Validation of a thin-layer chromatography for the determination of hydrocortisone acetate and lidocaine in a pharmaceutical preparation.

PubMed

Dołowy, Małgorzata; Kulpińska-Kucia, Katarzyna; Pyka, Alina

2014-01-01

A new specific, precise, accurate, and robust TLC-densitometry has been developed for the simultaneous determination of hydrocortisone acetate and lidocaine hydrochloride in combined pharmaceutical formulation. The chromatographic analysis was carried out using a mobile phase consisting of chloroform+acetone+ammonia (25%) in volume composition 8:2:0.1 and silica gel 60F254 plates. Densitometric detection was performed in UV at wavelengths 200 nm and 250 nm, respectively, for lidocaine hydrochloride and hydrocortisone acetate. The validation of the proposed method was performed in terms of specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, and robustness. The applied TLC procedure is linear in hydrocortisone acetate concentration range of 3.75÷12.50  μg·spot(-1), and from 1.00÷2.50  μg·spot(-1) for lidocaine hydrochloride. The developed method was found to be accurate (the value of the coefficient of variation CV [%] is less than 3%), precise (CV [%] is less than 2%), specific, and robust. LOQ of hydrocortisone acetate is 0.198  μg·spot(-1) and LOD is 0.066  μg·spot(-1). LOQ and LOD values for lidocaine hydrochloride are 0.270 and 0.090  μg·spot(-1), respectively. The assay value of both bioactive substances is consistent with the limits recommended by Pharmacopoeia.

An Evaluation of Different Statistical Targets for Assembling Parallel Forms in Item Response Theory

PubMed Central

Ali, Usama S.; van Rijn, Peter W.

2015-01-01

Assembly of parallel forms is an important step in the test development process. Therefore, choosing a suitable theoretical framework to generate well-defined test specifications is critical. The performance of different statistical targets of test specifications using the test characteristic curve (TCC) and the test information function (TIF) was investigated. Test length, the number of test forms, and content specifications are considered as well. The TCC target results in forms that are parallel in difficulty, but not necessarily in terms of precision. Vice versa, test forms created using a TIF target are parallel in terms of precision, but not necessarily in terms of difficulty. As sometimes the focus is either on TIF or TCC, differences in either difficulty or precision can arise. Differences in difficulty can be mitigated by equating, but differences in precision cannot. In a series of simulations using a real item bank, the two-parameter logistic model, and mixed integer linear programming for automated test assembly, these differences were found to be quite substantial. When both TIF and TCC are combined into one target with manipulation to relative importance, these differences can be made to disappear.

ISO/IEC 17025 Sysmex R-500 hematology reticulocyte analyzer validation.

PubMed

Dimopoulou, H A; Theodoridis, T; Galea, V; Christopoulou-Cokkinou, V; Spyridaki, M-H E; Georgakopoulos, C G

2007-01-01

The Sysmex R-500 (R-500) Hematology Analyzer is a bench-top system appropriate for the analysis of limited batches of blood samples. The R-500 provides percentage proportional (RET%), absolute reticulocyte (RET#), and absolute red blood cell (RBC#) counts. The system was validated at the Doping Control Laboratory of Athens, according to the International Committee for Standardization in Hematology, International Standards Organization (ISO/IEC) 17025, and World Antidoping Agency (WADA) specifications. The instrument calibration was performed according to the manufacturer and validation parameters comprised linearity, precision, uncertainty (intermediate and long-term precision), comparability, effect of drift, carryover, stability, and accuracy. The linearity and the comparability studies for RET#, RET%, and RBC# were expressed in regression factors (R2) and coefficients of correlation [r(x, y)], respectively. For the precision studies, the coefficients of variation for RET#, RET%, and RBC# were 9.49%, 9.83%, and <1.5%, respectively. For the intermediate precision studies, the coefficients of variation for RET#, RET%, and RBC# were 3.1%, 3.6%, and 0.6%, respectively. Carryover was found to be negligible. Sample stability was demonstrated at both room temperature and at 4 degrees C over a 24-hour period. Comparability studies for the R-500 were performed using a Sysmex SE-9500. The total evaluation led to the conclusion that the R-500 is an accurate and precise analyzer and because of to its relatively limited size, it can be considered a portable instrument, capable to be used in sports competition and training sites, where doping control and health tests are conducted. The analytical methodology of RET% measurement by the R-500 has been incorporated into the Doping Control Laboratory of Athens' Scope of Accreditation according to the ISO/IEC 17025 and WADA specifications.

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

PubMed

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

2010-01-10

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

Stability indicating high performance thin-layer chromatographic method for simultaneous estimation of pantoprazole sodium and itopride hydrochloride in combined dosage form

PubMed Central

Bageshwar, Deepak; Khanvilkar, Vineeta; Kadam, Vilasrao

2011-01-01

A specific, precise and stability indicating high-performance thin-layer chromatographic method for simultaneous estimation of pantoprazole sodium and itopride hydrochloride in pharmaceutical formulations was developed and validated. The method employed TLC aluminium plates precoated with silica gel 60F254 as the stationary phase. The solvent system consisted of methanol:water:ammonium acetate; 4.0:1.0:0.5 (v/v/v). This system was found to give compact and dense spots for both itopride hydrochloride (Rf value of 0.55±0.02) and pantoprazole sodium (Rf value of 0.85±0.04). Densitometric analysis of both drugs was carried out in the reflectance–absorbance mode at 289 nm. The linear regression analysis data for the calibration plots showed a good linear relationship with R2=0.9988±0.0012 in the concentration range of 100–400 ng for pantoprazole sodium. Also, the linear regression analysis data for the calibration plots showed a good linear relationship with R2=0.9990±0.0008 in the concentration range of 200–1200 ng for itopride hydrochloride. The method was validated for specificity, precision, robustness and recovery. Statistical analysis proves that the method is repeatable and selective for the estimation of both the said drugs. As the method could effectively separate the drug from its degradation products, it can be employed as a stability indicating method. PMID:29403710

Stability indicating high performance thin-layer chromatographic method for simultaneous estimation of pantoprazole sodium and itopride hydrochloride in combined dosage form.

PubMed

Bageshwar, Deepak; Khanvilkar, Vineeta; Kadam, Vilasrao

2011-11-01

A specific, precise and stability indicating high-performance thin-layer chromatographic method for simultaneous estimation of pantoprazole sodium and itopride hydrochloride in pharmaceutical formulations was developed and validated. The method employed TLC aluminium plates precoated with silica gel 60F 254 as the stationary phase. The solvent system consisted of methanol:water:ammonium acetate; 4.0:1.0:0.5 (v/v/v). This system was found to give compact and dense spots for both itopride hydrochloride ( R f value of 0.55±0.02) and pantoprazole sodium ( R f value of 0.85±0.04). Densitometric analysis of both drugs was carried out in the reflectance-absorbance mode at 289 nm. The linear regression analysis data for the calibration plots showed a good linear relationship with R 2 =0.9988±0.0012 in the concentration range of 100-400 ng for pantoprazole sodium. Also, the linear regression analysis data for the calibration plots showed a good linear relationship with R 2 =0.9990±0.0008 in the concentration range of 200-1200 ng for itopride hydrochloride. The method was validated for specificity, precision, robustness and recovery. Statistical analysis proves that the method is repeatable and selective for the estimation of both the said drugs. As the method could effectively separate the drug from its degradation products, it can be employed as a stability indicating method.

Microbiological assay for the determination of meropenem in pharmaceutical dosage form.

PubMed

Mendez, Andreas S L; Weisheimer, Vanessa; Oppe, Tércio P; Steppe, Martin; Schapoval, Elfrides E S

2005-04-01

Meropenem is a highly active carbapenem antibiotic used in the treatment of a wide range of serious infections. The present work reports a microbiological assay, applying the cylinder-plate method, for the determination of meropenem in powder for injection. The validation method yielded good results and included linearity, precision, accuracy and specificity. The assay is based on the inhibitory effect of meropenem upon the strain of Micrococcus luteus ATCC 9341 used as the test microorganism. The results of assay were treated statistically by analysis of variance (ANOVA) and were found to be linear (r=0.9999) in the range of 1.5-6.0 microg ml(-1), precise (intra-assay: R.S.D.=0.29; inter-assay: R.S.D.=0.94) and accurate. A preliminary stability study of meropenem was performed to show that the microbiological assay is specific for the determination of meropenem in the presence of its degradation products. The degraded samples were also analysed by the HPLC method. The proposed method allows the quantitation of meropenem in pharmaceutical dosage form and can be used for the drug analysis in routine quality control.

RP-HPLC method development and validation for simultaneous estimation of atorvastatin calcium and pioglitazone hydrochloride in pharmaceutical dosage form.

PubMed

Peraman, Ramalingam; Mallikarjuna, Sasikala; Ammineni, Pravalika; Kondreddy, Vinod kumar

2014-10-01

A simple, selective, rapid, precise and economical reversed-phase high-performance liquid chromatographic (RP-HPLC) method has been developed for simultaneous estimation of atorvastatin calcium (ATV) and pioglitazone hydrochloride (PIO) from pharmaceutical formulation. The method is carried out on a C8 (25 cm × 4.6 mm i.d., 5 μm) column with a mobile phase consisting of acetonitrile (ACN):water (pH adjusted to 6.2 using o-phosphoric acid) in the ratio of 45:55 (v/v). The retention time of ATV and PIO is 4.1 and 8.1 min, respectively, with the flow rate of 1 mL/min with diode array detector detection at 232 nm. The linear regression analysis data from the linearity plot showed good linear relationship with a correlation coefficient (R(2)) value for ATV and PIO of 0.9998 and 0.9997 in the concentration range of 10-80 µg mL(-1), respectively. The relative standard deviation for intraday precision has been found to be <2.0%. The method is validated according to the ICH guidelines. The developed method is validated in terms of specificity, selectivity, accuracy, precision, linearity, limit of detection, limit of quantitation and solution stability. The proposed method can be used for simultaneous estimation of these drugs in marketed dosage forms. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Development and Preliminary Testing of a High Precision Long Stroke Slit Change Mechanism for the SPICE Instrument

NASA Technical Reports Server (NTRS)

Paciotti, Gabriel; Humphries, Martin; Rottmeier, Fabrice; Blecha, Luc

2014-01-01

In the frame of ESA's Solar Orbiter scientific mission, Almatech has been selected to design, develop and test the Slit Change Mechanism of the SPICE (SPectral Imaging of the Coronal Environment) instrument. In order to guaranty optical cleanliness level while fulfilling stringent positioning accuracies and repeatability requirements for slit positioning in the optical path of the instrument, a linear guiding system based on a double flexible blade arrangement has been selected. The four different slits to be used for the SPICE instrument resulted in a total stroke of 16.5 mm in this linear slit changer arrangement. The combination of long stroke and high precision positioning requirements has been identified as the main design challenge to be validated through breadboard models testing. This paper presents the development of SPICE's Slit Change Mechanism (SCM) and the two-step validation tests successfully performed on breadboard models of its flexible blade support system. The validation test results have demonstrated the full adequacy of the flexible blade guiding system implemented in SPICE's Slit Change Mechanism in a stand-alone configuration. Further breadboard test results, studying the influence of the compliant connection to the SCM linear actuator on an enhanced flexible guiding system design have shown significant enhancements in the positioning accuracy and repeatability of the selected flexible guiding system. Preliminary evaluation of the linear actuator design, including a detailed tolerance analyses, has shown the suitability of this satellite roller screw based mechanism for the actuation of the tested flexible guiding system and compliant connection. The presented development and preliminary testing of the high-precision long-stroke Slit Change Mechanism for the SPICE Instrument are considered fully successful such that future tests considering the full Slit Change Mechanism can be performed, with the gained confidence, directly on a Qualification Model. The selected linear Slit Change Mechanism design concept, consisting of a flexible guiding system driven by a hermetically sealed linear drive mechanism, is considered validated for the specific application of the SPICE instrument, with great potential for other special applications where contamination and high precision positioning are dominant design drivers.

Estimation of suspended-sediment rating curves and mean suspended-sediment loads

USGS Publications Warehouse

Crawford, Charles G.

1991-01-01

A simulation study was done to evaluate: (1) the accuracy and precision of parameter estimates for the bias-corrected, transformed-linear and non-linear models obtained by the method of least squares; (2) the accuracy of mean suspended-sediment loads calculated by the flow-duration, rating-curve method using model parameters obtained by the alternative methods. Parameter estimates obtained by least squares for the bias-corrected, transformed-linear model were considerably more precise than those obtained for the non-linear or weighted non-linear model. The accuracy of parameter estimates obtained for the biascorrected, transformed-linear and weighted non-linear model was similar and was much greater than the accuracy obtained by non-linear least squares. The improved parameter estimates obtained by the biascorrected, transformed-linear or weighted non-linear model yield estimates of mean suspended-sediment load calculated by the flow-duration, rating-curve method that are more accurate and precise than those obtained for the non-linear model.

Amesos2 and Belos: Direct and Iterative Solvers for Large Sparse Linear Systems

DOE PAGES

Bavier, Eric; Hoemmen, Mark; Rajamanickam, Sivasankaran; ...

2012-01-01

Solvers for large sparse linear systems come in two categories: direct and iterative. Amesos2, a package in the Trilinos software project, provides direct methods, and Belos, another Trilinos package, provides iterative methods. Amesos2 offers a common interface to many different sparse matrix factorization codes, and can handle any implementation of sparse matrices and vectors, via an easy-to-extend C++ traits interface. It can also factor matrices whose entries have arbitrary “Scalar” type, enabling extended-precision and mixed-precision algorithms. Belos includes many different iterative methods for solving large sparse linear systems and least-squares problems. Unlike competing iterative solver libraries, Belos completely decouples themore » algorithms from the implementations of the underlying linear algebra objects. This lets Belos exploit the latest hardware without changes to the code. Belos favors algorithms that solve higher-level problems, such as multiple simultaneous linear systems and sequences of related linear systems, faster than standard algorithms. The package also supports extended-precision and mixed-precision algorithms. Together, Amesos2 and Belos form a complete suite of sparse linear solvers.« less

Validated modified Lycopodium spore method development for standardisation of ingredients of an ayurvedic powdered formulation Shatavaryadi churna.

PubMed

Kumar, Puspendra; Jha, Shivesh; Naved, Tanveer

2013-01-01

Validated modified lycopodium spore method has been developed for simple and rapid quantification of herbal powdered drugs. Lycopodium spore method was performed on ingredients of Shatavaryadi churna, an ayurvedic formulation used as immunomodulator, galactagogue, aphrodisiac and rejuvenator. Estimation of diagnostic characters of each ingredient of Shatavaryadi churna individually was carried out. Microscopic determination, counting of identifying number, measurement of area, length and breadth of identifying characters were performed using Leica DMLS-2 microscope. The method was validated for intraday precision, linearity, specificity, repeatability, accuracy and system suitability, respectively. The method is simple, precise, sensitive, and accurate, and can be used for routine standardisation of raw materials of herbal drugs. This method gives the ratio of individual ingredients in the powdered drug so that any adulteration of genuine drug with its adulterant can be found out. The method shows very good linearity value between 0.988-0.999 for number of identifying character and area of identifying character. Percentage purity of the sample drug can be determined by using the linear equation of standard genuine drug.

Precision Linear Actuator for Space Interferometry Mission (SIM) Siderostat Pointing

NASA Technical Reports Server (NTRS)

Cook, Brant; Braun, David; Hankins, Steve; Koenig, John; Moore, Don

2008-01-01

'SIM PlanetQuest will exploit the classical measuring tool of astrometry (interferometry) with unprecedented precision to make dramatic advances in many areas of astronomy and astrophysics'(1). In order to obtain interferometric data two large steerable mirrors, or Siderostats, are used to direct starlight into the interferometer. A gimbaled mechanism actuated by linear actuators is chosen to meet the unprecedented pointing and angle tracking requirements of SIM. A group of JPL engineers designed, built, and tested a linear ballscrew actuator capable of performing submicron incremental steps for 10 years of continuous operation. Precise, zero backlash, closed loop pointing control requirements, lead the team to implement a ballscrew actuator with a direct drive DC motor and a precision piezo brake. Motor control commutation using feedback from a precision linear encoder on the ballscrew output produced an unexpected incremental step size of 20 nm over a range of 120 mm, yielding a dynamic range of 6,000,000:1. The results prove linear nanometer positioning requires no gears, levers, or hydraulic converters. Along the way many lessons have been learned and will subsequently be shared.

Novel linear piezoelectric motor for precision position stage

NASA Astrophysics Data System (ADS)

Chen, Chao; Shi, Yunlai; Zhang, Jun; Wang, Junshan

2016-03-01

Conventional servomotor and stepping motor face challenges in nanometer positioning stages due to the complex structure, motion transformation mechanism, and slow dynamic response, especially directly driven by linear motor. A new butterfly-shaped linear piezoelectric motor for linear motion is presented. A two-degree precision position stage driven by the proposed linear ultrasonic motor possesses a simple and compact configuration, which makes the system obtain shorter driving chain. Firstly, the working principle of the linear ultrasonic motor is analyzed. The oscillation orbits of two driving feet on the stator are produced successively by using the anti-symmetric and symmetric vibration modes of the piezoelectric composite structure, and the slider pressed on the driving feet can be propelled twice in only one vibration cycle. Then with the derivation of the dynamic equation of the piezoelectric actuator and transient response model, start-upstart-up and settling state characteristics of the proposed linear actuator is investigated theoretically and experimentally, and is applicable to evaluate step resolution of the precision platform driven by the actuator. Moreover the structure of the two-degree position stage system is described and a special precision displacement measurement system is built. Finally, the characteristics of the two-degree position stage are studied. In the closed-loop condition the positioning accuracy of plus or minus <0.5 μm is experimentally obtained for the stage propelled by the piezoelectric motor. A precision position stage based the proposed butterfly-shaped linear piezoelectric is theoretically and experimentally investigated.

Cumulative Retrospective Exposure Assessment (REA) as a predictor of amphibole asbestos lung burden: validation procedures and results for industrial hygiene and pathology estimates.

PubMed

Rasmuson, James O; Roggli, Victor L; Boelter, Fred W; Rasmuson, Eric J; Redinger, Charles F

2014-01-01

A detailed evaluation of the correlation and linearity of industrial hygiene retrospective exposure assessment (REA) for cumulative asbestos exposure with asbestos lung burden analysis (LBA) has not been previously performed, but both methods are utilized for case-control and cohort studies and other applications such as setting occupational exposure limits. (a) To correlate REA with asbestos LBA for a large number of cases from varied industries and exposure scenarios; (b) to evaluate the linearity, precision, and applicability of both industrial hygiene exposure reconstruction and LBA; and (c) to demonstrate validation methods for REA. A panel of four experienced industrial hygiene raters independently estimated the cumulative asbestos exposure for 363 cases with limited exposure details in which asbestos LBA had been independently determined. LBA for asbestos bodies was performed by a pathologist by both light microscopy and scanning electron microscopy (SEM) and free asbestos fibers by SEM. Precision, reliability, correlation and linearity were evaluated via intraclass correlation, regression analysis and analysis of covariance. Plaintiff's answers to interrogatories, work history sheets, work summaries or plaintiff's discovery depositions that were obtained in court cases involving asbestos were utilized by the pathologist to provide a summarized brief asbestos exposure and work history for each of the 363 cases. Linear relationships between REA and LBA were found when adjustment was made for asbestos fiber-type exposure differences. Significant correlation between REA and LBA was found with amphibole asbestos lung burden and mixed fiber-types, but not with chrysotile. The intraclass correlation coefficients (ICC) for the precision of the industrial hygiene rater cumulative asbestos exposure estimates and the precision of repeated laboratory analysis were found to be in the excellent range. The ICC estimates were performed independent of specific asbestos fiber-type. Both REA and pathology assessment are reliable and complementary predictive methods to characterize asbestos exposures. Correlation analysis between the two methods effectively validates both REA methodology and LBA procedures within the determined precision, particularly for cumulative amphibole asbestos exposures since chrysotile fibers, for the most part, are not retained in the lung for an extended period of time.

Optimization and validation of liquid chromatography and headspace-gas chromatography based methods for the quantitative determination of capsaicinoids, salicylic acid, glycol monosalicylate, methyl salicylate, ethyl salicylate, camphor and l-menthol in a topical formulation.

PubMed

Pauwels, Jochen; D'Autry, Ward; Van den Bossche, Larissa; Dewever, Cédric; Forier, Michel; Vandenwaeyenberg, Stephanie; Wolfs, Kris; Hoogmartens, Jos; Van Schepdael, Ann; Adams, Erwin

2012-02-23

Capsaicinoids, salicylic acid, methyl and ethyl salicylate, glycol monosalicylate, camphor and l-menthol are widely used in topical formulations to relieve local pain. For each separate compound or simple mixtures, quantitative analysis methods are reported. However, for a mixture containing all above mentioned active compounds, no assay methods were found. Due to the differing physicochemical characteristics, two methods were developed and optimized simultaneously. The non-volatile capsaicinoids, salicylic acid and glycol monosalicylate were analyzed with liquid chromatography following liquid-liquid extraction, whereas the volatile compounds were analyzed with static headspace-gas chromatography. For the latter method, liquid paraffin was selected as compatible dilution solvent. The optimized methods were validated in terms of specificity, linearity, accuracy and precision in a range of 80% to 120% of the expected concentrations. For both methods, peaks were well separated without interference of other compounds. Linear relationships were demonstrated with R² values higher than 0.996 for all compounds. Accuracy was assessed by performing replicate recovery experiments with spiked blank samples. Mean recovery values were all between 98% and 102%. Precision was checked at three levels: system repeatability, method precision and intermediate precision. Both methods were found to be acceptably precise at all three levels. Finally, the method was successfully applied to the analysis of some real samples (cutaneous sticks). Copyright © 2011 Elsevier B.V. All rights reserved.

Linearity, Bias, and Precision of Hepatic Proton Density Fat Fraction Measurements by Using MR Imaging: A Meta-Analysis.

PubMed

Yokoo, Takeshi; Serai, Suraj D; Pirasteh, Ali; Bashir, Mustafa R; Hamilton, Gavin; Hernando, Diego; Hu, Houchun H; Hetterich, Holger; Kühn, Jens-Peter; Kukuk, Guido M; Loomba, Rohit; Middleton, Michael S; Obuchowski, Nancy A; Song, Ji Soo; Tang, An; Wu, Xinhuai; Reeder, Scott B; Sirlin, Claude B

2018-02-01

Purpose To determine the linearity, bias, and precision of hepatic proton density fat fraction (PDFF) measurements by using magnetic resonance (MR) imaging across different field strengths, imager manufacturers, and reconstruction methods. Materials and Methods This meta-analysis was performed in accordance with Preferred Reporting Items for Systematic Reviews and Meta-Analyses guidelines. A systematic literature search identified studies that evaluated the linearity and/or bias of hepatic PDFF measurements by using MR imaging (hereafter, MR imaging-PDFF) against PDFF measurements by using colocalized MR spectroscopy (hereafter, MR spectroscopy-PDFF) or the precision of MR imaging-PDFF. The quality of each study was evaluated by using the Quality Assessment of Studies of Diagnostic Accuracy 2 tool. De-identified original data sets from the selected studies were pooled. Linearity was evaluated by using linear regression between MR imaging-PDFF and MR spectroscopy-PDFF measurements. Bias, defined as the mean difference between MR imaging-PDFF and MR spectroscopy-PDFF measurements, was evaluated by using Bland-Altman analysis. Precision, defined as the agreement between repeated MR imaging-PDFF measurements, was evaluated by using a linear mixed-effects model, with field strength, imager manufacturer, reconstruction method, and region of interest as random effects. Results Twenty-three studies (1679 participants) were selected for linearity and bias analyses and 11 studies (425 participants) were selected for precision analyses. MR imaging-PDFF was linear with MR spectroscopy-PDFF (R 2 = 0.96). Regression slope (0.97; P < .001) and mean Bland-Altman bias (-0.13%; 95% limits of agreement: -3.95%, 3.40%) indicated minimal underestimation by using MR imaging-PDFF. MR imaging-PDFF was precise at the region-of-interest level, with repeatability and reproducibility coefficients of 2.99% and 4.12%, respectively. Field strength, imager manufacturer, and reconstruction method each had minimal effects on reproducibility. Conclusion MR imaging-PDFF has excellent linearity, bias, and precision across different field strengths, imager manufacturers, and reconstruction methods. © RSNA, 2017 Online supplemental material is available for this article. An earlier incorrect version of this article appeared online. This article was corrected on October 2, 2017.

On the linear relation between the mean and the standard deviation of a response time distribution.

PubMed

Wagenmakers, Eric-Jan; Brown, Scott

2007-07-01

Although it is generally accepted that the spread of a response time (RT) distribution increases with the mean, the precise nature of this relation remains relatively unexplored. The authors show that in several descriptive RT distributions, the standard deviation increases linearly with the mean. Results from a wide range of tasks from different experimental paradigms support a linear relation between RT mean and RT standard deviation. Both R. Ratcliff's (1978) diffusion model and G. D. Logan's (1988) instance theory of automatization provide explanations for this linear relation. The authors identify and discuss 3 specific boundary conditions for the linear law to hold. The law constrains RT models and supports the use of the coefficient of variation to (a) compare variability while controlling for differences in baseline speed of processing and (b) assess whether changes in performance with practice are due to quantitative speedup or qualitative reorganization. Copyright 2007 APA.

Determination of perfluorinated compounds in fish fillet homogenates: method validation and application to fillet homogenates from the Mississippi River.

PubMed

Malinsky, Michelle Duval; Jacoby, Cliffton B; Reagen, William K

2011-01-10

We report herein a simple protein precipitation extraction-liquid chromatography tandem mass spectrometry (LC/MS/MS) method, validation, and application for the analysis of perfluorinated carboxylic acids (C7-C12), perfluorinated sulfonic acids (C4, C6, and C8), and perfluorooctane sulfonamide (FOSA) in fish fillet tissue. The method combines a rapid homogenization and protein precipitation tissue extraction procedure using stable-isotope internal standard (IS) calibration. Method validation in bluegill (Lepomis macrochirus) fillet tissue evaluated the following: (1) method accuracy and precision in both extracted matrix-matched calibration and solvent (unextracted) calibration, (2) quantitation of mixed branched and linear isomers of perfluorooctanoate (PFOA) and perfluorooctanesulfonate (PFOS) with linear isomer calibration, (3) quantitation of low level (ppb) perfluorinated compounds (PFCs) in the presence of high level (ppm) PFOS, and (4) specificity from matrix interferences. Both calibration techniques produced method accuracy of at least 100±13% with a precision (%RSD) ≤18% for all target analytes. Method accuracy and precision results for fillet samples from nine different fish species taken from the Mississippi River in 2008 and 2009 are also presented. Copyright © 2010 Elsevier B.V. All rights reserved.

Simultaneous Determination of Ofloxacin and Flavoxate Hydrochloride by Absorption Ratio and Second Derivative UV Spectrophotometry

PubMed Central

Attimarad, Mahesh

2010-01-01

The objective of this study was to develop simple, precise, accurate and sensitive UV spectrophotometric methods for the simultaneous determination of ofloxacin (OFX) and flavoxate HCl (FLX) in pharmaceutical formulations. The first method is based on absorption ratio method, by formation of Q absorbance equation at 289 nm (λmax of OFX) and 322.4 nm (isoabsorptive point). The linearity range was found to be 1 to 30 μg/ml for FLX and OFX. In the method-II second derivative absorption at 311.4 nm for OFX (zero crossing for FLX) and at 246.2 nm for FLX (zero crossing for OFX) was used for the determination of the drugs and the linearity range was found to be 2 to 30 μg/ml for OFX and 2-75 μg /ml for FLX. The accuracy and precision of the methods were determined and validated statistically. Both the methods showed good reproducibility and recovery with % RSD less than 1.5%. Both the methods were found to be rapid, specific, precise and accurate and can be successfully applied for the routine analysis of OFX and FLX in combined dosage form PMID:24826003

High speed, precision motion strategies for lightweight structures

NASA Technical Reports Server (NTRS)

Book, Wayne J.

1987-01-01

Abstracts of published papers and dissertations generated during the reporting period are compiled. Work on fine motion control was completed. Specifically, real time control of flexible manipulator vibrations were experimentally investigated. A linear model based on the application of Lagrangian dynamics to a rigid body mode and a series of separable flexible modes was examined with respect to model order requirements, and modal candidate selection. State feedback control laws were implemented based upon linear quadratic regulator design. Specification of the closed loop poles in the regulator design process was obtained by inclusion of a prescribed degree of stability in the manipulator model. Work on gross motion planning and control is also summarized. A systematic method to symbolically derive the full nonlinear dynamic equations of motion of multi-link flexible manipulators was developed.

Myostatin inhibitors in sports drug testing: Detection of myostatin-neutralizing antibodies in plasma/serum by affinity purification and Western blotting.

PubMed

Walpurgis, Katja; Thomas, Andreas; Schänzer, Wilhelm; Thevis, Mario

2016-02-01

Myostatin is a key regulator of skeletal muscle growth and inhibition of its signaling pathway results in an increased muscle mass and function. The aim of this study was to develop a qualitative detection assay for myostatin-neutralizing antibodies for doping control purposes by using immunological approaches. To detect different types of myostatin-neutralizing antibodies irrespective of their amino acid sequence, an immunological assay specific for antibodies directed against myostatin and having a human Fc domain was established. Affinity purification and Western blotting strategies were combined to allow extracting and identifying relevant analytes from 200 μL of plasma/serum in a non-targeted approach. The assay was characterized regarding specificity, linearity, precision, robustness, and recovery. The assay was found to be highly specific, robust, and linear from 0.1 to 1 μg/mL. The precision was successfully specified at three different concentrations and the recovery of the affinity purification was 58%. Within this study, an immunological detection assay for myostatin-neutralizing antibodies present in plasma/serum specimens was developed and successfully characterized. The presented approach can easily be modified to include other therapeutic antibodies and serves as proof-of-concept for the detection of antibody-based myostatin inhibitors in doping control samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Validation of a commercial 1,2-o-dilauryl-rac-glycero glutaric acid-(6'-methylresorufin) ester lipase assay for diagnosis of canine pancreatitis.

PubMed

Goodband, Emily L; Serrano, Gonçalo; Constantino-Casas, Fernando; Archer, Joy; Watson, Penny J; Williams, Tim L

2018-01-01

The objectives of this study were fourfold: technical validation of a commercial canine 1,2-o-dilauryl-rac-glycero glutaric acid-(6'-methylresorufin) ester (DGGR) lipase assay, to calculate a reference interval for DGGR lipase by the indirect a posteriori method, to establish biological validity of the assay, and to assess agreement between DGGR lipase and specific canine pancreatic lipase (Spec cPL) assays. Dogs with histologically confirmed acute pancreatitis (n=3), chronic pancreatitis (n=8) and normal pancreatic tissue (n=7) with stored (-80°C) serum samples were identified. Relevant controls were selected. Precision, reproducibility and linearity of DGGR lipase, and the effect of sample haemolysis and freezing, were assessed. Sensitivity and specificity of DGGR lipase and Spec cPL were determined. Agreement between these two parameters was calculated using Cohen's kappa coefficient (κ). The DGGR lipase assay demonstrated excellent precision, reproducibility and linearity. Sample haemolysis and storage at -80°C for 12 months did not influence the assay. DGGR lipase (>245IU/l) and Spec cPL (>400µg/l) both showed poor sensitivity but excellent specificity for acute pancreatitis, and poor to moderate sensitivity but excellent specificity for chronic pancreatitis. Substantial agreement (κ=0.679) was found between DGGR lipase and Spec cPL. The validated DGGR lipase assay had similar sensitivity and specificity for the diagnosis of acute and chronic pancreatitis to Spec cPL. DGGR lipase is a reliable alternative to Spec cPL for the diagnosis of pancreatitis.

Superconducting linear actuator

NASA Technical Reports Server (NTRS)

Johnson, Bruce; Hockney, Richard

1993-01-01

Special actuators are needed to control the orientation of large structures in space-based precision pointing systems. Electromagnetic actuators that presently exist are too large in size and their bandwidth is too low. Hydraulic fluid actuation also presents problems for many space-based applications. Hydraulic oil can escape in space and contaminate the environment around the spacecraft. A research study was performed that selected an electrically-powered linear actuator that can be used to control the orientation of a large pointed structure. This research surveyed available products, analyzed the capabilities of conventional linear actuators, and designed a first-cut candidate superconducting linear actuator. The study first examined theoretical capabilities of electrical actuators and determined their problems with respect to the application and then determined if any presently available actuators or any modifications to available actuator designs would meet the required performance. The best actuator was then selected based on available design, modified design, or new design for this application. The last task was to proceed with a conceptual design. No commercially-available linear actuator or modification capable of meeting the specifications was found. A conventional moving-coil dc linear actuator would meet the specification, but the back-iron for this actuator would weigh approximately 12,000 lbs. A superconducting field coil, however, eliminates the need for back iron, resulting in an actuator weight of approximately 1000 lbs.

A European multicenter study on the analytical performance of the VERIS HBV assay.

PubMed

Braun, Patrick; Delgado, Rafael; Drago, Monica; Fanti, Diana; Fleury, Hervé; Izopet, Jacques; Lombardi, Alessandra; Mancon, Alessandro; Marcos, Maria Angeles; Sauné, Karine; O Shea, Siobhan; Pérez-Rivilla, Alfredo; Ramble, John; Trimoulet, Pascale; Vila, Jordi; Whittaker, Duncan; Artus, Alain; Rhodes, Daniel

Hepatitis B viral load monitoring is an essential part of managing patients with chronic Hepatits B infection. Beckman Coulter has developed the VERIS HBV Assay for use on the fully automated Beckman Coulter DxN VERIS Molecular Diagnostics System. 1 OBJECTIVES: To evaluate the analytical performance of the VERIS HBV Assay at multiple European virology laboratories. Precision, analytical sensitivity, negative sample performance, linearity and performance with major HBV genotypes/subtypes for the VERIS HBV Assay was evaluated. Precision showed an SD of 0.15 log 10 IU/mL or less for each level tested. Analytical sensitivity determined by probit analysis was between 6.8-8.0 IU/mL. Clinical specificity on 90 unique patient samples was 100.0%. Performance with 754 negative samples demonstrated 100.0% not detected results, and a carryover study showed no cross contamination. Linearity using clinical samples was shown from 1.23-8.23 log 10 IU/mL and the assay detected and showed linearity with major HBV genotypes/subtypes. The VERIS HBV Assay demonstrated comparable analytical performance to other currently marketed assays for HBV DNA monitoring. Copyright © 2017 Elsevier B.V. All rights reserved.

Comparison of EMIT II, CEDIA, and DPC RIA assays for the detection of lysergic acid diethylamide in forensic urine samples.

PubMed

Wiegand, Russell F; Klette, Kevin L; Stout, Peter R; Gehlhausen, Jay M

2002-10-01

In an effort to determine a practical, efficient, and economical alternative for the use of a radioimmunoassay (RIA) for the detection of lysergic acid diethylamide (LSD) in human urine, the performance of two photometric immunoassays (Dade Behring EMIT II and Microgenics CEDIA) and the Diagnostics Products Corp. (DPC) RIA were compared. Precision, accuracy, and linearity of the 3 assays were determined by testing 60 replicates (10 for RIA) at 5 different concentrations below and above the 500-pg/mL LSD cut-off. The CEDIA and RIA exhibited better accuracy and precision than the EMIT II immunoassay. In contrast, the EMIT II and CEDIA demonstrated superior linearity r2 = 0.9809 and 0.9540, respectively, as compared with the RIA (r2 = 0.9062). The specificity of the three assays was assessed using compounds that have structural and chemical properties similar to LSD, common over-the-counter products, prescription drugs and some of their metabolites, and other drugs of abuse. Of the 144 compounds studied, the EMIT II cross-reacted with twice as many compounds as did the CEDIA and RIA. Specificity was also assessed in 221 forensic human urine specimens that previously screened positive for LSD by the EMIT II assay. Of these, only 11 tested positive by CEDIA, and 3 were positive by RIA. This indicated a comparable specificity performance between CEDIA and RIA. This also was consistent with a previously reported high false-positive rate of EMIT II (low specificity). Each of the immunoassays correctly identified LSD in 23 out of 24 human urine specimens that had previously been found to contain LSD by gas chromatography-mass spectrometry at a cut-off concentration of 200 pg/mL. The CEDIA exhibited superior precision, accuracy, and decreased cross-reactivity to compounds other than LSD as compared with the EMIT II assay and does not necessitate the handling of radioactive materials.

Low-Amplitude Topographic Features and Textures on the Moon: Initial Results from Detrended Lunar Orbiter Laser Altimeter (LOLA) Topography

NASA Technical Reports Server (NTRS)

Kreslavsky, Mikhail A.; Head, James W.; Neumann, Gregory A.; Zuber, Maria T.; Smith, David E.

2016-01-01

Global lunar topographic data derived from ranging measurements by the Lunar Orbiter Laser Altimeter (LOLA) onboard LRO mission to the Moon have extremely high vertical precision. We use detrended topography as a means for utilization of this precision in geomorphological analysis. The detrended topography was calculated as a difference between actual topography and a trend surface defined as a median topography in a circular sliding window. We found that despite complicated distortions caused by the non-linear nature of the detrending procedure, visual inspection of these data facilitates identification of low-amplitude gently-sloping geomorphic features. We present specific examples of patterns of lava flows forming the lunar maria and revealing compound flow fields, a new class of lava flow complex on the Moon. We also highlight the identification of linear tectonic features that otherwise are obscured in the images and topographic data processed in a more traditional manner.

Development and Validation of RP-LC Method for the Determination of Cinnarizine/Piracetam and Cinnarizine/Heptaminol Acefyllinate in Presence of Cinnarizine Reported Degradation Products

PubMed Central

EL-Houssini, Ola M.; Zawilla, Nagwan H.; Mohammad, Mohammad A.

2013-01-01

Specific stability indicating reverse-phase liquid chromatography (RP-LC) assay method (SIAM) was developed for the determination of cinnarizine (Cinn)/piracetam (Pira) and cinnarizine (Cinn)/heptaminol acefyllinate (Hept) in the presence of the reported degradation products of Cinn. A C18 column and gradient mobile phase was applied for good resolution of all peaks. The detection was achieved at 210 nm and 254 nm for Cinn/Pira and Cinn/Hept, respectively. The responses were linear over concentration ranges of 20–200, 20–1000 and 25–1000 μgmL−1 for Cinn, Pira, and Hept respectively. The proposed method was validated for linearity, accuracy, repeatability, intermediate precision, and robustness via statistical analysis of the data. The method was shown to be precise, accurate, reproducible, sensitive, and selective for the analysis of Cinn/Pira and Cinn/Hept in laboratory prepared mixtures and in pharmaceutical formulations. PMID:24137049

Novel spectrophotometric methods for simultaneous determination of timolol and dorzolamide in their binary mixture.

PubMed

Lotfy, Hayam Mahmoud; Hegazy, Maha A; Rezk, Mamdouh R; Omran, Yasmin Rostom

2014-05-21

Two smart and novel spectrophotometric methods namely; absorbance subtraction (AS) and amplitude modulation (AM) were developed and validated for the determination of a binary mixture of timolol maleate (TIM) and dorzolamide hydrochloride (DOR) in presence of benzalkonium chloride without prior separation, using unified regression equation. Additionally, simple, specific, accurate and precise spectrophotometric methods manipulating ratio spectra were developed and validated for simultaneous determination of the binary mixture namely; simultaneous ratio subtraction (SRS), ratio difference (RD), ratio subtraction (RS) coupled with extended ratio subtraction (EXRS), constant multiplication method (CM) and mean centering of ratio spectra (MCR). The proposed spectrophotometric procedures do not require any separation steps. Accuracy, precision and linearity ranges of the proposed methods were determined and the specificity was assessed by analyzing synthetic mixtures of both drugs. They were applied to their pharmaceutical formulation and the results obtained were statistically compared to that of a reported spectrophotometric method. The statistical comparison showed that there is no significant difference between the proposed methods and the reported one regarding both accuracy and precision. Copyright © 2014 Elsevier B.V. All rights reserved.

Simultaneous quantification of withanolides in Withania somnifera by a validated high-performance thin-layer chromatographic method.

PubMed

Srivastava, Pooja; Tiwari, Neerja; Yadav, Akhilesh K; Kumar, Vijendra; Shanker, Karuna; Verma, Ram K; Gupta, Madan M; Gupta, Anil K; Khanuja, Suman P S

2008-01-01

This paper describes a sensitive, selective, specific, robust, and validated densitometric high-performance thin-layer chromatographic (HPTLC) method for the simultaneous determination of 3 key withanolides, namely, withaferin-A, 12-deoxywithastramonolide, and withanolide-A, in Ashwagandha (Withania somnifera) plant samples. The separation was performed on aluminum-backed silica gel 60F254 HPTLC plates using dichloromethane-methanol-acetone-diethyl ether (15 + 1 + 1 + 1, v/v/v/v) as the mobile phase. The withanolides were quantified by densitometry in the reflection/absorption mode at 230 nm. Precise and accurate quantification could be performed in the linear working concentration range of 66-330 ng/band with good correlation (r2 = 0.997, 0.999, and 0.996, respectively). The method was validated for recovery, precision, accuracy, robustness, limit of detection, limit of quantitation, and specificity according to International Conference on Harmonization guidelines. Specificity of quantification was confirmed using retention factor (Rf) values, UV-Vis spectral correlation, and electrospray ionization mass spectra of marker compounds in sample tracks.

