kinetic data gained during the transesterification reaction and, also partially serves as an indicator of the quality of biodiesel and mainly, as the indicator of the efficiency of the whole production process (i.e. the conversion of triacylglycerols to biodiesel and its time progress). The optimization of chromatographic conditions (e.g. the oven temperature program, injector setting, amount of derivatization reagent, and the derivatization reaction time) was performed. The method has been validated with crude samples of biodiesel made from waste-cooking oils in terms of linearity, precision, accuracy, sensitivity, and limits of detection and quantification. The results confirmed a satisfactory degree of accuracy and repeatability (the mean RSDs were usually below 2%) necessary for the reliable quantitative determination of all components in the considerable concentration range (e.g. 10-1100 μg/mL in case of methyl esters). Compound recoveries ranging from 96 to 104% were obtained. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Trehalose determination in linseed subjected to osmotic stress. HPAEC-PAD analysis: an inappropriate method.

PubMed

Quéro, Anthony; Béthencourt, Linda; Pilard, Serge; Fournet, Antoine; Guillot, Xavier; Sangwan, Rajbir S; Boitel-Conti, Michèle; Courtois, Josiane; Petit, Emmanuel

2013-03-01

Trehalose is a non-reducing disaccharide involved in stress tolerance in plants. To understand better the role of trehalose in the osmotic stress response in linseed (Linum usitatissimum), trehalose content in leaves was studied. First, the method commonly used for sugar determination, high performance anion exchange chromatography with pulsed amperometric detection (HPAEC-PAD), gave unsatisfactory results and the separation efficiency could not be improved by varying the elution conditions. The same problem was also found in the model plant: Arabidopsis thaliana. After clearly highlighting a co-elution of trehalose in these two species by a trehalase assay and liquid chromatography-high resolution mass spectrometry analysis, gas chromatography-mass spectrometry (GC-MS) was used as the analytical method instead. These results confirmed that trehalose content is currently overestimated by HPAEC-PAD analysis, approximately 7 and 13 times for A. thaliana and linseed respectively. Thus GC-MS gave more satisfactory results for trehalose quantification in plants. With this method, trehalose accumulation was observed in linseed during an osmotic stress (-0.30 MPa), the quantity (31.49 nmol g(-1) dry weight after 48 h) appears too low to assign an osmoprotector or osmoregulator role to trehalose in stressed linseed. Copyright © Physiologia Plantarum 2012.

A sensitive label-free amperometric CEA immunosensor based on graphene-nafion nanocomposite film as an enhanced sensing platform.

PubMed

Li, Yan; Yang, Wei-Kang; Fan, Man-Qi; Liu, Ao

2011-01-01

A novel approach to fabricate a label-free amperometric immunosensor for the detection of carcinoembryonic antigen (CEA) was described. Herein, methylene blue (MB), gold nanoparticles (AuNPs) and carcinoembryonic antibody (anti-CEA) were layer-by-layer assembled on the graphene-Nafion nanocomposite film-modified electrode by means of a self-assembling technique and the opposite-charged adsorption. Subsequently, the stepwise self-assembling procedure of the immunosensor was further characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The factors influencing the performance of the resulting immunosensor were studied in detail. The developed procedure showed improved features, including larger amount and higher immunoactivity of the immobilized antibody and repeatable regeneration of the sensor, as well as direct, rapid and simple determination for the antigen without multiple separation and labeling steps. The immunosensor could detect the target protein in a range of 0.5 to 120 ng/mL with a limit of 0.17 ng/mL (at 3σ). Finally, the immunosensing system was evaluated on several clinical samples. Analytical results were found to be in satisfactory agreement with those detected by the enzyme-linked immunosorbent assay (ELISA) method, indicating that this new method was a promising alternative tool for clinical diagnosis.

A quantitative determination of fluorochloridone in rat plasma by UPLC-MS/MS method: application to a pharmacokinetic study.

PubMed

Liu, Shihong; Shi, Jingmin; Fan, Junpei; Sun, Jie; Zhang, Suhui; Hu, Yue; Wei, Li; Wu, Chunhua; Chang, Xiuli; Tang, Liming; Zhou, Zhijun

2016-08-01

A precise, high-throughput and sensitive ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method has been developed for the determination of fluorochloridone (FLC) in rat plasma. The extraction of analytes from plasma samples was carried out by protein precipitation procedure using acetonitrile prior to UPLC-MS/MS analysis. Verapamil was proved as a proper internal standard (IS) among many candidates. The chromatographic separation based on UPLC was well optimized. Multiple reaction monitoring in positive electrospray ionization was used with the optimized MS transitions at: m/z 312.0 → 292.0 for FLC and m/z 456.4 → 165.2 for IS. This method was well validated with good linear response (r(2)  > 0.998) observed over the investigated range of 3-3000 ng/mL and with satisfactory stability. This method was also characterized with adequate intra- and inter-day precision and accuracy (within 12%) in the quality control samples, and with high selectivity and less matrix effect observed. Total running time was only 1.5 min. This method has been successfully applied to a pilot FLC pharmacokinetic study after oral administration. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Preparation and in vitro/in vivo evaluation of metformin hydrochloride rectal dosage forms for treatment of patients with type II diabetes.

PubMed

Zaghloul, Abdel-Azim; Lila, Ahmad; Abd-Allah, Fathy; Nada, Aly

2017-06-01

Metformin hydrochloride (MtHCL) is an oral antidiabetic drug and has many other therapeutic benefits. It has poor bioavailability, narrow absorption window and extensive liver metabolism. Moreover, children and elders face difficulty to swallow the commercial oral tablets. Preparation, in vitro/in vivo evaluation of MtHCL suppositories for rectal administration to solve some of these problems. Suppository fatty bases (Witepsol ® , Suppocire ® and Massa ® ; different grades) and PEG bases 1000, 4000 and 6000 (different ratios), were used to prepare rectal suppository formulations each containing 500 mg drug. These were characterized for manufacturing defects, and pharmacotechnical performance and formulations showing superior results were subjected to bioavailability testing in human volunteers compared with the commercial oral tablet (Ref) applying LC-MS/MS developed analytical technique. The preparation method produced suppositories with satisfactory characteristics and free of manufacturing defects. The fatty bases were superior compared with PEG bases regarding the physical characteristics. Three formulations were chosen for bioavailability testing and the results showed comparable bioavailability compared to the Ref. The fatty bases showed superior characteristics compared with the PEG bases. MtHCL formulated in selected fatty bases could be a potential alternative to the commercial oral tablets particularly for pediatric and geriatric patients.

High performance liquid chromatography used for quality control of Achyranthis Radix.

PubMed

Zhao, Bing Tian; Jeong, Su Yang; Moon, Dong Cheul; Son, Kun Ho; Son, Jong Keun; Woo, Mi Hee

2012-08-01

To establish a standard of quality control and to identify reliable Achyranthis Radix, three phytoecdysones including ecdysterone (1), 25R-inokosterone (2) and 25S-inokosterone (3) were determined by quantitative HPLC/UV analysis. Three phytoecdysones were separated with an YMC J'sphere ODS C(18) column (250 mm × 4.6 mm, 4 μm) by isocratic elution using 0.1% formic acid in water and acetonitrile (85:15, v/v%) as the mobile phase. The flow rate was 1.0 mL/min and the UV detector wavelength was set at 245 nm. The standards were quantified by HPLC/UV from Achyranthes bidentata Blume and Achyranthes japonica Nakai, as well as Cyathula capitata Moq. and Cyathula officinalis Kuan, which are of a different genus but are comparative herbs. The method was successfully used in the analysis of Achyranthis Radix of different geographical origin or genera with relatively simple conditions and procedures, and the assay results were satisfactory for linearity, recovery, precision, accuracy, stability and robustness. The HPLC analytical method for pattern recognition analysis was validated by repeated analysis of eighteen A. bidentata Blume samples and ten A. japonica Nakai samples. The results indicate that the established HPLC/UV method is suitable for quantitation and pattern recognition analyses for quality evaluation of Achyranthis Radix.