Validation of high throughput screening of human sera for detection of anti-PA IgG by Enzyme-Linked Immunosorbent Assay (ELISA) as an emergency response to an anthrax incident

PubMed Central

Semenova, Vera A.; Steward-Clark, Evelene; Maniatis, Panagiotis; Epperson, Monica; Sabnis, Amit; Schiffer, Jarad

2017-01-01

To improve surge testing capability for a response to a release of Bacillus anthracis, the CDC anti-Protective Antigen (PA) IgG Enzyme-Linked Immunosorbent Assay (ELISA) was re-designed into a high throughput screening format. The following assay performance parameters were evaluated: goodness of fit (measured as the mean reference standard r2), accuracy (measured as percent error), precision (measured as coefficient of variance (CV)), lower limit of detection (LLOD), lower limit of quantification (LLOQ), dilutional linearity, diagnostic sensitivity (DSN) and diagnostic specificity (DSP). The paired sets of data for each sample were evaluated by Concordance Correlation Coefficient (CCC) analysis. The goodness of fit was 0.999; percent error between the expected and observed concentration for each sample ranged from −4.6% to 14.4%. The coefficient of variance ranged from 9.0% to 21.2%. The assay LLOQ was 2.6 μg/mL. The regression analysis results for dilutional linearity data were r2 = 0.952, slope = 1.02 and intercept = −0.03. CCC between assays was 0.974 for the median concentration of serum samples. The accuracy and precision components of CCC were 0.997 and 0.977, respectively. This high throughput screening assay is precise, accurate, sensitive and specific. Anti-PA IgG concentrations determined using two different assays proved high levels of agreement. The method will improve surge testing capability 18-fold from 4 to 72 sera per assay plate. PMID:27814939

Validation of high throughput screening of human sera for detection of anti-PA IgG by Enzyme-Linked Immunosorbent Assay (ELISA) as an emergency response to an anthrax incident.

PubMed

Semenova, Vera A; Steward-Clark, Evelene; Maniatis, Panagiotis; Epperson, Monica; Sabnis, Amit; Schiffer, Jarad

2017-01-01

To improve surge testing capability for a response to a release of Bacillus anthracis, the CDC anti-Protective Antigen (PA) IgG Enzyme-Linked Immunosorbent Assay (ELISA) was re-designed into a high throughput screening format. The following assay performance parameters were evaluated: goodness of fit (measured as the mean reference standard r 2 ), accuracy (measured as percent error), precision (measured as coefficient of variance (CV)), lower limit of detection (LLOD), lower limit of quantification (LLOQ), dilutional linearity, diagnostic sensitivity (DSN) and diagnostic specificity (DSP). The paired sets of data for each sample were evaluated by Concordance Correlation Coefficient (CCC) analysis. The goodness of fit was 0.999; percent error between the expected and observed concentration for each sample ranged from -4.6% to 14.4%. The coefficient of variance ranged from 9.0% to 21.2%. The assay LLOQ was 2.6 μg/mL. The regression analysis results for dilutional linearity data were r 2  = 0.952, slope = 1.02 and intercept = -0.03. CCC between assays was 0.974 for the median concentration of serum samples. The accuracy and precision components of CCC were 0.997 and 0.977, respectively. This high throughput screening assay is precise, accurate, sensitive and specific. Anti-PA IgG concentrations determined using two different assays proved high levels of agreement. The method will improve surge testing capability 18-fold from 4 to 72 sera per assay plate. Published by Elsevier Ltd.

Development and validation of new spectrophotometric ratio H-point standard addition method and application to gastrointestinal acting drugs mixtures.

PubMed

Yehia, Ali M

2013-05-15

New, simple, specific, accurate and precise spectrophotometric technique utilizing ratio spectra is developed for simultaneous determination of two different binary mixtures. The developed ratio H-point standard addition method (RHPSAM) was managed successfully to resolve the spectral overlap in itopride hydrochloride (ITO) and pantoprazole sodium (PAN) binary mixture, as well as, mosapride citrate (MOS) and PAN binary mixture. The theoretical background and advantages of the newly proposed method are presented. The calibration curves are linear over the concentration range of 5-60 μg/mL, 5-40 μg/mL and 4-24 μg/mL for ITO, MOS and PAN, respectively. Specificity of the method was investigated and relative standard deviations were less than 1.5. The accuracy, precision and repeatability were also investigated for the proposed method according to ICH guidelines. Copyright © 2013 Elsevier B.V. All rights reserved.

Development and validation of new spectrophotometric ratio H-point standard addition method and application to gastrointestinal acting drugs mixtures

NASA Astrophysics Data System (ADS)

Yehia, Ali M.

2013-05-01

New, simple, specific, accurate and precise spectrophotometric technique utilizing ratio spectra is developed for simultaneous determination of two different binary mixtures. The developed ratio H-point standard addition method (RHPSAM) was managed successfully to resolve the spectral overlap in itopride hydrochloride (ITO) and pantoprazole sodium (PAN) binary mixture, as well as, mosapride citrate (MOS) and PAN binary mixture. The theoretical background and advantages of the newly proposed method are presented. The calibration curves are linear over the concentration range of 5-60 μg/mL, 5-40 μg/mL and 4-24 μg/mL for ITO, MOS and PAN, respectively. Specificity of the method was investigated and relative standard deviations were less than 1.5. The accuracy, precision and repeatability were also investigated for the proposed method according to ICH guidelines.

Novel spectrophotometric determination of flumethasone pivalate and clioquinol in their binary mixture and pharmaceutical formulation.

PubMed

Abdel-Aleem, Eglal A; Hegazy, Maha A; Sayed, Nour W; Abdelkawy, M; Abdelfatah, Rehab M

2015-02-05

This work is concerned with development and validation of three simple, specific, accurate and precise spectrophotometric methods for determination of flumethasone pivalate (FP) and clioquinol (CL) in their binary mixture and ear drops. Method A is a ratio subtraction spectrophotometric one (RSM). Method B is a ratio difference spectrophotometric one (RDSM), while method C is a mean center spectrophotometric one (MCR). The calibration curves are linear over the concentration range of 3-45 μg/mL for FP, and 2-25 μg/mL for CL. The specificity of the developed methods was assessed by analyzing different laboratory prepared mixtures of the FP and CL. The three methods were validated as per ICH guidelines; accuracy, precision and repeatability are found to be within the acceptable limits. Copyright © 2014 Elsevier B.V. All rights reserved.

New Stability-Indicating RP-HPLC Method for Determination of Diclofenac Potassium and Metaxalone from their Combined Dosage Form

PubMed Central

Panda, Sagar Suman; Patanaik, Debasis; Ravi Kumar, Bera V. V.

2012-01-01

A simple, precise and accurate isocratic RP-HPLC stability-indicating assay method has been developed to determine diclofenac potassium and metaxalone in their combined dosage forms. Isocratic separation was achieved on a Hibar-C18, Lichrosphere-100® (250 mm × 4.6 mm i.d., particle size 5 μm) column at room temperature in isocratic mode, the mobile phase consists of methanol: water (80:20, v/v) at a flow rate of 1.0 ml/min, the injection volume was 20 μl and UV detection was carried out at 280nm. The drug was subjected to acid and alkali hydrolysis, oxidation, photolysis and heat as stress conditions. The method was validated for specificity, linearity, precision, accuracy, robustness and system suitability. The method was linear in the drug concentration range of 2.5–30 μg/ml and 20–240 μg/ml for diclofenac potassium and metaxalone, respectively. The precision (RSD) of six samples was 0.83 and 0.93% for repeatability, and the intermediate precision (RSD) among six-sample preparation was 1.63 and 0.49% for diclofenac potassium and metaxalone, respectively. The mean recoveries were between 100.99–102.58% and 99.97–100.01% for diclofenac potassium and metaxalone, respectively. The proposed method can be used successfully for routine analysis of the drug in bulk and combined pharmaceutical dosage forms. PMID:22396909

Determination of illegal adulteration of dietary supplements with synthetic hair-growth compounds by UPLC and LC-Q-TOF/MS.

PubMed

Lee, Ji Hyun; Kang, Gihaeng; Park, Han Na; Kim, Jihee; Kim, Nam Sook; Park, Seongsoo; Park, Sung-Kwan; Baek, Sun Young; Kang, Hoil

2018-02-01

In this study, we developed a UPLC-PDA and LC-Q-TOF/MS method to identify and measure the following prohibited substances that may be found in dietary supplements:triaminodil, minoxidil, bimatoprost, alimemazine, diphenylcyclopropenone, α-tradiol, finasteride, methyltestosterone, spironolatone, flutamide, cyproterone, dutasteride, and testosterone 17-propionate.The method was validated according to International Conference on Harmonization guidelines in terms of specificity, linearity, accuracy, precision, LOD, LOQ, recovery, and stability. The method was completely validated showing satisfactory data for all method validation parameters. The linearity was good (R 2  > 0.999) with intra- and inter-day precision values of 0.2-3.4% and 0.3-2.9%, respectively. Moreover, the intra- and inter-day accuracies were 87-102% and 86-103%, respectively, and the precision was better than 9.4% (relative standard deviation).Hence, the proposed method is precise and has high quality,and can be utilised to comprehensively and continually monitor illegal drug adulteration in various forms of dietary supplements. Furthermore, to evaluate the applicability of the proposed method, we analysed 13 hair-growth compounds in 78 samples including food and dietary supplements. Minoxidil and triaminodil were detected in capsules at concentrations of 4.69 mg/g and 6.54 mg/g. In addition, finasteride was detected in a tablet at 13.45 mg/g. In addition, the major characteristic fragment ions were confirmed once again using LC-Q-TOF/MS for higher accuracy.

Simultaneous Determination of Soyasaponins and Isoflavones in Soy (Glycine max L.) Products by HPTLC-densitometry-Multiple Detection.

PubMed

Shawky, Eman; Sallam, Shaimaa M

2017-11-01

A new high-throughput method was developed for the simultaneous analysis of isoflavones and soyasaponnins in Soy (Glycine max L.) products by high-performance thin-layer chromatography with densitometry and multiple detection. Silica gel was used as the stationary phase and ethyl acetate:methanol:water:acetic acid (100:20:16:1, v/v/v/v) as the mobile phase. After chromatographic development, multi-wavelength scanning was carried out by: (i) UV-absorbance measurement at 265 nm for genistin, daidzin and glycitin, (ii) Vis-absorbance measurement at 650 nm for Soyasaponins I and III, after post-chromatographic derivatization with anisaldehyde/sulfuric acid reagent. Validation of the developed method was found to meet the acceptance criteria delineated by ICH guidelines with respect to linearity, accuracy, precision, specificity and robustness. Calibrations were linear with correlation coefficients of >0.994. Intra-day precisions relative standard deviation (RSD)% of all substances in matrix were determined to be between 0.7 and 0.9%, while inter-day precisions (RSD%) ranged between 1.2 and 1.8%. The validated method was successfully applied for determination of the studied analytes in soy-based infant formula and soybean products. The new method compares favorably to other reported methods in being as accurate and precise and in the same time more feasible and cost-effective. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Leveraging prognostic baseline variables to gain precision in randomized trials

PubMed Central

Colantuoni, Elizabeth; Rosenblum, Michael

2015-01-01

We focus on estimating the average treatment effect in a randomized trial. If baseline variables are correlated with the outcome, then appropriately adjusting for these variables can improve precision. An example is the analysis of covariance (ANCOVA) estimator, which applies when the outcome is continuous, the quantity of interest is the difference in mean outcomes comparing treatment versus control, and a linear model with only main effects is used. ANCOVA is guaranteed to be at least as precise as the standard unadjusted estimator, asymptotically, under no parametric model assumptions and also is locally semiparametric efficient. Recently, several estimators have been developed that extend these desirable properties to more general settings that allow any real-valued outcome (e.g., binary or count), contrasts other than the difference in mean outcomes (such as the relative risk), and estimators based on a large class of generalized linear models (including logistic regression). To the best of our knowledge, we give the first simulation study in the context of randomized trials that compares these estimators. Furthermore, our simulations are not based on parametric models; instead, our simulations are based on resampling data from completed randomized trials in stroke and HIV in order to assess estimator performance in realistic scenarios. We provide practical guidance on when these estimators are likely to provide substantial precision gains and describe a quick assessment method that allows clinical investigators to determine whether these estimators could be useful in their specific trial contexts. PMID:25872751

Acceleration of Linear Finite-Difference Poisson-Boltzmann Methods on Graphics Processing Units.

PubMed

Qi, Ruxi; Botello-Smith, Wesley M; Luo, Ray

2017-07-11

Electrostatic interactions play crucial roles in biophysical processes such as protein folding and molecular recognition. Poisson-Boltzmann equation (PBE)-based models have emerged as widely used in modeling these important processes. Though great efforts have been put into developing efficient PBE numerical models, challenges still remain due to the high dimensionality of typical biomolecular systems. In this study, we implemented and analyzed commonly used linear PBE solvers for the ever-improving graphics processing units (GPU) for biomolecular simulations, including both standard and preconditioned conjugate gradient (CG) solvers with several alternative preconditioners. Our implementation utilizes the standard Nvidia CUDA libraries cuSPARSE, cuBLAS, and CUSP. Extensive tests show that good numerical accuracy can be achieved given that the single precision is often used for numerical applications on GPU platforms. The optimal GPU performance was observed with the Jacobi-preconditioned CG solver, with a significant speedup over standard CG solver on CPU in our diversified test cases. Our analysis further shows that different matrix storage formats also considerably affect the efficiency of different linear PBE solvers on GPU, with the diagonal format best suited for our standard finite-difference linear systems. Further efficiency may be possible with matrix-free operations and integrated grid stencil setup specifically tailored for the banded matrices in PBE-specific linear systems.

Survival and aging of a small laboratory population of a marine mollusc, Aplysia californica.

PubMed

Hirsch, H R; Peretz, B

1984-09-01

In an investigation of the postmetamorphic survival of a population of 112 Aplysia californica, five animals died before 100 days of age and five after 200 days. The number of survivors among the 102 animals which died between 100 and 220 days declined approximately linearly with age. The median age at death was 155 days. The animals studied were those that died of natural causes within a laboratory population that was established to provide Aplysia for sacrifice in an experimental program. Actuarial separation of the former group from the latter was justified by theoretical consideration. Age-specific mortality rates were calculated from the survival data. Statistical fluctuation arising from the small size of the population was reduced by grouping the data in bins of unequal age duration. The durations were specified such that each bin contained approximately the same number of data points. An algorithm for choosing the number of data bins was based on the requirement that the precision with which the age of a group is determined should equal the precision with which the number of deaths in the groups is known. The Gompertz and power laws of mortality were fitted to the age-specific mortality-rate data with equally good results. The positive values of slope associated with the mortality-rate functions as well as the linear shape of the curve of survival provide actuarial evidence that Aplysia age. Since Aplysia grow linearly without approaching a limiting size, the existence of senescence indicates especially clearly the falsity of Bidder's hypothesis that aging is a by-product of the cessation of growth.

Experimental Robot Model Adjustments Based on Force–Torque Sensor Information

PubMed Central

2018-01-01

The computational complexity of humanoid robot balance control is reduced through the application of simplified kinematics and dynamics models. However, these simplifications lead to the introduction of errors that add to other inherent electro-mechanic inaccuracies and affect the robotic system. Linear control systems deal with these inaccuracies if they operate around a specific working point but are less precise if they do not. This work presents a model improvement based on the Linear Inverted Pendulum Model (LIPM) to be applied in a non-linear control system. The aim is to minimize the control error and reduce robot oscillations for multiple working points. The new model, named the Dynamic LIPM (DLIPM), is used to plan the robot behavior with respect to changes in the balance status denoted by the zero moment point (ZMP). Thanks to the use of information from force–torque sensors, an experimental procedure has been applied to characterize the inaccuracies and introduce them into the new model. The experiments consist of balance perturbations similar to those of push-recovery trials, in which step-shaped ZMP variations are produced. The results show that the responses of the robot with respect to balance perturbations are more precise and the mechanical oscillations are reduced without comprising robot dynamics. PMID:29534477

A Linear Variable-[theta] Model for Measuring Individual Differences in Response Precision

ERIC Educational Resources Information Center

Ferrando, Pere J.

2011-01-01

Models for measuring individual response precision have been proposed for binary and graded responses. However, more continuous formats are quite common in personality measurement and are usually analyzed with the linear factor analysis model. This study extends the general Gaussian person-fluctuation model to the continuous-response case and…

Double Arm Linkage precision Linear motion (DALL) Carriage, a simplified, rugged, high performance linear motion stage for the moving mirror of an Fourier Transform Spectrometer or other system requiring precision linear motion

NASA Astrophysics Data System (ADS)

Johnson, Kendall B.; Hopkins, Greg

2017-08-01

The Double Arm Linkage precision Linear motion (DALL) carriage has been developed as a simplified, rugged, high performance linear motion stage. Initially conceived as a moving mirror stage for the moving mirror of a Fourier Transform Spectrometer (FTS), it is applicable to any system requiring high performance linear motion. It is based on rigid double arm linkages connecting a base to a moving carriage through flexures. It is a monolithic design. The system is fabricated from one piece of material including the flexural elements, using high precision machining. The monolithic design has many advantages. There are no joints to slip or creep and there are no CTE (coefficient of thermal expansion) issues. This provides a stable, robust design, both mechanically and thermally and is expected to provide a wide operating temperature range, including cryogenic temperatures, and high tolerance to vibration and shock. Furthermore, it provides simplicity and ease of implementation, as there is no assembly or alignment of the mechanism. It comes out of the machining operation aligned and there are no adjustments. A prototype has been fabricated and tested, showing superb shear performance and very promising tilt performance. This makes it applicable to both corner cube and flat mirror FTS systems respectively.

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

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

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

2010-02-05

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

Application of Smart Infrastructure Systems approach to precision medicine.

PubMed

Govindaraju, Diddahally R; Annaswamy, Anuradha M

2015-12-01

All biological variation is hierarchically organized dynamic network system of genomic components, organelles, cells, tissues, organs, individuals, families, populations and metapopulations. Individuals are axial in this hierarchy, as they represent antecedent, attendant and anticipated aspects of health, disease, evolution and medical care. Humans show individual specific genetic and clinical features such as complexity, cooperation, resilience, robustness, vulnerability, self-organization, latent and emergent behavior during their development, growth and senescence. Accurate collection, measurement, organization and analyses of individual specific data, embedded at all stratified levels of biological, demographic and cultural diversity - the big data - is necessary to make informed decisions on health, disease and longevity; which is a central theme of precision medicine initiative (PMI). This initiative also calls for the development of novel analytical approaches to handle complex multidimensional data. Here we suggest the application of Smart Infrastructure Systems (SIS) approach to accomplish some of the goals set forth by the PMI on the premise that biological systems and the SIS share many common features. The latter has been successfully employed in managing complex networks of non-linear adaptive controls, commonly encountered in smart engineering systems. We highlight their concordance and discuss the utility of the SIS approach in precision medicine programs.

Simultaneous determination of related substances of telmisartan and hydrochlorothiazide in tablet dosage form by using reversed phase high performance liquid chromatographic method

PubMed Central

Mukhopadhyay, Sutirtho; Kadam, Kiran; Sawant, Laxman; Nachane, Dhanashree; Pandita, Nancy

2011-01-01

Objective: Telmisartan is a potent, long-lasting, nonpeptide antagonist of the angiotensin II type-1 (AT1) receptor that is indicated for the treatment of essential hypertension. Hydrochlorothiazide is a widely prescribed diuretic and it is indicated for the treatment of edema, control of essential hypertension and management of diabetes insipidus. In the current article a new, accurate, sensitive, precise, rapid, reversed phase high performance liquid chromatography (RP-HPLC) method was developed for determination of related substances of Telmisartan and Hydrochlorthiazide in tablet dosage form. Materials and Methods: Simultaneous determination of related substances was performed on Kromasil C18 analytical column (250 × 4.6 mm; 5μm pertical size) column at 40°C employing a gradient elution. Mobile phase consisting of solvent A (solution containing 2.0 g of potassium dihydrogen phosphate anhydrous and 1.04 g of Sodium 1- Hexane sulphonic acid monohydrate per liter of water, adjusted to pH 3.0 with orthophosphoric acid) and solvent B (mixture of Acetonitrile: Methanol in the ratio 80:20 v/v) was used at a flow rate of 1.0 ml min–1. UV detection was performed at 270 nm. Results: During method validation parameter such as precision, linearity, accuracy, specificity, limit of detection and quantification were evaluated, which remained within acceptable limits. Conclusions: HPLC analytical method is linear, accurate, precise, robust and specific, being able to separate the main drug from its degradation products. It may find application for the routine analysis of the related substances of both Telmisartan and Hydrochlorthiazide in this combination tablets. PMID:21966158

The Too-Much-Precision Effect.

PubMed

Loschelder, David D; Friese, Malte; Schaerer, Michael; Galinsky, Adam D

2016-12-01

Past research has suggested a fundamental principle of price precision: The more precise an opening price, the more it anchors counteroffers. The present research challenges this principle by demonstrating a too-much-precision effect. Five experiments (involving 1,320 experts and amateurs in real-estate, jewelry, car, and human-resources negotiations) showed that increasing the precision of an opening offer had positive linear effects for amateurs but inverted-U-shaped effects for experts. Anchor precision backfired because experts saw too much precision as reflecting a lack of competence. This negative effect held unless first movers gave rationales that boosted experts' perception of their competence. Statistical mediation and experimental moderation established the critical role of competence attributions. This research disentangles competing theoretical accounts (attribution of competence vs. scale granularity) and qualifies two putative truisms: that anchors affect experts and amateurs equally, and that more precise prices are linearly more potent anchors. The results refine current theoretical understanding of anchoring and have significant implications for everyday life.

Effect of electric potential and current on mandibular linear measurements in cone beam CT.

PubMed

Panmekiate, S; Apinhasmit, W; Petersson, A

2012-10-01

The purpose of this study was to compare mandibular linear distances measured from cone beam CT (CBCT) images produced by different radiographic parameter settings (peak kilovoltage and milliampere value). 20 cadaver hemimandibles with edentulous ridges posterior to the mental foramen were embedded in clear resin blocks and scanned by a CBCT machine (CB MercuRay(TM); Hitachi Medico Technology Corp., Chiba-ken, Japan). The radiographic parameters comprised four peak kilovoltage settings (60 kVp, 80 kVp, 100 kVp and 120 kVp) and two milliampere settings (10 mA and 15 mA). A 102.4 mm field of view was chosen. Each hemimandible was scanned 8 times with 8 different parameter combinations resulting in 160 CBCT data sets. On the cross-sectional images, six linear distances were measured. To assess the intraobserver variation, the 160 data sets were remeasured after 2 weeks. The measurement precision was calculated using Dahlberg's formula. With the same peak kilovoltage, the measurements yielded by different milliampere values were compared using the paired t-test. With the same milliampere value, the measurements yielded by different peak kilovoltage were compared using analysis of variance. A significant difference was considered when p < 0.05. Measurement precision varied from 0.03 mm to 0.28 mm. No significant differences in the distances were found among the different radiographic parameter combinations. Based upon the specific machine in the present study, low peak kilovoltage and milliampere value might be used for linear measurements in the posterior mandible.

Simultaneous Determination of Withanolide A and Bacoside A in Spansules by High-Performance Thin-Layer Chromatography

PubMed Central

Shinde, P B; Aragade, P D; Agrawal, M R; Deokate, U A; Khadabadi, S S

2011-01-01

The objective of this work was to develop and validate a simple, rapid, precise, and accurate high performance thin layer chromatography method for simultaneous determination of withanolide A and bacoside A in combined dosage form. The stationary phase used was silica gel G60F254. The mobile phase used was mixture of ethyl acetate: methanol: toluene: water (4:1:1:0.5 v/v/v/v). The detection of spots was carried out at 320 nm using absorbance reflectance mode. The method was validated in terms of linearity, accuracy, precision and specificity. The calibration curve was found to be linear between 200 to 800 ng/spot for withanolide A and 50 to 350 ng/spot for bacoside A. The limit of detection and limit of quantification for the withanolide A were found to be 3.05 and 10.06 ng/spot, respectively and for bacoside A 8.3 and 27.39 ng/spot, respectively. The proposed method can be successfully used to determine the drug content of marketed formulation. PMID:22303073

Simultaneous determination of withanolide a and bacoside a in spansules by high-performance thin-layer chromatography.

PubMed

Shinde, P B; Aragade, P D; Agrawal, M R; Deokate, U A; Khadabadi, S S

2011-03-01

The objective of this work was to develop and validate a simple, rapid, precise, and accurate high performance thin layer chromatography method for simultaneous determination of withanolide A and bacoside A in combined dosage form. The stationary phase used was silica gel G60F(254). The mobile phase used was mixture of ethyl acetate: methanol: toluene: water (4:1:1:0.5 v/v/v/v). The detection of spots was carried out at 320 nm using absorbance reflectance mode. The method was validated in terms of linearity, accuracy, precision and specificity. The calibration curve was found to be linear between 200 to 800 ng/spot for withanolide A and 50 to 350 ng/spot for bacoside A. The limit of detection and limit of quantification for the withanolide A were found to be 3.05 and 10.06 ng/spot, respectively and for bacoside A 8.3 and 27.39 ng/spot, respectively. The proposed method can be successfully used to determine the drug content of marketed formulation.

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

PubMed

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

2011-07-01

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

More Precise Estimation of Lower-Level Interaction Effects in Multilevel Models.

PubMed

Loeys, Tom; Josephy, Haeike; Dewitte, Marieke

2018-01-01

In hierarchical data, the effect of a lower-level predictor on a lower-level outcome may often be confounded by an (un)measured upper-level factor. When such confounding is left unaddressed, the effect of the lower-level predictor is estimated with bias. Separating this effect into a within- and between-component removes such bias in a linear random intercept model under a specific set of assumptions for the confounder. When the effect of the lower-level predictor is additionally moderated by another lower-level predictor, an interaction between both lower-level predictors is included into the model. To address unmeasured upper-level confounding, this interaction term ought to be decomposed into a within- and between-component as well. This can be achieved by first multiplying both predictors and centering that product term next, or vice versa. We show that while both approaches, on average, yield the same estimates of the interaction effect in linear models, the former decomposition is much more precise and robust against misspecification of the effects of cross-level and upper-level terms, compared to the latter.

UV Spectrophotometric Determination and Validation of Hydroquinone in Liposome.

PubMed

Khoshneviszadeh, Rabea; Fazly Bazzaz, Bibi Sedigheh; Housaindokht, Mohammad Reza; Ebrahim-Habibi, Azadeh; Rajabi, Omid

2015-01-01

The method has been developed and validated for the determination of hydroquinone in liposomal formulation. The samples were dissolved in methanol and evaluated in 293 nm. The validation parameters such as linearity, accuracy, precision, specificity, limit of detection (LOD) and limit of quantitation (LOQ) were determined. The calibration curve was linear in 1-50 µg/mL range of hydroquinone analyte with a regression coefficient of 0.9998. This study showed that the liposomal hydroquinone composed of phospholipid (7.8 %), cholesterol (1.5 %), alpha ketopherol (0.17 %) and hydroquinone (0.5 %) did not absorb wavelength of 293 nm if it diluted 500 times by methanol. The concentration of hydroquinone reached 10 µg/mL after 500 times of dilution. Furthermore, various validation parameters as per ICH Q2B guideline were tested and found accordingly. The recovery percentages of liposomal hydroquinone were found 102 ± 0.8, 99 ± 0.2 and 98 ± 0.4 for 80%, 100% and 120% respectively. The relative standard deviation values of inter and intra-day precisions were <%2. LOD and LOQ were 0.24 and 0.72 µg/mL respectively.

Estimation of L-dopa from Mucuna pruriens LINN and formulations containing M. pruriens by HPTLC method.

PubMed

Modi, Ketan Pravinbhai; Patel, Natvarlal Manilal; Goyal, Ramesh Kishorilal

2008-03-01

A selective, precise, and accurate high-performance thin-layer chromatographic (HPTLC) method has been developed for the analysis of L-dopa in Mucuna pruriens seed extract and its formulations. The method involves densitometric evaluation of L-dopa after resolving it by HPTLC on silica gel plates with n-butanol-acetic acid-water (4.0+1.0+1.0, v/v) as the mobile phase. Densitometric analysis of L-dopa was carried out in the absorbance mode at 280 nm. The relationship between the concentration of L-dopa and corresponding peak areas was found to be linear in the range of 100 to 1200 ng/spot. The method was validated for precision (inter and intraday), repeatability, and accuracy. Mean recovery was 100.30%. The relative standard deviation (RSD) values of the precision were found to be in the range 0.64-1.52%. In conclusion, the proposed TLC method was found to be precise, specific and accurate and can be used for identification and quantitative determination of L-dopa in herbal extract and its formulations.

Stress Degradation Studies on Varenicline Tartrate and Development of a Validated Stability-Indicating HPLC Method

PubMed Central

Pujeri, Sudhakar S.; Khader, Addagadde M. A.; Seetharamappa, Jaldappagari

2012-01-01

A simple, rapid and stability-indicating reversed-phase liquid chromatographic method was developed for the assay of varenicline tartrate (VRT) in the presence of its degradation products generated from forced decomposition studies. The HPLC separation was achieved on a C18 Inertsil column (250 mm × 4.6 mm i.d. particle size is 5 μm) employing a mobile phase consisting of ammonium acetate buffer containing trifluoroacetic acid (0.02M; pH 4) and acetonitrile in gradient program mode with a flow rate of 1.0 mL min−1. The UV detector was operated at 237 nm while column temperature was maintained at 40 °C. The developed method was validated as per ICH guidelines with respect to specificity, linearity, precision, accuracy, robustness and limit of quantification. The method was found to be simple, specific, precise and accurate. Selectivity of the proposed method was validated by subjecting the stock solution of VRT to acidic, basic, photolysis, oxidative and thermal degradation. The calibration curve was found to be linear in the concentration range of 0.1–192 μg mL−1 (R2 = 0.9994). The peaks of degradation products did not interfere with that of pure VRT. The utility of the developed method was examined by analyzing the tablets containing VRT. The results of analysis were subjected to statistical analysis. PMID:22396908

Assessment of Health-Cost Externalities of Air Pollution at the National Level using the EVA Model System

NASA Astrophysics Data System (ADS)

Brandt, Jørgen; Silver, Jeremy David; Heile Christensen, Jesper; Skou Andersen, Mikael; Geels, Camilla; Gross, Allan; Buus Hansen, Ayoe; Mantzius Hansen, Kaj; Brandt Hedegaard, Gitte; Ambelas Skjøth, Carsten

2010-05-01

Air pollution has significant negative impacts on human health and well-being, which entail substantial economic consequences. We have developed an integrated model system, EVA (External Valuation of Air pollution), to assess health-related economic externalities of air pollution resulting from specific emission sources/sectors. The EVA system was initially developed to assess externalities from power production, but in this study it is extended to evaluate costs at the national level. The EVA system integrates a regional-scale atmospheric chemistry transport model (DEHM), address-level population data, exposure-response functions and monetary values applicable for Danish/European conditions. Traditionally, systems that assess economic costs of health impacts from air pollution assume linear approximations in the source-receptor relationships. However, atmospheric chemistry is non-linear and therefore the uncertainty involved in the linear assumption can be large. The EVA system has been developed to take into account the non-linear processes by using a comprehensive, state-of-the-art chemical transport model when calculating how specific changes to emissions affect air pollution levels and the subsequent impacts on human health and cost. Furthermore, we present a new "tagging" method, developed to examine how specific emission sources influence air pollution levels without assuming linearity of the non-linear behaviour of atmospheric chemistry. This method is more precise than the traditional approach based on taking the difference between two concentration fields. Using the EVA system, we have estimated the total external costs from the main emission sectors in Denmark, representing the ten major SNAP codes. Finally, we assess the impacts and external costs of emissions from international ship traffic around Denmark, since there is a high volume of ship traffic in the region.

Development and application of a validated HPLC method for the analysis of dissolution samples of levothyroxine sodium drug products.

PubMed

Collier, J W; Shah, R B; Bryant, A R; Habib, M J; Khan, M A; Faustino, P J

2011-02-20

A rapid, selective, and sensitive gradient HPLC method was developed for the analysis of dissolution samples of levothyroxine sodium tablets. Current USP methodology for levothyroxine (L-T(4)) was not adequate to resolve co-elutants from a variety of levothyroxine drug product formulations. The USP method for analyzing dissolution samples of the drug product has shown significant intra- and inter-day variability. The sources of method variability include chromatographic interferences introduced by the dissolution media and the formulation excipients. In the present work, chromatographic separation of levothyroxine was achieved on an Agilent 1100 Series HPLC with a Waters Nova-pak column (250 mm × 3.9 mm) using a 0.01 M phosphate buffer (pH 3.0)-methanol (55:45, v/v) in a gradient elution mobile phase at a flow rate of 1.0 mL/min and detection UV wavelength of 225 nm. The injection volume was 800 μL and the column temperature was maintained at 28°C. The method was validated according to USP Category I requirements. The validation characteristics included accuracy, precision, specificity, linearity, and analytical range. The standard curve was found to have a linear relationship (r(2)>0.99) over the analytical range of 0.08-0.8 μg/mL. Accuracy ranged from 90 to 110% for low quality control (QC) standards and 95 to 105% for medium and high QC standards. Precision was <2% at all QC levels. The method was found to be accurate, precise, selective, and linear for L-T(4) over the analytical range. The HPLC method was successfully applied to the analysis of dissolution samples of marketed levothyroxine sodium tablets. Published by Elsevier B.V.

Development and application of a validated HPLC method for the analysis of dissolution samples of levothyroxine sodium drug products

PubMed Central

Collier, J.W.; Shah, R.B.; Bryant, A.R.; Habib, M.J.; Khan, M.A.; Faustino, P.J.

2011-01-01

A rapid, selective, and sensitive gradient HPLC method was developed for the analysis of dissolution samples of levothyroxine sodium tablets. Current USP methodology for levothyroxine (l-T4) was not adequate to resolve co-elutants from a variety of levothyroxine drug product formulations. The USP method for analyzing dissolution samples of the drug product has shown significant intra- and inter-day variability. The sources of method variability include chromatographic interferences introduced by the dissolution media and the formulation excipients. In the present work, chromatographic separation of levothyroxine was achieved on an Agilent 1100 Series HPLC with a Waters Nova-pak column (250mm × 3.9mm) using a 0.01 M phosphate buffer (pH 3.0)–methanol (55:45, v/v) in a gradient elution mobile phase at a flow rate of 1.0 mL/min and detection UV wavelength of 225 nm. The injection volume was 800 µL and the column temperature was maintained at 28 °C. The method was validated according to USP Category I requirements. The validation characteristics included accuracy, precision, specificity, linearity, and analytical range. The standard curve was found to have a linear relationship (r2 > 0.99) over the analytical range of 0.08–0.8 µg/mL. Accuracy ranged from 90 to 110% for low quality control (QC) standards and 95 to 105% for medium and high QC standards. Precision was <2% at all QC levels. The method was found to be accurate, precise, selective, and linear for l-T4 over the analytical range. The HPLC method was successfully applied to the analysis of dissolution samples of marketed levothyroxine sodium tablets. PMID:20947276

Evaluation of the COBAS Hepatitis C Virus (HCV) TaqMan analyte-specific reagent assay and comparison to the COBAS Amplicor HCV Monitor V2.0 and Versant HCV bDNA 3.0 assays.

PubMed

Konnick, Eric Q; Williams, Sheri M; Ashwood, Edward R; Hillyard, David R

2005-05-01

Performance characteristics of the COBAS hepatitis C virus (HCV) TaqMan analyte-specific reagent (TM-ASR) assay using the QIAGEN BioRobot 9604 for RNA extraction were evaluated and compared to the COBAS Amplicor HCV Monitor V2.0 (Amplicor) and Versant HCV bDNA 3.0 (Versant) assays using clinical samples. Calibration of TM-ASR using Armored RNA allowed determination of the distribution of HCV RNA in clinical samples, using 22,399 clinical samples. Limit of detection, linearity, and inter- and intraassay assay precision were determined for the TM-ASR assay using multiple clinical specimen panels across multiple determinations. Genotype specificity for the TM-ASR assay was determined using samples with different HCV RNA genotypes evaluated and compared against predetermined results. Contamination control of the TM-ASR assay was evaluated using pools of HCV RNA-positive and -negative samples tested in a checkerboard pattern over 12 runs of 96 samples. Correlation of the TM-ASR, Amplicor, and Versant assays was determined using 100 paired clinical samples and Deming regression analysis. The TM-ASR performed well with respect to linearity, precision, and contamination control. The correlation between TM-ASR and the Amplicor and Versant assays was poor, with large differences between assay results for individual samples. Calibration of the TM-ASR assay with Armored RNA allowed for a wide dynamic range and description of the distribution of HCV RNA in clinical samples.

Evaluation of the COBAS Hepatitis C Virus (HCV) TaqMan Analyte-Specific Reagent Assay and Comparison to the COBAS Amplicor HCV Monitor V2.0 and Versant HCV bDNA 3.0 Assays

PubMed Central

Konnick, Eric Q.; Williams, Sheri M.; Ashwood, Edward R.; Hillyard, David R.

2005-01-01

Performance characteristics of the COBAS hepatitis C virus (HCV) TaqMan analyte-specific reagent (TM-ASR) assay using the QIAGEN BioRobot 9604 for RNA extraction were evaluated and compared to the COBAS Amplicor HCV Monitor V2.0 (Amplicor) and Versant HCV bDNA 3.0 (Versant) assays using clinical samples. Calibration of TM-ASR using Armored RNA allowed determination of the distribution of HCV RNA in clinical samples, using 22,399 clinical samples. Limit of detection, linearity, and inter- and intraassay assay precision were determined for the TM-ASR assay using multiple clinical specimen panels across multiple determinations. Genotype specificity for the TM-ASR assay was determined using samples with different HCV RNA genotypes evaluated and compared against predetermined results. Contamination control of the TM-ASR assay was evaluated using pools of HCV RNA-positive and -negative samples tested in a checkerboard pattern over 12 runs of 96 samples. Correlation of the TM-ASR, Amplicor, and Versant assays was determined using 100 paired clinical samples and Deming regression analysis. The TM-ASR performed well with respect to linearity, precision, and contamination control. The correlation between TM-ASR and the Amplicor and Versant assays was poor, with large differences between assay results for individual samples. Calibration of the TM-ASR assay with Armored RNA allowed for a wide dynamic range and description of the distribution of HCV RNA in clinical samples. PMID:15872232

Development of a BK virus real-time quantitative assay using the bioMérieux analyte-specific reagents in plasma specimens.

PubMed

Rennert, Hanna; Fernandes, Helen; Gilani, Zahid; Sipley, John

2015-12-01

Viral load testing for BK virus (BKV) has become the standard of care for diagnosing BKV infection and monitoring therapy in kidney transplant patients. However, there are currently no US Food and Drug Administration-approved assays and no standardization among available tests. This study evaluated the performance of the analyte-specific reagent (ASR) BKV primers r-gene and probe r-gene reagents (bioMérieux, Marcy l'Étoile, France) soon to become available on the US market for accuracy, linearity, precision, analytical sensitivity, specificity, and correlation with the Qiagen (Germantown, MD) BKV ASR test using commercial material and patient plasma samples. The assay was linear from 204 to 3.92 million (2.31-6.6 log10) DNA copies/mL (coefficient of determination: R(2) =0.999). A dilution series demonstrated limits of detection and quantitation of 2.14 log10 and 2.30 log10 copies/mL (95% hit rate detection), respectively. Interrun precision was highly reproducible, with coefficients of variance ranging from 2.2% to 6.0%. A comparison of 34 matched samples showed a good agreement (R(2) = 0.87) between the bioMérieux BKV laboratory test and the Qiagen BKV ASR assay results, with an average negative bias (-0.28 log10 copies/mL). The laboratory-developed test with bioMérieux BKV reagents is a reliable and sensitive assay for BKV DNA quantitation compared with the Qiagen ASR test. Copyright© by the American Society for Clinical Pathology.

Characterization of single chain antibody targets through yeast two hybrid

PubMed Central

2010-01-01

Background Due to their unique ability to bind their targets with high fidelity, antibodies are used widely not only in biomedical research, but also in many clinical applications. Recombinant antibodies, including single chain variable fragments (scFv), are gaining momentum because they allow powerful in vitro selection and manipulation without loss of function. Regardless of the ultimate application or type of antibody used, precise understanding of the interaction between the antibody's binding site and its specific target epitope(s) is of great importance. However, such data is frequently difficult to obtain. Results We describe an approach that allows detailed characterization of a given antibody's target(s) using the yeast two-hybrid system. Several recombinant scFv were used as bait and screened against highly complex cDNA libraries. Systematic sequencing of all retained clones and statistical analysis allowed efficient ranking of the prey fragments. Multiple alignment of the obtained cDNA fragments provided a selected interacting domain (SID), efficiently narrowing the epitope-containing region. Interactions between antibodies and their respective targets were characterized for several scFv. For AA2 and ROF7, two conformation-specific sensors that exclusively bind the activated forms of the small GTPases Rab6 and Rab1 respectively, only fragments expressing the entire target protein's core region were retained. This strongly suggested interaction with a non-linear epitope. For two other scFv, TA10 and SF9, which recognize the large proteins giantin and non-muscle myosin IIA, respectively, precise antibody-binding regions within the target were defined. Finally, for some antibodies, secondary targets within and across species could be revealed. Conclusions Our method, utilizing the yeast two-hybrid technology and scFv as bait, is a simple yet powerful approach for the detailed characterization of antibody targets. It allows precise domain mapping for linear epitopes, confirmation of non-linear epitopes for conformational sensors, and detection of secondary binding partners. This approach may thus prove to be an elegant and rapid method for the target characterization of newly obtained scFv antibodies. It may be considered prior to any research application and particularly before any use of such recombinant antibodies in clinical medicine. PMID:20727208

Weighted linear least squares estimation of diffusion MRI parameters: strengths, limitations, and pitfalls.