What Do They Have in Common? Drivers of Streamflow Spatial Correlation and Prediction of Flow Regimes in Ungauged Locations

NASA Astrophysics Data System (ADS)

Betterle, A.; Radny, D.; Schirmer, M.; Botter, G.

2017-12-01

The spatial correlation of daily streamflows represents a statistical index encapsulating the similarity between hydrographs at two arbitrary catchment outlets. In this work, a process-based analytical framework is utilized to investigate the hydrological drivers of streamflow spatial correlation through an extensive application to 78 pairs of stream gauges belonging to 13 unregulated catchments in the eastern United States. The analysis provides insight on how the observed heterogeneity of the physical processes that control flow dynamics ultimately affect streamflow correlation and spatial patterns of flow regimes. Despite the variability of recession properties across the study catchments, the impact of heterogeneous drainage rates on the streamflow spatial correlation is overwhelmed by the spatial variability of frequency and intensity of effective rainfall events. Overall, model performances are satisfactory, with root mean square errors between modeled and observed streamflow spatial correlation below 10% in most cases. We also propose a method for estimating streamflow correlation in the absence of discharge data, which proves useful to predict streamflow regimes in ungauged areas. The method consists in setting a minimum threshold on the modeled flow correlation to individuate hydrologically similar sites. Catchment outlets that are most correlated (ρ>0.9) are found to be characterized by analogous streamflow distributions across a broad range of flow regimes.

New method for the determination of metolachlor and buprofezin in natural water using orthophthalaldehyde by thermochemically-induced fluorescence derivatization (TIFD).

PubMed

Mendy, Alphonse; Thiaré, Diène Diégane; Sambou, Souleymane; Khonté, Abdourahmane; Coly, Atanasse; Gaye-Seye, Mame Diabou; Delattre, François; Tine, Alphonse

2016-05-01

Herbicide metolachlor (MET) and insecticide buprofezin (BUP) were determined in natural waters by means of a newly-developed, simple and sensitive thermochemically-induced fluorescence derivatization (TIFD) method. The TIFD approach is based on the thermolysis transformation of naturally non-fluorescent pesticides into fluorescent complex O-phthalaldehyde-thermoproduct(s) in water at 70°C for MET and at 80°C for BUP. The TIFD method was optimized with respect to the temperature, pH, complex formation kinetic and pesticides concentrations. The limit of detection (LOD=0.8ngmL(-1) for MET and 3.0ngmL(-1) for BUP) and quantification (LOQ=2.6ngmL(-1) for MET and 9.5 ngmL(-1) for BUP) values were low, and the relative standard deviation (RSD) values were small (between 1.2% and 1.8%), which indicates a good analytical sensitivity and a great repeatability of TIFD method. Recovery studies were performed on spiked well, sea and draining waters samples collected in the Niayes area by using the solid phase extraction (SPE) procedure. Satisfactory recovery results (84-118%) were obtained for the determination of MET and BUP in these natural waters. Copyright © 2016 Elsevier B.V. All rights reserved.

PET Image Reconstruction Incorporating 3D Mean-Median Sinogram Filtering

NASA Astrophysics Data System (ADS)

Mokri, S. S.; Saripan, M. I.; Rahni, A. A. Abd; Nordin, A. J.; Hashim, S.; Marhaban, M. H.

2016-02-01

Positron Emission Tomography (PET) projection data or sinogram contained poor statistics and randomness that produced noisy PET images. In order to improve the PET image, we proposed an implementation of pre-reconstruction sinogram filtering based on 3D mean-median filter. The proposed filter is designed based on three aims; to minimise angular blurring artifacts, to smooth flat region and to preserve the edges in the reconstructed PET image. The performance of the pre-reconstruction sinogram filter prior to three established reconstruction methods namely filtered-backprojection (FBP), Maximum likelihood expectation maximization-Ordered Subset (OSEM) and OSEM with median root prior (OSEM-MRP) is investigated using simulated NCAT phantom PET sinogram as generated by the PET Analytical Simulator (ASIM). The improvement on the quality of the reconstructed images with and without sinogram filtering is assessed according to visual as well as quantitative evaluation based on global signal to noise ratio (SNR), local SNR, contrast to noise ratio (CNR) and edge preservation capability. Further analysis on the achieved improvement is also carried out specific to iterative OSEM and OSEM-MRP reconstruction methods with and without pre-reconstruction filtering in terms of contrast recovery curve (CRC) versus noise trade off, normalised mean square error versus iteration, local CNR versus iteration and lesion detectability. Overall, satisfactory results are obtained from both visual and quantitative evaluations.