PubMed

Veraart, Jelle; Sijbers, Jan; Sunaert, Stefan; Leemans, Alexander; Jeurissen, Ben

2013-11-01

Linear least squares estimators are widely used in diffusion MRI for the estimation of diffusion parameters. Although adding proper weights is necessary to increase the precision of these linear estimators, there is no consensus on how to practically define them. In this study, the impact of the commonly used weighting strategies on the accuracy and precision of linear diffusion parameter estimators is evaluated and compared with the nonlinear least squares estimation approach. Simulation and real data experiments were done to study the performance of the weighted linear least squares estimators with weights defined by (a) the squares of the respective noisy diffusion-weighted signals; and (b) the squares of the predicted signals, which are reconstructed from a previous estimate of the diffusion model parameters. The negative effect of weighting strategy (a) on the accuracy of the estimator was surprisingly high. Multi-step weighting strategies yield better performance and, in some cases, even outperformed the nonlinear least squares estimator. If proper weighting strategies are applied, the weighted linear least squares approach shows high performance characteristics in terms of accuracy/precision and may even be preferred over nonlinear estimation methods. Copyright © 2013 Elsevier Inc. All rights reserved.

An extended sequence specificity for UV-induced DNA damage.

PubMed

Chung, Long H; Murray, Vincent

2018-01-01

The sequence specificity of UV-induced DNA damage was determined with a higher precision and accuracy than previously reported. UV light induces two major damage adducts: cyclobutane pyrimidine dimers (CPDs) and pyrimidine(6-4)pyrimidone photoproducts (6-4PPs). Employing capillary electrophoresis with laser-induced fluorescence and taking advantages of the distinct properties of the CPDs and 6-4PPs, we studied the sequence specificity of UV-induced DNA damage in a purified DNA sequence using two approaches: end-labelling and a polymerase stop/linear amplification assay. A mitochondrial DNA sequence that contained a random nucleotide composition was employed as the target DNA sequence. With previous methodology, the UV sequence specificity was determined at a dinucleotide or trinucleotide level; however, in this paper, we have extended the UV sequence specificity to a hexanucleotide level. With the end-labelling technique (for 6-4PPs), the consensus sequence was found to be 5'-GCTC*AC (where C* is the breakage site); while with the linear amplification procedure, it was 5'-TCTT*AC. With end-labelling, the dinucleotide frequency of occurrence was highest for 5'-TC*, 5'-TT* and 5'-CC*; whereas it was 5'-TT* for linear amplification. The influence of neighbouring nucleotides on the degree of UV-induced DNA damage was also examined. The core sequences consisted of pyrimidine nucleotides 5'-CTC* and 5'-CTT* while an A at position "1" and C at position "2" enhanced UV-induced DNA damage. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.

Mechanism Underlying IκB Kinase Activation Mediated by the Linear Ubiquitin Chain Assembly Complex

PubMed Central

Fujita, Hiroaki; Akita, Mariko; Kato, Ryuichi; Sasaki, Yoshiteru; Wakatsuki, Soichi

2014-01-01

The linear ubiquitin chain assembly complex (LUBAC) ligase, consisting of HOIL-1L, HOIP, and SHARPIN, specifically generates linear polyubiquitin chains. LUBAC-mediated linear polyubiquitination has been implicated in NF-κB activation. NEMO, a component of the IκB kinase (IKK) complex, is a substrate of LUBAC, but the precise molecular mechanism underlying linear chain-mediated NF-κB activation has not been fully elucidated. Here, we demonstrate that linearly polyubiquitinated NEMO activates IKK more potently than unanchored linear chains. In mutational analyses based on the crystal structure of the complex between the HOIP NZF1 and NEMO CC2-LZ domains, which are involved in the HOIP-NEMO interaction, NEMO mutations that impaired linear ubiquitin recognition activity and prevented recognition by LUBAC synergistically suppressed signal-induced NF-κB activation. HOIP NZF1 bound to NEMO and ubiquitin simultaneously, and HOIP NZF1 mutants defective in interaction with either NEMO or ubiquitin could not restore signal-induced NF-κB activation. Furthermore, linear chain-mediated activation of IKK2 involved homotypic interaction of the IKK2 kinase domain. Collectively, these results demonstrate that linear polyubiquitination of NEMO plays crucial roles in IKK activation and that this modification involves the HOIP NZF1 domain and recognition of NEMO-conjugated linear ubiquitin chains by NEMO on another IKK complex. PMID:24469399

A methodology based on reduced complexity algorithm for system applications using microprocessors

NASA Technical Reports Server (NTRS)

Yan, T. Y.; Yao, K.

1988-01-01

The paper considers a methodology on the analysis and design of a minimum mean-square error criterion linear system incorporating a tapped delay line (TDL) where all the full-precision multiplications in the TDL are constrained to be powers of two. A linear equalizer based on the dispersive and additive noise channel is presented. This microprocessor implementation with optimized power of two TDL coefficients achieves a system performance comparable to the optimum linear equalization with full-precision multiplications for an input data rate of 300 baud.

Formation Control for the MAXIM Mission

NASA Technical Reports Server (NTRS)

Luquette, Richard J.; Leitner, Jesse; Gendreau, Keith; Sanner, Robert M.

2004-01-01

Over the next twenty years, a wave of change is occurring in the space-based scientific remote sensing community. While the fundamental limits in the spatial and angular resolution achievable in spacecraft have been reached, based on today s technology, an expansive new technology base has appeared over the past decade in the area of Distributed Space Systems (DSS). A key subset of the DSS technology area is that which covers precision formation flying of space vehicles. Through precision formation flying, the baselines, previously defined by the largest monolithic structure which could fit in the largest launch vehicle fairing, are now virtually unlimited. Several missions including the Micro-Arcsecond X-ray Imaging Mission (MAXIM), and the Stellar Imager will drive the formation flying challenges to achieve unprecedented baselines for high resolution, extended-scene, interferometry in the ultraviolet and X-ray regimes. This paper focuses on establishing the feasibility for the formation control of the MAXIM mission. MAXIM formation flying requirements are on the order of microns, while Stellar Imager mission requirements are on the order of nanometers. This paper specifically addresses: (1) high-level science requirements for these missions and how they evolve into engineering requirements; and (2) the development of linearized equations of relative motion for a formation operating in an n-body gravitational field. Linearized equations of motion provide the ground work for linear formation control designs.

Probing New Long-Range Interactions by Isotope Shift Spectroscopy

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

Berengut, Julian C.; Budker, Dmitry; Delaunay, Cédric

We explore a method to probe new long- and intermediate-range interactions using precision atomic isotope shift spectroscopy. We develop a formalism to interpret linear King plots as bounds on new physics with minimal theory inputs. We focus only on bounding the new physics contributions that can be calculated independently of the standard model nuclear effects. We apply our method to existing Ca + data and project its sensitivity to conjectured new bosons with spin-independent couplings to the electron and the neutron using narrow transitions in other atoms and ions, specifically, Sr and Yb. Future measurements are expected to improve themore » relative precision by 5 orders of magnitude, and they can potentially lead to an unprecedented sensitivity for bosons within the 0.3 to 10 MeV mass range.« less

Probing New Long-Range Interactions by Isotope Shift Spectroscopy.

PubMed

Berengut, Julian C; Budker, Dmitry; Delaunay, Cédric; Flambaum, Victor V; Frugiuele, Claudia; Fuchs, Elina; Grojean, Christophe; Harnik, Roni; Ozeri, Roee; Perez, Gilad; Soreq, Yotam

2018-03-02

We explore a method to probe new long- and intermediate-range interactions using precision atomic isotope shift spectroscopy. We develop a formalism to interpret linear King plots as bounds on new physics with minimal theory inputs. We focus only on bounding the new physics contributions that can be calculated independently of the standard model nuclear effects. We apply our method to existing Ca^{+} data and project its sensitivity to conjectured new bosons with spin-independent couplings to the electron and the neutron using narrow transitions in other atoms and ions, specifically, Sr and Yb. Future measurements are expected to improve the relative precision by 5 orders of magnitude, and they can potentially lead to an unprecedented sensitivity for bosons within the 0.3 to 10 MeV mass range.

Probing New Long-Range Interactions by Isotope Shift Spectroscopy

DOE PAGES

Berengut, Julian C.; Budker, Dmitry; Delaunay, Cédric; ...

2018-02-26

We explore a method to probe new long- and intermediate-range interactions using precision atomic isotope shift spectroscopy. We develop a formalism to interpret linear King plots as bounds on new physics with minimal theory inputs. We focus only on bounding the new physics contributions that can be calculated independently of the standard model nuclear effects. We apply our method to existing Ca + data and project its sensitivity to conjectured new bosons with spin-independent couplings to the electron and the neutron using narrow transitions in other atoms and ions, specifically, Sr and Yb. Future measurements are expected to improve themore » relative precision by 5 orders of magnitude, and they can potentially lead to an unprecedented sensitivity for bosons within the 0.3 to 10 MeV mass range.« less

Time-resolved optical spectrometer based on a monolithic array of high-precision TDCs and SPADs

NASA Astrophysics Data System (ADS)

Tamborini, Davide; Markovic, Bojan; Di Sieno, Laura; Contini, Davide; Bassi, Andrea; Tisa, Simone; Tosi, Alberto; Zappa, Franco

2013-12-01

We present a compact time-resolved spectrometer suitable for optical spectroscopy from 400 nm to 1 μm wavelengths. The detector consists of a monolithic array of 16 high-precision Time-to-Digital Converters (TDC) and Single-Photon Avalanche Diodes (SPAD). The instrument has 10 ps resolution and reaches 70 ps (FWHM) timing precision over a 160 ns full-scale range with a Differential Non-Linearity (DNL) better than 1.5 % LSB. The core of the spectrometer is the application-specific integrated chip composed of 16 pixels with 250 μm pitch, containing a 20 μm diameter SPAD and an independent TDC each, fabricated in a 0.35 μm CMOS technology. In front of this array a monochromator is used to focus different wavelengths into different pixels. The spectrometer has been used for fluorescence lifetime spectroscopy: 5 nm spectral resolution over an 80 nm bandwidth is achieved. Lifetime spectroscopy of Nile blue is demonstrated.

Morphologies of precise polyethylene-based acid copolymers and ionomers

NASA Astrophysics Data System (ADS)

Buitrago, C. Francisco

Acid copolymers and ionomers are polymers that contain a small fraction of covalently bound acidic or ionic groups, respectively. For the specific case of polyethylene (PE), acid and ionic pendants enhance many of the physical properties such as toughness, adhesion and rheological properties. These improved properties result from microphase separated aggregates of the polar pendants in the non-polar PE matrix. Despite the widespread industrial use of these materials, rigorous chemical structure---morphology---property relationships remain elusive due to the inevitable structural heterogeneities in the historically-available acid copolymers and ionomers. Recently, precise acid copolymers and ionomers were successfully synthesized by acyclic diene metathesis (ADMET) polymerization. These precise materials are linear, high molecular weight PEs with pendant acid or ionic functional groups separated by a precisely controlled number of carbon atoms. The morphologies of nine precise acid copolymers and eleven precise ionomers were investigated by X-ray scattering, solid-state 13C nuclear magnetic resonance (NMR) and differential scanning calorimetry (DSC). For comparison, the morphologies of linear PEs with pseudo-random placement of the pendant groups were also studied. Previous studies of precise copolymers with acrylic acid (AA) found that the microstructural precision produces a new morphology in which PE crystals drive the acid aggregates into layers perpendicular to the chain axes and presumably at the interface between crystalline and amorphous phases. In this dissertation, a second new morphology for acid copolymers is identified in which the aggregates arrange on cubic lattices. The fist report of a cubic morphology was observed at room and elevated temperatures for a copolymer functionalized with two phosphonic acid (PA) groups on every 21st carbon atom. The cubic lattice has been identified as face-centered cubic (FCC). Overall, three morphology types have been identified for precise acid copolymers and ionomers at room temperature: (1) liquid-like order of aggregates dispersed throughout an amorphous PE matrix, (2) one-dimensional long-range order of aggregates in layers coexisting with PE crystals, and (3) three-dimensional periodicity of aggregates in cubic lattices in a PE matrix featuring defective packing. The liquid-like morphology is a result of high content of acid or ionic substituents deterring PE crystallinity due to steric hindrance. The layered morphology occurs when the content of pendants is low and the PE segments are long enough to crystallize. The cubic morphologies occur in precise copolymers with geminal substitution of phosphonic acid (PA) groups and long, flexible PE segments. At temperatures above the thermal transitions of the PE matrix, all but one material present a liquid-like morphology. Those conditions are ideal to study the evolution of the interaggregate spacing (d*) in X-ray scattering as a function of PE segment length between pendants, pendant type and pendant architecture (specifically, mono or geminal substitution). Also at elevated temperatures, the morphologies of precise acrylic acid (AA) copolymers and ionomers were investigated further via atomistic molecular dynamics (MD) simulations. The simulations complement X-ray scattering by providing real space visualization of the aggregates, demonstrating the occurrence of isolated, string-like and even percolated aggregate structures. This is the first dissertation completely devoted to the morphology of precise acid copolymers and precise ionomers. The complete analysis of the morphologies in these novel materials provides new insights into the shapes of aggregates in acid copolymers and ionomers in general. A key aspect of this thesis is the complementary use of experimental and simulation methods to unlock a wealth of new understanding.

A phase match based frequency estimation method for sinusoidal signals

NASA Astrophysics Data System (ADS)

Shen, Yan-Lin; Tu, Ya-Qing; Chen, Lin-Jun; Shen, Ting-Ao

2015-04-01

Accurate frequency estimation affects the ranging precision of linear frequency modulated continuous wave (LFMCW) radars significantly. To improve the ranging precision of LFMCW radars, a phase match based frequency estimation method is proposed. To obtain frequency estimation, linear prediction property, autocorrelation, and cross correlation of sinusoidal signals are utilized. The analysis of computational complex shows that the computational load of the proposed method is smaller than those of two-stage autocorrelation (TSA) and maximum likelihood. Simulations and field experiments are performed to validate the proposed method, and the results demonstrate the proposed method has better performance in terms of frequency estimation precision than methods of Pisarenko harmonic decomposition, modified covariance, and TSA, which contribute to improving the precision of LFMCW radars effectively.

Precision Interval Estimation of the Response Surface by Means of an Integrated Algorithm of Neural Network and Linear Regression

NASA Technical Reports Server (NTRS)

Lo, Ching F.

1999-01-01

The integration of Radial Basis Function Networks and Back Propagation Neural Networks with the Multiple Linear Regression has been accomplished to map nonlinear response surfaces over a wide range of independent variables in the process of the Modem Design of Experiments. The integrated method is capable to estimate the precision intervals including confidence and predicted intervals. The power of the innovative method has been demonstrated by applying to a set of wind tunnel test data in construction of response surface and estimation of precision interval.

Quantification of endocrine disruptors and pesticides in water by gas chromatography-tandem mass spectrometry. Method validation using weighted linear regression schemes.

PubMed

Mansilha, C; Melo, A; Rebelo, H; Ferreira, I M P L V O; Pinho, O; Domingues, V; Pinho, C; Gameiro, P

2010-10-22

A multi-residue methodology based on a solid phase extraction followed by gas chromatography-tandem mass spectrometry was developed for trace analysis of 32 compounds in water matrices, including estrogens and several pesticides from different chemical families, some of them with endocrine disrupting properties. Matrix standard calibration solutions were prepared by adding known amounts of the analytes to a residue-free sample to compensate matrix-induced chromatographic response enhancement observed for certain pesticides. Validation was done mainly according to the International Conference on Harmonisation recommendations, as well as some European and American validation guidelines with specifications for pesticides analysis and/or GC-MS methodology. As the assumption of homoscedasticity was not met for analytical data, weighted least squares linear regression procedure was applied as a simple and effective way to counteract the greater influence of the greater concentrations on the fitted regression line, improving accuracy at the lower end of the calibration curve. The method was considered validated for 31 compounds after consistent evaluation of the key analytical parameters: specificity, linearity, limit of detection and quantification, range, precision, accuracy, extraction efficiency, stability and robustness. Copyright © 2010 Elsevier B.V. All rights reserved.

Reverse phase HPLC method for detection and quantification of lupin seed γ-conglutin.

PubMed

Mane, Sharmilee; Bringans, Scott; Johnson, Stuart; Pareek, Vishnu; Utikar, Ranjeet

2017-09-15

A simple, selective and accurate reverse phase HPLC method was developed for detection and quantitation of γ-conglutin from lupin seed extract. A linear gradient of water and acetonitrile containing trifluoroacetic acid (TFA) on a reverse phase column (Agilent Zorbax 300SB C-18), with a flow rate of 0.8ml/min was able to produce a sharp and symmetric peak of γ-conglutin with a retention time at 29.16min. The identity of γ-conglutin in the peak was confirmed by mass spectrometry (MS/MS identification) and sodium dodecyl sulphate polyacrylamide gel electrophoresis (SDS-PAGE) analysis. The data obtained from MS/MS analysis was matched against the specified database to obtain the exact match for the protein of interest. The proposed method was validated in terms of specificity, linearity, sensitivity, precision, recovery and accuracy. The analytical parameters revealed that the validated method was capable of selectively performing a good chromatographic separation of γ-conglutin from the lupin seed extract with no interference of the matrix. The detection and quantitation limit of γ-conglutin were found to be 2.68μg/ml and 8.12μg/ml respectively. The accuracy (precision and recovery) analysis of the method was conducted under repeatable conditions on different days. Intra-day and inter-day precision values less than 0.5% and recovery greater than 97% indicated high precision and accuracy of the method for analysis of γ-conglutin. The method validation findings were reproducible and can be successfully applied for routine analysis of γ-conglutin from lupin seed extract. Copyright © 2017 Elsevier B.V. All rights reserved.

Precision linear ramp function generator

DOEpatents

Jatko, W.B.; McNeilly, D.R.; Thacker, L.H.

1984-08-01

A ramp function generator is provided which produces a precise linear ramp function which is repeatable and highly stable. A derivative feedback loop is used to stabilize the output of an integrator in the forward loop and control the ramp rate. The ramp may be started from a selected baseline voltage level and the desired ramp rate is selected by applying an appropriate constant voltage to the input of the integrator.

Precision linear ramp function generator

DOEpatents

Jatko, W. Bruce; McNeilly, David R.; Thacker, Louis H.

1986-01-01

A ramp function generator is provided which produces a precise linear ramp unction which is repeatable and highly stable. A derivative feedback loop is used to stabilize the output of an integrator in the forward loop and control the ramp rate. The ramp may be started from a selected baseline voltage level and the desired ramp rate is selected by applying an appropriate constant voltage to the input of the integrator.

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

PubMed

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

2017-10-13

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

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

PubMed Central

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

2011-01-01

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

Simultaneous determination of triacetin, acetic ether, butyl acetate and amorolfine hydrochloride in amorolfine liniment by HPLC.

PubMed

Gao, Yuan; Li, Li; Zhang, Jianjun; Shu, Wenjuan; Gao, Liqiong

2012-04-01

A simple, rapid, specific and precise reversed-phase high-performance liquid chromatographic method was developed for simultaneous estimation of triacetin, acetic ether, butyl acetate and amorolfine in marketed pharmaceutical liniment. Chromatographic separation was performed on a Shimadzu VP-ODS C(18) column using the mixture of citric acid-hydrochloric acid-sodium hydrate buffer (pH 3.0), acetonitrile and methanol (32:30:38) as the mobile phase at a flow rate of 1.0 mL/min with UV-detection at 215 nm. The method separated the four components simultaneously in less than 10 min. The validation of the method was performed with respect to specificity, linearity, accuracy, and precision. The calibration curves were linear in the range of 35.1-81.9 μ/mL for triacetin, 431.1-1005.9 μ/mL for acetic ether, 167.0-389.7 μ/mL for butyl acetate and 151.0-352.3 μ/mL for amorolfine. The mean 100% spiked recovery for triacetin, acetic ether, butyl acetate and amorolfine is 99.43 ± 0.42, 101.5 ± 1.09, 101.4 ± 1.02 and 100.8 ± 0.69, respectively. The intra-day and inter-day relative standard deviation values were <2.0%. The limits of detection of these compounds ranged from 0.08 to 5.88 ng. The utility of the procedure was verified by its application to the commercial liniment.

Development and validation of sensitive LC/MS/MS method for quantitative bioanalysis of levonorgestrel in rat plasma and application to pharmacokinetics study.

PubMed

Ananthula, Suryatheja; Janagam, Dileep R; Jamalapuram, Seshulatha; Johnson, James R; Mandrell, Timothy D; Lowe, Tao L

2015-10-15

Rapid, sensitive, selective and accurate LC/MS/MS method was developed for quantitative determination of levonorgestrel (LNG) in rat plasma and further validated for specificity, linearity, accuracy, precision, sensitivity, matrix effect, recovery efficiency and stability. Liquid-liquid extraction procedure using hexane:ethyl acetate mixture at 80:20 v:v ratio was employed to efficiently extract LNG from rat plasma. Reversed phase Luna column C18(2) (50×2.0mm i.d., 3μM) installed on a AB SCIEX Triple Quad™ 4500 LC/MS/MS system was used to perform chromatographic separation. LNG was identified within 2min with high specificity. Linear calibration curve was drawn within 0.5-50ng·mL(-1) concentration range. The developed method was validated for intra-day and inter-day accuracy and precision whose values fell in the acceptable limits. Matrix effect was found to be minimal. Recovery efficiency at three quality control (QC) concentrations 0.5 (low), 5 (medium) and 50 (high) ng·mL(-1) was found to be >90%. Stability of LNG at various stages of experiment including storage, extraction and analysis was evaluated using QC samples, and the results showed that LNG was stable at all the conditions. This validated method was successfully used to study the pharmacokinetics of LNG in rats after SubQ injection, providing its applicability in relevant preclinical studies. Copyright © 2015 Elsevier B.V. All rights reserved.

The compression–error trade-off for large gridded data sets

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

Silver, Jeremy D.; Zender, Charles S.

The netCDF-4 format is widely used for large gridded scientific data sets and includes several compression methods: lossy linear scaling and the non-lossy deflate and shuffle algorithms. Many multidimensional geoscientific data sets exhibit considerable variation over one or several spatial dimensions (e.g., vertically) with less variation in the remaining dimensions (e.g., horizontally). On such data sets, linear scaling with a single pair of scale and offset parameters often entails considerable loss of precision. We introduce an alternative compression method called "layer-packing" that simultaneously exploits lossy linear scaling and lossless compression. Layer-packing stores arrays (instead of a scalar pair) of scalemore » and offset parameters. An implementation of this method is compared with lossless compression, storing data at fixed relative precision (bit-grooming) and scalar linear packing in terms of compression ratio, accuracy and speed. When viewed as a trade-off between compression and error, layer-packing yields similar results to bit-grooming (storing between 3 and 4 significant figures). Bit-grooming and layer-packing offer significantly better control of precision than scalar linear packing. Relative performance, in terms of compression and errors, of bit-groomed and layer-packed data were strongly predicted by the entropy of the exponent array, and lossless compression was well predicted by entropy of the original data array. Layer-packed data files must be "unpacked" to be readily usable. The compression and precision characteristics make layer-packing a competitive archive format for many scientific data sets.« less

The compression–error trade-off for large gridded data sets

DOE PAGES

Silver, Jeremy D.; Zender, Charles S.

2017-01-27

The netCDF-4 format is widely used for large gridded scientific data sets and includes several compression methods: lossy linear scaling and the non-lossy deflate and shuffle algorithms. Many multidimensional geoscientific data sets exhibit considerable variation over one or several spatial dimensions (e.g., vertically) with less variation in the remaining dimensions (e.g., horizontally). On such data sets, linear scaling with a single pair of scale and offset parameters often entails considerable loss of precision. We introduce an alternative compression method called "layer-packing" that simultaneously exploits lossy linear scaling and lossless compression. Layer-packing stores arrays (instead of a scalar pair) of scalemore » and offset parameters. An implementation of this method is compared with lossless compression, storing data at fixed relative precision (bit-grooming) and scalar linear packing in terms of compression ratio, accuracy and speed. When viewed as a trade-off between compression and error, layer-packing yields similar results to bit-grooming (storing between 3 and 4 significant figures). Bit-grooming and layer-packing offer significantly better control of precision than scalar linear packing. Relative performance, in terms of compression and errors, of bit-groomed and layer-packed data were strongly predicted by the entropy of the exponent array, and lossless compression was well predicted by entropy of the original data array. Layer-packed data files must be "unpacked" to be readily usable. The compression and precision characteristics make layer-packing a competitive archive format for many scientific data sets.« less

NCLscan: accurate identification of non-co-linear transcripts (fusion, trans-splicing and circular RNA) with a good balance between sensitivity and precision.

PubMed

Chuang, Trees-Juen; Wu, Chan-Shuo; Chen, Chia-Ying; Hung, Li-Yuan; Chiang, Tai-Wei; Yang, Min-Yu

2016-02-18

Analysis of RNA-seq data often detects numerous 'non-co-linear' (NCL) transcripts, which comprised sequence segments that are topologically inconsistent with their corresponding DNA sequences in the reference genome. However, detection of NCL transcripts involves two major challenges: removal of false positives arising from alignment artifacts and discrimination between different types of NCL transcripts (trans-spliced, circular or fusion transcripts). Here, we developed a new NCL-transcript-detecting method ('NCLscan'), which utilized a stepwise alignment strategy to almost completely eliminate false calls (>98% precision) without sacrificing true positives, enabling NCLscan outperform 18 other publicly-available tools (including fusion- and circular-RNA-detecting tools) in terms of sensitivity and precision, regardless of the generation strategy of simulated dataset, type of intragenic or intergenic NCL event, read depth of coverage, read length or expression level of NCL transcript. With the high accuracy, NCLscan was applied to distinguishing between trans-spliced, circular and fusion transcripts on the basis of poly(A)- and nonpoly(A)-selected RNA-seq data. We showed that circular RNAs were expressed more ubiquitously, more abundantly and less cell type-specifically than trans-spliced and fusion transcripts. Our study thus describes a robust pipeline for the discovery of NCL transcripts, and sheds light on the fundamental biology of these non-canonical RNA events in human transcriptome. © The Author(s) 2015. Published by Oxford University Press on behalf of Nucleic Acids Research.

Purity assessment of recombinant human granulocyte colony-stimulating factor in finished drug product by capillary zone electrophoresis.

PubMed

Benković, Goran; Skrlin, Ana; Madić, Tomislav; Debeljak, Zeljko; Medić-Šarić, Marica

2014-09-01

Current methods for determination of impurities with different charge-to-volume ratio are limited especially in terms of sensitivity and precision. The main goal of this research was to establish a quantitative method for determination of impurities with charges differing from that of recombinant human granulocyte colony-stimulating factor (rhG-CSF, filgrastim) with superior precision and sensitivity compared to existing methods. A CZE method has been developed, optimized, and validated for a purity assessment of filgrastim in liquid pharmaceutical formulations. Optimal separation of filgrastim from the related impurities with different charges was achieved on a 50 μm id fused-silica capillary of a total length of 80.5 cm. A BGE that contains 100 mM phosphoric acid adjusted to pH 7.0 with triethanolamine was used. The applied voltage was 20 kV while the temperature was maintained at 25°C. UV detection was set to 200 nm. Method was validated in terms of selectivity/specificity, linearity, precision, LOD, LOQ, stability, and robustness. Linearity was observed in the concentration range of 6-600 μg/mL and the LOQ was determined to be 0.3% relative to the concentration of filgrastim of 0.6 mg/mL. Other validation parameters were also found to be acceptable; thus the method was successfully applied for a quantitative purity assessment of filgrastim in a finished drug product. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A rapid method for the simultaneous determination of 25 anti-hypertensive compounds in dietary supplements using ultra-high-pressure liquid chromatography.

PubMed

Heo, Seok; Yoo, Geum Joo; Choi, Ji Yeon; Park, Hyoung Joon; Park, Sung-Kwan; Baek, Sun Young

2016-11-01

A novel, stable, simple and specific ultra-performance liquid chromatography method with ultraviolet detection (205 nm) for the simultaneous analysis of 25 anti-hypertensive substances was developed. The method was validated according to the International Conference of Harmonisation guidelines with respect to linearity, accuracy, precision, limit of detection (LOD), limit of quantitation (LOQ) and stability. From the ultra-performance liquid chromatography results, we identified the LOD and LOQ of solid samples to be 0.20-1.00 and 0.60-3.00 μg ml -1 , respectively, while those of liquid samples were 0.30-1.20 and 0.90-3.60 μg ml -1 , respectively. The linearity exceeded 0.9999, and the intra- and inter-day precisions were 0.15-6.48% and 0.28-8.67%, respectively. The intra- and inter-day accuracies were 82.25-111.42% and 80.70-115.64%, respectively, and the stability was lower than 12.9% (relative standard deviation). This method was applied to the monitoring of 97 commercially available dietary supplements obtained in Korea, such as pills, soft capsules, hard capsules, liquids, powders and tablets. The proposed method is accurate, precise and of high quality, and can be used for the routine, reproducible analysis and control of 25 anti-hypertensive substances in various dietary supplements. The work presented herein may help to prevent incidents related to food adulteration and restrict the illegal food market.

Standardisation of DNA quantitation by image analysis: quality control of instrumentation.

PubMed

Puech, M; Giroud, F

1999-05-01

DNA image analysis is frequently performed in clinical practice as a prognostic tool and to improve diagnosis. The precision of prognosis and diagnosis depends on the accuracy of analysis and particularly on the quality of image analysis systems. It has been reported that image analysis systems used for DNA quantification differ widely in their characteristics (Thunissen et al.: Cytometry 27: 21-25, 1997). This induces inter-laboratory variations when the same sample is analysed in different laboratories. In microscopic image analysis, the principal instrumentation errors arise from the optical and electronic parts of systems. They bring about problems of instability, non-linearity, and shading and glare phenomena. The aim of this study is to establish tools and standardised quality control procedures for microscopic image analysis systems. Specific reference standard slides have been developed to control instability, non-linearity, shading and glare phenomena and segmentation efficiency. Some systems have been controlled with these tools and these quality control procedures. Interpretation criteria and accuracy limits of these quality control procedures are proposed according to the conclusions of a European project called PRESS project (Prototype Reference Standard Slide). Beyond these limits, tested image analysis systems are not qualified to realise precise DNA analysis. The different procedures presented in this work determine if an image analysis system is qualified to deliver sufficiently precise DNA measurements for cancer case analysis. If the controlled systems are beyond the defined limits, some recommendations are given to find a solution to the problem.

Validation of an enzyme-linked immunosorbent assay for the quantification of citrullinated histone H3 as a marker for neutrophil extracellular traps in human plasma.

PubMed

Thålin, Charlotte; Daleskog, Maud; Göransson, Sophie Paues; Schatzberg, Daphne; Lasselin, Julie; Laska, Ann-Charlotte; Kallner, Anders; Helleday, Thomas; Wallén, Håkan; Demers, Mélanie

2017-06-01

There is an emerging interest in the diverse functions of neutrophil extracellular traps (NETs) in a variety of disease settings. However, data on circulating NETs rely largely upon surrogate NET markers such as cell-free DNA, nucleosomes, and NET-associated enzymes. Citrullination of histone H3 by peptidyl arginine deiminase 4 (PAD4) is central for NET formation, and citrullinated histone H3 (H3Cit) is considered a NET-specific biomarker. We therefore aimed to optimize and validate a new enzyme-linked immunosorbent assay (ELISA) to quantify the levels of H3Cit in human plasma. A standard curve made of in vitro PAD4-citrullinated histones H3 allows for the quantification of H3Cit in plasma using an anti-histone antibody as capture antibody and an anti-histone H3 citrulline antibody for detection. The assay was evaluated for linearity, stability, specificity, and precision on plasma samples obtained from a human model of inflammation before and after lipopolysaccharide injection. The results revealed linearity and high specificity demonstrated by the inability of detecting non-citrullinated histone H3. Coefficients of variation for intra- and inter-assay variability ranged from 2.1 to 5.1% and from 5.8 to 13.5%, respectively, allowing for a high precision. Furthermore, our results support an inflammatory induction of a systemic NET burden by showing, for the first time, clear intra-individual elevations of plasma H3Cit in a human model of lipopolysaccharide-induced inflammation. Taken together, our work demonstrates the development of a new method for the quantification of H3Cit by ELISA that can reliably be used for the detection of NETs in human plasma.

Microhartree precision in density functional theory calculations

NASA Astrophysics Data System (ADS)

Gulans, Andris; Kozhevnikov, Anton; Draxl, Claudia

2018-04-01

To address ultimate precision in density functional theory calculations we employ the full-potential linearized augmented plane-wave + local-orbital (LAPW + lo) method and justify its usage as a benchmark method. LAPW + lo and two completely unrelated numerical approaches, the multiresolution analysis (MRA) and the linear combination of atomic orbitals, yield total energies of atoms with mean deviations of 0.9 and 0.2 μ Ha , respectively. Spectacular agreement with the MRA is reached also for total and atomization energies of the G2-1 set consisting of 55 molecules. With the example of α iron we demonstrate the capability of LAPW + lo to reach μ Ha /atom precision also for periodic systems, which allows also for the distinction between the numerical precision and the accuracy of a given functional.

Optimization and qualification of an Fc Array assay for assessments of antibodies against HIV-1/SIV.

PubMed

Brown, Eric P; Weiner, Joshua A; Lin, Shu; Natarajan, Harini; Normandin, Erica; Barouch, Dan H; Alter, Galit; Sarzotti-Kelsoe, Marcella; Ackerman, Margaret E

2018-04-01

The Fc Array is a multiplexed assay that assesses the Fc domain characteristics of antigen-specific antibodies with the potential to evaluate up to 500 antigen specificities simultaneously. Antigen-specific antibodies are captured on antigen-conjugated beads and their functional capacity is probed via an array of Fc-binding proteins including antibody subclassing reagents, Fcγ receptors, complement proteins, and lectins. Here we present the results of the optimization and formal qualification of the Fc Array, performed in compliance with Good Clinical Laboratory Practice (GCLP) guidelines. Assay conditions were optimized for performance and reproducibility, and the final version of the assay was then evaluated for specificity, accuracy, precision, limits of detection and quantitation, linearity, range and robustness. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

Lack of transferability between two automated immunoassays for serum IGF-I measurement.

PubMed

Gomez-Gomez, Carolina; Iglesias, Eva M; Barallat, Jaume; Moreno, Fernando; Biosca, Carme; Pastor, Mari-Cruz; Granada, Maria-Luisa

2014-01-01

IGF-I is a clinically relevant protein in the diagnosis and monitoring of treatment of growth disor- ders. The Growth Hormone Research Society and the International IGF Research Society have encouraged the adoption of a universal calibration for immunoassays to improve standardization of IGF-I measurements, but currently commercial assays are calibrated either against the old WHO IRR 87/518 or the new WHO 02/254. We compared two IGF-I immunochemiluminescent assays: IMMULITE® 2000 (Siemens) and LIAISON® (DiaSorin), which differ in their standardization, and verified their precision according to quality specifications based on biological variation and their linear range. 62 patient serum samples were analyzed for both assays and compared according to standards of the Clinical and Laboratory Standards Institute (CLSI), EP9-A2-IR. Precision was verified according to CLSI EP15- A2. Optimal coefficient of variation (CVo) and desirable coefficient of variation (CVd) for IGF-I assays were calculated as quality specifications based on the biological variability, in order to assess if the interassay analytical CV (CVa1) in the two methods were appropriate. Two dilution series using the 1st WHO International Standard (WHO IS) for IGF-I 02/254 were used to verify and compare the linearity range. The regression analysis showed constant and proportional differences for serum samples (slope b = 0.8115 (CI 95% CI; 0.7575-0.8556); intercept a = 33.6873 (95% CI: 23.3613-44.0133) between assays and similar pro- portional differences for WHO IS 02/254 standard dilutions series (slope b = 0.8024 (CI 95% CI; 0.7560-0.8616); intercept a = 6.9623 (95% CI: -2.0819-18.4383) between assays. Within-laboratory coefficients of variation for low and high levels were 2.82% and 3.80% for IMMULITE® 2000 and 3.58% and 2.14% for LIAISON®, respecttively. IGF-I concentrations measured by both assays are not transferable. The results emphasize the need to express IGF-I concentrations in standard deviation score (SDS) according to a matched normal population of the same age and gender. Within-laboratory precision in both methods met quality specifications derived from biological variation.

Tri-axial tactile sensing element

NASA Astrophysics Data System (ADS)

Castellanos-Ramos, Julián.; Navas-González, Rafael; Vidal-Verdú, F.

2013-05-01

A 13 x 13 square millimetre tri-axial taxel is presented which is suitable for some medical applications, for instance in assistive robotics that involves contact with humans or in prosthetics. Finite Element Analysis is carried out to determine what structure is the best to obtain a uniform distribution of pressure on the sensing areas underneath the structure. This structure has been fabricated in plastic with a 3D printer and a commercial tactile sensor has been used to implement the sensing areas. A three axis linear motorized translation stage with a tri-axial precision force sensor is used to find the parameters of the linear regression model and characterize the proposed taxel. The results are analysed to see to what extent the goal has been reached in this specific implementation.

Group delay variations of GPS transmitting and receiving antennas

NASA Astrophysics Data System (ADS)

Wanninger, Lambert; Sumaya, Hael; Beer, Susanne

2017-09-01

GPS code pseudorange measurements exhibit group delay variations at the transmitting and the receiving antenna. We calibrated C1 and P2 delay variations with respect to dual-frequency carrier phase observations and obtained nadir-dependent corrections for 32 satellites of the GPS constellation in early 2015 as well as elevation-dependent corrections for 13 receiving antenna models. The combined delay variations reach up to 1.0 m (3.3 ns) in the ionosphere-free linear combination for specific pairs of satellite and receiving antennas. Applying these corrections to the code measurements improves code/carrier single-frequency precise point positioning, ambiguity fixing based on the Melbourne-Wübbena linear combination, and determination of ionospheric total electron content. It also affects fractional cycle biases and differential code biases.

Precise measurement of coupling strength and high temperature quantum effect in a nonlinearly coupled qubit-oscillator system

NASA Astrophysics Data System (ADS)

Ge, Li; Zhao, Nan

2018-04-01

We study the coherence dynamics of a qubit coupled to a harmonic oscillator with both linear and quadratic interactions. As long as the linear coupling strength is much smaller than the oscillator frequency, the long time behavior of the coherence is dominated by the quadratic coupling strength g 2. The coherence decays and revives at a period , with the width of coherence peak decreasing as the temperature increases, hence providing a way to measure g 2 precisely without cooling. Unlike the case of linear coupling, here the coherence dynamics never reduces to the classical limit in which the oscillator is classical. Finally, the validity of linear coupling approximation is discussed and the coherence under Hahn-echo is evaluated.

Digital Simulation Of Precise Sensor Degradations Including Non-Linearities And Shift Variance

NASA Astrophysics Data System (ADS)

Kornfeld, Gertrude H.

1987-09-01

Realistic atmospheric and Forward Looking Infrared Radiometer (FLIR) degradations were digitally simulated. Inputs to the routine are environmental observables and the FLIR specifications. It was possible to achieve realism in the thermal domain within acceptable computer time and random access memory (RAM) requirements because a shift variant recursive convolution algorithm that well describes thermal properties was invented and because each picture element (pixel) has radiative temperature, a materials parameter and range and altitude information. The computer generation steps start with the image synthesis of an undegraded scene. Atmospheric and sensor degradation follow. The final result is a realistic representation of an image seen on the display of a specific FLIR.

Quantum-inspired algorithm for estimating the permanent of positive semidefinite matrices

NASA Astrophysics Data System (ADS)

Chakhmakhchyan, L.; Cerf, N. J.; Garcia-Patron, R.

2017-08-01

We construct a quantum-inspired classical algorithm for computing the permanent of Hermitian positive semidefinite matrices by exploiting a connection between these mathematical structures and the boson sampling model. Specifically, the permanent of a Hermitian positive semidefinite matrix can be expressed in terms of the expected value of a random variable, which stands for a specific photon-counting probability when measuring a linear-optically evolved random multimode coherent state. Our algorithm then approximates the matrix permanent from the corresponding sample mean and is shown to run in polynomial time for various sets of Hermitian positive semidefinite matrices, achieving a precision that improves over known techniques. This work illustrates how quantum optics may benefit algorithm development.

Influence of the air’s refractive index on precision angle metrology with autocollimators

NASA Astrophysics Data System (ADS)

Geckeler, Ralf D.; Křen, Petr; Just, Andreas; Schumann, Matthias; Krause, Michael

2018-07-01

In this paper, we discuss a substantial—though previously neglected—error source in precision metrology with autocollimators, specifically, changes in the air’s refractive index, with a focus on the dominant impact of pressure changes. Pressure decreases with increasing elevation above sea level and is subject to substantial variation due to weather changes. It causes changes in an autocollimator’s angle response which are proportional to the measured angle and which increase linearly with the beam length and air pressure. We characterise this important influence in detail by using extended theoretical and experimental investigations and derive strategies for correcting it. We discuss its implications for the comparison of autocollimator calibrations performed at different metrology institutes which is crucial for validating their calibration capabilities. This work aims at approaching fundamental limits in angle metrology with autocollimators.

A creatinine biosensor based on admittance measurement

NASA Astrophysics Data System (ADS)

Ching, Congo Tak-Shing; Sun, Tai-Ping; Jheng, Deng-Yun; Tsai, Hou-Wei; Shieh, Hsiu-Li

2015-08-01

Regular check of blood creatinine level is very important as it is a measurement of renal function. Therefore, the objective of this study is to develop a simple and reliable creatinine biosensor based on admittance measurement for precise determination of creatinine. The creatinine biosensor was fabricated with creatinine deiminase immobilized on screen-printed carbon electrodes. Admittance measurement at a specific frequency ranges (22.80 - 84.71 Hz) showed that the biosensor has an excellent linear (r2 > 0.95) response range (50 - 250 uM), which covers the normal physiological and pathological ranges of blood creatinine levels. Intraclass correlation coefficient (ICC) showed that the biosensor has excellent reliability and validity (ICC = 0.98). In conclusion, a simple and reliable creatinine biosensor was developed and it is capable of precisely determining blood creatinine levels in both the normal physiological and pathological ranges.

The Fermi-Pasta-Ulam Problem and Its Underlying Integrable Dynamics: An Approach Through Lyapunov Exponents

NASA Astrophysics Data System (ADS)

Benettin, G.; Pasquali, S.; Ponno, A.

2018-05-01

FPU models, in dimension one, are perturbations either of the linear model or of the Toda model; perturbations of the linear model include the usual β -model, perturbations of Toda include the usual α +β model. In this paper we explore and compare two families, or hierarchies, of FPU models, closer and closer to either the linear or the Toda model, by computing numerically, for each model, the maximal Lyapunov exponent χ . More precisely, we consider statistically typical trajectories and study the asymptotics of χ for large N (the number of particles) and small ɛ (the specific energy E / N), and find, for all models, asymptotic power laws χ ˜eq Cɛ ^a, C and a depending on the model. The asymptotics turns out to be, in general, rather slow, and producing accurate results requires a great computational effort. We also revisit and extend the analytic computation of χ introduced by Casetti, Livi and Pettini, originally formulated for the β -model. With great evidence the theory extends successfully to all models of the linear hierarchy, but not to models close to Toda.

Complexity in estimation of esomeprazole and its related impurities' stability in various stress conditions in low-dose aspirin and esomeprazole magnesium capsules.

PubMed

Reddy, Palavai Sripal; Hotha, Kishore Kumar; Sait, Shakil

2013-01-01

A complex, sensitive, and precise high-performance liquid chromatographic method for the profiling of impurities of esomeprazole in low-dose aspirin and esomeprazole capsules has been developed, validated, and used for the determination of impurities in pharmaceutical products. Esomeprazole and its related impurities' development in the presence of aspirin was traditionally difficult due to aspirin's sensitivity to basic conditions and esomeprazole's sensitivity to acidic conditions. When aspirin is under basic, humid, and extreme temperature conditions, it produces salicylic acid and acetic acid moieties. These two byproducts create an acidic environment for the esomeprazole. Due to the volatility and migration phenomenon of the produced acetic acid and salicylic acid from aspirin in the capsule dosage form, esomeprazole's purity, stability, and quantification are affected. The objective of the present research work was to develop a gradient reversed-phase liquid chromatographic method to separate all the degradation products and process-related impurities from the main peak. The impurities were well-separated on a RP8 column (150 mm × 4.6mm, X-terra, RP8, 3.5μm) by the gradient program using a glycine buffer (0.08 M, pH adjusted to 9.0 with 50% NaOH), acetonitrile, and methanol at a flow rate of 1.0 mL min(-1) with detection wavelength at 305 nm and column temperature at 30°C. The developed method was found to be specific, precise, linear, accurate, rugged, and robust. LOQ values for all of the known impurities were below reporting thresholds. The drug was subjected to stress conditions of hydrolysis, oxidation, photolysis, and thermal degradation in the presence of aspirin. The developed RP-HPLC method was validated according to the present ICH guidelines for specificity, linearity, accuracy, precision, limit of detection, limit of quantification, ruggedness, and robustness.

voom: precision weights unlock linear model analysis tools for RNA-seq read counts

PubMed Central

2014-01-01

New normal linear modeling strategies are presented for analyzing read counts from RNA-seq experiments. The voom method estimates the mean-variance relationship of the log-counts, generates a precision weight for each observation and enters these into the limma empirical Bayes analysis pipeline. This opens access for RNA-seq analysts to a large body of methodology developed for microarrays. Simulation studies show that voom performs as well or better than count-based RNA-seq methods even when the data are generated according to the assumptions of the earlier methods. Two case studies illustrate the use of linear modeling and gene set testing methods. PMID:24485249

voom: Precision weights unlock linear model analysis tools for RNA-seq read counts.

PubMed

Law, Charity W; Chen, Yunshun; Shi, Wei; Smyth, Gordon K

2014-02-03

New normal linear modeling strategies are presented for analyzing read counts from RNA-seq experiments. The voom method estimates the mean-variance relationship of the log-counts, generates a precision weight for each observation and enters these into the limma empirical Bayes analysis pipeline. This opens access for RNA-seq analysts to a large body of methodology developed for microarrays. Simulation studies show that voom performs as well or better than count-based RNA-seq methods even when the data are generated according to the assumptions of the earlier methods. Two case studies illustrate the use of linear modeling and gene set testing methods.

The research of radar target tracking observed information linear filter method

NASA Astrophysics Data System (ADS)

Chen, Zheng; Zhao, Xuanzhi; Zhang, Wen

2018-05-01

Aiming at the problems of low precision or even precision divergent is caused by nonlinear observation equation in radar target tracking, a new filtering algorithm is proposed in this paper. In this algorithm, local linearization is carried out on the observed data of the distance and angle respectively. Then the kalman filter is performed on the linearized data. After getting filtered data, a mapping operation will provide the posteriori estimation of target state. A large number of simulation results show that this algorithm can solve above problems effectively, and performance is better than the traditional filtering algorithm for nonlinear dynamic systems.

Linear signal noise summer accurately determines and controls S/N ratio

NASA Technical Reports Server (NTRS)

Sundry, J. L.

1966-01-01

Linear signal noise summer precisely controls the relative power levels of signal and noise, and mixes them linearly in accurately known ratios. The S/N ratio accuracy and stability are greatly improved by this technique and are attained simultaneously.

Sample Introduction Using the Hildebrand Grid Nebulizer for Plasma Spectrometry

DTIC Science & Technology

1988-01-01

linear dynamic ranges, precision, and peak width were de- termined for elements in methanol and acetonitrile solutions. , (1)> The grid nebulizer was...FIA) with ICP-OES detection were evaluated. Detec- tion limits, linear dynamic ranges, precision, and peak width were de- termined for elements in...Concentration vs. Log Peak Area for Mn, 59 Cd, Zn, Au, Ni in Methanol (CMSC) 3-28 Log Concentration vs. Log Peak Area for Mn, 60 Cd, Au, Ni in

Linear Covariance Analysis for a Lunar Lander

NASA Technical Reports Server (NTRS)

Jang, Jiann-Woei; Bhatt, Sagar; Fritz, Matthew; Woffinden, David; May, Darryl; Braden, Ellen; Hannan, Michael

2017-01-01

A next-generation lunar lander Guidance, Navigation, and Control (GNC) system, which includes a state-of-the-art optical sensor suite, is proposed in a concept design cycle. The design goal is to allow the lander to softly land within the prescribed landing precision. The achievement of this precision landing requirement depends on proper selection of the sensor suite. In this paper, a robust sensor selection procedure is demonstrated using a Linear Covariance (LinCov) analysis tool developed by Draper.

Sedimentation of knotted polymers

NASA Astrophysics Data System (ADS)

Piili, J.; Marenduzzo, D.; Kaski, K.; Linna, R. P.

2013-01-01

We investigate the sedimentation of knotted polymers by means of stochastic rotation dynamics, a molecular dynamics algorithm that takes hydrodynamics fully into account. We show that the sedimentation coefficient s, related to the terminal velocity of the knotted polymers, increases linearly with the average crossing number nc of the corresponding ideal knot. This provides direct computational confirmation of this relation, postulated on the basis of sedimentation experiments by Rybenkov [J. Mol. Biol.10.1006/jmbi.1996.0876 267, 299 (1997)]. Such a relation was previously shown to hold with simulations for knot electrophoresis. We also show that there is an accurate linear dependence of s on the inverse of the radius of gyration Rg-1, more specifically with the inverse of the Rg component that is perpendicular to the direction along which the polymer sediments. When the polymer sediments in a slab, the walls affect the results appreciably. However, Rg-1 remains to a good precision linearly dependent on nc. Therefore, Rg-1 is a good measure of a knot's complexity.

Fractal geometry of music.

PubMed Central

Hsü, K J; Hsü, A J

1990-01-01

Music critics have compared Bach's music to the precision of mathematics. What "mathematics" and what "precision" are the questions for a curious scientist. The purpose of this short note is to suggest that the mathematics is, at least in part, Mandelbrot's fractal geometry and the precision is the deviation from a log-log linear plot. PMID:11607061

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.

Programmable DNA scaffolds for spatially-ordered protein assembly

NASA Astrophysics Data System (ADS)

Chandrasekaran, Arun Richard

2016-02-01

Ever since the notion of using DNA as a material was realized, it has been employed in the construction of complex structures that facilitate the assembly of nanoparticles or macromolecules with nanometer-scale precision. Specifically, tiles fashioned from DNA strands and DNA origami sheets have been shown to be suitable as scaffolds for immobilizing proteins with excellent control over their spatial positioning. Supramolecular assembly of proteins into periodic arrays in one or more dimensions is one of the most challenging aspects in the design of scaffolds for biomolecular investigations and macromolecular crystallization. This review provides a brief overview of how various biomolecular interactions with high degree of specificity such as streptavidin-biotin, antigen-antibody, and aptamer-protein interactions have been used to fabricate linear and multidimensional assemblies of structurally intact and functional proteins. The use of DNA-binding proteins as adaptors, polyamide recognition on DNA scaffolds and oligonucleotide linkers for protein assembly are also discussed.Ever since the notion of using DNA as a material was realized, it has been employed in the construction of complex structures that facilitate the assembly of nanoparticles or macromolecules with nanometer-scale precision. Specifically, tiles fashioned from DNA strands and DNA origami sheets have been shown to be suitable as scaffolds for immobilizing proteins with excellent control over their spatial positioning. Supramolecular assembly of proteins into periodic arrays in one or more dimensions is one of the most challenging aspects in the design of scaffolds for biomolecular investigations and macromolecular crystallization. This review provides a brief overview of how various biomolecular interactions with high degree of specificity such as streptavidin-biotin, antigen-antibody, and aptamer-protein interactions have been used to fabricate linear and multidimensional assemblies of structurally intact and functional proteins. The use of DNA-binding proteins as adaptors, polyamide recognition on DNA scaffolds and oligonucleotide linkers for protein assembly are also discussed. Dedicated to my advisor Ned Seeman on the occasion of his 70th birthday.

Positioner with long travel in two dimensions

DOEpatents

Trumper, David L.; Williams, Mark E.

1997-12-23

A precision positioning system is provided which provides long travel in two of the linear dimensions, while using non-contact bearings for both a first subassembly which provides long travel in one of the linear dimension and a second subassembly which provides long travel in the second linear dimension. The first or upper subassembly is preferably a magnetic subassembly which, in addition to providing long travel, also compensates or positions in three rotary dimensions and in the third linear dimension. The second subassembly is preferably either an air bearing or magnetic subassembly and is normally used only to provide long travel. Angled surfaces may be provided for magnetic bearings and capacitive or other gap sensing probes may be mounted to the stage and ground flush with the bearing actuators to provide more precise gap measurements.

A comparative study of smart spectrophotometric methods for simultaneous determination of a skeletal muscle relaxant and an analgesic in combined dosage form

NASA Astrophysics Data System (ADS)

Salem, Hesham; Mohamed, Dalia

2015-04-01

Six simple, specific, accurate and precise spectrophotometric methods were developed and validated for the simultaneous determination of the analgesic drug; paracetamol (PARA) and the skeletal muscle relaxant; dantrolene sodium (DANT). Three methods are manipulating ratio spectra namely; ratio difference (RD), ratio subtraction (RS) and mean centering (MC). The other three methods are utilizing the isoabsorptive point either at zero order namely; absorbance ratio (AR) and absorbance subtraction (AS) or at ratio spectrum namely; amplitude modulation (AM). The proposed spectrophotometric procedures do not require any preliminary separation step. The accuracy, precision and linearity ranges of the proposed methods were determined. The selectivity of the developed methods was investigated by analyzing laboratory prepared mixtures of the drugs and their combined dosage form. Standard deviation values are less than 1.5 in the assay of raw materials and capsules. The obtained results were statistically compared with each other and with those of reported spectrophotometric ones. The comparison showed that there is no significant difference between the proposed methods and the reported methods regarding both accuracy and precision.

Complex thiolated mannose/quinone film modified on EQCM/Au electrode for recognizing specific carbohydrate-proteins.

PubMed

Zeng, Hongjuan; Yu, Junsheng; Jiang, Yadong; Zeng, Xiangqun

2014-05-15

A complex thiolated mannose (TM)/quinone functionalised polythiophene (QFPT) thin film was modified on EQCM/Au electrode for recognition of specific carbohydrate-proteins. Different lectins such as those from Sambucus nigra (elder berry), Arachis hypogaea (peanut), Ulex europaeus (gorse, furze), Triticum vulgaris and Concanavalin A (ConA) was used for probes to evaluate bio-sensing performance of the TM/QFPT film. A specific response was observed for ConA from lectins when using the TM/QFPT film as sensing material and employing either elelctrochemical or the QCM method. No response was detected between thiolated mannose and other lectins. The linear relationship between current and ConA concentration is in the range of 0.5-17.5 nM by the elelctrochemical method and the linear relationship between frequency change and ConA concentration is in the range of 0.5-4.5 nM by the QCM method. This shows that the TM/QFPT-modified EQCM biosensor presents a paralleled determination by using electrochemical and the QCM method. The elelctrochemical method of the biosensor can be applicable in a large concentration range and its frequency change can be more precise. © 2013 Published by Elsevier B.V.

Verification of spectrophotometric method for nitrate analysis in water samples

NASA Astrophysics Data System (ADS)

Kurniawati, Puji; Gusrianti, Reny; Dwisiwi, Bledug Bernanti; Purbaningtias, Tri Esti; Wiyantoko, Bayu

2017-12-01

The aim of this research was to verify the spectrophotometric method to analyze nitrate in water samples using APHA 2012 Section 4500 NO3-B method. The verification parameters used were: linearity, method detection limit, level of quantitation, level of linearity, accuracy and precision. Linearity was obtained by using 0 to 50 mg/L nitrate standard solution and the correlation coefficient of standard calibration linear regression equation was 0.9981. The method detection limit (MDL) was defined as 0,1294 mg/L and limit of quantitation (LOQ) was 0,4117 mg/L. The result of a level of linearity (LOL) was 50 mg/L and nitrate concentration 10 to 50 mg/L was linear with a level of confidence was 99%. The accuracy was determined through recovery value was 109.1907%. The precision value was observed using % relative standard deviation (%RSD) from repeatability and its result was 1.0886%. The tested performance criteria showed that the methodology was verified under the laboratory conditions.

A Very Fast and Angular Momentum Conserving Tree Code

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

Marcello, Dominic C., E-mail: dmarce504@gmail.com

There are many methods used to compute the classical gravitational field in astrophysical simulation codes. With the exception of the typically impractical method of direct computation, none ensure conservation of angular momentum to machine precision. Under uniform time-stepping, the Cartesian fast multipole method of Dehnen (also known as the very fast tree code) conserves linear momentum to machine precision. We show that it is possible to modify this method in a way that conserves both angular and linear momenta.

A precision isotonic measuring system for isolated tissues.

PubMed

Mellor, P M

1984-12-01

An isotonic measuring system is described which utilizes an angular position transducer of the linear differential voltage transformer type. Resistance to corrosion, protection against the ingress of solutions, and ease of mounting and setting up were the mechanical objectives. Accuracy, linearity, and freedom from drift were essential requirements of the electrical specification. A special housing was designed to accommodate the transducer to overcome these problems. A control unit incorporating a power supply and electronic filtering components was made to serve up to four such transducers. The transducer output voltage is sufficiently high to drive directly even low sensitivity chart recorders. Constructional details and a circuit diagram are included. Fifty such transducers have been in use for up to four years in these laboratories. Examples of some of the published work done using this transducer system are referenced.

Using linear algebra for protein structural comparison and classification

PubMed Central

2009-01-01

In this article, we describe a novel methodology to extract semantic characteristics from protein structures using linear algebra in order to compose structural signature vectors which may be used efficiently to compare and classify protein structures into fold families. These signatures are built from the pattern of hydrophobic intrachain interactions using Singular Value Decomposition (SVD) and Latent Semantic Indexing (LSI) techniques. Considering proteins as documents and contacts as terms, we have built a retrieval system which is able to find conserved contacts in samples of myoglobin fold family and to retrieve these proteins among proteins of varied folds with precision of up to 80%. The classifier is a web tool available at our laboratory website. Users can search for similar chains from a specific PDB, view and compare their contact maps and browse their structures using a JMol plug-in. PMID:21637532

Using linear algebra for protein structural comparison and classification.

PubMed

Gomide, Janaína; Melo-Minardi, Raquel; Dos Santos, Marcos Augusto; Neshich, Goran; Meira, Wagner; Lopes, Júlio César; Santoro, Marcelo

2009-07-01

In this article, we describe a novel methodology to extract semantic characteristics from protein structures using linear algebra in order to compose structural signature vectors which may be used efficiently to compare and classify protein structures into fold families. These signatures are built from the pattern of hydrophobic intrachain interactions using Singular Value Decomposition (SVD) and Latent Semantic Indexing (LSI) techniques. Considering proteins as documents and contacts as terms, we have built a retrieval system which is able to find conserved contacts in samples of myoglobin fold family and to retrieve these proteins among proteins of varied folds with precision of up to 80%. The classifier is a web tool available at our laboratory website. Users can search for similar chains from a specific PDB, view and compare their contact maps and browse their structures using a JMol plug-in.

Simultaneous Determination of Eight Hypotensive Drugs of Various Chemical Groups in Pharmaceutical Preparations by HPLC-DAD.

PubMed

Stolarczyk, Mariusz; Hubicka, Urszula; Żuromska-Witek, Barbara; Krzek, Jan

2015-01-01

A new sensitive, simple, rapid, and precise HPLC method with diode array detection has been developed for separation and simultaneous determination of hydrochlorothiazide, furosemide, torasemide, losartane, quinapril, valsartan, spironolactone, and canrenone in combined pharmaceutical dosage forms. The chromatographic analysis of the tested drugs was performed on an ACE C18, 100 Å, 250×4.6 mm, 5 μm particle size column with 0.0.05 M phosphate buffer (pH=3.00)-acetonitrile-methanol (30+20+50 v/v/v) mobile phase at a flow rate of 1.0 mL/min. The column was thermostatted at 25°C. UV detection was performed at 230 nm. Analysis time was 10 min. The elaborated method meets the acceptance criteria for specificity, linearity, sensitivity, accuracy, and precision. The proposed method was successfully applied for the determination of the studied drugs in the selected combined dosage forms.

Three different spectrophotometric methods manipulating ratio spectra for determination of binary mixture of Amlodipine and Atorvastatin

NASA Astrophysics Data System (ADS)

Darwish, Hany W.; Hassan, Said A.; Salem, Maissa Y.; El-Zeiny, Badr A.

2011-12-01

Three simple, specific, accurate and precise spectrophotometric methods manipulating ratio spectra are developed for the simultaneous determination of Amlodipine besylate (AM) and Atorvastatin calcium (AT) in tablet dosage forms. The first method is first derivative of the ratio spectra ( 1DD), the second is ratio subtraction and the third is the method of mean centering of ratio spectra. The calibration curve is linear over the concentration range of 3-40 and 8-32 μg/ml for AM and AT, respectively. These methods are tested by analyzing synthetic mixtures of the above drugs and they are applied to commercial pharmaceutical preparation of the subjected drugs. Standard deviation is <1.5 in the assay of raw materials and tablets. Methods are validated as per ICH guidelines and accuracy, precision, repeatability and robustness are found to be within the acceptable limit.

Three different methods for determination of binary mixture of Amlodipine and Atorvastatin using dual wavelength spectrophotometry

NASA Astrophysics Data System (ADS)

Darwish, Hany W.; Hassan, Said A.; Salem, Maissa Y.; El-Zeany, Badr A.

2013-03-01

Three simple, specific, accurate and precise spectrophotometric methods depending on the proper selection of two wavelengths are developed for the simultaneous determination of Amlodipine besylate (AML) and Atorvastatin calcium (ATV) in tablet dosage forms. The first method is the new Ratio Difference method, the second method is the Bivariate method and the third one is the Absorbance Ratio method. The calibration curve is linear over the concentration range of 4-40 and 8-32 μg/mL for AML and ATV, respectively. These methods are tested by analyzing synthetic mixtures of the above drugs and they are applied to commercial pharmaceutical preparation of the subjected drugs. Methods are validated according to the ICH guidelines and accuracy, precision, repeatability and robustness are found to be within the acceptable limit. The mathematical explanation of the procedures is illustrated.

Approach to method development and validation in capillary electrophoresis for enantiomeric purity testing of active basic pharmaceutical ingredients.

PubMed

Sokoliess, Torsten; Köller, Gerhard

2005-06-01

A chiral capillary electrophoresis system allowing the determination of the enantiomeric purity of an investigational new drug was developed using a generic method development approach for basic analytes. The method was optimized in terms of type and concentration of both cyclodextrin (CD) and electrolyte, buffer pH, temperature, voltage, and rinsing procedure. Optimal chiral separation of the analyte was obtained using an electrolyte with 2.5% carboxymethyl-beta-CD in 25 mM NaH2PO4 (pH 4.0). Interchanging the inlet and outlet vials after each run improved the method's precision. To assure the method's suitability for the control of enantiomeric impurities in pharmaceutical quality control, its specificity, linearity, precision, accuracy, and robustness were validated according to the requirements of the International Conference on Harmonization. The usefulness of our generic method development approach for the validation of robustness was demonstrated.

Design of the 15 GHz BPM test bench for the CLIC test facility to perform precise stretched-wire RF measurements

NASA Astrophysics Data System (ADS)

Zorzetti, Silvia; Fanucci, Luca; Galindo Muñoz, Natalia; Wendt, Manfred

2015-09-01

The Compact Linear Collider (CLIC) requires a low emittance beam transport and preservation, thus a precise control of the beam orbit along up to 50 km of the accelerator components in the sub-μm regime is required. Within the PACMAN3 (Particle Accelerator Components Metrology and Alignment to the Nanometer Scale) PhD training action a study with the objective of pre-aligning the electrical centre of a 15 GHz cavity beam position monitor (BPM) to the magnetic centre of the main beam quadrupole is initiated. Of particular importance is the design of a specific test bench to study the stretched-wire setup for the CLIC Test Facility (CTF3) BPM, focusing on the aspects of microwave signal excitation, transmission and impedance-matching, as well as the mechanical setup and reproducibility of the measurement method.

Development and Analytical Validation of an Immunoassay for Quantifying Serum Anti-Pertussis Toxin Antibodies Resulting from Bordetella pertussis Infection ▿

PubMed Central

Menzies, Sandra L.; Kadwad, Vijay; Pawloski, Lucia C.; Lin, Tsai-Lien; Baughman, Andrew L.; Martin, Monte; Tondella, Maria Lucia C.; Meade, Bruce D.

2009-01-01

Adequately sensitive and specific methods to diagnose pertussis in adolescents and adults are not widely available. Currently, no Food and Drug Administration-approved diagnostic assays are available for the serodiagnosis of Bordetella pertussis. Since concentrations of B. pertussis-specific antibodies tend to be high during the later phases of disease, a simple, rapid, easily transferable serodiagnostic test was developed. This article describes test development, initial evaluation of a prototype kit enzyme-linked immunosorbent assay (ELISA) in an interlaboratory collaborative study, and analytical validation. The data presented here demonstrate that the kit met all prespecified criteria for precision, linearity, and accuracy for samples with anti-pertussis toxin (PT) immunoglobulin G (IgG) antibody concentrations in the range of 50 to 150 ELISA units (EU)/ml, the range believed to be most relevant for serodiagnosis. The assay met the precision and linearity criteria for a wider range, namely, from 50 to 200 EU/ml; however, the accuracy criterion was not met at 200 EU/ml. When the newly adopted World Health Organization International Standard for pertussis antiserum (human) reference reagent was used to evaluate accuracy, the accuracy criteria were met from 50 to 200 international units/ml. In conclusion, the IgG anti-PT ELISA met all assay validation parameters within the range considered most relevant for serodiagnosis. This ELISA was developed and analytically validated as a user-friendly kit that can be used in both qualitative and quantitative formats. The technology for producing the kit is transferable to public health laboratories. PMID:19864485

Performance characteristics of an ion chromatographic method for the quantitation of citrate and phosphate in pharmaceutical solutions.

PubMed

Jenke, Dennis; Sadain, Salma; Nunez, Karen; Byrne, Frances

2007-01-01

The performance of an ion chromatographic method for measuring citrate and phosphate in pharmaceutical solutions is evaluated. Performance characteristics examined include accuracy, precision, specificity, response linearity, robustness, and the ability to meet system suitability criteria. In general, the method is found to be robust within reasonable deviations from its specified operating conditions. Analytical accuracy is typically 100 +/- 3%, and short-term precision is not more than 1.5% relative standard deviation. The instrument response is linear over a range of 50% to 150% of the standard preparation target concentrations (12 mg/L for phosphate and 20 mg/L for citrate), and the results obtained using a single-point standard versus a calibration curve are essentially equivalent. A small analytical bias is observed and ascribed to the relative purity of the differing salts, used as raw materials in tested finished products and as reference standards in the analytical method. The assay is specific in that no phosphate or citrate peaks are observed in a variety of method-related solutions and matrix blanks (with and without autoclaving). The assay with manual preparation of the eluents is sensitive to the composition of the eluent in the sense that the eluent must be effectively degassed and protected from CO(2) ingress during use. In order for the assay to perform effectively, extensive system equilibration and conditioning is required. However, a properly conditioned and equilibrated system can be used to test a number of samples via chromatographic runs that include many (> 50) injections.

Use of Longitudinal Data in Genetic Studies in the Genome-wide Association Studies Era: Summary of Group 14

PubMed Central

Kerner, Berit; North, Kari E; Fallin, M Daniele

2010-01-01

Participants analyzed actual and simulated longitudinal data from the Framingham Heart Study for various metabolic and cardiovascular traits. The genetic information incorporated into these investigations ranged from selected single-nucleotide polymorphisms to genome-wide association arrays. Genotypes were incorporated using a broad range of methodological approaches including conditional logistic regression, linear mixed models, generalized estimating equations, linear growth curve estimation, growth modeling, growth mixture modeling, population attributable risk fraction based on survival functions under the proportional hazards models, and multivariate adaptive splines for the analysis of longitudinal data. The specific scientific questions addressed by these different approaches also varied, ranging from a more precise definition of the phenotype, bias reduction in control selection, estimation of effect sizes and genotype associated risk, to direct incorporation of genetic data into longitudinal modeling approaches and the exploration of population heterogeneity with regard to longitudinal trajectories. The group reached several overall conclusions: 1) The additional information provided by longitudinal data may be useful in genetic analyses. 2) The precision of the phenotype definition as well as control selection in nested designs may be improved, especially if traits demonstrate a trend over time or have strong age-of-onset effects. 3) Analyzing genetic data stratified for high-risk subgroups defined by a unique development over time could be useful for the detection of rare mutations in common multi-factorial diseases. 4) Estimation of the population impact of genomic risk variants could be more precise. The challenges and computational complexity demanded by genome-wide single-nucleotide polymorphism data were also discussed. PMID:19924713

Evaluation of automated assays for immunoglobulin G, M, and A measurements in dog and cat serum.

PubMed

Tvarijonaviciute, Asta; Martínez-Subiela, Silvia; Caldin, Marco; Tecles, Fernando; Ceron, Jose J

2013-09-01

Measurements of immunoglobulins (Igs) in companion animals can be useful to detect deficiencies of the humoral immune system, that can be associated with opportunistic or chronic infections, or other immune-mediated disorders including B-cell neoplasms. The purpose of this study was to evaluate commercially available automated immunoturbidimetric assays designed for human IgG, M, and A measurements in canine and feline serum using species-specific calibrators. Canine and feline serum samples with different IgG, M, and A concentrations were used for the analytical validation of the assays. Intra- and inter-assay precision, linearity under dilution, spiking recovery, and limit of detection were determined. In addition, effects of lipemia, hemolysis, and bilirubinemia were evaluated. Finally, Ig concentrations were determined in small groups of diseased dogs and cats, and compared with healthy groups. Spiking recovery and linearity under dilution tests showed that the assays measured Igs in canine and feline serum samples precisely and accurately. Intra- and inter-assay imprecisions were lower than 15% in all cases. Significantly higher IgG, IgM, and IgA levels were observed in dogs with leishmaniasis, while dogs with pyometra showed a statistically significant increase in IgM and IgA concentrations in comparison with healthy dogs. Significantly higher IgG and IgM levels were observed in FIV-infected cats compared with healthy ones. The automated human Ig assays showed adequate precision and accuracy with serum samples from dogs and cats. Also, they were able to discriminate different concentrations of Igs in healthy and diseased animals. © 2013 American Society for Veterinary Clinical Pathology.

Precision Control of Multiple Quantum Cascade Lasers for Calibration Systems

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

Taubman, Matthew S.; Myers, Tanya L.; Pratt, Richard M.

We present a precision, digitally interfaced current controller for quantum cascade lasers, with demonstrated DC and modulated temperature coefficients of 1- 2 ppm/ºC and 15 ppm/ºC respectively. High linearity digital to analog converters (DACs) together with an ultra-precision voltage reference, produce highly stable, precision voltages. These are in turn selected by a low charge-injection multiplexer (MUX) chip, which are then used to set output currents via a linear current regulator. The controller is operated in conjunction with a power multiplexing unit, allowing one of three lasers to be driven by the controller while ensuring protection of controller and all lasersmore » during operation, standby and switching. Simple ASCII commands sent over a USB connection to a microprocessor located in the current controller operate both the controller (via the DACs and MUX chip) and the power multiplexer.« less

Improved measurement linearity and precision for AMCW time-of-flight range imaging cameras.

PubMed

Payne, Andrew D; Dorrington, Adrian A; Cree, Michael J; Carnegie, Dale A

2010-08-10

Time-of-flight range imaging systems utilizing the amplitude modulated continuous wave (AMCW) technique often suffer from measurement nonlinearity due to the presence of aliased harmonics within the amplitude modulation signals. Typically a calibration is performed to correct these errors. We demonstrate an alternative phase encoding approach that attenuates the harmonics during the sampling process, thereby improving measurement linearity in the raw measurements. This mitigates the need to measure the system's response or calibrate for environmental changes. In conjunction with improved linearity, we demonstrate that measurement precision can also be increased by reducing the duty cycle of the amplitude modulated illumination source (while maintaining overall illumination power).

Comparison of linear and nonlinear implementation of the compartmental tissue uptake model for dynamic contrast-enhanced MRI.

PubMed

Kallehauge, Jesper F; Sourbron, Steven; Irving, Benjamin; Tanderup, Kari; Schnabel, Julia A; Chappell, Michael A

2017-06-01

Fitting tracer kinetic models using linear methods is much faster than using their nonlinear counterparts, although this comes often at the expense of reduced accuracy and precision. The aim of this study was to derive and compare the performance of the linear compartmental tissue uptake (CTU) model with its nonlinear version with respect to their percentage error and precision. The linear and nonlinear CTU models were initially compared using simulations with varying noise and temporal sampling. Subsequently, the clinical applicability of the linear model was demonstrated on 14 patients with locally advanced cervical cancer examined with dynamic contrast-enhanced magnetic resonance imaging. Simulations revealed equal percentage error and precision when noise was within clinical achievable ranges (contrast-to-noise ratio >10). The linear method was significantly faster than the nonlinear method, with a minimum speedup of around 230 across all tested sampling rates. Clinical analysis revealed that parameters estimated using the linear and nonlinear CTU model were highly correlated (ρ ≥ 0.95). The linear CTU model is computationally more efficient and more stable against temporal downsampling, whereas the nonlinear method is more robust to variations in noise. The two methods may be used interchangeably within clinical achievable ranges of temporal sampling and noise. Magn Reson Med 77:2414-2423, 2017. © 2016 The Authors Magnetic Resonance in Medicine published by Wiley Periodicals, Inc. on behalf of International Society for Magnetic Resonance in Medicine. This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited. © 2016 The Authors Magnetic Resonance in Medicine published by Wiley Periodicals, Inc. on behalf of International Society for Magnetic Resonance in Medicine.

Measuring changes in Plasmodium falciparum transmission: Precision, accuracy and costs of metrics

PubMed Central

Tusting, Lucy S.; Bousema, Teun; Smith, David L.; Drakeley, Chris

2016-01-01

As malaria declines in parts of Africa and elsewhere, and as more countries move towards elimination, it is necessary to robustly evaluate the effect of interventions and control programmes on malaria transmission. To help guide the appropriate design of trials to evaluate transmission-reducing interventions, we review eleven metrics of malaria transmission, discussing their accuracy, precision, collection methods and costs, and presenting an overall critique. We also review the non-linear scaling relationships between five metrics of malaria transmission; the entomological inoculation rate, force of infection, sporozoite rate, parasite rate and the basic reproductive number, R0. Our review highlights that while the entomological inoculation rate is widely considered the gold standard metric of malaria transmission and may be necessary for measuring changes in transmission in highly endemic areas, it has limited precision and accuracy and more standardised methods for its collection are required. In areas of low transmission, parasite rate, sero-conversion rates and molecular metrics including MOI and mFOI may be most appropriate. When assessing a specific intervention, the most relevant effects will be detected by examining the metrics most directly affected by that intervention. Future work should aim to better quantify the precision and accuracy of malaria metrics and to improve methods for their collection. PMID:24480314

Simultaneous quantification of paracetamol, acetylsalicylic acid and papaverine with a validated HPLC method.

PubMed

Kalmár, Eva; Gyuricza, Anett; Kunos-Tóth, Erika; Szakonyi, Gerda; Dombi, György

2014-01-01

Combined drug products have the advantages of better patient compliance and possible synergic effects. The simultaneous application of several active ingredients at a time is therefore frequently chosen. However, the quantitative analysis of such medicines can be challenging. The aim of this study is to provide a validated method for the investigation of a multidose packed oral powder that contained acetylsalicylic acid, paracetamol and papaverine-HCl. Reversed-phase high-pressure liquid chromatography was used. The Agilent Zorbax SB-C18 column was found to be the most suitable of the three different stationary phases tested for the separation of the components of this sample. The key parameters in the method development (apart from the nature of the column) were the pH of the aqueous phase (set to 3.4) and the ratio of the organic (acetonitrile) and the aqueous (25 mM phosphate buffer) phases, which was varied from 7:93 (v/v) to 25:75 (v/v) in a linear gradient, preceded by an initial hold. The method was validated: linearity, precision (repeatability and intermediate precision), accuracy, specificity and robustness were all tested, and the results met the ICH guidelines. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Identifiability of PBPK Models with Applications to ...

EPA Pesticide Factsheets

Any statistical model should be identifiable in order for estimates and tests using it to be meaningful. We consider statistical analysis of physiologically-based pharmacokinetic (PBPK) models in which parameters cannot be estimated precisely from available data, and discuss different types of identifiability that occur in PBPK models and give reasons why they occur. We particularly focus on how the mathematical structure of a PBPK model and lack of appropriate data can lead to statistical models in which it is impossible to estimate at least some parameters precisely. Methods are reviewed which can determine whether a purely linear PBPK model is globally identifiable. We propose a theorem which determines when identifiability at a set of finite and specific values of the mathematical PBPK model (global discrete identifiability) implies identifiability of the statistical model. However, we are unable to establish conditions that imply global discrete identifiability, and conclude that the only safe approach to analysis of PBPK models involves Bayesian analysis with truncated priors. Finally, computational issues regarding posterior simulations of PBPK models are discussed. The methodology is very general and can be applied to numerous PBPK models which can be expressed as linear time-invariant systems. A real data set of a PBPK model for exposure to dimethyl arsinic acid (DMA(V)) is presented to illustrate the proposed methodology. We consider statistical analy

Microbiological assay for the analysis of certain macrolides in pharmaceutical dosage forms.

PubMed

Mahmoudi, A; Fourar, R E-A; Boukhechem, M S; Zarkout, S

2015-08-01

Clarithromycin (CLA) and roxithromycin (ROX) are macrolide antibiotics with an expanded spectrum of activity that are commercially available as tablets. A microbiological assay, applying the cylinder-plate method and using a strain of Micrococcus luteus ATCC 9341 as test organism, has been used and validated for the quantification of two macrolide drugs; CLA and ROX in pure and pharmaceutical formulations. The validation of the proposed method was carried out for linearity, precision, accuracy and specificity. The linear dynamic ranges were from 0.1 to 0.5μg/mL for both compounds. Logarithmic calibration curve was obtained for each macrolide (r>0.989) with statistically equal slopes varying from 3.275 to 4.038, and a percentage relative standard deviation in the range of 0.24-0.92%. Moreover, the method was applied successfully for the assay of the studied drugs in pharmaceutical tablet dosage forms. Recovery from standard addition experiments in commercial products was 94.71-96.91% regarding clarithromycin and 93.94-98.12% regarding roxithromycin, with a precision (%RSD) 1.32-2.11%. Accordingly, this microbiological assay can be used for routine quality control analysis of titled drugs in tablet formulations. Copyright © 2015 Elsevier B.V. All rights reserved.

Development and validation of a reversed-phase HPLC method for simultaneous estimation of ambroxol hydrochloride and azithromycin in tablet dosage form.

PubMed

Shaikh, K A; Patil, S D; Devkhile, A B

2008-12-15

A simple, precise and accurate reversed-phase liquid chromatographic method has been developed for the simultaneous estimation of ambroxol hydrochloride and azithromycin in tablet formulations. The chromatographic separation was achieved on a Xterra RP18 (250 mm x 4.6 mm, 5 microm) analytical column. A Mixture of acetonitrile-dipotassium phosphate (30 mM) (50:50, v/v) (pH 9.0) was used as the mobile phase, at a flow rate of 1.7 ml/min and detector wavelength at 215 nm. The retention time of ambroxol and azithromycin was found to be 5.0 and 11.5 min, respectively. The validation of the proposed method was carried out for specificity, linearity, accuracy, precision, limit of detection, limit of quantitation and robustness. The linear dynamic ranges were from 30-180 to 250-1500 microg/ml for ambroxol hydrochloride and azithromycin, respectively. The percentage recovery obtained for ambroxol hydrochloride and azithromycin were 99.40 and 99.90%, respectively. Limit of detection and quantification for azithromycin were 0.8 and 2.3 microg/ml, for ambroxol hydrochloride 0.004 and 0.01 microg/ml, respectively. The developed method can be used for routine quality control analysis of titled drugs in combination in tablet formulation.

N-nitrosamines as "special case" leachables in a metered dose inhaler drug product.

PubMed

Norwood, Daniel L; Mullis, James O; Feinberg, Thomas N; Davis, Letha K

2009-01-01

N-nitrosamines are chemical entities, some of which are considered to be possible human carcinogens, which can be found at trace levels in some types of foods, tobacco smoke, certain cosmetics, and certain types of rubber. N-nitrosamines are of regulatory concern as leachables in inhalation drug products, particularly metered dose inhalers, which incorporate rubber seals into their container closure systems. The United States Food and Drug Administration considers N-nitrosamines (along with polycyclic aromatic hydrocarbons and 2-mercaptobenzothiazole) to be "special case" leachables in inhalation drug products, meaning that there are no recognized safety or analytical thresholds and these compounds must therefore be identified and quantitated at the lowest practical level. This report presents the development of a quantitative analytical method for target volatile N-nitrosamines in a metered dose inhaler drug product, Atrovent HFA. The method incorporates a target analyte recovery procedure from the drug product matrix with analysis by gas chromatography/thermal energy analysis detection. The capability of the method was investigated with respect to specificity, linearity/range, accuracy (linearity of recovery), precision (repeatability, intermediate precision), limits of quantitation, standard/sample stability, and system suitability. Sample analyses showed that Atrovent HFA contains no target N-nitrosamines at the trace level of 1 ng/canister.

Rivaroxaban Levels in Patients' Plasmas are Comparable by Using Two Different Anti Xa Assay/Coagulometer Systems Calibrated with Two Different Calibrators.

PubMed

Martinuzzo, Marta E; Duboscq, Cristina; Lopez, Marina S; Barrera, Luis H; Vinuales, Estela S; Ceresetto, Jose; Forastiero, Ricardo R; Oyhamburu, Jose

2018-06-01

Rivaroxaban oral anticoagulant does not need laboratory monitoring, but in some situations plasma level measurement is useful. The objective of this paper was to verify analytical performance and compare two rivaroxaban calibrated anti Xa assays/coagulometer systems with specific or other branch calibrators. In 59 samples drawn at trough or peak from patients taking rivaroxaban, plasma levels were measured by HemosIL Liquid anti Xa in ACLTOP 300/500, and STA liquid Anti Xa in TCoag Destiny Plus. HemosIL and STA rivaroxaban calibrators and controls were used. CLSI guideline procedures EP15A3 for precision and trueness, EP6 for linearity, and EP9 for methods comparison were used. Coefficient of variation within run and total precision (CVR and CVWL respectively) of plasmatic rivaroxaban were < 4.2 and < 4.85% and BIAS < 7.4 and < 6.5%, for HemosIL-ACL TOP and STA-Destiny systems, respectively. Linearity verification 8 - 525 ng/mL a Deming regression for methods comparison presented R 0.963, 0.968 and 0.982, with a mean CV 13.3% when using different systems and calibrations. The analytical performance of plasma rivaroxaban was acceptable in both systems, and results from reagent/coagulometer systems are comparable even when calibrating with different branch material.

Clinical laboratory urine analysis: comparison of the UriSed automated microscopic analyzer and the manual microscopy.