Controlling Capillary-Driven Fluid Transport in Paper-Based Microfluidic Devices Using a Movable Valve.

PubMed

Li, Bowei; Yu, Lijuan; Qi, Ji; Fu, Longwen; Zhang, Peiqing; Chen, Lingxin

2017-06-06

This paper describes a novel strategy for fabricating the movable valve on paper-based microfluidic devices to manipulate capillary-driven fluids. The movable valve fabrication is first realized using hollow rivets as the holding center to control the paper channel in different layer movement that results in the channel's connection or disconnection. The relatively simple valve fabrication procedure is robust, versatile, and compatible with microfluidic paper-based analytical devices (μPADs) with differing levels of complexity. It is remarkable that the movable valve can be convenient and free to control fluid without the timing setting, advantages that make it user-friendly for untrained users to carry out the complex multistep operations. For the performance of the movable valve to be verified, several different designs of μPADs were tested and obtained with satisfactory results. In addition, in the proof-of-concept enzyme-linked immunosorbent assay experiments, we demonstrate the use of these valves in μPADs for the successful analysis of samples of carcino-embryonic antigen, showing good sensitivity and reproducibility. We hope this technique will open new avenues for the fabrication of paper-based valves in an easily adoptable and widely available way on μPADs and provide potential point-of-care applications in the future.

Problem of quantifying quantum correlations with non-commutative discord

NASA Astrophysics Data System (ADS)

Majtey, A. P.; Bussandri, D. G.; Osán, T. M.; Lamberti, P. W.; Valdés-Hernández, A.

2017-09-01

In this work we analyze a non-commutativity measure of quantum correlations recently proposed by Guo (Sci Rep 6:25241, 2016). By resorting to a systematic survey of a two-qubit system, we detected an undesirable behavior of such a measure related to its representation-dependence. In the case of pure states, this dependence manifests as a non-satisfactory entanglement measure whenever a representation other than the Schmidt's is used. In order to avoid this basis-dependence feature, we argue that a minimization procedure over the set of all possible representations of the quantum state is required. In the case of pure states, this minimization can be analytically performed and the optimal basis turns out to be that of Schmidt's. In addition, the resulting measure inherits the main properties of Guo's measure and, unlike the latter, it reduces to a legitimate entanglement measure in the case of pure states. Some examples involving general mixed states are also analyzed considering such an optimization. The results show that, in most cases of interest, the use of Guo's measure can result in an overestimation of quantum correlations. However, since Guo's measure has the advantage of being easily computable, it might be used as a qualitative estimator of the presence of quantum correlations.

Development of a scale to measure consumer perception of the risks involved in consuming raw vegetable salad in full-service restaurants.

PubMed

Danelon, Mariana Schievano; Salay, Elisabete

2012-12-01

The importance of the number of meals taken away-from-home represents an opportunity to promote consumption of vegetables in this context. However, the perception of risk may interfere with the food consumption behavior. The objective of this research was to develop a scale to measure consumer perception of the risks involved in consuming raw vegetable salad in full-service restaurants. The following research steps were carried out: item elaboration; content validity; scale purification (item-total correlation, internal consistency and exploratory factor analysis); and construct validity (confirmatory factor analysis). Non-probabilistic samples of consumers were interviewed (a total of 672 individuals) in the city of Campinas, Brazil. Several analyses were carried out using the Predictive Analytics Software 18.0 and LISREL 8.80. The final scale contained 26 items with an adequate content validity index (0.97) and Cronbach's alpha coefficient (0.93). The confirmatory factor analysis validates a six risk type factor model: physical, psychological, social, time, financial and performance (chi-square/degrees of freedom=2.29, root mean square error of approximation - RMSEA=0.060 and comparative fit index - CFI=0.98). The scale developed presented satisfactory reliability and validity results and could therefore be employed in further studies. Copyright © 2012 Elsevier Ltd. All rights reserved.