PubMed

Ma, Junlong; Wang, Chengbin; Yue, Jiaxin; Li, Mianyang; Zhang, Hongrui; Ma, Xiaojing; Li, Xincui; Xue, Dandan; Qing, Xiaoyan; Wang, Shengjiang; Xiang, Daijun; Cong, Yulong

2013-01-01

Several automated urine sediment analyzers have been introduced to clinical laboratories. Automated microscopic pattern recognition is a new technique for urine particle analysis. We evaluated the analytical and diagnostic performance of the UriSed automated microscopic analyzer and compared with manual microscopy for urine sediment analysis. Precision, linearity, carry-over, and method comparison were carried out. A total of 600 urine samples sent for urinalysis were assessed using the UriSed automated microscopic analyzer and manual microscopy. Within-run and between-run precision of the UriSed for red blood cells (RBC) and white blood cells (WBC) were acceptable at all levels (CV < 20%). Within-run and between-run imprecision of the UriSed testing for cast, squamous epithelial cells (EPI), and bacteria (BAC) were good at middle level and high level (CV < 20%). The linearity analysis revealed substantial agreement between the measured value and the theoretical value of the UriSed for RBC, WBC, cast, EPI, and BAC (r > 0.95). There was no carry-over. RBC, WBC, and squamous epithelial cells with sensitivities and specificities were more than 80% in this study. There is substantial agreement between the UriSed automated microscopic analyzer and the manual microscopy methods. The UriSed provides for a rapid turnaround time.

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.

Validation and Uncertainty Estimation of an Ecofriendly and Stability-Indicating HPLC Method for Determination of Diltiazem in Pharmaceutical Preparations

PubMed Central

Sadeghi, Fahimeh; Navidpour, Latifeh; Bayat, Sima; Afshar, Minoo

2013-01-01

A green, simple, and stability-indicating RP-HPLC method was developed for the determination of diltiazem in topical preparations. The separation was based on a C18 analytical column using a mobile phase consisted of ethanol: phosphoric acid solution (pH = 2.5) (35 : 65, v/v). Column temperature was set at 50°C and quantitation was achieved with UV detection at 240 nm. In forced degradation studies, the drug was subjected to oxidation, hydrolysis, photolysis, and heat. The method was validated for specificity, selectivity, linearity, precision, accuracy, and robustness. The applied procedure was found to be linear in diltiazem concentration range of 0.5–50 μg/mL (r 2 = 0.9996). Precision was evaluated by replicate analysis in which % relative standard deviation (RSD) values for areas were found below 2.0. The recoveries obtained (99.25%–101.66%) ensured the accuracy of the developed method. The degradation products as well as the pharmaceutical excipients were well resolved from the pure drug. The expanded uncertainty (5.63%) of the method was also estimated from method validation data. Accordingly, the proposed validated and sustainable procedure was proved to be suitable for routine analyzing and stability studies of diltiazem in pharmaceutical preparations. PMID:24163778

Integrated Analytic and Linearized Inverse Kinematics for Precise Full Body Interactions

NASA Astrophysics Data System (ADS)

Boulic, Ronan; Raunhardt, Daniel

Despite the large success of games grounded on movement-based interactions the current state of full body motion capture technologies still prevents the exploitation of precise interactions with complex environments. This paper focuses on ensuring a precise spatial correspondence between the user and the avatar. We build upon our past effort in human postural control with a Prioritized Inverse Kinematics framework. One of its key advantage is to ease the dynamic combination of postural and collision avoidance constraints. However its reliance on a linearized approximation of the problem makes it vulnerable to the well-known full extension singularity of the limbs. In such context the tracking performance is reduced and/or less believable intermediate postural solutions are produced. We address this issue by introducing a new type of analytic constraint that smoothly integrates within the prioritized Inverse Kinematics framework. The paper first recalls the background of full body 3D interactions and the advantages and drawbacks of the linearized IK solution. Then the Flexion-EXTension constraint (FLEXT in short) is introduced for the partial position control of limb-like articulated structures. Comparative results illustrate the interest of this new type of integrated analytical and linearized IK control.

The fastclime Package for Linear Programming and Large-Scale Precision Matrix Estimation in R.

PubMed

Pang, Haotian; Liu, Han; Vanderbei, Robert

2014-02-01

We develop an R package fastclime for solving a family of regularized linear programming (LP) problems. Our package efficiently implements the parametric simplex algorithm, which provides a scalable and sophisticated tool for solving large-scale linear programs. As an illustrative example, one use of our LP solver is to implement an important sparse precision matrix estimation method called CLIME (Constrained L 1 Minimization Estimator). Compared with existing packages for this problem such as clime and flare, our package has three advantages: (1) it efficiently calculates the full piecewise-linear regularization path; (2) it provides an accurate dual certificate as stopping criterion; (3) it is completely coded in C and is highly portable. This package is designed to be useful to statisticians and machine learning researchers for solving a wide range of problems.

Comparative artificial neural network and partial least squares models for analysis of Metronidazole, Diloxanide, Spiramycin and Cliquinol in pharmaceutical preparations.

PubMed

Elkhoudary, Mahmoud M; Abdel Salam, Randa A; Hadad, Ghada M

2014-09-15

Metronidazole (MNZ) is a widely used antibacterial and amoebicide drug. Therefore, it is important to develop a rapid and specific analytical method for the determination of MNZ in mixture with Spiramycin (SPY), Diloxanide (DIX) and Cliquinol (CLQ) in pharmaceutical preparations. This work describes simple, sensitive and reliable six multivariate calibration methods, namely linear and nonlinear artificial neural networks preceded by genetic algorithm (GA-ANN) and principle component analysis (PCA-ANN) as well as partial least squares (PLS) either alone or preceded by genetic algorithm (GA-PLS) for UV spectrophotometric determination of MNZ, SPY, DIX and CLQ in pharmaceutical preparations with no interference of pharmaceutical additives. The results manifest the problem of nonlinearity and how models like ANN can handle it. Analytical performance of these methods was statistically validated with respect to linearity, accuracy, precision and specificity. The developed methods indicate the ability of the previously mentioned multivariate calibration models to handle and solve UV spectra of the four components' mixtures using easy and widely used UV spectrophotometer. Copyright © 2014 Elsevier B.V. All rights reserved.

Comparative artificial neural network and partial least squares models for analysis of Metronidazole, Diloxanide, Spiramycin and Cliquinol in pharmaceutical preparations

NASA Astrophysics Data System (ADS)

Elkhoudary, Mahmoud M.; Abdel Salam, Randa A.; Hadad, Ghada M.

2014-09-01

Metronidazole (MNZ) is a widely used antibacterial and amoebicide drug. Therefore, it is important to develop a rapid and specific analytical method for the determination of MNZ in mixture with Spiramycin (SPY), Diloxanide (DIX) and Cliquinol (CLQ) in pharmaceutical preparations. This work describes simple, sensitive and reliable six multivariate calibration methods, namely linear and nonlinear artificial neural networks preceded by genetic algorithm (GA-ANN) and principle component analysis (PCA-ANN) as well as partial least squares (PLS) either alone or preceded by genetic algorithm (GA-PLS) for UV spectrophotometric determination of MNZ, SPY, DIX and CLQ in pharmaceutical preparations with no interference of pharmaceutical additives. The results manifest the problem of nonlinearity and how models like ANN can handle it. Analytical performance of these methods was statistically validated with respect to linearity, accuracy, precision and specificity. The developed methods indicate the ability of the previously mentioned multivariate calibration models to handle and solve UV spectra of the four components’ mixtures using easy and widely used UV spectrophotometer.

Probabilistic measurement of non-physical constructs during early childhood: Epistemological implications for advancing psychosocial science

NASA Astrophysics Data System (ADS)

Bezruczko, N.; Fatani, S. S.

2010-07-01

Social researchers commonly compute ordinal raw scores and ratings to quantify human aptitudes, attitudes, and abilities but without a clear understanding of their limitations for scientific knowledge. In this research, common ordinal measures were compared to higher order linear (equal interval) scale measures to clarify implications for objectivity, precision, ontological coherence, and meaningfulness. Raw score gains, residualized raw gains, and linear gains calculated with a Rasch model were compared between Time 1 and Time 2 for observations from two early childhood learning assessments. Comparisons show major inconsistencies between ratings and linear gains. When gain distribution was dense, relatively compact, and initial status near item mid-range, linear measures and ratings were indistinguishable. When Time 1 status was distributed more broadly and magnitude of change variable, ratings were unrelated to linear gain, which emphasizes problematic implications of ordinal measures. Surprisingly, residualized gain scores did not significantly improve ordinal measurement of change. In general, raw scores and ratings may be meaningful in specific samples to establish order and high/low rank, but raw score differences suffer from non-uniform units. Even meaningfulness of sample comparisons, as well as derived proportions and percentages, are seriously affected by rank order distortions and should be avoided.

Statistical analysis of an RNA titration series evaluates microarray precision and sensitivity on a whole-array basis

PubMed Central

Holloway, Andrew J; Oshlack, Alicia; Diyagama, Dileepa S; Bowtell, David DL; Smyth, Gordon K

2006-01-01

Background Concerns are often raised about the accuracy of microarray technologies and the degree of cross-platform agreement, but there are yet no methods which can unambiguously evaluate precision and sensitivity for these technologies on a whole-array basis. Results A methodology is described for evaluating the precision and sensitivity of whole-genome gene expression technologies such as microarrays. The method consists of an easy-to-construct titration series of RNA samples and an associated statistical analysis using non-linear regression. The method evaluates the precision and responsiveness of each microarray platform on a whole-array basis, i.e., using all the probes, without the need to match probes across platforms. An experiment is conducted to assess and compare four widely used microarray platforms. All four platforms are shown to have satisfactory precision but the commercial platforms are superior for resolving differential expression for genes at lower expression levels. The effective precision of the two-color platforms is improved by allowing for probe-specific dye-effects in the statistical model. The methodology is used to compare three data extraction algorithms for the Affymetrix platforms, demonstrating poor performance for the commonly used proprietary algorithm relative to the other algorithms. For probes which can be matched across platforms, the cross-platform variability is decomposed into within-platform and between-platform components, showing that platform disagreement is almost entirely systematic rather than due to measurement variability. Conclusion The results demonstrate good precision and sensitivity for all the platforms, but highlight the need for improved probe annotation. They quantify the extent to which cross-platform measures can be expected to be less accurate than within-platform comparisons for predicting disease progression or outcome. PMID:17118209

Five degree-of-freedom control of an ultra-precision magnetically-suspended linear bearing. Ph.D. Thesis - MIT

NASA Technical Reports Server (NTRS)

Trumper, David L.; Slocum, A. H.

1991-01-01

The authors constructed a high precision linear bearing. A 10.7 kg platen measuring 125 mm by 125 mm by 350 mm is suspended and controlled in five degrees of freedom by seven electromagnets. The position of the platen is measured by five capacitive probes which have nanometer resolution. The suspension acts as a linear bearing, allowing linear travel of 50 mm in the sixth degree of freedom. In the laboratory, this bearing system has demonstrated position stability of 5 nm peak-to-peak. This is believed to be the highest position stability yet demonstrated in a magnetic suspension system. Performance at this level confirms that magnetic suspensions can address motion control requirements at the nanometer level. The experimental effort associated with this linear bearing system is described. Major topics are the development of models for the suspension, implementation of control algorithms, and measurement of the actual bearing performance. Suggestions for the future improvement of the bearing system are given.

Validation of the Filovirus Plaque Assay for Use in Preclinical Studies

PubMed Central

Shurtleff, Amy C.; Bloomfield, Holly A.; Mort, Shannon; Orr, Steven A.; Audet, Brian; Whitaker, Thomas; Richards, Michelle J.; Bavari, Sina

2016-01-01

A plaque assay for quantitating filoviruses in virus stocks, prepared viral challenge inocula and samples from research animals has recently been fully characterized and standardized for use across multiple institutions performing Biosafety Level 4 (BSL-4) studies. After standardization studies were completed, Good Laboratory Practices (GLP)-compliant plaque assay method validation studies to demonstrate suitability for reliable and reproducible measurement of the Marburg Virus Angola (MARV) variant and Ebola Virus Kikwit (EBOV) variant commenced at the United States Army Medical Research Institute of Infectious Diseases (USAMRIID). The validation parameters tested included accuracy, precision, linearity, robustness, stability of the virus stocks and system suitability. The MARV and EBOV assays were confirmed to be accurate to ±0.5 log10 PFU/mL. Repeatability precision, intermediate precision and reproducibility precision were sufficient to return viral titers with a coefficient of variation (%CV) of ≤30%, deemed acceptable variation for a cell-based bioassay. Intraclass correlation statistical techniques for the evaluation of the assay’s precision when the same plaques were quantitated by two analysts returned values passing the acceptance criteria, indicating high agreement between analysts. The assay was shown to be accurate and specific when run on Nonhuman Primates (NHP) serum and plasma samples diluted in plaque assay medium, with negligible matrix effects. Virus stocks demonstrated stability for freeze-thaw cycles typical of normal usage during assay retests. The results demonstrated that the EBOV and MARV plaque assays are accurate, precise and robust for filovirus titration in samples associated with the performance of GLP animal model studies. PMID:27110807

Precision of dehydroascorbic acid quantitation with the use of the subtraction method--validation of HPLC-DAD method for determination of total vitamin C in food.

PubMed

Mazurek, Artur; Jamroz, Jerzy

2015-04-15

In food analysis, a method for determination of vitamin C should enable measuring of total content of ascorbic acid (AA) and dehydroascorbic acid (DHAA) because both chemical forms exhibit biological activity. The aim of the work was to confirm applicability of HPLC-DAD method for analysis of total content of vitamin C (TC) and ascorbic acid in various types of food by determination of validation parameters such as: selectivity, precision, accuracy, linearity and limits of detection and quantitation. The results showed that the method applied for determination of TC and AA was selective, linear and precise. Precision of DHAA determination by the subtraction method was also evaluated. It was revealed that the results of DHAA determination obtained by the subtraction method were not precise which resulted directly from the assumption of this method and the principles of uncertainty propagation. The proposed chromatographic method should be recommended for routine determinations of total vitamin C in various food. Copyright © 2014 Elsevier Ltd. All rights reserved.

Portable Linear Sled (PLS) for biomedical research

NASA Technical Reports Server (NTRS)

Vallotton, Will; Matsuhiro, Dennis; Wynn, Tom; Temple, John

1993-01-01

The PLS is a portable linear motion generating device conceived by researchers at Ames Research Center's Vestibular Research Facility and designed by engineers at Ames for the study of motion sickness in space. It is an extremely smooth apparatus, powered by linear motors and suspended on air bearings which ride on precision ground ceramic ways.

Mechanical design of a precision linear flexural stage for 3D x-ray diffraction microscope at the Advanced Photon Source

NASA Astrophysics Data System (ADS)

Shu, D.; Liu, W.; Kearney, S.; Anton, J.; Tischler, J. Z.

2015-09-01

The 3-D X-ray diffraction microscope is a new nondestructive tool for the three-dimensional characterization of mesoscopic materials structure. A flexural-pivot-based precision linear stage has been designed to perform a wire scan as a differential aperture for the 3-D diffraction microscope at the Advanced Photon Source, Argonne National Laboratory. The mechanical design and finite element analyses of the flexural stage, as well as its initial mechanical test results with laser interferometer are described in this paper.

Trueness, Precision, and Detectability for Sampling and Analysis of Organic Species in Airborne Particulate Matter

EPA Science Inventory

Recovery. precision, limits of detection and quantitation, blank levels, calibration linearity, and agreement with certified reference materials were determined for two classes of organic components of airborne particulate matter, polycyclic aromatic hydrocarbons and hopanes usin...

Smart manipulation of ratio spectra for resolving a pharmaceutical mixture of Methocarbamol and Paracetamol

NASA Astrophysics Data System (ADS)

Essam, Hebatallah M.; Abd-El Rahman, Mohamed K.

2015-04-01

Two smart, specific, accurate and precise spectrophotometric methods manipulating ratio spectra are developed for simultaneous determination of Methocarbamol (METH) and Paracetamol (PAR) in their combined pharmaceutical formulation without preliminary separation. Method A, is an extended ratio subtraction one (EXRSM) coupled with ratio subtraction method (RSM), which depends on subtraction of the plateau values from the ratio spectrum. Method B is a ratio difference spectrophotometric one (RDM) which measures the difference in amplitudes of ratio spectra between 278 and 286 nm for METH and 247 and 260 nm for PAR. The calibration curves are linear over the concentration range of 10-100 μg mL-1 and 2-20 μg mL-1 for METH and PAR, respectively. The specificity of the developed methods was investigated by analyzing different laboratory prepared mixtures of the two drugs. Both methods were applied successfully for the determination of the selected drugs in their combined dosage form. Furthermore, validation was performed according to ICH guidelines; accuracy, precision and repeatability are found to be within the acceptable limits. Statistical studies showed that both methods can be competitively applied in quality control laboratories.

Linear-dichroic infrared spectroscopy—Validation and experimental design of the new orientation technique of solid samples as suspension in nematic liquid crystal

NASA Astrophysics Data System (ADS)

Ivanova, B. B.; Simeonov, V. D.; Arnaudov, M. G.; Tsalev, D. L.

2007-05-01

A validation of the developed new orientation method of solid samples as suspension in nematic liquid crystal (NLC), applied in linear-dichroic infrared (IR-LD) spectroscopy has been carried out using a model system DL-isoleucine ( DL-isoleu). Accuracy, precision and the influence of the liquid crystal medium on peak positions and integral absorbances of guest molecules have been presented. Optimization of experimental conditions has been performed as well. An experimental design for quantitative evaluation of the impact of four input factors: the number of scans, the rubbing-out of KBr-pellets, the amount of studied compounds included in the liquid crystal medium and the ratios of Lorentzian to Gaussian peak functions in the curve fitting procedure on the spectroscopic signal at five different frequencies, indicating important specifities of the system has been studied.

International ring trial for the validation of an event-specific Golden Rice 2 quantitative real-time polymerase chain reaction method.

PubMed

Jacchia, Sara; Nardini, Elena; Bassani, Niccolò; Savini, Christian; Shim, Jung-Hyun; Trijatmiko, Kurniawan; Kreysa, Joachim; Mazzara, Marco

2015-05-27

This article describes the international validation of the quantitative real-time polymerase chain reaction (PCR) detection method for Golden Rice 2. The method consists of a taxon-specific assay amplifying a fragment of rice Phospholipase D α2 gene, and an event-specific assay designed on the 3' junction between transgenic insert and plant DNA. We validated the two assays independently, with absolute quantification, and in combination, with relative quantification, on DNA samples prepared in haploid genome equivalents. We assessed trueness, precision, efficiency, and linearity of the two assays, and the results demonstrate that both the assays independently assessed and the entire method fulfill European and international requirements for methods for genetically modified organism (GMO) testing, within the dynamic range tested. The homogeneity of the results of the collaborative trial between Europe and Asia is a good indicator of the robustness of the method.

Cutting force measurement of electrical jigsaw by strain gauges

NASA Astrophysics Data System (ADS)

Kazup, L.; Varadine Szarka, A.

2016-11-01

This paper describes a measuring method based on strain gauges for accurate specification of electric jigsaw's cutting force. The goal of the measurement is to provide an overall perspective about generated forces in a jigsaw's gearbox during a cutting period. The lifetime of the tool is affected by these forces primarily. This analysis is part of the research and development project aiming to develop a special linear magnetic brake for realizing automatic lifetime tests of electric jigsaws or similar handheld tools. The accurate specification of cutting force facilitates to define realistic test cycles during the automatic lifetime test. The accuracy and precision resulted by the well described cutting force characteristic and the possibility of automation provide new dimension for lifetime testing of the handheld tools with alternating movement.

A comparative study of smart spectrophotometric methods for simultaneous determination of a skeletal muscle relaxant and an analgesic in combined dosage form.

PubMed

Salem, Hesham; Mohamed, Dalia

2015-04-05

Six simple, specific, accurate and precise spectrophotometric methods were developed and validated for the simultaneous determination of the analgesic drug; paracetamol (PARA) and the skeletal muscle relaxant; dantrolene sodium (DANT). Three methods are manipulating ratio spectra namely; ratio difference (RD), ratio subtraction (RS) and mean centering (MC). The other three methods are utilizing the isoabsorptive point either at zero order namely; absorbance ratio (AR) and absorbance subtraction (AS) or at ratio spectrum namely; amplitude modulation (AM). The proposed spectrophotometric procedures do not require any preliminary separation step. The accuracy, precision and linearity ranges of the proposed methods were determined. The selectivity of the developed methods was investigated by analyzing laboratory prepared mixtures of the drugs and their combined dosage form. Standard deviation values are less than 1.5 in the assay of raw materials and capsules. The obtained results were statistically compared with each other and with those of reported spectrophotometric ones. The comparison showed that there is no significant difference between the proposed methods and the reported methods regarding both accuracy and precision. Copyright © 2015 Elsevier B.V. All rights reserved.

Combining simplicity with cost-effectiveness: Investigation of potential counterfeit of proton pump inhibitors through simulated formulations using thin-layer chromatography.

PubMed

Bhatt, Nejal M; Chavada, Vijay D; Sanyal, Mallika; Shrivastav, Pranav S

2016-11-18

A simple, accurate and precise high-performance thin-layer chromatographic method has been developed and validated for the analysis of proton pump inhibitors (PPIs) and their co-formulated drugs, available as binary combination. Planar chromatographic separation was achieved using a single mobile phase comprising of toluene: iso-propranol: acetone: ammonia 5.0:2.3:2.5:0.2 (v/v/v/v) for the analysis of 14 analytes on aluminium-backed layer of silica gel 60 FG 254 . Densitometric determination of the separated spots was done at 290nm. The method was validated according to ICH guidelines for linearity, precision and accuracy, sensitivity, specificity and robustness. The method showed good linear response for the selected drugs as indicated by the high values of correlation coefficients (≥0.9993). The limit of detection and limit of quantiation were in the range of 6.9-159.2ng/band and 20.8-478.1ng/band respectively for all the analytes. The optimized conditions afforded adequate resolution of each PPI from their co-formulated drugs and provided unambiguous identification of the co-formulated drugs from their homologous retardation factors (hR f ). The only limitation of the method was the inability to separate two PPIs, rabeprazole and lansoprazole from each other. Nevertheless, it is proposed that peak spectra recording and comparison with standard drug spot can be a viable option for assignment of TLC spots. The method performance was assessed by analyzing different laboratory simulated mixtures and some marketed formulations of the selected drugs. The developed method was successfully used to investigate potential counterfeit of PPIs through a series of simulated formulations with good accuracy and precision. Copyright © 2016 Elsevier B.V. All rights reserved.

Development and validation of a UPLC method for the determination of duloxetine hydrochloride residues on pharmaceutical manufacturing equipment surfaces

PubMed Central

Kumar, Navneet; Sangeetha, D.; Balakrishna, P.

2011-01-01

Background: In pharmaceutical industries, it is very important to remove drug residues from the equipment and areas used. The cleaning procedure must be validated, so special attention must be devoted to the methods used for analysis of trace amounts of drugs. A rapid, sensitive, and specific reverse phase ultra-performance liquid chromatographic (UPLC) method was developed for the quantitative determination of duloxetine in cleaning validation swab samples. Material and Methods: The method was validated using an Acquity UPLC™ HSS T3 (100 × 2.1 mm2) 1.8 μm column with a isocratic mobile phase containing a mixture of 0.01 M potassium dihydrogen orthophosphate, pH adjusted to 3.0 with orthophosphoric acid and acetonitrile (60:40 v/v). The flow rate of the mobile phase was 0.4 ml/min with a column temperature of 40°C and detection wavelength at 230 nm. Cotton swabs, moisten with extraction solution (90% methanol and 10% water), were used to remove any residue of drug from stainless steel, glass and silica surfaces, and give recoveries >80% at four concentration levels. Results: The precision of the results, reported as the relative standard deviation, were below 1.5%. The calibration curve was linear over a concentration range from 0.02 to 5.0 μg/ml with a correlation coefficient of 0.999. The detection limit and quantitation limit were 0.006 and 0.02 μg/ml, respectively. The method was validated over a concentration range of 0.05–5.0 μg/ml. Conclusion: The developed method was validated with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, and robustness. PMID:23781449

Influence of non-ideal performance of lasers on displacement precision in single-grating heterodyne interferometry

NASA Astrophysics Data System (ADS)

Wang, Guochao; Xie, Xuedong; Yan, Shuhua

2010-10-01

Principle of the dual-wavelength single grating nanometer displacement measuring system, with a long range, high precision, and good stability, is presented. As a result of the nano-level high-precision displacement measurement, the error caused by a variety of adverse factors must be taken into account. In this paper, errors, due to the non-ideal performance of the dual-frequency laser, including linear error caused by wavelength instability and non-linear error caused by elliptic polarization of the laser, are mainly discussed and analyzed. On the basis of theoretical modeling, the corresponding error formulas are derived as well. Through simulation, the limit value of linear error caused by wavelength instability is 2nm, and on the assumption that 0.85 x T = , 1 Ty = of the polarizing beam splitter(PBS), the limit values of nonlinear-error caused by elliptic polarization are 1.49nm, 2.99nm, 4.49nm while the non-orthogonal angle is selected correspondingly at 1°, 2°, 3° respectively. The law of the error change is analyzed based on different values of Tx and Ty .

A Simple and Specific Stability- Indicating RP-HPLC Method for Routine Assay of Adefovir Dipivoxil in Bulk and Tablet Dosage Form.

PubMed

Darsazan, Bahar; Shafaati, Alireza; Mortazavi, Seyed Alireza; Zarghi, Afshin

2017-01-01

A simple and reliable stability-indicating RP-HPLC method was developed and validated for analysis of adefovir dipivoxil (ADV).The chromatographic separation was performed on a C 18 column using a mixture of acetonitrile-citrate buffer (10 mM at pH 5.2) 36:64 (%v/v) as mobile phase, at a flow rate of 1.5 mL/min. Detection was carried out at 260 nm and a sharp peak was obtained for ADV at a retention time of 5.8 ± 0.01 min. No interferences were observed from its stress degradation products. The method was validated according to the international guidelines. Linear regression analysis of data for the calibration plot showed a linear relationship between peak area and concentration over the range of 0.5-16 μg/mL; the regression coefficient was 0.9999and the linear regression equation was y = 24844x-2941.3. The detection (LOD) and quantification (LOQ) limits were 0.12 and 0.35 μg/mL, respectively. The results proved the method was fast (analysis time less than 7 min), precise, reproducible, and accurate for analysis of ADV over a wide range of concentration. The proposed specific method was used for routine quantification of ADV in pharmaceutical bulk and a tablet dosage form.

Electrochemical Impedance Spectrometer with an Environmental Chamber for Rapid Screening of New Precise Copolymers

DTIC Science & Technology

2017-10-07

polymerization to make linear polyethylenes with carboxylic acid groups at precise intervals along the polymer . Precise acid- containing polymers provide...acid polyethylene and the a polymerized ionic liquids based on cyclopropenium. The instrument is also be used to study polymer segmental dynamics...Advances in batteries, fuel cells, and permselective membranes are materials limited. New acid- and ion-containing polymers must be designed and

Optimal moving grids for time-dependent partial differential equations

NASA Technical Reports Server (NTRS)

Wathen, A. J.

1989-01-01

Various adaptive moving grid techniques for the numerical solution of time-dependent partial differential equations were proposed. The precise criterion for grid motion varies, but most techniques will attempt to give grids on which the solution of the partial differential equation can be well represented. Moving grids are investigated on which the solutions of the linear heat conduction and viscous Burgers' equation in one space dimension are optimally approximated. Precisely, the results of numerical calculations of optimal moving grids for piecewise linear finite element approximation of partial differential equation solutions in the least squares norm.

Optimal moving grids for time-dependent partial differential equations

NASA Technical Reports Server (NTRS)

Wathen, A. J.

1992-01-01

Various adaptive moving grid techniques for the numerical solution of time-dependent partial differential equations were proposed. The precise criterion for grid motion varies, but most techniques will attempt to give grids on which the solution of the partial differential equation can be well represented. Moving grids are investigated on which the solutions of the linear heat conduction and viscous Burgers' equation in one space dimension are optimally approximated. Precisely, the results of numerical calculations of optimal moving grids for piecewise linear finite element approximation of PDE solutions in the least-squares norm are reported.

Simultaneous determination of isochamaejasmin, neochamaejasmin A and aphnoretinin rat plasma by UPLC-MS/MS and its application to a pharmacokinetic study of Stellera chamaejasme L. extract.

PubMed

Wang, Ludi; Yang, Wei; Wu, Siyang; Wang, Shuyao; Kang, Chen; Ma, Xiaoli; Li, Yingfei; Li, Chuan

2018-05-01

Isochamaejasmin, neochamaejasmin A and daphnoretin derived from Stellera chamaejasme L. are important because of their reported anticancer properties. In this study, a sensitive UPLC-MS/MS method for the determination of isochamaejasmin, neochamaejasmin A and daphnoretin in rat plasma was developed. The analyte and IS were separated on an Acquity UPLC HSS T3 column (100 × 2.1 mm, 1.8 μm) using gradient elution with the mobile phase of aqueous solution (methanol-water, 1:99, v/v, containing 1 mm formic acid) and organic solution (methanol-water, 99:1, v/v, containing 1 mm formic acid) at a flow rate of 0.3 mL/min. Multiple reaction monitoring mode with negative electrospray ionization interface was carried out to detect the components. The method was validated in terms of specificity, linearity, accuracy, precision, stability, etc. Excellent linear behavior was observed over the certain concentration ranges with the correlation coefficient values >0.99. Intra- and inter-day precisions (RSD) were <6.7% and accuracy (RE) ranged from -7.0 to 12.0%. The validated method was successfully applied to investigate the pharmacokinetics of three chemical ingredients after oral administration of S. chamaejasme L. extract to rats. Copyright © 2017 John Wiley & Sons, Ltd.

A validated RP-HPLC method for simultaneous determination of propranolol and valsartan in bulk drug and gel formulation

PubMed Central

Imam, Syed Sarim; Ahad, Abdul; Aqil, Mohammed; Sultana, Yasmin; Ali, Asgar

2013-01-01

Objective: A simple, precise, and stability indicating high performance liquid chromatography (HPLC) method was developed and validated for the simultaneous determination of propranolol hydrochloride and valsartan in pharmaceutical dosage form. Materials and Methods: The method involves the use of easily available inexpensive laboratory reagents. The separation was achieved on Hypersil ODS C-18 column (250*4.6 mm, i.d., 5 μm particle size) with isocratic flow with UV detector. The mobile phase at a flow rate of 1.0 mL/min consisted of acetonitrile, methanol, and 0.01 M disodium hydrogen phosphate (pH 3.5) in the ratio of 50:35:15 v/v. Results: A linear response was observed over the concentration range 5-50 μg/mL of propranolol and the concentration range 4-32 μg/mL of valsartan. Limit of detection and limit of quantitation for propranolol were 0.27 μg/mL and 0.85 μg/mL, and for valsartan were 0.45 μg/mL and 1.39 μg/mL, respectively. The method was successfully validated in accordance to ICH guidelines acceptance criteria for linearity, accuracy, precision, specificity, robustness. Conclusion: The analysis concluded that the method was selective for simultaneous estimation of propranolol and valsartan can be potentially used for the estimation of these drugs in combined dosage form. PMID:23559826

Application of portable X-ray fluorescence spectrometry in environmental investigation of heavy metal-contaminated sites and comparison with laboratory analysis

NASA Astrophysics Data System (ADS)

Ding, Liang; Wang, Shui; Cai, Bingjie; Zhang, Mancheng; Qu, Changsheng

2018-02-01

In this study, portable X-ray fluorescence spectrometry (pXRF) was used to measure the heavy metal contents of As, Cu, Cr, Ni, Pb and Zn in the soils of heavy metal-contaminated sites. The precision, accuracy and system errors of pXRF were evaluated and compared with traditional laboratory methods to examine the suitability of in situ pXRF. The results show that the pXRF analysis achieved satisfactory accuracy and precision in measuring As, Cr, Cu, Ni, Pb, and Zn in soils, and meets the requirements of the relevant detection technology specifications. For the certified reference soil samples, the pXRF results of As, Cr, Cu, Ni, Pb, and Zn show good linear relationships and coefficients of determination with the values measured using the reference analysis methods; with the exception of Ni, all the measured values were within the 95% confidence level. In the soil samples, the coefficients of determination between Cu, Zn, Pb, and Ni concentrations measured laboratory pXRF and the values measured with laboratory analysis all reach 0.9, showing a good linear relationship; however, there were large deviations between methods for Cr and As. This study provides reference data and scientific support for rapid detection of heavy metals in soils using pXRF in site investigation, which can better guide the practical application of pXRF.

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

PubMed

Shirkhedkar, Atul A; Surana, Sanjay J

2010-01-01

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

Perinatal BPA exposure alters body weight and composition in a dose specific and sex specific manner: The addition of peripubertal exposure exacerbates adverse effects in female mice

PubMed Central

Rubin, Beverly S.; Paranjpe, Maneesha; DaFonte, Tracey; Schaeberle, Cheryl; Soto, Ana M.; Obin, Martin; Greenberg, Andrew S.

2017-01-01

Body weight (BW) and body composition were examined in CD-1 mice exposed perinatally or perinatally and peripubertally to 0, 0.25, 2.5, 25, or 250 μg BPA/kg BW/day. Our goal was to identify the BPA dose (s) and the exposure window(s) that increased BW and adiposity, and to assess potential sex differences in this response. Both perinatal exposure alone and perinatal plus peripubertal exposure to environmentally relevant levels of BPA resulted in lasting effects on body weight and body composition. The effects were dose specific and sex specific and were influenced by the precise window of BPA exposure. The addition of peripubertal BPA exposure following the initial perinatal exposure exacerbated adverse effects in the females but appeared to reduce differences in body weight and body composition between control and BPA exposed males. Some effects of BPA on body weight and body composition showed a non-linear dose response. PMID:27496714

Clinical evaluation of the Technico Stat/Ion system.

PubMed

Slaunwhite, D; Clements, J C; Reynoso, G

1977-02-01

1. We describe our evaluation of the Technicon Stat/Ion, an instrument which performs sodium, chloride and bicarbonate analysis simultaneously. 2. All four of the assays resulted in linear response over the entire clinical range with insignificant carryover between specimens. 3. Precision studies for within-run variation were: sodium 0.3 percent, potassium 0.7 percent, chloride 0.5 percent and bicarbonate 1.6 percent. Day-to-day precision was similar to the within-run precision. 4. Comparison methods for sodium, potassium, chloride and bicarbonate utilizing flame photometry, chloridometry and titration of released carbon dioxide respectively showed the following linear regression and correlation coefficients: sodium y=0.96+5.5 (a=0.988) potassium y=1.01x+0.0 (a=.996) chloride y=0.99x+1.0 (a=.993)bicarbonate y=1.0x+1.2 (alpha=.969).

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

PubMed

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

2009-01-01

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

A new linear least squares method for T1 estimation from SPGR signals with multiple TRs

NASA Astrophysics Data System (ADS)

Chang, Lin-Ching; Koay, Cheng Guan; Basser, Peter J.; Pierpaoli, Carlo

2009-02-01

The longitudinal relaxation time, T1, can be estimated from two or more spoiled gradient recalled echo x (SPGR) images with two or more flip angles and one or more repetition times (TRs). The function relating signal intensity and the parameters are nonlinear; T1 maps can be computed from SPGR signals using nonlinear least squares regression. A widely-used linear method transforms the nonlinear model by assuming a fixed TR in SPGR images. This constraint is not desirable since multiple TRs are a clinically practical way to reduce the total acquisition time, to satisfy the required resolution, and/or to combine SPGR data acquired at different times. A new linear least squares method is proposed using the first order Taylor expansion. Monte Carlo simulations of SPGR experiments are used to evaluate the accuracy and precision of the estimated T1 from the proposed linear and the nonlinear methods. We show that the new linear least squares method provides T1 estimates comparable in both precision and accuracy to those from the nonlinear method, allowing multiple TRs and reducing computation time significantly.

Precision Efficacy Analysis for Regression.

ERIC Educational Resources Information Center

Brooks, Gordon P.

When multiple linear regression is used to develop a prediction model, sample size must be large enough to ensure stable coefficients. If the derivation sample size is inadequate, the model may not predict well for future subjects. The precision efficacy analysis for regression (PEAR) method uses a cross- validity approach to select sample sizes…

Research on precise pneumatic-electric displacement sensor with large measurement range

NASA Astrophysics Data System (ADS)

Yin, Zhehao; Yuan, Yibao; Liu, Baoshuai

2017-10-01

This research mainly focuses on precise pneumatic-electric displacement sensor which has large measurement range. Under the high precision, measurement range can be expanded so that the need of high precision as well as large range can be satisfied in the field of machining inspection technology. This research was started by the analysis of pneumatic-measuring theory. Then, an gas circuit measuring system which is based on differential pressure was designed. This designed system can reach two aims: Firstly, to convert displacement signal into gas signal; Secondly, to reduce the measurement error which caused by pressure and environmental turbulence. Furthermore, in consideration of the high requirement for linearity, sensitivity and stability, the project studied the pneumatic-electric transducer which puts the SCX series pressure sensor as a key part. The main purpose of this pneumatic-electric transducer is to convert gas signal to suitable electrical signal. Lastly, a broken line subsection linearization circuit was designed, which can nonlinear correct the output characteristic curve so as to enlarge the linear measurement range. The final result could be briefly described like this: under the condition that measuring error is less than 1μm, measurement range could be extended to approximately 200μm which is much higher than the measurement range of traditional pneumatic measuring instrument. Meanwhile, it can reach higher exchangeability and stability in order to become more suitable to engineering application.

Determination of emamectin benzoate in medicated fish feed: a multisite study.

PubMed

Farer, Leslie J

2005-01-01

A new method was developed for the quantitation of emamectin benzoate in medicated fish feed at levels between 1 and 30 ppm. The new procedure, based on a previously reported assay, consists of a wet methanolic extraction of ground feed, followed by solid-phase extraction and injection onto a gradient liquid chromatographic system. A multisite study involving 3 laboratories (the developing laboratory and 2 independent laboratories) was performed to evaluate precision, recovery, linearity, and sensitivity. Mean recove;ries for triplicate analyses at 3 levels, performed by 2 analysts per laboratory, were between 89 and 97%, with coefficients of variation ranging from 1.6 to 8.6%. Coefficients of determination (r2) obtained from the plotted data were > or =0.993. The precision of the method, determined from 6 replicate preparations from the same batch of medicated feed assayed in 3 separate trials per laboratory, was between 0.6 and 5.8%. The quantitation limit was established at 0.5 ppm. Specificity and robustness studies were performed by the developing laboratory.

High-precision optical measurements of 13C/12C isotope ratios in organic compounds at natural abundance

PubMed Central

Zare, Richard N.; Kuramoto, Douglas S.; Haase, Christa; Tan, Sze M.; Crosson, Eric R.; Saad, Nabil M. R.

2009-01-01

A continuous-flow cavity ring-down spectroscopy (CRDS) system integrating a chromatographic separation technique, a catalytic combustor, and an isotopic 13C/12C optical analyzer is described for the isotopic analysis of a mixture of organic compounds. A demonstration of its potential is made for the geochemically important class of short-chain hydrocarbons. The system proved to be linear over a 3-fold injection volume dynamic range with an average precision of 0.95‰ and 0.67‰ for ethane and propane, respectively. The calibrated accuracy for methane, ethane, and propane is within 3‰ of the values determined using isotope ratio mass spectrometry (IRMS), which is the current method of choice for compound-specific isotope analysis. With anticipated improvements, the low-cost, portable, and easy-to-use CRDS-based instrumental setup is poised to evolve into a credible challenge to the high-cost and complex IRMS-based technique. PMID:19564619

Simultaneous determination of diclofenac potassium and methocarbamol in ternary mixture with guaifenesin by reversed phase liquid chromatography.

PubMed

Elkady, Ehab F

2010-09-15

New, simple, rapid and precise reversed phase liquid chromatographic (RP-LC) method has been developed for the simultaneous determination of diclofenac potassium (DP) and methocarbamol (MT) in ternary mixture with guaifenesin (GF), degradation product of methocarbamol. Chromatographic separation was achieved on a Symmetry Waters C18 column (150 mm x 4. 6mm, 5 microm). Gradient elution based on phosphate buffer pH (8)-acetonitrile at a flow rate of 1 mL min(-1) was applied. The UV detector was operated at 282 nm for DP and 274 nm for MT and GF. Linearity, accuracy and precision were found to be acceptable over the concentration ranges of 0.05-16, 0.5-160 and 0.5-160 microg mL(-1) for DP, MT and GF, respectively. The optimized method proved to be specific, robust and accurate for the quality control of the cited drugs in pharmaceutical preparation. Copyright (c) 2010 Elsevier B.V. All rights reserved.

3D DNA origami as programmable anchoring points for bioreceptors in fiber optic surface plasmon resonance biosensing.

PubMed

Daems, Devin; Pfeifer, Wolfgang; Rutten, Iene; Sacca, Barbara; Spasic, Dragana; Lammertyn, Jeroen

2018-06-27

Many challenges in biosensing originate from the fact that the all-important nano-architecture of the biosensor's surface, including precise density and orientation of bioreceptors, is not entirely comprehended. Here we introduced a 3D DNA origami as bioreceptor carrier to functionalize the fiber optic surface plasmon resonance (FO-SPR) sensor with nanoscale precision. Starting from a 24-helix bundle, two distinct DNA origami structures were designed to position thrombin-specific aptamers with different density and distance (27 and 113 nm) from the FO-SPR surface. The origami-based biosensors proved to be not only capable of reproducible, label-free thrombin detection, but revealed also valuable innovative features: (1) a significantly better performance in the absence of backfilling, known as essential in biosensing field, suggesting improved bioreceptor orientation and accessibility and (2) a wider linear range compared to previously reported thrombin biosensors. We envisage that our method will be beneficial both for scientists and clinicians looking for new surface (bio)chemistry and improved diagnostics.

A validated high-performance liquid chromatographic method for the determination of glibenclamide in human plasma and its application to pharmacokinetic studies.

PubMed

Niopas, Ioannis; Daftsios, Athanasios C

2002-05-15

Glibenclamide is a potent second generation oral sulfonylurea antidiabetic agent widely used for the treatment of type II diabetes melitus. A rapid, sensitive, precise, accurate and specific HPLC assay for the determination of glibenclamide in human plasma was developed and validated. After addition of flufenamic acid as internal standard, the analytes were isolated from human plasma by liquid-liquid extraction. The method was linear in the 10-400 ng/ml concentration range (r > 0.999). Recovery for glibenclamide was greater than 91.5% and for internal standard was 93.5%. Within-day and between-day precision, expressed as the relative standard deviation (RSD%), ranged from 1.4 to 5.9% and 5.8 to 6.6%, respectively. Assay accuracy was better than 93.4%. The assay was used to estimate the pharmacokinetics of glibenclamide after oral administration of a 5 mg tablet of glibenclamide to 18 healthy volunteers.

Validation of quantitative method for azoxystrobin residues in green beans and peas.

PubMed

Abdelraheem, Ehab M H; Hassan, Sayed M; Arief, Mohamed M H; Mohammad, Somaia G

2015-09-01

This study presents a method validation for extraction and quantitative analysis of azoxystrobin residues in green beans and peas using HPLC-UV and the results confirmed by GC-MS. The employed method involved initial extraction with acetonitrile after the addition of salts (magnesium sulfate and sodium chloride), followed by a cleanup step by activated neutral carbon. Validation parameters; linearity, matrix effect, LOQ, specificity, trueness and repeatability precision were attained. The spiking levels for the trueness and the precision experiments were (0.1, 0.5, 3 mg/kg). For HPLC-UV analysis, mean recoveries ranged between 83.69% to 91.58% and 81.99% to 107.85% for green beans and peas, respectively. For GC-MS analysis, mean recoveries ranged from 76.29% to 94.56% and 80.77% to 100.91% for green beans and peas, respectively. According to these results, the method has been proven to be efficient for extraction and determination of azoxystrobin residues in green beans and peas. Copyright © 2015 Elsevier Ltd. All rights reserved.

A novel spectrofluorimetric method for the assay of pseudoephedrine hydrochloride in pharmaceutical formulations via derivatization with 4-chloro-7-nitrobenzofurazan.

PubMed

El-Didamony, Akram M; Gouda, Ayman A

2011-01-01

A new highly sensitive and specific spectrofluorimetric method has been developed to determine a sympathomimetic drug pseudoephedrine hydrochloride. The present method was based on derivatization with 4-chloro-7-nitrobenzofurazan in phosphate buffer at pH 7.8 to produce a highly fluorescent product which was measured at 532 nm (excitation at 475 nm). Under the optimized conditions a linear relationship and good correlation was found between the fluorescence intensity and pseudoephedrine hydrochloride concentration in the range of 0.5-5 µg mL(-1). The proposed method was successfully applied to the assay of pseudoephedrine hydrochloride in commercial pharmaceutical formulations with good accuracy and precision and without interferences from common additives. Statistical comparison of the results with a well-established method showed excellent agreement and proved that there was no significant difference in the accuracy and precision. The stoichiometry of the reaction was determined and the reaction pathway was postulated. Copyright © 2010 John Wiley & Sons, Ltd.

Proposing a Parkinson's disease-specific tremor scale from the MDS-UPDRS.

PubMed

Forjaz, Maria João; Ayala, Alba; Testa, Claudia M; Bain, Peter G; Elble, Rodger; Haubenberger, Dietrich; Rodriguez-Blazquez, Carmen; Deuschl, Günther; Martinez-Martin, Pablo

2015-07-01

This article proposes an International Parkinson and Movement Disorder Society (MDS)-UPDRS tremor-based scale and describes its measurement properties, with a view to developing an improved scale for assessing tremor in Parkinson's disease (PD). This was a cross-sectional, multicenter study of 435 PD patients. Rasch analysis was performed on the 11 MDS-UPDRS tremor items. Construct validity, precision, and test-retest reliability were also analyzed. After some modifications, which included removal of an item owing to redundancy, the obtained MDS-UPDRS tremor scale showed moderate reliability, unidimensionality, absence of differential item functioning, satisfactory convergent validity with medication, and better precision than the raw sum score. However, the scale displayed a floor effect and a need for more items measuring lower levels of tremor. The MDS-UPDRS tremor scale provides linear scores that can be used to assess tremor in PD in a valid, reliable way. The scale might benefit from modifications and studies that analyze its responsiveness. © 2015 International Parkinson and Movement Disorder Society.

Fitting and forecasting coupled dark energy in the non-linear regime

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

Casas, Santiago; Amendola, Luca; Pettorino, Valeria

2016-01-01

We consider cosmological models in which dark matter feels a fifth force mediated by the dark energy scalar field, also known as coupled dark energy. Our interest resides in estimating forecasts for future surveys like Euclid when we take into account non-linear effects, relying on new fitting functions that reproduce the non-linear matter power spectrum obtained from N-body simulations. We obtain fitting functions for models in which the dark matter-dark energy coupling is constant. Their validity is demonstrated for all available simulations in the redshift range 0z=–1.6 and wave modes below 0k=1 h/Mpc. These fitting formulas can be used tomore » test the predictions of the model in the non-linear regime without the need for additional computing-intensive N-body simulations. We then use these fitting functions to perform forecasts on the constraining power that future galaxy-redshift surveys like Euclid will have on the coupling parameter, using the Fisher matrix method for galaxy clustering (GC) and weak lensing (WL). We find that by using information in the non-linear power spectrum, and combining the GC and WL probes, we can constrain the dark matter-dark energy coupling constant squared, β{sup 2}, with precision smaller than 4% and all other cosmological parameters better than 1%, which is a considerable improvement of more than an order of magnitude compared to corresponding linear power spectrum forecasts with the same survey specifications.« less

An accuracy improvement method for the topology measurement of an atomic force microscope using a 2D wavelet transform.

PubMed

Yoon, Yeomin; Noh, Suwoo; Jeong, Jiseong; Park, Kyihwan

2018-05-01

The topology image is constructed from the 2D matrix (XY directions) of heights Z captured from the force-feedback loop controller. For small height variations, nonlinear effects such as hysteresis or creep of the PZT-driven Z nano scanner can be neglected and its calibration is quite straightforward. For large height variations, the linear approximation of the PZT-driven Z nano scanner fail and nonlinear behaviors must be considered because this would cause inaccuracies in the measurement image. In order to avoid such inaccuracies, an additional strain gauge sensor is used to directly measure displacement of the PZT-driven Z nano scanner. However, this approach also has a disadvantage in its relatively low precision. In order to obtain high precision data with good linearity, we propose a method of overcoming the low precision problem of the strain gauge while its feature of good linearity is maintained. We expect that the topology image obtained from the strain gauge sensor showing significant noise at high frequencies. On the other hand, the topology image obtained from the controller output showing low noise at high frequencies. If the low and high frequency signals are separable from both topology images, the image can be constructed so that it is represented with high accuracy and low noise. In order to separate the low frequencies from high frequencies, a 2D Haar wavelet transform is used. Our proposed method use the 2D wavelet transform for obtaining good linearity from strain gauge sensor and good precision from controller output. The advantages of the proposed method are experimentally validated by using topology images. Copyright © 2018 Elsevier B.V. All rights reserved.

Evaluation of Beckman Coulter DxI 800 immunoassay system using clinically oriented performance goals.

PubMed

Akbas, Neval; Schryver, Patricia G; Algeciras-Schimnich, Alicia; Baumann, Nikola A; Block, Darci R; Budd, Jeffrey R; Gaston, S J Stephen; Klee, George G

2014-11-01

We evaluated the analytical performance of 24 immunoassays using the Beckman Coulter DxI 800 immunoassay systems at Mayo Clinic, Rochester, MN for trueness, precision, detection limits, linearity, and consistency (across instruments and reagent lots). Clinically oriented performance goals were defined using the following methods: trueness-published desirable accuracy limits, precision-published desirable biologic variation; detection limits - 0.1 percentile of patient test values, linearity - 50% of total error, and consistency-percentage test values crossing key decision points. Local data were collected for precision, linearity, and consistency. Data were provided by Beckman Coulter, Inc. for trueness and detection limits. All evaluated assays except total thyroxine were within the proposed goals for trueness. Most of the assays met the proposed goals for precision (86% of intra-assay results and 75% of inter-assay results). Five assays had more than 15% of the test results below the minimum detection limits. Carcinoembryonic antigen, total thyroxine and free triiodothyronine exceeded the proposed goals of ±6.3%, ±5% and ±5.7% for dilution linearity. All evaluated assays were within the proposed goals for instrument consistency. Lot-to-lot consistency results for cortisol, ferritin and total thyroxine exceeded the proposed goals of 3.3%, 11.4% and 7% at one medical decision level, while vitamin B12 exceeded the proposed goals of 5.2% and 3.8% at two decision levels. The Beckman Coulter DxI 800 immunoassay system meets most of these proposed goals, even though these clinically focused performance goals represent relatively stringent limits. Copyright © 2014 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Anodic Oxidation of Etodolac and its Linear Sweep, Square Wave and Differential Pulse Voltammetric Determination in Pharmaceuticals

PubMed Central

Yilmaz, B.; Kaban, S.; Akcay, B. K.

2015-01-01

In this study, simple, fast and reliable cyclic voltammetry, linear sweep voltammetry, square wave voltammetry and differential pulse voltammetry methods were developed and validated for determination of etodolac in pharmaceutical preparations. The proposed methods were based on electrochemical oxidation of etodolac at platinum electrode in acetonitrile solution containing 0.1 M lithium perchlorate. The well-defined oxidation peak was observed at 1.03 V. The calibration curves were linear for etodolac at the concentration range of 2.5-50 μg/ml for linear sweep, square wave and differential pulse voltammetry methods, respectively. Intra- and inter-day precision values for etodolac were less than 4.69, and accuracy (relative error) was better than 2.00%. The mean recovery of etodolac was 100.6% for pharmaceutical preparations. No interference was found from three tablet excipients at the selected assay conditions. Developed methods in this study are accurate, precise and can be easily applied to Etol, Tadolak and Etodin tablets as pharmaceutical preparation. PMID:26664057

Efficient calculation of cosmological neutrino clustering in the non-linear regime

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

Archidiacono, Maria; Hannestad, Steen, E-mail: archi@phys.au.dk, E-mail: sth@phys.au.dk

2016-06-01

We study in detail how neutrino perturbations can be followed in linear theory by using only terms up to l =2 in the Boltzmann hierarchy. We provide a new approximation to the third moment and demonstrate that the neutrino power spectrum can be calculated to a precision of better than ∼ 5% for masses up to ∼ 1 eV and k ∼< 10 h /Mpc. The matter power spectrum can be calculated far more precisely and typically at least a factor of a few better than with existing approximations. We then proceed to study how the neutrino power spectrum canmore » be reliably calculated even in the non-linear regime by using the non-linear gravitational potential, sourced by dark matter overdensities, as it is derived from semi-analytic methods based on N -body simulations in the Boltzmann evolution hierarchy. Our results agree extremely well with results derived from N -body simulations that include cold dark matter and neutrinos as independent particles with different properties.« less

A comparison of multiple imputation methods for handling missing values in longitudinal data in the presence of a time-varying covariate with a non-linear association with time: a simulation study.

PubMed

De Silva, Anurika Priyanjali; Moreno-Betancur, Margarita; De Livera, Alysha Madhu; Lee, Katherine Jane; Simpson, Julie Anne

2017-07-25

Missing data is a common problem in epidemiological studies, and is particularly prominent in longitudinal data, which involve multiple waves of data collection. Traditional multiple imputation (MI) methods (fully conditional specification (FCS) and multivariate normal imputation (MVNI)) treat repeated measurements of the same time-dependent variable as just another 'distinct' variable for imputation and therefore do not make the most of the longitudinal structure of the data. Only a few studies have explored extensions to the standard approaches to account for the temporal structure of longitudinal data. One suggestion is the two-fold fully conditional specification (two-fold FCS) algorithm, which restricts the imputation of a time-dependent variable to time blocks where the imputation model includes measurements taken at the specified and adjacent times. To date, no study has investigated the performance of two-fold FCS and standard MI methods for handling missing data in a time-varying covariate with a non-linear trajectory over time - a commonly encountered scenario in epidemiological studies. We simulated 1000 datasets of 5000 individuals based on the Longitudinal Study of Australian Children (LSAC). Three missing data mechanisms: missing completely at random (MCAR), and a weak and a strong missing at random (MAR) scenarios were used to impose missingness on body mass index (BMI) for age z-scores; a continuous time-varying exposure variable with a non-linear trajectory over time. We evaluated the performance of FCS, MVNI, and two-fold FCS for handling up to 50% of missing data when assessing the association between childhood obesity and sleep problems. The standard two-fold FCS produced slightly more biased and less precise estimates than FCS and MVNI. We observed slight improvements in bias and precision when using a time window width of two for the two-fold FCS algorithm compared to the standard width of one. We recommend the use of FCS or MVNI in a similar longitudinal setting, and when encountering convergence issues due to a large number of time points or variables with missing values, the two-fold FCS with exploration of a suitable time window.

Age-Related Decline of Wrist Position Sense and its Relationship to Specific Physical Training

PubMed Central

Van de Winckel, Ann; Tseng, Yu-Ting; Chantigian, Daniel; Lorant, Kaitlyn; Zarandi, Zinat; Buchanan, Jeffrey; Zeffiro, Thomas A.; Larson, Mia; Olson-Kellogg, Becky; Konczak, Jürgen; Keller-Ross, Manda L.

2017-01-01

Perception of limb and body positions is known as proprioception. Sensory feedback, especially from proprioceptive receptors, is essential for motor control. Aging is associated with a decline in position sense at proximal joints, but there is inconclusive evidence of distal joints being equally affected by aging. In addition, there is initial evidence that physical activity attenuates age-related decline in proprioception. Our objectives were, first, to establish wrist proprioceptive acuity in a large group of seniors and compare their perception to young adults, and second, to determine if specific types of training or regular physical activity are associated with preserved wrist proprioception. We recruited community-dwelling seniors (n = 107, mean age, 70 ± 5 years, range, 65–84 years) without cognitive decline (Mini Mental State Examination-brief version ≥13/16) and young adult students (n = 51, mean age, 20 ± 1 years, range, 19–26 years). Participants performed contralateral and ipsilateral wrist position sense matching tasks with a bimanual wrist manipulandum to a 15° flexion reference position. Systematic error or proprioceptive bias was computed as the mean difference between matched and reference position. The respective standard deviation over five trials constituted a measure of random error or proprioceptive precision. Current levels of physical activity and previous sport, musical, or dance training were obtained through a questionnaire. We employed longitudinal mixed effects linear models to calculate the effects of trial number, sex, type of matching task and age on wrist proprioceptive bias and precision. The main results were that relative proprioceptive bias was greater in older when compared to young adults (mean difference: 36% ipsilateral, 88% contralateral, p < 0.01). Proprioceptive precision for contralateral but not for ipsilateral matching was smaller in older than in young adults (mean difference: 38% contralateral, p < 0.01). Longer years of dance training were associated with smaller bias during ipsilateral matching (p < 0.01). Other types of training or physical activity levels did not affect bias or precision. Our findings demonstrate that aging is associated with a decline in proprioceptive bias in distal arm joints, but age does not negatively affect proprioceptive precision. Further, specific types of long-term dance related training may attenuate age-related decline in proprioceptive bias. PMID:29209188

Age-Related Decline of Wrist Position Sense and its Relationship to Specific Physical Training.

PubMed

Van de Winckel, Ann; Tseng, Yu-Ting; Chantigian, Daniel; Lorant, Kaitlyn; Zarandi, Zinat; Buchanan, Jeffrey; Zeffiro, Thomas A; Larson, Mia; Olson-Kellogg, Becky; Konczak, Jürgen; Keller-Ross, Manda L

2017-01-01

Perception of limb and body positions is known as proprioception. Sensory feedback, especially from proprioceptive receptors, is essential for motor control. Aging is associated with a decline in position sense at proximal joints, but there is inconclusive evidence of distal joints being equally affected by aging. In addition, there is initial evidence that physical activity attenuates age-related decline in proprioception. Our objectives were, first, to establish wrist proprioceptive acuity in a large group of seniors and compare their perception to young adults, and second, to determine if specific types of training or regular physical activity are associated with preserved wrist proprioception. We recruited community-dwelling seniors ( n = 107, mean age, 70 ± 5 years, range, 65-84 years) without cognitive decline (Mini Mental State Examination-brief version ≥13/16) and young adult students ( n = 51, mean age, 20 ± 1 years, range, 19-26 years). Participants performed contralateral and ipsilateral wrist position sense matching tasks with a bimanual wrist manipulandum to a 15° flexion reference position. Systematic error or proprioceptive bias was computed as the mean difference between matched and reference position. The respective standard deviation over five trials constituted a measure of random error or proprioceptive precision . Current levels of physical activity and previous sport, musical, or dance training were obtained through a questionnaire. We employed longitudinal mixed effects linear models to calculate the effects of trial number, sex, type of matching task and age on wrist proprioceptive bias and precision. The main results were that relative proprioceptive bias was greater in older when compared to young adults (mean difference: 36% ipsilateral, 88% contralateral, p < 0.01). Proprioceptive precision for contralateral but not for ipsilateral matching was smaller in older than in young adults (mean difference: 38% contralateral, p < 0.01). Longer years of dance training were associated with smaller bias during ipsilateral matching ( p < 0.01). Other types of training or physical activity levels did not affect bias or precision. Our findings demonstrate that aging is associated with a decline in proprioceptive bias in distal arm joints, but age does not negatively affect proprioceptive precision. Further, specific types of long-term dance related training may attenuate age-related decline in proprioceptive bias.

Soft tissue differentiation by diffuse reflectance spectroscopy

NASA Astrophysics Data System (ADS)

Zam, Azhar; Stelzle, Florian; Nkenke, Emeka; Tangermann-Gerk, Katja; Schmidt, Michael; Adler, Werner; Douplik, Alexandre

2009-07-01

Laser surgery gives the possibility to work remotely which leads to high precision, little trauma and high level sterility. However these advantages are coming with the lack of haptic feedback during the laser ablation of tissue. Therefore additional means are required to control tissue-specific ablation during laser surgery supporting the surgeon regardless of experience and skills. Diffuse Reflectance Spectroscopy provides a straightforward and simple approach for optical tissue differentiation. We measured diffuse reflectance from four various tissue types ex vivo. We applied Linear Discriminant Analysis (LDA) to differentiate the four tissue types and computed the area under the ROC curve (AUC). Special emphasis was taken on the identification of nerve as the most crucial tissue for maxillofacial surgery. The results show a promise for differentiating soft tissues as guidance for tissue-specific laser surgery by means of the diffuse reflectance.

High performance liquid chromatography: Tandem mass spectrometric determination of cisplatin levels in different visceral pleura layers of rats.

PubMed

Xia, Hui; Zhang, Wen; Li, Yingjie; Yu, Changhai

2015-05-01

The aim of the present study was to investigate the concentration of cisplatin in different layers of the visceral pleura in rats, following drug administration. In this study, a sensitive and specific liquid chromatography method coupled with electrospray ionization-tandem mass spectrometry was established to investigate the disposition of cisplatin in different layers of the visceral pleura in rats. Methodological data, including specificity, linearity, accuracy, recovery, precision and lower limits of quantification, confirmed that this novel method may be used to efficiently quantify the cisplatin concentrations in visceral pleura of rats following administration of the drug. Furthermore, the results demonstrated that the desired drug concentration was not achieved in the outer or inner elastic layers of the visceral pleura following injection with cisplatin through various administration methods.

High efficiency machining technology and equipment for edge chamfer of KDP crystals

NASA Astrophysics Data System (ADS)

Chen, Dongsheng; Wang, Baorui; Chen, Jihong

2016-10-01

Potassium dihydrogen phosphate (KDP) is a type of nonlinear optical crystal material. To Inhibit the transverse stimulated Raman scattering of laser beam and then enhance the optical performance of the optics, the edges of the large-sized KDP crystal needs to be removed to form chamfered faces with high surface quality (RMS<5 nm). However, as the depth of cut (DOC) of fly cutting is usually several, its machining efficiency is too low to be accepted for chamfering of the KDP crystal as the amount of materials to be removed is in the order of millimeter. This paper proposes a novel hybrid machining method, which combines precision grinding with fly cutting, for crackless and high efficiency chamfer of KDP crystal. A specialized machine tool, which adopts aerostatic bearing linear slide and aerostatic bearing spindle, was developed for chamfer of the KDP crystal. The aerostatic bearing linear slide consists of an aerostatic bearing guide with linearity of 0.1 μm/100mm and a linear motor to achieve linear feeding with high precision and high dynamic performance. The vertical spindle consists of an aerostatic bearing spindle with the rotation accuracy (axial) of 0.05 microns and Fork type flexible connection precision driving mechanism. The machining experiment on flying and grinding was carried out, the optimize machining parameters was gained by a series of experiment. Surface roughness of 2.4 nm has been obtained. The machining efficiency can be improved by six times using the combined method to produce the same machined surface quality.

Precision genome editing using CRISPR-Cas9 and linear repair templates in C. elegans.

PubMed

Paix, Alexandre; Folkmann, Andrew; Seydoux, Geraldine

2017-05-15

The ability to introduce targeted edits in the genome of model organisms is revolutionizing the field of genetics. State-of-the-art methods for precision genome editing use RNA-guided endonucleases to create double-strand breaks (DSBs) and DNA templates containing the edits to repair the DSBs. Following this strategy, we have developed a protocol to create precise edits in the C. elegans genome. The protocol takes advantage of two innovations to improve editing efficiency: direct injection of CRISPR-Cas9 ribonucleoprotein complexes and use of linear DNAs with short homology arms as repair templates. The protocol requires no cloning or selection, and can be used to generate base and gene-size edits in just 4days. Point mutations, insertions, deletions and gene replacements can all be created using the same experimental pipeline. Copyright © 2017 The Authors. Published by Elsevier Inc. All rights reserved.

Master-slave micromanipulator apparatus

DOEpatents

Morimoto, A.K.; Kozlowski, D.M.; Charles, S.T.; Spalding, J.A.

1999-08-31

An apparatus is disclosed based on precision X-Y stages that are stacked. Attached to arms projecting from each X-Y stage are a set of two axis gimbals. Attached to the gimbals is a rod, which provides motion along the axis of the rod and rotation around its axis. A dual-planar apparatus that provides six degrees of freedom of motion precise to within microns of motion. Precision linear stages along with precision linear motors, encoders, and controls provide a robotics system. The motors can be positioned in a remote location by incorporating a set of bellows on the motors and can be connected through a computer controller that will allow one to be a master and the other one to be a slave. Position information from the master can be used to control the slave. Forces of interaction of the slave with its environment can be reflected back to the motor control of the master to provide a sense of force sensed by the slave. Forces import onto the master by the operator can be fed back into the control of the slave to reduce the forces required to move it. 12 figs.

Master-slave micromanipulator method

DOEpatents

Morimoto, Alan K.; Kozlowski, David M.; Charles, Steven T.; Spalding, James A.

1999-01-01

A method based on precision X-Y stages that are stacked. Attached to arms projecting from each X-Y stage are a set of two axis gimbals. Attached to the gimbals is a rod, which provides motion along the axis of the rod and rotation around its axis. A dual-planar apparatus that provides six degrees of freedom of motion precise to within microns of motion. Precision linear stages along with precision linear motors, encoders, and controls provide a robotics system. The motors can be remotized by incorporating a set of bellows on the motors and can be connected through a computer controller that will allow one to be a master and the other one to be a slave. Position information from the master can be used to control the slave. Forces of interaction of the slave with its environment can be reflected back to the motor control of the master to provide a sense of force sensed by the slave. Forces import onto the master by the operator can be fed back into the control of the slave to reduce the forces required to move it.

Master-slave micromanipulator apparatus

DOEpatents

Morimoto, Alan K.; Kozlowski, David M.; Charles, Steven T.; Spalding, James A.

1999-01-01

An apparatus based on precision X-Y stages that are stacked. Attached to arms projecting from each X-Y stage are a set of two axis gimbals. Attached to the gimbals is a rod, which provides motion along the axis of the rod and rotation around its axis. A dual-planar apparatus that provides six degrees of freedom of motion precise to within microns of motion. Precision linear stages along with precision linear motors, encoders, and controls provide a robotics system. The motors can be positioned in a remote location by incorporating a set of bellows on the motors and can be connected through a computer controller that will allow one to be a master and the other one to be a slave. Position information from the master can be used to control the slave. Forces of interaction of the slave with its environment can be reflected back to the motor control of the master to provide a sense of force sensed by the slave. Forces import onto the master by the operator can be fed back into the control of the slave to reduce the forces required to move it.

Study on Fuzzy Adaptive Fractional Order PIλDμ Control for Maglev Guiding System

NASA Astrophysics Data System (ADS)

Hu, Qing; Hu, Yuwei

The mathematical model of the linear elevator maglev guiding system is analyzed in this paper. For the linear elevator needs strong stability and robustness to run, the integer order PID was expanded to the fractional order, in order to improve the steady state precision, rapidity and robustness of the system, enhance the accuracy of the parameter in fractional order PIλDμ controller, the fuzzy control is combined with the fractional order PIλDμ control, using the fuzzy logic achieves the parameters online adjustment. The simulations reveal that the system has faster response speed, higher tracking precision, and has stronger robustness to the disturbance.

Reference geometry-based detection of (4D-)CT motion artifacts: a feasibility study

NASA Astrophysics Data System (ADS)

Werner, René; Gauer, Tobias

2015-03-01

Respiration-correlated computed tomography (4D or 3D+t CT) can be considered as standard of care in radiation therapy treatment planning for lung and liver lesions. The decision about an application of motion management devices and the estimation of patient-specific motion effects on the dose distribution relies on precise motion assessment in the planning 4D CT data { which is impeded in case of CT motion artifacts. The development of image-based/post-processing approaches to reduce motion artifacts would benefit from precise detection and localization of the artifacts. Simple slice-by-slice comparison of intensity values and threshold-based analysis of related metrics suffer from- depending on the threshold- high false-positive or -negative rates. In this work, we propose exploiting prior knowledge about `ideal' (= artifact free) reference geometries to stabilize metric-based artifact detection by transferring (multi-)atlas-based concepts to this specific task. Two variants are introduced and evaluated: (S1) analysis and comparison of warped atlas data obtained by repeated non-linear atlas-to-patient registration with different levels of regularization; (S2) direct analysis of vector field properties (divergence, curl magnitude) of the atlas-to-patient transformation. Feasibility of approaches (S1) and (S2) is evaluated by motion-phantom data and intra-subject experiments (four patients) as well as - adopting a multi-atlas strategy- inter-subject investigations (twelve patients involved). It is demonstrated that especially sorting/double structure artifacts can be precisely detected and localized by (S1). In contrast, (S2) suffers from high false positive rates.

[Development and validation of event-specific quantitative PCR method for genetically modified maize LY038].

PubMed

Mano, Junichi; Masubuchi, Tomoko; Hatano, Shuko; Futo, Satoshi; Koiwa, Tomohiro; Minegishi, Yasutaka; Noguchi, Akio; Kondo, Kazunari; Akiyama, Hiroshi; Teshima, Reiko; Kurashima, Takeyo; Takabatake, Reona; Kitta, Kazumi

2013-01-01

In this article, we report a novel real-time PCR-based analytical method for quantitation of the GM maize event LY038. We designed LY038-specific and maize endogenous reference DNA-specific PCR amplifications. After confirming the specificity and linearity of the LY038-specific PCR amplification, we determined the conversion factor required to calculate the weight-based content of GM organism (GMO) in a multilaboratory evaluation. Finally, in order to validate the developed method, an interlaboratory collaborative trial according to the internationally harmonized guidelines was performed with blind DNA samples containing LY038 at the mixing levels of 0, 0.5, 1.0, 5.0 and 10.0%. The precision of the method was evaluated as the RSD of reproducibility (RSDR), and the values obtained were all less than 25%. The limit of quantitation of the method was judged to be 0.5% based on the definition of ISO 24276 guideline. The results from the collaborative trial suggested that the developed quantitative method would be suitable for practical testing of LY038 maize.

Precision magnetic suspension linear bearing

NASA Technical Reports Server (NTRS)

Trumper, David L.; Queen, Michael A.

1992-01-01

We have shown the design and analyzed the electromechanics of a linear motor suitable for independently controlling two suspension degrees of freedom. This motor, at least on paper, meets the requirements for driving an X-Y stage of 10 Kg mass with about 4 m/sq sec acceleration, with travel of several hundred millimeters in X and Y, and with reasonable power dissipation. A conceptual design for such a stage is presented. The theoretical feasibility of linear and planar bearings using single or multiple magnetic suspension linear motors is demonstrated.

Dynamic in-lake spawning migrations by female sockeye salmon

USGS Publications Warehouse

Young, Daniel B.; Woody, C.A.

2007-01-01

Precise homing by salmon to natal habitats is considered the primary mechanism in the evolution of population-specific traits, yet few studies have focused on this final phase of their spawning migration. We radio tagged 157 female sockeye salmon (Oncorhynchus nerka) as they entered Lake Clark, Alaska, and tracked them every 1-10 days to their spawning locations. Contrary to past research, no specific shoreline migration pattern was observed (e.g., clockwise) nor did fish enter a tributary unless they spawned in that tributary. Tributary spawning fish migrated faster (mean = 4.7 km??day-1, SD = 2.7, vs. 1.6 km??day-1, SD = 2.1) and more directly (mean linearity = 0.8, SD = 0.2, vs. 0.4, SD = 0.2) than Lake Clark beach spawning fish. Although radio-tagged salmon migrated to within 5 km of their final spawning location in an average of 21.2 days (SD = 13.2), some fish migrated five times the distance necessary and over 50 days to reach their spawning destination. These results demonstrate the dynamic nature of this final phase of migration and support studies indicating a higher degree of homing precision by tributary spawning fish. ?? Journal compilation 2007 Blackwell Munksgaard No claim to original US government works.

Active transport improves the precision of linear long distance molecular signalling

NASA Astrophysics Data System (ADS)

Godec, Aljaž; Metzler, Ralf

2016-09-01

Molecular signalling in living cells occurs at low copy numbers and is thereby inherently limited by the noise imposed by thermal diffusion. The precision at which biochemical receptors can count signalling molecules is intimately related to the noise correlation time. In addition to passive thermal diffusion, messenger RNA and vesicle-engulfed signalling molecules can transiently bind to molecular motors and are actively transported across biological cells. Active transport is most beneficial when trafficking occurs over large distances, for instance up to the order of 1 metre in neurons. Here we explain how intermittent active transport allows for faster equilibration upon a change in concentration triggered by biochemical stimuli. Moreover, we show how intermittent active excursions induce qualitative changes in the noise in effectively one-dimensional systems such as dendrites. Thereby they allow for significantly improved signalling precision in the sense of a smaller relative deviation in the concentration read-out by the receptor. On the basis of linear response theory we derive the exact mean field precision limit for counting actively transported molecules. We explain how intermittent active excursions disrupt the recurrence in the molecular motion, thereby facilitating improved signalling accuracy. Our results provide a deeper understanding of how recurrence affects molecular signalling precision in biological cells and novel medical-diagnostic devices.

A novel methodology for non-linear system identification of battery cells used in non-road hybrid electric vehicles

NASA Astrophysics Data System (ADS)

Unger, Johannes; Hametner, Christoph; Jakubek, Stefan; Quasthoff, Marcus

2014-12-01

An accurate state of charge (SoC) estimation of a traction battery in hybrid electric non-road vehicles, which possess higher dynamics and power densities than on-road vehicles, requires a precise battery cell terminal voltage model. This paper presents a novel methodology for non-linear system identification of battery cells to obtain precise battery models. The methodology comprises the architecture of local model networks (LMN) and optimal model based design of experiments (DoE). Three main novelties are proposed: 1) Optimal model based DoE, which aims to high dynamically excite the battery cells at load ranges frequently used in operation. 2) The integration of corresponding inputs in the LMN to regard the non-linearities SoC, relaxation, hysteresis as well as temperature effects. 3) Enhancements to the local linear model tree (LOLIMOT) construction algorithm, to achieve a physical appropriate interpretation of the LMN. The framework is applicable for different battery cell chemistries and different temperatures, and is real time capable, which is shown on an industrial PC. The accuracy of the obtained non-linear battery model is demonstrated on cells with different chemistries and temperatures. The results show significant improvement due to optimal experiment design and integration of the battery non-linearities within the LMN structure.

Near-optimal matrix recovery from random linear measurements.

PubMed

Romanov, Elad; Gavish, Matan

2018-06-25

In matrix recovery from random linear measurements, one is interested in recovering an unknown M-by-N matrix [Formula: see text] from [Formula: see text] measurements [Formula: see text], where each [Formula: see text] is an M-by-N measurement matrix with i.i.d. random entries, [Formula: see text] We present a matrix recovery algorithm, based on approximate message passing, which iteratively applies an optimal singular-value shrinker-a nonconvex nonlinearity tailored specifically for matrix estimation. Our algorithm typically converges exponentially fast, offering a significant speedup over previously suggested matrix recovery algorithms, such as iterative solvers for nuclear norm minimization (NNM). It is well known that there is a recovery tradeoff between the information content of the object [Formula: see text] to be recovered (specifically, its matrix rank r) and the number of linear measurements n from which recovery is to be attempted. The precise tradeoff between r and n, beyond which recovery by a given algorithm becomes possible, traces the so-called phase transition curve of that algorithm in the [Formula: see text] plane. The phase transition curve of our algorithm is noticeably better than that of NNM. Interestingly, it is close to the information-theoretic lower bound for the minimal number of measurements needed for matrix recovery, making it not only state of the art in terms of convergence rate, but also near optimal in terms of the matrices it successfully recovers. Copyright © 2018 the Author(s). Published by PNAS.

Image guided IMRT dosimetry using anatomy specific MOSFET configurations.

PubMed

Amin, Md Nurul; Norrlinger, Bern; Heaton, Robert; Islam, Mohammad

2008-06-23

We have investigated the feasibility of using a set of multiple MOSFETs in conjunction with the mobile MOSFET wireless dosimetry system, to perform a comprehensive and efficient quality assurance (QA) of IMRT plans. Anatomy specific MOSFET configurations incorporating 5 MOSFETs have been developed for a specially designed IMRT dosimetry phantom. Kilovoltage cone beam computed tomography (kV CBCT) imaging was used to increase the positional precision and accuracy of the detectors and phantom, and so minimize dosimetric uncertainties in high dose gradient regions. The effectiveness of the MOSFET based dose measurements was evaluated by comparing the corresponding doses measured by an ion chamber. For 20 head and neck IMRT plans the agreement between the MOSFET and ionization chamber dose measurements was found to be within -0.26 +/- 0.88% and 0.06 +/- 1.94% (1 sigma) for measurement points in the high dose and low dose respectively. A precision of 1 mm in detector positioning was achieved by using the X-Ray Volume Imaging (XVI) kV CBCT system available with the Elekta Synergy Linear Accelerator. Using the anatomy specific MOSFET configurations, simultaneous measurements were made at five strategically located points covering high dose and low dose regions. The agreement between measurements and calculated doses by the treatment planning system for head and neck and prostate IMRT plans was found to be within 0.47 +/- 2.45%. The results indicate that a cylindrical phantom incorporating multiple MOSFET detectors arranged in an anatomy specific configuration, in conjunction with image guidance, can be utilized to perform a comprehensive and efficient quality assurance of IMRT plans.

Research on the precision measurement of super-low reflectivity

NASA Astrophysics Data System (ADS)

Yuan, Hao-yu; Lu, Zong-gui; Xia, Yan-wen; Peng, Zhi-tao; Liu, Hua; Xu, Long-bo; Sun, Zhi-hong; Tang, Jun

2010-10-01

Introduced a high-precision measurement of measured the super-low reflectivity and small sampling angle. Using single reflect way measured, and compare with re-swatch. Testing the reflectance of the sampling mirror which be used on TIL, and analyze the error. Research results indicate, the main factor which affect result is energy detector error and energy detector linearity. This methods is easy and have high-precision, it can be used to measure the super-low reflectivity sampling mirror reflectance.

Imprints of dark energy on cosmic structure formation - I. Realistic quintessence models and the non-linear matter power spectrum

NASA Astrophysics Data System (ADS)

Alimi, J.-M.; Füzfa, A.; Boucher, V.; Rasera, Y.; Courtin, J.; Corasaniti, P.-S.

2010-01-01

Quintessence has been proposed to account for dark energy (DE) in the Universe. This component causes a typical modification of the background cosmic expansion, which, in addition to its clustering properties, can leave a potentially distinctive signature on large-scale structures. Many previous studies have investigated this topic, particularly in relation to the non-linear regime of structure formation. However, no careful pre-selection of viable quintessence models with high precision cosmological data was performed. Here we show that this has led to a misinterpretation (and underestimation) of the imprint of quintessence on the distribution of large-scale structures. To this purpose, we perform a likelihood analysis of the combined Supernova Ia UNION data set and Wilkinson Microwave Anisotropy Probe 5-yr data to identify realistic quintessence models. These are specified by different model parameter values, but still statistically indistinguishable from the vanilla Λ cold dark matter (ΛCDM). Differences are especially manifest in the predicted amplitude and shape of the linear matter power spectrum though these remain within the uncertainties of the Sloan Digital Sky Survey data. We use these models as a benchmark for studying the clustering properties of dark matter haloes by performing a series of high-resolution N-body simulations. In this first paper, we specifically focus on the non-linear matter power spectrum. We find that realistic quintessence models allow for relevant differences of the dark matter distribution with respect to the ΛCDM scenario well into the non-linear regime, with deviations of up to 40 per cent in the non-linear power spectrum. Such differences are shown to depend on the nature of DE, as well as the scale and epoch considered. At small scales (k ~ 1-5hMpc-1, depending on the redshift), the structure formation process is about 20 per cent more efficient than in ΛCDM. We show that these imprints are a specific record of the cosmic structure formation history in DE cosmologies and therefore cannot be accounted for in standard fitting functions of the non-linear matter power spectrum.

MIrExpress: A Database for Gene Coexpression Correlation in Immune Cells Based on Mutual Information and Pearson Correlation

PubMed Central

Wang, Luman; Mo, Qiaochu; Wang, Jianxin

2015-01-01

Most current gene coexpression databases support the analysis for linear correlation of gene pairs, but not nonlinear correlation of them, which hinders precisely evaluating the gene-gene coexpression strengths. Here, we report a new database, MIrExpress, which takes advantage of the information theory, as well as the Pearson linear correlation method, to measure the linear correlation, nonlinear correlation, and their hybrid of cell-specific gene coexpressions in immune cells. For a given gene pair or probe set pair input by web users, both mutual information (MI) and Pearson correlation coefficient (r) are calculated, and several corresponding values are reported to reflect their coexpression correlation nature, including MI and r values, their respective rank orderings, their rank comparison, and their hybrid correlation value. Furthermore, for a given gene, the top 10 most relevant genes to it are displayed with the MI, r, or their hybrid perspective, respectively. Currently, the database totally includes 16 human cell groups, involving 20,283 human genes. The expression data and the calculated correlation results from the database are interactively accessible on the web page and can be implemented for other related applications and researches. PMID:26881263

Programmable Quantitative DNA Nanothermometers.

PubMed

Gareau, David; Desrosiers, Arnaud; Vallée-Bélisle, Alexis

2016-07-13

Developing molecules, switches, probes or nanomaterials that are able to respond to specific temperature changes should prove of utility for several applications in nanotechnology. Here, we describe bioinspired strategies to design DNA thermoswitches with programmable linear response ranges that can provide either a precise ultrasensitive response over a desired, small temperature interval (±0.05 °C) or an extended linear response over a wide temperature range (e.g., from 25 to 90 °C). Using structural modifications or inexpensive DNA stabilizers, we show that we can tune the transition midpoints of DNA thermometers from 30 to 85 °C. Using multimeric switch architectures, we are able to create ultrasensitive thermometers that display large quantitative fluorescence gains within small temperature variation (e.g., > 700% over 10 °C). Using a combination of thermoswitches of different stabilities or a mix of stabilizers of various strengths, we can create extended thermometers that respond linearly up to 50 °C in temperature range. Here, we demonstrate the reversibility, robustness, and efficiency of these programmable DNA thermometers by monitoring temperature change inside individual wells during polymerase chain reactions. We discuss the potential applications of these programmable DNA thermoswitches in various nanotechnology fields including cell imaging, nanofluidics, nanomedecine, nanoelectronics, nanomaterial, and synthetic biology.

MIrExpress: A Database for Gene Coexpression Correlation in Immune Cells Based on Mutual Information and Pearson Correlation.

PubMed

Wang, Luman; Mo, Qiaochu; Wang, Jianxin

2015-01-01

Most current gene coexpression databases support the analysis for linear correlation of gene pairs, but not nonlinear correlation of them, which hinders precisely evaluating the gene-gene coexpression strengths. Here, we report a new database, MIrExpress, which takes advantage of the information theory, as well as the Pearson linear correlation method, to measure the linear correlation, nonlinear correlation, and their hybrid of cell-specific gene coexpressions in immune cells. For a given gene pair or probe set pair input by web users, both mutual information (MI) and Pearson correlation coefficient (r) are calculated, and several corresponding values are reported to reflect their coexpression correlation nature, including MI and r values, their respective rank orderings, their rank comparison, and their hybrid correlation value. Furthermore, for a given gene, the top 10 most relevant genes to it are displayed with the MI, r, or their hybrid perspective, respectively. Currently, the database totally includes 16 human cell groups, involving 20,283 human genes. The expression data and the calculated correlation results from the database are interactively accessible on the web page and can be implemented for other related applications and researches.

Segmentation of vessel-like patterns using mathematical morphology and curvature evaluation.