Simultaneous determination of penicillin G salts by infrared spectroscopy: Evaluation of combining orthogonal signal correction with radial basis function-partial least squares regression

NASA Astrophysics Data System (ADS)

Talebpour, Zahra; Tavallaie, Roya; Ahmadi, Seyyed Hamid; Abdollahpour, Assem

2010-09-01

In this study, a new method for the simultaneous determination of penicillin G salts in pharmaceutical mixture via FT-IR spectroscopy combined with chemometrics was investigated. The mixture of penicillin G salts is a complex system due to similar analytical characteristics of components. Partial least squares (PLS) and radial basis function-partial least squares (RBF-PLS) were used to develop the linear and nonlinear relation between spectra and components, respectively. The orthogonal signal correction (OSC) preprocessing method was used to correct unexpected information, such as spectral overlapping and scattering effects. In order to compare the influence of OSC on PLS and RBF-PLS models, the optimal linear (PLS) and nonlinear (RBF-PLS) models based on conventional and OSC preprocessed spectra were established and compared. The obtained results demonstrated that OSC clearly enhanced the performance of both RBF-PLS and PLS calibration models. Also in the case of some nonlinear relation between spectra and component, OSC-RBF-PLS gave satisfactory results than OSC-PLS model which indicated that the OSC was helpful to remove extrinsic deviations from linearity without elimination of nonlinear information related to component. The chemometric models were tested on an external dataset and finally applied to the analysis commercialized injection product of penicillin G salts.

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.

36 CFR 51.44 - How will the Director determine if a concessioner was satisfactory for purposes of a right of...

Code of Federal Regulations, 2010 CFR

2010-07-01

... determine if a concessioner was satisfactory for purposes of a right of preference? 51.44 Section 51.44... satisfactory for purposes of a right of preference? To be a satisfactory concessioner for the purposes of a... concessioner made subsequent to May 17, 2000 are less than satisfactory for any two or more years of operation...

Development of self-acting seals for helicopter engines

NASA Technical Reports Server (NTRS)

Lynwander, P.

1974-01-01

An experimental evaluation of a NASA-designed self-acting face seal for use in advanced gas turbine main shaft positions was conducted. The seal incorporated Rayleigh step pads (self-acting geometry) for lift augmentation. Satisfactory performance of the gas film seal was demonstrated in a 500-hour endurance test at speeds to 183 m/s (600 ft/sec, 54,000 rpm) and air pressure differential of 137 newtons per square centimeter (198.7 psi). Carbon wear was minor. Tests were also conducted with seal seat runout greater than that expected in engine operation and in a severe sand and dust environment. Seal operation was satisfactory in both these detrimental modes of operation.

Registration of 'Prevail' hard red spring wheat

USDA-ARS?s Scientific Manuscript database

Grower and end-user acceptance of new Hard Red Spring Wheat (HRSW; Triticum aestivum L.) cultivars is largely contingent upon satisfactory agronomic performance, end-use quality potential, and disease resistance levels. Additional characteristics, such as desirable plant height, can also contribute...

Design parameters and methodology for mechanically stabilized earth (MSE) walls.

DOT National Transportation Integrated Search

2014-10-01

Since its appearance in 1970s, mechanically stabilized earth (MSE) walls have become a majority among all types of retaining walls due to their economics and satisfactory performance. The Texas Department of Transportation (TxDOT) has primarily adopt...

Ultrasensitive analysis of lysergic acid diethylamide and its C-8 isomer in hair by capillary zone electrophoresis in combination with a stacking technique and laser induced fluorescence detection.