PubMed

Zana, F; Klein, J C

2001-01-01

This paper presents an algorithm based on mathematical morphology and curvature evaluation for the detection of vessel-like patterns in a noisy environment. Such patterns are very common in medical images. Vessel detection is interesting for the computation of parameters related to blood flow. Its tree-like geometry makes it a usable feature for registration between images that can be of a different nature. In order to define vessel-like patterns, segmentation is performed with respect to a precise model. We define a vessel as a bright pattern, piece-wise connected, and locally linear, mathematical morphology is very well adapted to this description, however other patterns fit such a morphological description. In order to differentiate vessels from analogous background patterns, a cross-curvature evaluation is performed. They are separated out as they have a specific Gaussian-like profile whose curvature varies smoothly along the vessel. The detection algorithm that derives directly from this modeling is based on four steps: (1) noise reduction; (2) linear pattern with Gaussian-like profile improvement; (3) cross-curvature evaluation; (4) linear filtering. We present its theoretical background and illustrate it on real images of various natures, then evaluate its robustness and its accuracy with respect to noise.

Evaluation of empirical rule of linearly correlated peptide selection (ERLPS) for proteotypic peptide-based quantitative proteomics.

PubMed

Liu, Kehui; Zhang, Jiyang; Fu, Bin; Xie, Hongwei; Wang, Yingchun; Qian, Xiaohong

2014-07-01

Precise protein quantification is essential in comparative proteomics. Currently, quantification bias is inevitable when using proteotypic peptide-based quantitative proteomics strategy for the differences in peptides measurability. To improve quantification accuracy, we proposed an "empirical rule for linearly correlated peptide selection (ERLPS)" in quantitative proteomics in our previous work. However, a systematic evaluation on general application of ERLPS in quantitative proteomics under diverse experimental conditions needs to be conducted. In this study, the practice workflow of ERLPS was explicitly illustrated; different experimental variables, such as, different MS systems, sample complexities, sample preparations, elution gradients, matrix effects, loading amounts, and other factors were comprehensively investigated to evaluate the applicability, reproducibility, and transferability of ERPLS. The results demonstrated that ERLPS was highly reproducible and transferable within appropriate loading amounts and linearly correlated response peptides should be selected for each specific experiment. ERLPS was used to proteome samples from yeast to mouse and human, and in quantitative methods from label-free to O18/O16-labeled and SILAC analysis, and enabled accurate measurements for all proteotypic peptide-based quantitative proteomics over a large dynamic range. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analog-to-digital conversion techniques for precision photometry

NASA Technical Reports Server (NTRS)

Opal, Chet B.

1988-01-01

Three types of analog-to-digital converters are described: parallel, successive-approximation, and integrating. The functioning of comparators and sample-and-hold amplifiers is explained. Differential and integral linearity are defined, and good and bad examples are illustrated. The applicability and relative advantages of the three types of converters for precision astronomical photometric measurements are discussed. For most measurements, integral linearity is more important than differential linearity. Successive-approximation converters should be used with multielement solid state detectors because of their high speed, but dual slope integrating converters may be superior for use with single element solid state detectors where speed of digitization is not a factor. In all cases, the input signal should be tailored so that they occupy the upper part of the converter's dynamic range; this can be achieved by providing adjustable gain, or better by varying the integration time of the observation if possible.

Precision Magnetic Bearing Six Degree of Freedom Stage

NASA Technical Reports Server (NTRS)

Williams, M. E.; Trumper, David L.

1996-01-01

Magnetic bearings are capable of applying force and torque to a suspended object without rigidly constraining any degrees of freedom. Additionally, the resolution of magnetic bearings is limited only by sensors and control, and not by the finish of a bearing surface. For these reasons, magnetic bearings appear to be ideal for precision wafer positioning in lithography systems. To demonstrate this capability a linear magnetic bearing has been constructed which uses variable reluctance actuators to control the motion of a 14.5 kg suspended platen in five degrees of freedom. A Lorentz type linear motor of our own design and construction is used to provide motion and position control in the sixth degree of freedom. The stage performance results verify that the positioning requirements of photolithography can be met with a system of this type. This paper describes the design, control, and performance of the linear magnetic bearing.

Theory, simulation and experiments for precise deflection control of radiotherapy electron beams.

PubMed

Figueroa, R; Leiva, J; Moncada, R; Rojas, L; Santibáñez, M; Valente, M; Velásquez, J; Young, H; Zelada, G; Yáñez, R; Guillen, Y

2018-03-08

Conventional radiotherapy is mainly applied by linear accelerators. Although linear accelerators provide dual (electron/photon) radiation beam modalities, both of them are intrinsically produced by a megavoltage electron current. Modern radiotherapy treatment techniques are based on suitable devices inserted or attached to conventional linear accelerators. Thus, precise control of delivered beam becomes a main key issue. This work presents an integral description of electron beam deflection control as required for novel radiotherapy technique based on convergent photon beam production. Theoretical and Monte Carlo approaches were initially used for designing and optimizing device´s components. Then, dedicated instrumentation was developed for experimental verification of electron beam deflection due to the designed magnets. Both Monte Carlo simulations and experimental results support the reliability of electrodynamics models used to predict megavoltage electron beam control. Copyright © 2018 Elsevier Ltd. All rights reserved.

Accuracy of the Precision® point-of-care ketone test examined by liquid chromatography tandem-mass spectrometry (LC-MS/MS) in the same fingerstick sample.

PubMed

Janssen, Marcel J W; Hendrickx, Ben H E; Habets-van der Poel, Carin D; van den Bergh, Joop P W; Haagen, Anton A M; Bakker, Jaap A

2010-12-01

The Precision(®) (Abbott Diabetes Care) point-of-care biosensor test strips are widely used by patients with diabetes and clinical laboratories for measurement of plasma β-hydroxybutyrate (β-HB) concentrations in capillary blood samples obtained by fingerstick. In the literature, this procedure has been validated only against the enzymatic determination of β-HB in venous plasma, i.e., the method to which the Precision(®) has been calibrated. In this study, the Precision(®) Xceed was compared to a methodologically different and superior procedure: determination of β-HB by liquid chromatography tandem-mass spectrometry (LC-MS/MS) in capillary blood spots. Blood spots were obtained from the same fingerstick sample from out of which Precision(®) measurements were performed. Linearity was tested by adding varying amounts of standard to an EDTA venous whole blood matrix. The Precision(®) was in good agreement with LC-MS/MS within the measuring range of 0.0-6.0 mmol/L (Passing and Bablok regression: slope=1.20 and no significant intercept, R=0.97, n=59). Surprisingly, the Precision(®) showed non-linearity and full saturation at concentrations above 6.0 mmol/L, which were confirmed by a standard addition experiment. Results obtained at the saturation level varied between 3.0 and 6.5 mmol/L. The Precision(®) β-HB test strips demonstrate good comparison with LC-MS/MS. Inter-individual variation around the saturation level, however, is large. Therefore, we advise reporting readings above 3.0 as >3.0 mmol/L. The test is valid for use in the clinically relevant range of 0.0-3.0 mmol/L.

Prevention and control of emergent infectious disease with high specific antigen sensor.

PubMed

Zhang, Hongzhe; Zhang, Shanshan; Liu, Nan

2017-11-01

This study aims to evaluate the application of a new type of high specificity antigen sensor in detecting the viruses in sudden infectious diseases. Influenza A (H1N1) virus immunosensor was used for the respective determination of the six kinds of antigens of H1N1, H3N2 viral protein, HA protein of H7N9, influenza B virus, adenovirus, and EV71 virus of same dilution degree on the Screen Printed Carbon Electrode (SPCE), so as to test the specificity of the detection method. In addition, various batches of chick embryo allantoic saliva dilution simulation samples were also detected on their recovery (accuracy), repeatability (precision), and stability. The results were as follows: the linear equation was y = 121.33x + 168; the slope of the linear equation was 121.33 nA/HA unit, representing the sensitivity; correlation coefficient was R 2 =0.9921 > 0.90. Using Statistical Analysis System (SAS) software, we found that: the W values of seven sets of data after Shapiro-Wilk detection were 0.853, 0.991, 0.901, 0.906, 0.825, 0.974, and 0.992, respectively; P values were 0.247, 0.831, 0.386, 0.405, 0.174, 0.691, and 0.821, respectively, all of which were greater than 0.05, suggesting that normality was met. The results of homogeneity test for variance were as follows: F = 2.44, P = 0.0775 > 0.05, suggesting that homogeneity of variance was met. The parametric test results were as follows: F = 19114.0, P < 0.0001, suggesting that there were obvious differences between testing data of the seven groups. The determination recovery rate of electrochemical immunosensor was 80-110%. Relative Standard Deviation (RSD) values of repeatability (precision) test of H1N1 influenza virus electrochemical immunosensor were 7.74%, 3.54%, and 2.01%, all of which were smaller than 10%. The signal response of H1N1 electrochemical immune biological sensor could still maintain more than 85% of the original signal within 30 days of storage. In conclusion, H1N1 electrochemical immune biosensor has good specificity and the test results are not affected by other viruses of the same type. Besides, it has good accuracy which can realize the accurate determination of A (H1N1) influenza virus in actual detection. Thus, the requirement of precision measurement of A (H1N1) flu virus detection can be met. Therefore, H1N1 electrochemical immune biosensors can be used in actual detection with good stability.

Classical and sequential limit analysis revisited

NASA Astrophysics Data System (ADS)

Leblond, Jean-Baptiste; Kondo, Djimédo; Morin, Léo; Remmal, Almahdi

2018-04-01

Classical limit analysis applies to ideal plastic materials, and within a linearized geometrical framework implying small displacements and strains. Sequential limit analysis was proposed as a heuristic extension to materials exhibiting strain hardening, and within a fully general geometrical framework involving large displacements and strains. The purpose of this paper is to study and clearly state the precise conditions permitting such an extension. This is done by comparing the evolution equations of the full elastic-plastic problem, the equations of classical limit analysis, and those of sequential limit analysis. The main conclusion is that, whereas classical limit analysis applies to materials exhibiting elasticity - in the absence of hardening and within a linearized geometrical framework -, sequential limit analysis, to be applicable, strictly prohibits the presence of elasticity - although it tolerates strain hardening and large displacements and strains. For a given mechanical situation, the relevance of sequential limit analysis therefore essentially depends upon the importance of the elastic-plastic coupling in the specific case considered.

Development and validation of RP-UHPLC procedure for estimation of 5-amino salicyclic acid in 5-amino salicyclic acid rectal suppositories

NASA Astrophysics Data System (ADS)

Balaji, Jayagopal; Shivashankar, Murugesh

2017-11-01

The present study describes a simple and robust reverse phase ultra performance liquid chromatography (RP-UPLC) method for the quantification of 5-amino salicyclic acid in 5-amino salicyclic acid rectal capsules. Successful separation of Mesalamine peak from excipient peaks and diluent were achieved on a Acquity C8 (50 × 2.1 mm, 1.7 μm) and UV detector at 254 nm, 0.3 mL/min as a flow rate, and 3 μL as an injection volume. For the RP-UPLC method, phosphate buffer and methanol was used as mobile phases at ratio of 83:17 and the column temperature was 25 °C. Percentage recovery obtained in the range of 98.7 - 99.7 % and the method is linear for Mesalamine for specified concentration range with coefficient of variation (r) not less than 0.99. The proposed RP-UPLC method was found to be specific, linear, precise, accurate and robust.

Characterization of the International Linear Collider damping ring optics

NASA Astrophysics Data System (ADS)

Shanks, J.; Rubin, D. L.; Sagan, D.

2014-10-01

A method is presented for characterizing the emittance dilution and dynamic aperture for an arbitrary closed lattice that includes guide field magnet errors, multipole errors and misalignments. This method, developed and tested at the Cornell Electron Storage Ring Test Accelerator (CesrTA), has been applied to the damping ring lattice for the International Linear Collider (ILC). The effectiveness of beam based emittance tuning is limited by beam position monitor (BPM) measurement errors, number of corrector magnets and their placement, and correction algorithm. The specifications for damping ring magnet alignment, multipole errors, number of BPMs, and precision in BPM measurements are shown to be consistent with the required emittances and dynamic aperture. The methodology is then used to determine the minimum number of position monitors that is required to achieve the emittance targets, and how that minimum depends on the location of the BPMs. Similarly, the maximum tolerable multipole errors are evaluated. Finally, the robustness of each BPM configuration with respect to random failures is explored.

AUTOMOTIVE DIESEL MAINTENANCE 1. UNIT X, USE OF MEASURING TOOLS IN DIESEL MAINTENANCE.

ERIC Educational Resources Information Center

Human Engineering Inst., Cleveland, OH.

THIS MODULE OF A 30-MODULE COURSE IS DESIGNED TO DEVELOP AN UNDERSTANDING OF THE PRECISION MEASURING TOOLS USED IN DIESEL ENGINE MAINTENANCE. TOPICS ARE (1) LINEAR MEASURE, (2) MEASURING WITH RULES AND TAPES, (3) GETTING PRECISION WITH MICROMETERS, (4) DIAL INDICATORS, (5) TACHOMETERS, (6) TORQUE WRENCH, (7) THICKNESS (TECHER) GAGE, AND (8) VALVE…

Movement Precision and Amplitude as Separate Factors in the Control of Movement.

ERIC Educational Resources Information Center

Kerr, Robert

The purpose of this study was to assess Welford's dual controlling factor interpretation of Fitts' Law--describing movement time as being a linear function of movement distance (or amplitude) and the required precision of the movement (or target width). Welford's amplification of the theory postulates that two separate processes ought to be…

A high-throughput LC-MS/MS screen for GHRP in equine and human urine, featuring peptide derivatization for improved chromatography.

PubMed

Timms, Mark; Hall, Nikki; Levina, Vita; Vine, John; Steel, Rohan

2014-10-01

The growth hormone releasing peptides (GHRPs) hexarelin, ipamorelin, alexamorelin, GHRP-1, GHRP-2, GHRP-4, GHRP-5, and GHRP-6 are all synthetic met-enkephalin analogues that include unnatural D-amino acids. They were designed specifically for their ability to stimulate growth hormone release and may serve as performance enhancing drugs. To regulate the use of these peptides within the horse racing industry and by human athletes, a method is presented for the extraction, derivatization, and detection of GHRPs from equine and human urine. This method takes advantage of a highly specific solid-phase extraction combined with a novel derivatization method to improve the chromatography of basic peptides. The method was validated with respect to linearity, repeatability, intermediate precision, specificity, limits of detection, limits of confirmation, ion suppression, and stability. As proof of principle, all eight GHRPs or their metabolites could be detected in urine collected from rats after intravenous administration. Copyright © 2014 John Wiley & Sons, Ltd.

Complement dependent cytotoxicity (CDC) activity of a humanized anti Lewis-Y antibody: FACS-based assay versus the 'classical' radioactive method -- qualification, comparison and application of the FACS-based approach.

PubMed

Nechansky, A; Szolar, O H J; Siegl, P; Zinoecker, I; Halanek, N; Wiederkum, S; Kircheis, R

2009-05-01

The fully humanized Lewis-Y carbohydrate specific monoclonal antibody (mAb) IGN311 is currently tested in a passive immunotherapy approach in a clinical phase I trail and therefore regulatory requirements demand qualified assays for product analysis. To demonstrate the functionality of its Fc-region, the capacity of IGN311 to mediate complement dependent cytotoxicity (CDC) against human breast cancer cells was evaluated. The "classical" radioactive method using chromium-51 and a FACS-based assay were established and qualified according to ICH guidelines. Parameters evaluated were specificity, response function, bias, repeatability (intra-day precision), intermediate precision (operator-time different), and linearity (assay range). In the course of a fully nested design, a four-parameter logistic equation was identified as appropriate calibration model for both methods. For the radioactive assay, the bias ranged from -6.1% to -3.6%. The intermediate precision for future means of duplicate measurements revealed values from 12.5% to 15.9% and the total error (beta-expectation tolerance interval) of the method was found to be <40%. For the FACS-based assay, the bias ranged from -8.3% to 0.6% and the intermediate precision for future means of duplicate measurements revealed values from 4.2% to 8.0%. The total error of the method was found to be <25%. The presented data demonstrate that the FACS-based CDC is more accurate than the radioactive assay. Also, the elimination of radioactivity and the 'real-time' counting of apoptotic cells further justifies the implementation of this method which was subsequently applied for testing the influence of storage at 4 degrees C and 25 degrees C ('stability testing') on the potency of IGN311 drug product. The obtained results demonstrate that the qualified functional assay represents a stability indicating test method.

An ultraviolet-spectrophotometric method for the determination of glimepiride in solid dosage forms.

PubMed

Afieroho, Ozadheoghene E; Okorie, Ogbonna; Okonkwo, Tochukwu J N

2011-06-01

Considering the cost of acquiring a liquid chromatographic instrument in underdeveloped economies, the rising incidence of diabetes mellitus, the need to evaluate the quality performance of glimepiride generics, and the need for less toxic processes, this research is an imperative. The method was validated for linearity, recovery accuracy, intra- and inter-day precision, specificity in the presence of excipients, and inter-day stability under laboratory conditions. Student's t test at the 95% confidence limit was used for statistics. Using 96% ethanol as solvent, a less toxic and cost-effective spectrophotometric method for the determination of glimepiride in solid dosage forms was developed and validated. The results of the validated parameters showed a λ(max) of 231 nm, linearity range of 0.5-22 μg/mL, precision with relative SD of <1.0%, recovery accuracy of 100.8%, regression equation of y = 45.741x + 0.0202, R(2) = 0.999, limit of detection of 0.35 μg/mL, and negligible interference from common excipients and colorants. The method was found to be accurate at the 95% confidence limit compared with the standard liquid chromatographic method with comparable reproducibility when used to assay the formulated products Amaryl(®) (sanofi-aventis, Paris, France) and Mepyril(®) (May & Baker Nigeria PLC, Ikeja, Nigeria). The results obtained for the validated parameters were within allowable limits. This method is recommended for routine quality control analysis.

Simultaneous determination of bifonazole and tinctures of calendula flower in pharmaceutical creams by reversed-phase liquid chromatography.

PubMed

Ferreyra, Carola F; Ortiz, Cristina S

2005-01-01

The aim of this research was to develop and validate a sensitive, rapid, easy, and precise reversed-phase liquid chromatography (LC) method for stability studies of bifonazole (I) formulated with tinctures of calendula flower (II). The method was especially developed for the analysis and quantitative determination of I and II in pure and combined forms in cream pharmaceutical formulations without using gradient elution and at room temperature. The influence on the stability of compound I of temperature, artificial radiation, and drug II used for the new pharmaceutical design was evaluated. The LC separation was carried out using a Supelcosil LC-18 column (25 cm x 4.6 mm id, 5 microm particle size); the mobile phase was composed of methanol-0.1 M ammonium acetate buffer (85 + 15, v/v) pumped isocratically at a flow rate of 1 mL/min; and ultraviolet detection was at 254 nm. The analysis time was less than 10 min. Calibration graphs were found to be linear in the 0.125-0.375 mg/mL (rI = 0.9991) and 0.639-1.916 mg/mL (rII = 0.9995) ranges for I and II, respectively. The linearity, precision, recovery, and limits of detection and quantification were satisfactory for I and II. The results obtained suggested that the developed LC method is selective and specific for the analysis of I and II in pharmaceutical products, and that it can be applied to stability studies.

Stability-indicating method for simultaneous estimation of olmesartan medoxomile, amlodipine besylate and hydrochlorothiazide by RP-HPLC in tablet dosage form.

PubMed

Jain, P S; Patel, M K; Gorle, A P; Chaudhari, A J; Surana, S J

2012-09-01

A simple, specific, accurate and precise stability-indicating reversed-phase high-performance liquid chromatographic method was developed for simultaneous estimation of olmesartan medoxomile (OLME), amlodipine besylate (AMLO) and hydrochlorothiazide (HCTZ) in tablet dosage form. The method was developed using an RP C18 base deactivated silica column (250 × 4.6 mm, 5 µm) with a mobile phase consisting of triethylamine (pH 3.0) adjusted with orthophosphoric acid (A) and acetonitrile (B), with a timed gradient program of T/%B: 0/30, 7/70, 8/30, 10/30 with a flow rate of 1.4 mL/min. Ultraviolet detection was used at 236 nm. The retention times for OLME, AMLO and HCTZ were found to be 6.72, 4.28 and 2.30, respectively. The proposed method was validated for precision, accuracy, linearity, range, robustness, ruggedness and force degradation study. The calibration curves of OLME, AMLO and HCTZ were linear over the range of 50-150, 12.5-37.5 and 31-93 µg/mL, respectively. The method was found to be sensitive. The limits of detection of OLME, AMLO and HCTZ were determined 0.19, 0.16 and 0.22 µg/mL and limits of quantification of OLME, AMLO and HCTZ were determined 0.57, 0.49 and 0.66, respectively. Forced degradation study was performed according to International Conference on Harmonization guidelines.

Development and validation of a rapid reverse-phase HPLC method for the determination of methotrexate from nanostructured liquid crystalline systems.

PubMed

Zuben, E S Von; Oliveira, A G; Chorilli, M; Scarpa, M V

2018-03-05

A reversed-phase liquid chromatography (RP-LC) method was successfully developed and validated for the determination of methotrexate in nanostructured liquid crystalline systems composed by polyether functional siloxane and silicone polyether copolymer. The LC method was performed on RP C18-ODS column, Agilent Zorbax® (4.6 x 250 mm, 5 μm), maintained at room temperature, with a mobile phase constituted by a mixture of 50 mM ammonium acetate buffer (pH 6.0) and methanol (77:23,v/v) with a flow rate of 1.0 mL/min, using ultraviolet detection at 313 nm. The parameters used in the validation process were linearity, specificity, intra and inter-day precision, accuracy, robustness. The quantitation and detection limits yielded good results. The calibration plot assumed linear behavior from 5.0-150.0 μg. mL-1 (r2 = 0.9999). The methotrexate was subjected to oxidation, acid, base and neutral degradation, photolysis and heat as stress conditions. There were no interfering peaks at or near the retention time of methotrexate. The nanostructured liquid crystalline systems did not interfere with the analysis and the recovery was quantitative. The intra and inter-day assay relative standard deviation were less than 0.20 %. The method developed proved to be simple, sensitive, accurate, precise, reproducible and therefore adequate for routine analysis of methotrexate in nanostructured liquid crystalline systems.

Validated spectrofluorimetric methods for the determination of apixaban and tirofiban hydrochloride in pharmaceutical formulations.

PubMed

El-Bagary, Ramzia I; Elkady, Ehab F; Farid, Naira A; Youssef, Nadia F

2017-03-05

Apixaban and Tirofiban Hydrochloride are low molecular weight anticoagulants. The two drugs exhibit native fluorescence that allow the development of simple and valid spectrofluorimetric methods for the determination of Apixaban at λ ex/λ em=284/450nm and tirofiban HCl at λ ex/λ em=227/300nm in aqueous media. Different experimental parameters affecting fluorescence intensities were carefully studied and optimized. The fluorescence intensity-concentration plots were linear over the ranges of 0.2-6μgml -1 for apixaban and 0.2-5μgml -1 for tirofiban HCl. The limits of detection were 0.017 and 0.019μgml -1 and quantification limits were 0.057 and 0.066μgml -1 for apixaban and tirofiban HCl, respectively. The fluorescence quantum yield of apixaban and tirofiban were calculated with values of 0.43 and 0.49. Method validation was evaluated for linearity, specificity, accuracy, precision and robustness as per ICH guidelines. The proposed spectrofluorimetric methods were successfully applied for the determination of apixaban in Eliquis tablets and tirofiban HCl in Aggrastat intravenous infusion. Tolerance ratio was tested to study the effect of foreign interferences from dosage forms excipients. Using Student's t and F tests, revealed no statistically difference between the developed spectrofluorimetric methods and the comparison methods regarding the accuracy and precision, so can be contributed to the analysis of apixaban and tirofiban HCl in QC laboratories as an alternative method. Copyright © 2016 Elsevier B.V. All rights reserved.

A UPLC-MS/MS method for simultaneous determination of five flavonoids from Stellera chamaejasme L. in rat plasma and its application to a pharmacokinetic study.

PubMed

Li, Yun-Qing; Li, Cheng-Jian; Lv, Lei; Cao, Qing-Qing; Qian, Xian; Li, Si Wei; Wang, Hui; Zhao, Liang

2018-06-01

Stellera chamaejasme L. has been used as a traditional Chinese medicine for the treatment of scabies, tinea, stubborn skin ulcers, chronic tracheitis, cancer and tuberculosis. A sensitive and selective ultra-high liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the simultaneous determination of five flavonoids (stelleranol, chamaechromone, neochamaejasmin A, chamaejasmine and isochamaejasmin) of S. chamaejasme L. in rat plasma. Chromatographic separation was accomplished on an Agilent Poroshell 120 EC-C 18 column (2.1 × 100 mm, 2.7 μm) with gradient elution at a flow rate of 0.4 mL/min and the total analysis time was 7 min. The analytes were detected using multiple reaction monitoring in positive ionization mode. The samples were prepared by liquid-liquid extraction with ethyl acetate. The UPLC-MS/MS method was validated for specificity, linearity, sensitivity, accuracy and precision, recovery, matrix effect and stability. The validated method exhibited good linearity (r ≥ 0.9956), and the lower limits of quantification ranged from 0.51 to 0.64 ng/mL for five flavonoids. The intra- and inter-day precision were both <10.2%, and the accuracy ranged from -11.79 to 9.21%. This method was successfully applied to a pharmacokinetic study of five flavonoids in rats after oral administration of ethyl acetate extract of S. chamaejasme L. Copyright © 2018 John Wiley & Sons, Ltd.

Quality by design: a systematic and rapid liquid chromatography and mass spectrometry method for eprosartan mesylate and its related impurities using a superficially porous particle column.

PubMed

Kalariya, Pradipbhai D; Kumar Talluri, Murali V N; Gaitonde, Vinay D; Devrukhakar, Prashant S; Srinivas, Ragampeta

2014-08-01

The present work describes the systematic development of a robust, precise, and rapid reversed-phase liquid chromatography method for the simultaneous determination of eprosartan mesylate and its six impurities using quality-by-design principles. The method was developed in two phases, screening and optimization. During the screening phase, the most suitable stationary phase, organic modifier, and pH were identified. The optimization was performed for secondary influential parameters--column temperature, gradient time, and flow rate using eight experiments--to examine multifactorial effects of parameters on the critical resolution and generated design space representing the robust region. A verification experiment was performed within the working design space and the model was found to be accurate. This study also describes other operating features of the column packed with superficially porous particles that allow very fast separations at pressures available in most liquid chromatography instruments. Successful chromatographic separation was achieved in less than 7 min using a fused-core C18 (100 mm × 2.1 mm, 2.6 μm) column with linear gradient elution of 10 mM ammonium formate (pH 3.0) and acetonitrile as the mobile phase. The method was validated for specificity, linearity, accuracy, precision, and robustness in compliance with the International Conference on Harmonization Q2 (R1) guidelines. The impurities were identified by liquid chromatography with mass spectrometry. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous densitometric determination of anthelmintic drug albendazole and its metabolite albendazole sulfoxide by HPTLC in human plasma and pharmaceutical formulations.

PubMed

Pandya, Jui J; Sanyal, Mallika; Shrivastav, Pranav S

2017-09-01

A new, simple, accurate and precise high-performance thin-layer chromatographic method has been developed and validated for simultaneous determination of an anthelmintic drug, albendazole, and its active metabolite albendazole, sulfoxide. Planar chromatographic separation was performed on aluminum-backed layer of silica gel 60G F 254 using a mixture of toluene-acetonitrile-glacial acetic acid (7.0:2.9:0.1, v/v/v) as the mobile phase. For quantitation, the separated spots were scanned densitometrically at 225 nm. The retention factors (R f ) obtained under the established conditions were 0.76 ± 0.01 and 0.50 ± 0.01 and the regression plots were linear (r 2  ≥ 0.9997) in the concentration ranges 50-350 and 100-700 ng/band for albendazole and albendazole sulfoxide, respectively. The method was validated for linearity, specificity, accuracy (recovery) and precision, repeatability, stability and robustness. The limit of detection and limit of quantitation found were 9.84 and 29.81 ng/band for albendazole and 21.60 and 65.45 ng/band for albendazole sulfoxide, respectively. For plasma samples, solid-phase extraction of analytes yielded mean extraction recoveries of 87.59 and 87.13% for albendazole and albendazole sulfoxide, respectively. The method was successfully applied for the analysis of albendazole in pharmaceutical formulations with accuracy ≥99.32%. Copyright © 2017 John Wiley & Sons, Ltd.

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

PubMed Central

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

2017-01-01

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

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

PubMed

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

2006-04-11

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

Concurrent determination of olanzapine, risperidone and 9-hydroxyrisperidone in human plasma by ultra performance liquid chromatography with diode array detection method: application to pharmacokinetic study.

PubMed

Siva Selva Kumar, M; Ramanathan, M

2016-02-01

A simple and sensitive ultra-performance liquid chromatography (UPLC) method has been developed and validated for simultaneous estimation of olanzapine (OLZ), risperidone (RIS) and 9-hydroxyrisperidone (9-OHRIS) in human plasma in vitro. The sample preparation was performed by simple liquid-liquid extraction technique. The analytes were chromatographed on a Waters Acquity H class UPLC system using isocratic mobile phase conditions at a flow rate of 0.3 mL/min and Acquity UPLC BEH shield RP18 column maintained at 40°C. Quantification was performed on a photodiode array detector set at 277 nm and clozapine was used as internal standard (IS). OLZ, RIS, 9-OHRIS and IS retention times were found to be 0.9, 1.4, .1.8 and 3.1 min, respectively, and the total run time was 4 min. The method was validated for selectivity, specificity, recovery, linearity, accuracy, precision and sample stability. The calibration curve was linear over the concentration range 1-100 ng/mL for OLZ, RIS and 9-OHRIS. Intra- and inter-day precisions for OLZ, RIS and 9-OHRIS were found to be good with the coefficient of variation <6.96%, and the accuracy ranging from 97.55 to 105.41%, in human plasma. The validated UPLC method was successfully applied to the pharmacokinetic study of RIS and 9-OHRIS in human plasma. Copyright © 2015 John Wiley & Sons, Ltd.

Fast and parallel determination of PCB 77 and PCB 180 in plasma using ultra performance liquid chromatography with diode array detection: A pharmacokinetic study in Swiss albino mouse.

PubMed

Ramanujam, N; Sivaselvakumar, M; Ramalingam, S

2017-11-01

A simple, sensitive and reproducible ultra-performance liquid chromatography (UPLC) method has been developed and validated for simultaneous estimation of polychlorinated biphenyl (PCB) 77 and PCB 180 in mouse plasma. The sample preparation was performed by simple liquid-liquid extraction technique. The analytes were chromatographed on a Waters Acquity H class UPLC system using isocratic mobile phase conditions at a flow rate of 0.3 mL/min and Acquity UPLC BEH shield RP 18 column maintained at 35°C. Quantification was performed on a photodiode array detector set at 215 nm and PCB 101 was used as internal standard (IS). PCB 77, PCB 180, and IS retention times were 2.6, 4.7 and 2.8 min, respectively, and the total run time was 6 min. The method was validated for specificity, selectivity, recovery, linearity, accuracy, precision and sample stability. The calibration curve was linear over the concentration range 10-3000 ng/mL for PCB 77 and PCB 180. Intra- and inter-day precisions for PCBs 77 and 180 were found to be good with CV <4.64%, and the accuracy ranged from 98.90 to 102.33% in mouse plasma. The validated UPLC method was successfully applied to the pharmacokinetic study of PCBs 77 and 180 in mouse plasma. Copyright © 2017 John Wiley & Sons, Ltd.

AN ADA LINEAR ALGEBRA PACKAGE MODELED AFTER HAL/S

NASA Technical Reports Server (NTRS)

Klumpp, A. R.

1994-01-01

This package extends the Ada programming language to include linear algebra capabilities similar to those of the HAL/S programming language. The package is designed for avionics applications such as Space Station flight software. In addition to the HAL/S built-in functions, the package incorporates the quaternion functions used in the Shuttle and Galileo projects, and routines from LINPAK that solve systems of equations involving general square matrices. Language conventions in this package follow those of HAL/S to the maximum extent practical and minimize the effort required for writing new avionics software and translating existent software into Ada. Valid numeric types in this package include scalar, vector, matrix, and quaternion declarations. (Quaternions are fourcomponent vectors used in representing motion between two coordinate frames). Single precision and double precision floating point arithmetic is available in addition to the standard double precision integer manipulation. Infix operators are used instead of function calls to define dot products, cross products, quaternion products, and mixed scalar-vector, scalar-matrix, and vector-matrix products. The package contains two generic programs: one for floating point, and one for integer. The actual component type is passed as a formal parameter to the generic linear algebra package. The procedures for solving systems of linear equations defined by general matrices include GEFA, GECO, GESL, and GIDI. The HAL/S functions include ABVAL, UNIT, TRACE, DET, INVERSE, TRANSPOSE, GET, PUT, FETCH, PLACE, and IDENTITY. This package is written in Ada (Version 1.2) for batch execution and is machine independent. The linear algebra software depends on nothing outside the Ada language except for a call to a square root function for floating point scalars (such as SQRT in the DEC VAX MATHLIB library). This program was developed in 1989, and is a copyrighted work with all copyright vested in NASA.

A Simple Approach to the Technical Aspects of Radiosurgery Treatments

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

Prasad, S.C.; Bassano, D.A.; King, G.A.

2015-01-15

An approach to radiosurgery treatment that can be readily adopted in most radiotherapy centers with linear accelerators is presented. In our institution, a Leksell-type of neurosurgical frame, a computed tomography scanner, locally fabricated cones, and 6 MV X-ray beams are used to perform radiosurgery treatments. Collimated arcs with dose distributions that conform to the shape of the lesion in the transverse and the sagittal planes are used. It is argued that the uncertainties in the localization of the isocenter within a lesion and the specifications of the size of the target volume do not justify high precision mechanical devices formore » most radiosurgery treatments.« less

A tilt and roll device for automated correction of rotational setup errors.

PubMed

Hornick, D C; Litzenberg, D W; Lam, K L; Balter, J M; Hetrick, J; Ten Haken, R K

1998-09-01

A tilt and roll device has been developed to add two additional degrees of freedom to an existing treatment table. This device allows computer-controlled rotational motion about the inferior-superior and left-right patient axes. The tilt and roll device comprises three supports between the tabletop and base. An automotive type universal joint welded to the end of a steel pipe supports the center of the table. Two computer-controlled linear electric actuators utilizing high accuracy stepping motors support the foot of table and control the tilt and roll of the tabletop. The current system meets or exceeds all pre-design specifications for precision, weight capacity, rigidity, and range of motion.

Linear Self-Referencing Techiques for Short-Optical-Pulse Characterization

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

Dorrer, C.; Kang, I.

2008-04-04

Linear self-referencing techniques for the characterization of the electric field of short optical pulses are presented. The theoretical and practical advantages of these techniques are developed. Experimental implementations are described, and their performance is compared to the performance of their nonlinear counterparts. Linear techniques demonstrate unprecedented sensitivity and are a perfect fit in many domains where the precise, accurate measurement of the electric field of an optical pulse is required.

Towards TeV-scale electron-positron collisions: the Compact Linear Collider (CLIC)

NASA Astrophysics Data System (ADS)

Doebert, Steffen; Sicking, Eva

2018-02-01

The Compact Linear Collider (CLIC), a future electron-positron collider at the energy frontier, has the potential to change our understanding of the universe. Proposed to follow the Large Hardron Collider (LHC) programme at CERN, it is conceived for precision measurements as well as for searches for new phenomena.

Precision of the upgraded cottonscan instrument for measuring the average fiber linear density (fineness) of cotton lint samples

USDA-ARS?s Scientific Manuscript database

An inter-laboratory trial was conducted to validate the operation of the CottonscanTM technology as useful technique for determining the average fiber linear density of cotton. A significant inter-laboratory trial was completed and confirmed that the technology is quite acceptable. For fibers fin...

DAC-board based X-band EPR spectrometer with arbitrary waveform control

NASA Astrophysics Data System (ADS)

Kaufmann, Thomas; Keller, Timothy J.; Franck, John M.; Barnes, Ryan P.; Glaser, Steffen J.; Martinis, John M.; Han, Songi

2013-10-01

We present arbitrary control over a homogenous spin system, demonstrated on a simple, home-built, electron paramagnetic resonance (EPR) spectrometer operating at 8-10 GHz (X-band) and controlled by a 1 GHz arbitrary waveform generator (AWG) with 42 dB (i.e. 14-bit) of dynamic range. Such a spectrometer can be relatively easily built from a single DAC (digital to analog converter) board with a modest number of stock components and offers powerful capabilities for automated digital calibration and correction routines that allow it to generate shaped X-band pulses with precise amplitude and phase control. It can precisely tailor the excitation profiles "seen" by the spins in the microwave resonator, based on feedback calibration with experimental input. We demonstrate the capability to generate a variety of pulse shapes, including rectangular, triangular, Gaussian, sinc, and adiabatic rapid passage waveforms. We then show how one can precisely compensate for the distortion and broadening caused by transmission into the microwave cavity in order to optimize corrected waveforms that are distinctly different from the initial, uncorrected waveforms. Specifically, we exploit a narrow EPR signal whose width is finer than the features of any distortions in order to map out the response to a short pulse, which, in turn, yields the precise transfer function of the spectrometer system. This transfer function is found to be consistent for all pulse shapes in the linear response regime. In addition to allowing precise waveform shaping capabilities, the spectrometer presented here offers complete digital control and calibration of the spectrometer that allows one to phase cycle the pulse phase with 0.007° resolution and to specify the inter-pulse delays and pulse durations to ⩽250 ps resolution. The implications and potential applications of these capabilities will be discussed.

[Technological innovations in radiation oncology require specific quality controls].

PubMed

Lenaerts, E; Mathot, M

2014-01-01

During the last decade, the field of radiotherapy has benefited from major technological innovations and continuously improving treatment efficacy, comfort and safety of patients. This mainly concerns the imaging techniques that allow 4D CT scan recording the respiratory phases, on-board imaging on linear accelerators that ensure perfect positioning of the patient for treatment and irradiation techniques that reduce very significantly the duration of treatment sessions without compromising quality of the treatment plan, including IMRT (Intensity Modulated Radiation Therapy) and VMAT (Volumetric Modulated Arc therapy). In this context of rapid technological change, it is the responsibility of medical physicists to regularly and precisely monitor the perfect functioning of new techniques to ensure patient safety. This requires the use of specific quality control equipment best suited to these new techniques. We will briefly describe the measurement system Delta4 used to control individualized treatment plan for each patient treated with VMAT technology.

Using the ADAP Learning Algorithm to Forecast the Onset of Diabetes Mellitus

PubMed Central

Smith, Jack W.; Everhart, J.E.; Dickson, W.C.; Knowler, W.C.; Johannes, R.S.

1988-01-01

Neural networks or connectionist models for parallel processing are not new. However, a resurgence of interest in the past half decade has occurred. In part, this is related to a better understanding of what are now referred to as hidden nodes. These algorithms are considered to be of marked value in pattern recognition problems. Because of that, we tested the ability of an early neural network model, ADAP, to forecast the onset of diabetes mellitus in a high risk population of Pima Indians. The algorithm's performance was analyzed using standard measures for clinical tests: sensitivity, specificity, and a receiver operating characteristic curve. The crossover point for sensitivity and specificity is 0.76. We are currently further examining these methods by comparing the ADAP results with those obtained from logistic regression and linear perceptron models using precisely the same training and forecasting sets. A description of the algorithm is included.

Programmable DNA scaffolds for spatially-ordered protein assembly.

PubMed

Chandrasekaran, Arun Richard

2016-02-28

Ever since the notion of using DNA as a material was realized, it has been employed in the construction of complex structures that facilitate the assembly of nanoparticles or macromolecules with nanometer-scale precision. Specifically, tiles fashioned from DNA strands and DNA origami sheets have been shown to be suitable as scaffolds for immobilizing proteins with excellent control over their spatial positioning. Supramolecular assembly of proteins into periodic arrays in one or more dimensions is one of the most challenging aspects in the design of scaffolds for biomolecular investigations and macromolecular crystallization. This review provides a brief overview of how various biomolecular interactions with high degree of specificity such as streptavidin-biotin, antigen-antibody, and aptamer-protein interactions have been used to fabricate linear and multidimensional assemblies of structurally intact and functional proteins. The use of DNA-binding proteins as adaptors, polyamide recognition on DNA scaffolds and oligonucleotide linkers for protein assembly are also discussed.

Optimization and Validation of ELISA for Pre-Clinical Trials of Influenza Vaccine.

PubMed

Mitic, K; Muhandes, L; Minic, R; Petrusic, V; Zivkovic, I

2016-01-01

Testing of every new vaccine involves investigation of its immunogenicity, which is based on monitoring its ability to induce specific antibodies in animals. The fastest and most sensitive method used for this purpose is enzyme-linked immunosorbent assay (ELISA). However, commercial ELISA kits with whole influenza virus antigens are not available on the market, and it is therefore essential to establish an adequate assay for testing influenza virusspecific antibodies. We developed ELISA with whole influenza virus strains for the season 2011/2012 as antigens and validated it by checking its specificity, accuracy, linearity, range, precision, and sensitivity. The results show that we developed high-quality ELISA that can be used to test immunogenicity of newly produced seasonal or pandemic vaccines in mice. The pre-existence of validated ELISA enables shortening the time from the process of vaccine production to its use in patients, which is particularly important in the case of a pandemic.

Rapid capillary electrophoresis approach for the quantification of ewe milk adulteration with cow milk.