PubMed

Airado-Rodríguez, Diego; Cruces-Blanco, Carmen; García-Campaña, Ana M

2015-03-25

This article deals with the development and validation of a novel capillary zone electrophoresis (CZE) with laser induced fluorescence detection method for the analysis of lysergic acid diethylamide (LSD) and its isomer iso-LSD in hair samples. The separation of both analytes has been achieved in less than 13 min in a 72-cm effective length capillary with 75-μm internal diameter. As running buffer 25 mM citrate, pH 6.0 has been employed and separation temperature and voltage of 20 °C and 13 kV respectively, were applied. Field amplified sample injection (FASI) has been employed for on-line sample preconcentration, using ultrapure water containing 117 μM H3PO4 as optimum injection medium. Injection voltage and time have been optimized by means of experimental design, obtaining values of 7 kV and 15s, respectively. Methylergonovine has been employed as internal standard in order to compensate irreproducibility from electrokinetic injection. The analytical method has been applied to hair samples, previous extraction of the target analytes by ultrasound assisted solid-liquid extraction at 40 °C for 2.5 h, employing acetonitrile as extracting solvent. Linear responses were found for LSD and iso-LSD in matrix-matched calibrations from around 0.400 up to 50.0 pg mg(-1). LODs (3 S/N) in the order of 0.100 pg mg(-1) were calculated for both analytes, obtaining satisfactory recovery percentages for this kind of sample. Copyright © 2015 Elsevier B.V. All rights reserved.

Development and application of GC-MS method for monitoring of long-term exposure to the pesticide cypermethrin.

PubMed

Kavvalakis, Matthaios P; Tzatzarakis, Manolis N; Alegakis, Athanasios K; Vynias, Dionysios; Tsakalof, Andreas K; Tsatsakis, Aristidis M

2014-06-01

Cypermethrin (CPMN) is a synthetic pyrethroid used as an insecticide in large-scale commercial agricultural applications as well as for domestic purposes. In the present study a gas chromatography-mass spectrometry (GC-MS) based method was developed and validated for the quantitation of CPMN metabolites, 3-phenoxybenzoic acid (3-PBA) and cis- and trans- 3-(2,2-dichlorovinyl)-2,2-dimethyl-1-cyclopropane (cis- and trans- Cl2 CA). The developed method was applied for the monitoring of CPMN metabolites in hair of laboratory animals (rabbits) intentionally exposed per os to CPMN at 40 (low dose) and 80 (high dose) mg/kg weight/day for 16 weeks. The analytical method comprises three main steps: isolation of analytes from hair, analytes derivatization, and subsequent instrumental analysis by GC-MS. The limits of detection ensured by the method are 4.0, 3.9 and 1.0 pg/mg hair for cis-Cl2 CA, trans-Cl2 CA and 3-PBA, respectively. The instrument responce is linear (r(2)  > 0.99) in the investigated concentrations range from 25 to 1000 pg/mg. With and between-run precision as well as accuracy were estimated and found satisfactory. Analytes were efficiently isolated by solid-liquid extraction from hair with recoveries greater than 84.8% for cis-Cl2 CA, 87.2% for trans-Cl2 CA and 96.4% for 3-PBA. Rabbit's hair showed increasing levels for all metabolites (metabolites accumulation in a time and dose dependent manner) over time and in a dose-dependent manner. The developed experimental procedure could be used for biomonitoring of population exposure to CPMN. Copyright © 2014 John Wiley & Sons, Ltd.

Development of an analytical method for the simultaneous analysis of MCPD esters and glycidyl esters in oil-based foodstuffs.

PubMed

Ermacora, Alessia; Hrnčiřík, Karel

2014-01-01

Substantial progress has been recently made in the development and optimisation of analytical methods for the quantification of 2-MCPD, 3-MCPD and glycidyl esters in oils and fats, and there are a few methods currently available that allow a reliable quantification of these contaminants in bulk oils and fats. On the other hand, no standard method for the analysis of foodstuffs has yet been established. The aim of this study was the development and validation of a new method for the simultaneous quantification of 2-MCPD, 3-MCPD and glycidyl esters in oil-based food products. The developed protocol includes a first step of liquid-liquid extraction and purification of the lipophilic substances of the sample, followed by the application of a previously developed procedure based on acid transesterification, for the indirect quantification of these contaminants in oils and fats. The method validation was carried out on food products (fat-based spreads, creams, margarine, mayonnaise) manufactured in-house, in order to control the manufacturing process and account for any food matrix-analyte interactions (the sample spiking was carried out on the single components used for the formulations rather than the final products). The method showed good accuracy (the recoveries ranged from 97% to 106% for bound 3-MCPD and 2-MCPD and from 88% to 115% for bound glycidol) and sensitivity (the LOD was 0.04 and 0.05 mg kg(-1) for bound MCPD and glycidol, respectively). Repeatability and reproducibility were satisfactory (RSD below 2% and 5%, respectively) for all analytes. The levels of salts and surface-active compounds in the formulation were found to have no impact on the accuracy and the other parameters of the method.

Extensive intestinal first-pass metabolism of arctigenin: evidenced by simultaneous monitoring of both parent drug and its major metabolites.

PubMed

Gao, Qiong; Zhang, Yufeng; Wo, Siukwan; Zuo, Zhong

2014-03-01

The current study aims to investigate intestinal absorption and metabolism of arctigenin (AR) through simultaneous monitoring of AR and its major metabolites in rat plasma. An UPLC/MS/MS assay was developed with chromatographic separation of all analytes achieved by a C18 Column (3.9mm×150mm, 3.5μm) and a gradient elution with acetonitrile and 0.1% formic acid within 9min. Sample extraction with acetonitrile was optimized to achieve satisfactory recovery for both AR and its major metabolites. The lower limit of quantification (LLOQ) for all analytes was 25ng/ml. The intra-day and inter-day precision and accuracy of each analyte at LLOQ and three quality control (QC) concentrations (low, middle and high) in rat plasma was within 15.0% RSD and 15.0% bias. The extraction recoveries were within the range of 83.8-94.0% for all analytes. The developed and validated assay was then applied to the absorption study of AR in both Caco-2 cell monolayer model and in situ single-pass rat intestinal perfusion model. High absorption permeability of AR was demonstrated in both models with Papp of (1.76±0.48)×10(-5) (A→B) (Caco-2) and Pblood of (8.6±3.0)×10(-6)cm/s (intestinal perfusion). Extensive first-pass metabolism of AR to arctigenic acid (AA) and arctigenin-4'-O-glucuronide (AG) was identified in rat intestinal perfusion study with Cummins's extraction ratios of 0.458±0.012 and 0.085±0.013, respectively. The current assay method demonstrated to be a practical tool for pharmacokinetics investigation of AR with complicated metabolism pathways and multiple metabolites. Copyright © 2013 Elsevier B.V. All rights reserved.

Comparison of performance criteria for evaluating stake test data

Treesearch

Stan T. Lebow; Patricia K. Lebow; Grant T. Kirker

2017-01-01

Stake tests are a critical part of evaluating durability of wood in ground-contact, but there is a lack of criteria for interpreting stake test results. This paper discusses criteria that might be used to determine if short term ratings indicate satisfactory longterm performance. Ratings of 19 by 19 mm stakes from multiple plots in the Harrison Experimental Forest,...

SNAP 19 Viking Program. Bimonthly technical progress report, October 1979-November 1979

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

Not Available

1979-12-01

Monitoring and evaluation of Viking 1 Lander power system data continued. The RTG series power range as measured at the PCDA was 65 to 68 watts at fin root temperatures between 280/sup 0/F and 310/sup 0/F. The Mars landed performance history of Viking 1 include both the minimum and maximum data for each of the SOL days. Monitoring and evaluation of Viking 2 Lander power system data continued. The RTG series power range as measured at the PCDA was 71 to 72 watts at fin root temperatures between 230/sup 0/F and 260/sup 0/F. The Mars landed performance history of Vikingmore » 2 include both the minimum and maximum data for each of the SOL days. The performance of both power systems continues to be very satisfactory. Power system performance data for Pioneer 10 and Pioneer 11 spacecraft were monitored through the reporting period. The estimated RTG system net power was 116 watts for Pioneer 10 and 118 watts for Pioneer Saturn. The September 1 encounter with Saturn appears to have had no deleterious effect on the RTG's of the spacecraft power system. The telemetry signals from both spacecrafts remain satisfactory.« less