PubMed

Trimboli, Francesca; Morittu, Valeria Maria; Cicino, Caterina; Palmieri, Camillo; Britti, Domenico

2017-10-13

The substitution of ewe milk with more economic cow milk is a common fraud. Here we present a capillary electrophoresis method for the quantification of ewe milk in ovine/bovine milk mixtures, which allows for the rapid and inexpensive recognition of ewe milk adulteration with cow milk. We utilized a routine CE method for human blood and urine proteins analysis, which fulfilled the separation of skimmed milk proteins in alkaline buffer. Under this condition, ovine and bovine milk exhibited a recognizable and distinct CE protein profiles, with a specific ewe peak showing a reproducible migration zone in ovine/bovine mixtures. Based on ewe specific CE peak, we developed a method for ewe milk quantification in ovine/bovine skimmed milk mixtures, which showed good linearity, precision and accuracy, and a minimum amount of detectable fraudulent cow milk equal to 5%. Copyright © 2017 Elsevier B.V. All rights reserved.

Precision-feeding dairy heifers a high rumen-undegradable protein diet with different proportions of dietary fiber and forage-to-concentrate ratios.

PubMed

Koch, L E; Gomez, N A; Bowyer, A; Lascano, G J

2017-12-01

The addition of dietary fiber can alter nutrient and N utilization in precision-fed dairy heifers and may further benefit from higher inclusion levels of RUP. The objective of this experiment was to determine the effects of feeding a high-RUP diet when dietary fiber content was manipulated within differing forage-to-concentrate ratios (F:C) on nutrient utilization of precision-fed dairy heifers. Six rumen-cannulated Holstein heifers (555.4 ± 31.4 kg BW; 17.4 ± 0.1 mo) were randomly assigned to 2 levels of forage, high forage (HF; 60% forage) or low forage (LF; 45% forage), and to a fiber proportion sequence (low fiber: 100% oat hay and silage [OA], 0% wheat straw [WS]; medium fiber: 83.4% OA, 16.6% WS; and high fiber: 66.7% OA, 33.3% WS) administered according to a split-plot 3 × 3 Latin square design (21-d periods). Similar levels of N intake (1.70 g N/kg BW) and RUP (55% of CP) were provided. Data were analyzed as a split-plot, 3 × 3 Latin square design using a mixed model with fixed effects of period and treatment. A repeated measures model was used with data that had multiple measurements over time. No differences were observed for DM, OM, NDF, or ADF apparent digestibility coefficients (dC) between HF- and LF-fed heifers. Heifers receiving LF diets had greater starch dC compared to HF heifers. Increasing the fiber level through WS addition resulted in a linear reduction of OM dC. There was a linear interaction for DM dC with a concurrent linear interaction in NDF dC. Nitrogen intake, dC, and retention did not differ; however, urine and total N excretion increased linearly with added fiber. Predicted microbial CP flow (MP) linearly decreased with WS inclusion mainly in LF heifers, as indicated by a significant interaction between F:C and WS. Rumen pH linearly increased with WS addition, although no F:C effect was detected. Ruminal ammonia concentration had an opposite linear effect with respect to MP as WS increased. Diets with the higher proportion of fiber benefited the most from a high RUP supply, complementing the substantial reduction in predicted MP caused by the incremental dietary fiber concentration. These results suggest that RUP supplementation is a practical method for reestablishing optimal ruminal N balance in the event of increased dietary fiber through forage inclusion in precision-fed dairy heifer diets.

Ultra-Low-Dropout Linear Regulator

NASA Technical Reports Server (NTRS)

Thornton, Trevor; Lepkowski, William; Wilk, Seth

2011-01-01

A radiation-tolerant, ultra-low-dropout linear regulator can operate between -150 and 150 C. Prototype components were demonstrated to be performing well after a total ionizing dose of 1 Mrad (Si). Unlike existing components, the linear regulator developed during this activity is unconditionally stable over all operating regimes without the need for an external compensation capacitor. The absence of an external capacitor reduces overall system mass/volume, increases reliability, and lowers cost. Linear regulators generate a precisely controlled voltage for electronic circuits regardless of fluctuations in the load current that the circuit draws from the regulator.

Perinatal BPA exposure alters body weight and composition in a dose specific and sex specific manner: The addition of peripubertal exposure exacerbates adverse effects in female mice.

PubMed

Rubin, Beverly S; Paranjpe, Maneesha; DaFonte, Tracey; Schaeberle, Cheryl; Soto, Ana M; Obin, Martin; Greenberg, Andrew S

2017-03-01

Body weight (BW) and body composition were examined in CD-1 mice exposed perinatally or perinatally and peripubertally to 0, 0.25, 2.5, 25, or 250μg BPA/kg BW/day. Our goal was to identify the BPA dose (s) and the exposure window(s) that increased BW and adiposity, and to assess potential sex differences in this response. Both perinatal exposure alone and perinatal plus peripubertal exposure to environmentally relevant levels of BPA resulted in lasting effects on body weight and body composition. The effects were dose specific and sex specific and were influenced by the precise window of BPA exposure. The addition of peripubertal BPA exposure following the initial perinatal exposure exacerbated adverse effects in the females but appeared to reduce differences in body weight and body composition between control and BPA exposed males. Some effects of BPA on body weight and body composition showed a non-linear dose response. Copyright © 2016. Published by Elsevier Inc.

Development and Validation of GC-ECD Method for the Determination of Metamitron in Soil

PubMed Central

Tandon, Shishir; Kumar, Satyendra; Sand, N. K.

2015-01-01

This paper aims at developing and validating a convenient, rapid, and sensitive method for estimation of metamitron from soil samples.Determination andquantification was carried out by Gas Chromatography on microcapillary column with an Electron Capture Detector source. The compound was extracted from soil using methanol and cleanup by C-18 SPE. After optimization, the method was validated by evaluating the analytical curves, linearity, limits of detection, and quantification, precision (repeatability and intermediate precision), and accuracy (recovery). Recovery values ranged from 89 to 93.5% within 0.05- 2.0 µg L−1 with average RSD 1.80%. The precision (repeatability) ranged from 1.7034 to 1.9144% and intermediate precision from 1.5685 to 2.1323%. Retention time was 6.3 minutes, and minimum detectable and quantifiable limits were 0.02 ng mL−1 and 0.05 ng g−1, respectively. Good linearity (R 2 = 0.998) of the calibration curves was obtained over the range from 0.05 to 2.0 µg L−1. Results indicated that the developed method is rapid and easy to perform, making it applicable for analysis in large pesticide monitoring programmes. PMID:25733978

Accurate determination of reference materials and natural isolates by means of quantitative (1)h NMR spectroscopy.

PubMed

Frank, Oliver; Kreissl, Johanna Karoline; Daschner, Andreas; Hofmann, Thomas

2014-03-26

A fast and precise proton nuclear magnetic resonance (qHNMR) method for the quantitative determination of low molecular weight target molecules in reference materials and natural isolates has been validated using ERETIC 2 (Electronic REference To access In vivo Concentrations) based on the PULCON (PULse length based CONcentration determination) methodology and compared to the gravimetric results. Using an Avance III NMR spectrometer (400 MHz) equipped with a broad band observe (BBO) probe, the qHNMR method was validated by determining its linearity, range, precision, and accuracy as well as robustness and limit of quantitation. The linearity of the method was assessed by measuring samples of l-tyrosine, caffeine, or benzoic acid in a concentration range between 0.3 and 16.5 mmol/L (r(2) ≥ 0.99), whereas the interday and intraday precisions were found to be ≤2%. The recovery of a range of reference compounds was ≥98.5%, thus demonstrating the qHNMR method as a precise tool for the rapid quantitation (~15 min) of food-related target compounds in reference materials and natural isolates such as nucleotides, polyphenols, or cyclic peptides.

Computing Generalized Matrix Inverse on Spiking Neural Substrate.

PubMed

Shukla, Rohit; Khoram, Soroosh; Jorgensen, Erik; Li, Jing; Lipasti, Mikko; Wright, Stephen

2018-01-01

Emerging neural hardware substrates, such as IBM's TrueNorth Neurosynaptic System, can provide an appealing platform for deploying numerical algorithms. For example, a recurrent Hopfield neural network can be used to find the Moore-Penrose generalized inverse of a matrix, thus enabling a broad class of linear optimizations to be solved efficiently, at low energy cost. However, deploying numerical algorithms on hardware platforms that severely limit the range and precision of representation for numeric quantities can be quite challenging. This paper discusses these challenges and proposes a rigorous mathematical framework for reasoning about range and precision on such substrates. The paper derives techniques for normalizing inputs and properly quantizing synaptic weights originating from arbitrary systems of linear equations, so that solvers for those systems can be implemented in a provably correct manner on hardware-constrained neural substrates. The analytical model is empirically validated on the IBM TrueNorth platform, and results show that the guarantees provided by the framework for range and precision hold under experimental conditions. Experiments with optical flow demonstrate the energy benefits of deploying a reduced-precision and energy-efficient generalized matrix inverse engine on the IBM TrueNorth platform, reflecting 10× to 100× improvement over FPGA and ARM core baselines.

Wii Balance Board: Reliability and Clinical Use in Assessment of Balance in Healthy Elderly Women.

PubMed

Monteiro-Junior, Renato Sobral; Ferreira, Arthur Sá; Puell, Vivian Neiva; Lattari, Eduardo; Machado, Sérgio; Otero Vaghetti, César Augusto; da Silva, Elirez Bezerra

2015-01-01

Force plate is considered gold standard tool to assess body balance. However the Wii Balance Board (WBB) platform is a trustworthy equipment to assess stabilometric components in young people. Thus, we aim to examine the reliability of measures of center of pressure with WBB in healthy elderly women. Twenty one healthy and physically active women were enrolled in the study (age: 64 ± 7 years; body mass index: 29 ± 5 kg/m2. The WBB was used to assess the center of pressure measures in the individuals. Pressure was linearly applied to different points to test the platform precision. Three assessments were performed, with two of them being held on the same day at a 5- to 10-minute interval, and the third one was performed 48 h later. A linear regression analysis was used to find out linearity, while the intraclass correlation coefficient was used to assess reliability. The platform precision was adequate (R2 = 0.997, P = 0.01). Center of pressure measures showed an excellent reliability (all intraclass correlation coefficient values were > 0.90; p < 0.01). The WBB is a precise and reliable tool of body stability quantitative measure in healthy active elderly women and its use should be encouraged in clinical settings.

Method of Individual Adjustment for 3D CT Analysis: Linear Measurement.

PubMed

Kim, Dong Kyu; Choi, Dong Hun; Lee, Jeong Woo; Yang, Jung Dug; Chung, Ho Yun; Cho, Byung Chae; Choi, Kang Young

2016-01-01

Introduction . We aim to regularize measurement values in three-dimensional (3D) computed tomography (CT) reconstructed images for higher-precision 3D analysis, focusing on length-based 3D cephalometric examinations. Methods . We measure the linear distances between points on different skull models using Vernier calipers (real values). We use 10 differently tilted CT scans for 3D CT reconstruction of the models and measure the same linear distances from the picture archiving and communication system (PACS). In both cases, each measurement is performed three times by three doctors, yielding nine measurements. The real values are compared with the PACS values. Each PACS measurement is revised based on the display field of view (DFOV) values and compared with the real values. Results . The real values and the PACS measurement changes according to tilt value have no significant correlations ( p > 0.05). However, significant correlations appear between the real values and DFOV-adjusted PACS measurements ( p < 0.001). Hence, we obtain a correlation expression that can yield real physical values from PACS measurements. The DFOV value intervals for various age groups are also verified. Conclusion . Precise confirmation of individual preoperative length and precise analysis of postoperative improvements through 3D analysis is possible, which is helpful for facial-bone-surgery symmetry correction.

Application of a microplate-based ORAC-pyrogallol red assay for the estimation ofantioxidant capacity: First Action 2012.03.

PubMed

Ortiz, Rocío; Antilén, Mónica; Speisky, Hernán; Aliaga, Margarita E; López-Alarcón, Camilo; Baugh, Steve

2012-01-01

A method was developed for microplate-based oxygen radicals absorbance capacity (ORAC) using pyrogallol red (PGR) as probe (ORAC-PGR). The method was evaluated for linearity, precision, and accuracy. In addition, the antioxidant capacity of commercial beverages, such as wines, fruit juices, and iced teas, was measured. Linearity of the area under the curve (AUC) versus Trolox concentration plots was [AUC = (845 +/- 110) + (23 +/- 2) [Trolox, microM]; R = 0.9961, n = 19]. Analyses showed better precision and accuracy at the highest Trolox concentration (40 microM) with RSD and recovery (REC) values of 1.7 and 101.0%, respectively. The method also showed good linearity for red wine [AUC = (787 +/- 77) + (690 +/- 60) [red wine, microL/mL]; R = 0.9926, n = 17], precision and accuracy with RSD values from 1.4 to 8.3%, and REC values that ranged from 89.7 to 103.8%. Red wines showed higher ORAC-PGR values than white wines, while the ORAC-PGR index of fruit juices and iced teas presented a wide range of results, from 0.6 to 21.6 mM of Trolox equivalents. Product-to-product variability was also observed for juices of the same fruit, showing the differences between brands on the ORAC-PGR index.

Fourier Transform Fringe-Pattern Analysis of an Absolute Distance Michelson Interferometer for Space-Based Laser Metrology.

NASA Astrophysics Data System (ADS)

Talamonti, James Joseph

1995-01-01

Future NASA proposals include the placement of optical interferometer systems in space for a wide variety of astrophysical studies including a vastly improved deflection test of general relativity, a precise and direct calibration of the Cepheid distance scale, and the determination of stellar masses (Reasenberg et al., 1988). There are also plans for placing large array telescopes on the moon with the ultimate objective of being able to measure angular separations of less than 10 mu-arc seconds (Burns, 1990). These and other future projects will require interferometric measurement of the (baseline) distance between the optical elements comprising the systems. Eventually, space qualifiable interferometers capable of picometer (10^{-12}m) relative precision and nanometer (10^{ -9}m) absolute precision will be required. A numerical model was developed to emulate the capabilities of systems performing interferometric noncontact absolute distance measurements. The model incorporates known methods to minimize signal processing and digital sampling errors and evaluates the accuracy limitations imposed by spectral peak isolation using Hanning, Blackman, and Gaussian windows in the Fast Fourier Transform Technique. We applied this model to the specific case of measuring the relative lengths of a compound Michelson interferometer using a frequency scanned laser. By processing computer simulated data through our model, the ultimate precision is projected for ideal data, and data containing AM/FM noise. The precision is shown to be limited by non-linearities in the laser scan. A laboratory system was developed by implementing ultra-stable external cavity diode lasers into existing interferometric measuring techniques. The capabilities of the system were evaluated and increased by using the computer modeling results as guidelines for the data analysis. Experimental results measured 1-3 meter baselines with <20 micron precision. Comparison of the laboratory and modeling results showed that the laboratory precisions obtained were of the same order of magnitude as those predicted for computer generated results under similar conditions. We believe that our model can be implemented as a tool in the design for new metrology systems capable of meeting the precisions required by space-based interferometers.

Pre-treatment patient-specific stopping power by combining list-mode proton radiography and x-ray CT

NASA Astrophysics Data System (ADS)

Collins-Fekete, Charles-Antoine; Brousmiche, Sébastien; Hansen, David C.; Beaulieu, Luc; Seco, Joao

2017-09-01

The relative stopping power (RSP) uncertainty is the largest contributor to the range uncertainty in proton therapy. The purpose of this work was to develop a systematic method that yields accurate and patient-specific RSPs by combining (1) pre-treatment x-ray CT and (2) daily proton radiography of the patient. The method was formulated as a penalized least squares optimization problem (argmin(\\Vert {A}{x}-{b}\\Vert _22 )). The parameter A represents the cumulative path-length crossed by the proton in each material, separated by thresholding on the HU. The material RSPs (water equivalent thickness/physical thickness) are denoted by x. The parameter b is the list-mode proton radiography produced using Geant4 simulations. The problem was solved using a non-negative linear-solver with {x}≥slant0 . A was computed by superposing proton trajectories calculated with a cubic or linear spline approach to the CT. The material’s RSP assigned in Geant4 were used for reference while the clinical HU-RSP calibration curve was used for comparison. The Gammex RMI-467 phantom was first investigated. The standard deviation between the estimated material RSP and the calculated RSP is 0.45%. The robustness of the techniques was then assessed as a function of the number of projections and initial proton energy. Optimization with two initial projections yields precise RSP (⩽1.0%) for 330 MeV protons. 250 MeV protons have shown higher uncertainty (⩽2.0%) due to the loss of precision in the path estimate. Anthropomorphic phantoms of the head, pelvis, and lung were subsequently evaluated. Accurate RSP has been obtained for the head (μ =0.21+/-1.63% ), the lung (μ=0.06+/-0.99% ) and the pelvis (μ=0.90+/-3.87% ). The range precision has been optimized using the calibration curves obtained with the algorithm, yielding a mean R80 difference to the reference of 0.11  ±0.09%, 0.28  ±  0.34% and 0.05 +/- 0.06% in the same order. The solution’s accuracy is limited by the assumed HU/RSP bijection, neglecting inherent degeneracy. The proposed formulation of the problem with prior knowledge x-ray CT demonstrates potential to increase the accuracy of present RSP estimates.

Pre-treatment patient-specific stopping power by combining list-mode proton radiography and x-ray CT.

PubMed

Collins-Fekete, Charles-Antoine; Brousmiche, Sébastien; Hansen, David C; Beaulieu, Luc; Seco, Joao

2017-08-03

The relative stopping power (RSP) uncertainty is the largest contributor to the range uncertainty in proton therapy. The purpose of this work was to develop a systematic method that yields accurate and patient-specific RSPs by combining (1) pre-treatment x-ray CT and (2) daily proton radiography of the patient. The method was formulated as a penalized least squares optimization problem (argmin([Formula: see text])). The parameter A represents the cumulative path-length crossed by the proton in each material, separated by thresholding on the HU. The material RSPs (water equivalent thickness/physical thickness) are denoted by x. The parameter b is the list-mode proton radiography produced using Geant4 simulations. The problem was solved using a non-negative linear-solver with [Formula: see text]. A was computed by superposing proton trajectories calculated with a cubic or linear spline approach to the CT. The material's RSP assigned in Geant4 were used for reference while the clinical HU-RSP calibration curve was used for comparison. The Gammex RMI-467 phantom was first investigated. The standard deviation between the estimated material RSP and the calculated RSP is 0.45%. The robustness of the techniques was then assessed as a function of the number of projections and initial proton energy. Optimization with two initial projections yields precise RSP (⩽1.0%) for 330 MeV protons. 250 MeV protons have shown higher uncertainty (⩽2.0%) due to the loss of precision in the path estimate. Anthropomorphic phantoms of the head, pelvis, and lung were subsequently evaluated. Accurate RSP has been obtained for the head ([Formula: see text]), the lung ([Formula: see text]) and the pelvis ([Formula: see text]). The range precision has been optimized using the calibration curves obtained with the algorithm, yielding a mean [Formula: see text] difference to the reference of 0.11  ±0.09%, 0.28  ±  0.34% and [Formula: see text] in the same order. The solution's accuracy is limited by the assumed HU/RSP bijection, neglecting inherent degeneracy. The proposed formulation of the problem with prior knowledge x-ray CT demonstrates potential to increase the accuracy of present RSP estimates.

Uranium Detection - Technique Validation Report

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

Colletti, Lisa Michelle; Garduno, Katherine; Lujan, Elmer J.

As a LANL activity for DOE/NNSA in support of SHINE Medical Technologies™ ‘Accelerator Technology’ we have been investigating the application of UV-vis spectroscopy for uranium analysis in solution. While the technique has been developed specifically for sulfate solutions, the proposed SHINE target solutions, it can be adapted to a range of different solution matrixes. The FY15 work scope incorporated technical development that would improve accuracy, specificity, linearity & range, precision & ruggedness, and comparative analysis. Significant progress was achieved throughout FY 15 addressing these technical challenges, as is summarized in this report. In addition, comparative analysis of unknown samples usingmore » the Davies-Gray titration technique highlighted the importance of controlling temperature during analysis (impacting both technique accuracy and linearity/range). To fully understand the impact of temperature, additional experimentation and data analyses were performed during FY16. The results from this FY15/FY16 work were presented in a detailed presentation, LA-UR-16-21310, and an update of this presentation is included with this short report summarizing the key findings. The technique is based on analysis of the most intense U(VI) absorbance band in the visible region of the uranium spectra in 1 M H 2SO 4, at λ max = 419.5 nm.« less

Development and validity of an instrumented handbike: initial results of propulsion kinetics.

PubMed

van Drongelen, Stefan; van den Berg, Jos; Arnet, Ursina; Veeger, Dirkjan H E J; van der Woude, Lucas H V

2011-11-01

To develop an instrumented handbike system to measure the forces applied to the handgrip during handbiking. A 6 degrees of freedom force sensor was built into the handgrip of an attach-unit handbike, together with two optical encoders to measure the orientation of the handgrip and crank in space. Linearity, precision, and percent error were determined for static and dynamic tests. High linearity was demonstrated for both the static and the dynamic condition (r=1.01). Precision was high under the static condition (standard deviation of 0.2N), however the precision decreased with higher loads during the dynamic condition. Percent error values were between 0.3 and 5.1%. This is the first instrumented handbike system that can register 3-dimensional forces. It can be concluded that the instrumented handbike system allows for an accurate force analysis based on forces registered at the handle bars. Copyright © 2011 IPEM. Published by Elsevier Ltd. All rights reserved.

Development of an ultrasonic linear motor with ultra-positioning capability and four driving feet.

PubMed

Zhu, Cong; Chu, Xiangcheng; Yuan, Songmei; Zhong, Zuojin; Zhao, Yanqiang; Gao, Shuning

2016-12-01

This paper presents a novel linear piezoelectric motor which is suitable for rapid ultra-precision positioning. The finite element analysis (FEA) was applied for optimal design and further analysis, then experiments were conducted to investigate its performance. By changing the input signal, the proposed motor was found capable of working in the fast driving mode as well as in the precision positioning mode. When working in the fast driving mode, the motor acts as an ultrasonic motor with maximum no-load speed up to 181.2mm/s and maximum thrust of 1.7N at 200Vp-p. Also, when working in precision positioning mode, the motor can be regarded as a flexible hinge piezoelectric actuator with arbitrary motion in the range of 8μm. The measurable minimum output displacement was found to be 0.08μm, but theoretically, can be even smaller. More importantly, the motor can be quickly and accurately positioned in a large stroke. Copyright © 2016 Elsevier B.V. All rights reserved.

Analytical characteristics and comparative evaluation of Aptima HCV quant Dx assay with the Abbott RealTime HCV assay and Roche COBAS AmpliPrep/COBAS TaqMan HCV quantitative test v2.0.

PubMed

Worlock, A; Blair, D; Hunsicker, M; Le-Nguyen, T; Motta, C; Nguyen, C; Papachristou, E; Pham, J; Williams, A; Vi, M; Vinluan, B; Hatzakis, A

2017-04-04

The Aptima HCV Quant Dx assay (Aptima assay) is a fully automated quantitative assay on the Panther® system. This assay is intended for confirmation of diagnosis and monitoring of HCV RNA in plasma and serum specimens. The purpose of the testing described in this paper was to evaluate the performance of the Aptima assay. The analytical sensitivity, analytical specificity, precision, and linearity of the Aptima assay were assessed. The performance of the Aptima assay was compared to two commercially available HCV assays; the Abbott RealTime HCV assay (Abbott assay, Abbott Labs Illinois, USA) and the Roche COBAS Ampliprep/COBAS Taqman HCV Quantitative Test v2.0 (Roche Assay, Roche Molecular Systems, Pleasanton CA, USA). The 95% Lower Limit of Detection (LoD) of the assay was determined from dilutions of the 2nd HCV WHO International Standard (NIBSC 96/798 genotype 1) and HCV positive clinical specimens in HCV negative human plasma and serum. Probit analysis was performed to generate the 95% predicted detection limits. The Lower Limit of Quantitation (LLoQ) was established for each genotype by diluting clinical specimens and the 2nd HCV WHO International Standard (NIBSC 96/798 genotype 1) in HCV negative human plasma and serum. Specificity was determined using 200 fresh and 536 frozen HCV RNA negative clinical specimens including 370 plasma specimens and 366 serum specimens. Linearity for genotypes 1 to 6 was established by diluting armored RNA or HCV positive clinical specimens in HCV negative serum or plasma from 8.08 log IU/mL to below 1 log IU/mL. Precision was tested using a 10 member panel made by diluting HCV positive clinical specimens or spiking armored RNA into HCV negative plasma and serum. A method comparison was conducted against the Abbott assay using 1058 clinical specimens and against the Roche assay using 608 clinical specimens from HCV infected patients. In addition, agreement between the Roche assay and the Aptima assay using specimens with low HCV concentrations (

Simultaneous determination of kolliphor HS15 and miglyol 812 in microemulsion formulation by ultra-high performance liquid chromatography coupled with nano quantity analyte detector.

PubMed

Zhang, Honggen; Wang, Zhenyu; Liu, Oscar

2016-02-01

A novel method for simultaneous determination of kolliphor HS15 and miglyol 812 in microemulsion formulation was developed using ultra-high performance liquid chromatography coupled with a nano quantitation analytical detector (UHPLC-NQAD). All components in kolliphor HS15 and miglyol 812 were well separated on an Acquity BEH C 18 column. Mobile phase A was 0.1% trifluoroacetic acid (TFA) in water and mobile phase B was acetonitrile. A gradient elution sequence was programed initially with 60% organic solvent, slowly increased to 100% within 8 min. The flow rate was 0.7 mL/min. Good linearity ( r >0.95) was obtained in the range of 27.6-1381.1 μg/mL for polyoxyl 15 hydroxystearate in kolliphor HS15, 0.8-202.0 μg/mL for caprylic acid triglyceride and 2.7-221.9 μg/mL for capric acid triglyceride in miglyol 812. The relative standard deviations (RSD) ranged from 0.6% to 1.7% for intra-day precision and from 0.4% to 2.7% for inter-day precision. The overall recoveries (accuracy) were 99.7%-101.4% for polyoxyl 15 hydroxystearate in kolliphor HS15, 96.7%-99.6% for caprylic acid triglyceride, and 94.1%-103.3% for capric acid triglyceride in miglyol 812. Quantification limits (QL) were determined as 27.6 μg/mL for polyoxyl 15 hydroxystearate in kolliphor HS15, 0.8 μg/mL for caprylic acid triglyceride, and 2.7 μg/mL for capric acid triglyceride in miglyol 812. No interferences were observed in the retention time ranges of kolliphor HS15 and miglyol 812. The method was validated in terms of specificity, linearity, precision, accuracy, QL, and robustness. The proposed method has been applied to microemulsion formulation analyses with good recoveries (82.2%-103.4%).

Development of a Stability-Indicating Stereoselective Method for Quantification of the Enantiomer in the Drug Substance and Pharmaceutical Dosage Form of Rosuvastatin Calcium by an Enhanced Approach

PubMed Central

Rajendra Reddy, Gangireddy; Ravindra Reddy, Papammagari; Siva Jyothi, Polisetty

2015-01-01

A novel, simple, precise, and stability-indicating stereoselective method was developed and validated for the accurate quantification of the enantiomer in the drug substance and pharmaceutical dosage forms of Rosuvastatin Calcium. The method is capable of quantifying the enantiomer in the presence of other related substances. The chromatographic separation was achieved with an immobilized cellulose stationary phase (Chiralpak IB) 250 mm x 4.6 mm x 5.0 μm particle size column with a mobile phase containing a mixture of n-hexane, dichloromethane, 2-propanol, and trifluoroacetic acid in the ratio 82:10:8:0.2 (v/v/v/v). The eluted compounds were monitored at 243 nm and the run time was 18 min. Multivariate analysis and statistical tools were used to develop this highly robust method in a short span of time. The stability-indicating power of the method was established by subjecting Rosuvastatin Calcium to the stress conditions (forced degradation) of acid, base, oxidative, thermal, humidity, and photolytic degradation. Major degradation products were identified and found to be well-resolved from the enantiomer peak, proving the stability-indicating power of the method. The developed method was validated as per International Conference on Harmonization (ICH) guidelines with respect to specificity, limit of detection and limit of quantification, precision, linearity, accuracy, and robustness. The method exhibited consistent, high-quality recoveries (100 ± 10%) with a high precision for the enantiomer. Linear regression analysis revealed an excellent correlation between the peak responses and concentrations (r2 value of 0.9977) for the enantiomer. The method is sensitive enough to quantify the enantiomer above 0.04% and detect the enantiomer above 0.015% in Rosuvastatin Calcium. The stability tests were also performed on the drug substances as per ICH norms. PMID:26839815

Validation of a rapid micellar electrokinetic capillary chromatographic method for the simultaneous determination of isoniazid and pyridoxine hydrochloride in pharmaceutical formulation.

PubMed

Nemutlu, E; Celebier, M; Uyar, B; Altinöz, S

2007-07-01

An efficient and reliable micellar electrokinetic capillary chromatography (MEKC) method has been developed for the simultaneous determination of isoniazid (ISO) and pyridoxine hydrochloride (PYR) in pharmaceutical formulations. A chemometric two level full factorial design approach was used to search for the optimum conditions of separation. Three parameters were selected for this study: the buffer pH, the buffer concentration and sodium dodecyl sulphate (SDS) concentrations. Resolution, peak symmetry and analysis time were established as response. The two analytes were separated within 6 min with the optimized conditions: 50 mM borate buffer, 25 mM SDS pH 7.8, 35 degrees C, at 50 mbar 4s injection and 30 kV by using a fused silica capillary (72 cm effective length, 50 microm i.d.). The detection wavelength was set to 205 nm. Meloxicam was used as internal standard. The method was validated with respect to stability, linearity range, limit of quantitation and detection, precision, accuracy, specificity and robustness. The detection limits of the method were 1.0 microg mL(-1) for ISO and 0.40 microg mL(-1) for PYR and the method was linear at least in the range of 3.0-100 microg mL(-1) for ISO and 1.0-100 microg mL(-1) for PYR with excellent correlation coefficients (0.9995 for ISO and 0.9998 for PYR). Relative standard deviations (R.S.D.s) of the described method ranged between 0.54 and 2.27% for intra-day precision and between 0.65 and 2.69% for inter-day precision. The developed method was applied to the tablet form of ISO and PYR-containing the pharmaceutical preparations and the data were compared with obtained from the standard addition method. No statistically significant difference was found.

Mechanical design of deformation compensated flexural pivots structured for linear nanopositioning stages

DOEpatents

Shu, Deming; Kearney, Steven P.; Preissner, Curt A.

2015-02-17

A method and deformation compensated flexural pivots structured for precision linear nanopositioning stages are provided. A deformation-compensated flexural linear guiding mechanism includes a basic parallel mechanism including a U-shaped member and a pair of parallel bars linked to respective pairs of I-link bars and each of the I-bars coupled by a respective pair of flexural pivots. The basic parallel mechanism includes substantially evenly distributed flexural pivots minimizing center shift dynamic errors.

Bit Grooming: statistically accurate precision-preserving quantization with compression, evaluated in the netCDF Operators (NCO, v4.4.8+)

NASA Astrophysics Data System (ADS)

Zender, Charles S.

2016-09-01

Geoscientific models and measurements generate false precision (scientifically meaningless data bits) that wastes storage space. False precision can mislead (by implying noise is signal) and be scientifically pointless, especially for measurements. By contrast, lossy compression can be both economical (save space) and heuristic (clarify data limitations) without compromising the scientific integrity of data. Data quantization can thus be appropriate regardless of whether space limitations are a concern. We introduce, implement, and characterize a new lossy compression scheme suitable for IEEE floating-point data. Our new Bit Grooming algorithm alternately shaves (to zero) and sets (to one) the least significant bits of consecutive values to preserve a desired precision. This is a symmetric, two-sided variant of an algorithm sometimes called Bit Shaving that quantizes values solely by zeroing bits. Our variation eliminates the artificial low bias produced by always zeroing bits, and makes Bit Grooming more suitable for arrays and multi-dimensional fields whose mean statistics are important. Bit Grooming relies on standard lossless compression to achieve the actual reduction in storage space, so we tested Bit Grooming by applying the DEFLATE compression algorithm to bit-groomed and full-precision climate data stored in netCDF3, netCDF4, HDF4, and HDF5 formats. Bit Grooming reduces the storage space required by initially uncompressed and compressed climate data by 25-80 and 5-65 %, respectively, for single-precision values (the most common case for climate data) quantized to retain 1-5 decimal digits of precision. The potential reduction is greater for double-precision datasets. When used aggressively (i.e., preserving only 1-2 digits), Bit Grooming produces storage reductions comparable to other quantization techniques such as Linear Packing. Unlike Linear Packing, whose guaranteed precision rapidly degrades within the relatively narrow dynamic range of values that it can compress, Bit Grooming guarantees the specified precision throughout the full floating-point range. Data quantization by Bit Grooming is irreversible (i.e., lossy) yet transparent, meaning that no extra processing is required by data users/readers. Hence Bit Grooming can easily reduce data storage volume without sacrificing scientific precision or imposing extra burdens on users.

Magnetic resonance imaging for precise radiotherapy of small laboratory animals.

PubMed

Frenzel, Thorsten; Kaul, Michael Gerhard; Ernst, Thomas Michael; Salamon, Johannes; Jäckel, Maria; Schumacher, Udo; Krüll, Andreas

2017-03-01

Radiotherapy of small laboratory animals (SLA) is often not as precisely applied as in humans. Here we describe the use of a dedicated SLA magnetic resonance imaging (MRI) scanner for precise tumor volumetry, radiotherapy treatment planning, and diagnostic imaging in order to make the experiments more accurate. Different human cancer cells were injected at the lower trunk of pfp/rag2 and SCID mice to allow for local tumor growth. Data from cross sectional MRI scans were transferred to a clinical treatment planning system (TPS) for humans. Manual palpation of the tumor size was compared with calculated tumor size of the TPS and with tumor weight at necropsy. As a feasibility study MRI based treatment plans were calculated for a clinical 6MV linear accelerator using a micro multileaf collimator (μMLC). In addition, diagnostic MRI scans were used to investigate animals which did clinical poorly during the study. MRI is superior in precise tumor volume definition whereas manual palpation underestimates their size. Cross sectional MRI allow for treatment planning so that conformal irradiation of mice with a clinical linear accelerator using a μMLC is in principle feasible. Several internal pathologies were detected during the experiment using the dedicated scanner. MRI is a key technology for precise radiotherapy of SLA. The scanning protocols provided are suited for tumor volumetry, treatment planning, and diagnostic imaging. Copyright © 2016. Published by Elsevier GmbH.

Detector Outline Document for the Fourth Concept Detector ("4th") at the International Linear Collider

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

Barbareschi, Daniele; et al.

We describe a general purpose detector ( "Fourth Concept") at the International Linear Collider (ILC) that can measure with high precision all the fundamental fermions and bosons of the standard model, and thereby access all known physics processes. The 4th concept consists of four basic subsystems: a pixel vertex detector for high precision vertex definitions, impact parameter tagging and near-beam occupancy reduction; a Time Projection Chamber for robust pattern recognition augmented with three high-precision pad rows for precision momentum measurement; a high precision multiple-readout fiber calorimeter, complemented with an EM dual-readout crystal calorimeter, for the energy measurement of hadrons, jets,more » electrons, photons, missing momentum, and the tagging of muons; and, an iron-free dual-solenoid muon system for the inverse direction bending of muons in a gas volume to achieve high acceptance and good muon momentum resolution. The pixel vertex chamber, TPC and calorimeter are inside the solenoidal magnetic field. All four subsytems separately achieve the important scientific goal to be 2-to-10 times better than the already excellent LEP detectors, ALEPH, DELPHI, L3 and OPAL. All four basic subsystems contribute to the identification of standard model partons, some in unique ways, such that consequent physics studies are cogent. As an integrated detector concept, we achieve comprehensive physics capabilities that puts all conceivable physics at the ILC within reach.« less

Validation of HPLC and UV spectrophotometric methods for the determination of meropenem in pharmaceutical dosage form.

PubMed

Mendez, Andreas S L; Steppe, Martin; Schapoval, Elfrides E S

2003-12-04

A high-performance liquid chromatographic method and a UV spectrophotometric method for the quantitative determination of meropenem, a highly active carbapenem antibiotic, in powder for injection were developed in present work. The parameters linearity, precision, accuracy, specificity, robustness, limit of detection and limit of quantitation were studied according to International Conference on Harmonization guidelines. Chromatography was carried out by reversed-phase technique on an RP-18 column with a mobile phase composed of 30 mM monobasic phosphate buffer and acetonitrile (90:10; v/v), adjusted to pH 3.0 with orthophosphoric acid. The UV spectrophotometric method was performed at 298 nm. The samples were prepared in water and the stability of meropenem in aqueous solution at 4 and 25 degrees C was studied. The results were satisfactory with good stability after 24 h at 4 degrees C. Statistical analysis by Student's t-test showed no significant difference between the results obtained by the two methods. The proposed methods are highly sensitive, precise and accurate and can be used for the reliable quantitation of meropenem in pharmaceutical dosage form.

Development and validation of liquid chromatographic and UV derivative spectrophotometric methods for the determination of famciclovir in pharmaceutical dosage forms.

PubMed

Srinubabu, Gedela; Sudharani, Batchu; Sridhar, Lade; Rao, Jvln Seshagiri

2006-06-01

A high-performance liquid chromatographic method and a UV derivative spectrophotometric method for the determination of famciclovir, a highly active antiviral agent, in tablets were developed in the present work. The various parameters, such as linearity, precision, accuracy, specificity, robustness, limit of detection and limit of quantitation were studied according to International Conference on Harmonization guidelines. HPLC was carried out by using the reversed-phase technique on an RP-18 column with a mobile phase composed of 50 mM monobasic phosphate buffer and methanol (50 : 50; v/v), adjusted to pH 3.05 with orthophosphoric acid. The mobile phase was pumped at a flow rate of 1 ml/min and detection was made at 242 nm with UV dual absorbance detector. The first derivative UV spectrophotometric method was performed at 226.5 nm. Statistical analysis was done by Student's t-test and F-test, which showed no significant difference between the results obtained by the two methods. The proposed methods are highly sensitive, precise and accurate and therefore can be used for its Intended purpose.

Validation of 2 commercially available enzyme-linked immunosorbent assays for adiponectin determination in canine serum samples.

PubMed

Tvarijonaviciute, Asta; Martínez-Subiela, Silvia; Ceron, José J

2010-10-01

The aim of this study was to validate 2 commercially available enzyme-linked immunosorbent assays (ELISAs) for adiponectin in dogs, 1 canine-specific and 1 originally designed for measurements in humans. Intra-assay and interassay precision was evaluated by multiple measurements in canine serum samples, and assay accuracy was indirectly determined by linearity under dilution. Interference caused by hemolysis and lipemia was also studied. Both assays were subsequently used for measuring adiponectin concentrations in clinically healthy dogs and those with different grades of obesity. The intra-assay and inter-assay precision was less than 7.5% and 13.5% in serum samples with low and high adiponectin concentrations, respectively. Lipemia and hemolysis did not affect the results of any of the assays. Both assays were able to differentiate lean dogs from those that were overweight or obese on the basis of the measured adiponectin concentrations. From these results it can be concluded that canine adiponectin concentrations can be measured reliably by means of the 2 ELISAs evaluated in this study.

Validation of 2 commercially available enzyme-linked immunosorbent assays for adiponectin determination in canine serum samples

PubMed Central

Tvarijonaviciute, Asta; Martínez-Subiela, Silvia; Ceron, José J.

2010-01-01

The aim of this study was to validate 2 commercially available enzyme-linked immunosorbent assays (ELISAs) for adiponectin in dogs, 1 canine-specific and 1 originally designed for measurements in humans. Intra-assay and interassay precision was evaluated by multiple measurements in canine serum samples, and assay accuracy was indirectly determined by linearity under dilution. Interference caused by hemolysis and lipemia was also studied. Both assays were subsequently used for measuring adiponectin concentrations in clinically healthy dogs and those with different grades of obesity. The intra-assay and inter-assay precision was less than 7.5% and 13.5% in serum samples with low and high adiponectin concentrations, respectively. Lipemia and hemolysis did not affect the results of any of the assays. Both assays were able to differentiate lean dogs from those that were overweight or obese on the basis of the measured adiponectin concentrations. From these results it can be concluded that canine adiponectin concentrations can be measured reliably by means of the 2 ELISAs evaluated in this study. PMID:21197228

Spectrophotometric methods for simultaneous determination of betamethasone valerate and fusidic acid in their binary mixture.

PubMed

Lotfy, Hayam Mahmoud; Salem, Hesham; Abdelkawy, Mohammad; Samir, Ahmed

2015-04-05

Five spectrophotometric methods were successfully developed and validated for the determination of betamethasone valerate and fusidic acid in their binary mixture. Those methods are isoabsorptive point method combined with the first derivative (ISO Point--D1) and the recently developed and well established methods namely ratio difference (RD) and constant center coupled with spectrum subtraction (CC) methods, in addition to derivative ratio (1DD) and mean centering of ratio spectra (MCR). New enrichment technique called spectrum addition technique was used instead of traditional spiking technique. The proposed spectrophotometric procedures do not require any separation steps. Accuracy, precision and linearity ranges of the proposed methods were determined and the specificity was assessed by analyzing synthetic mixtures of both drugs. They were applied to their pharmaceutical formulation and the results obtained were statistically compared to that of official methods. The statistical comparison showed that there is no significant difference between the proposed methods and the official ones regarding both accuracy and precision. Copyright © 2015 Elsevier B.V. All rights reserved.

Precise Point Positioning Using Triple GNSS Constellations in Various Modes

PubMed Central

Afifi, Akram; El-Rabbany, Ahmed

2016-01-01

This paper introduces a new dual-frequency precise point positioning (PPP) model, which combines the observations from three different global navigation satellite system (GNSS) constellations, namely GPS, Galileo, and BeiDou. Combining measurements from different GNSS systems introduces additional biases, including inter-system bias and hardware delays, which require rigorous modelling. Our model is based on the un-differenced and between-satellite single-difference (BSSD) linear combinations. BSSD linear combination cancels out some receiver-related biases, including receiver clock error and non-zero initial phase bias of the receiver oscillator. Forming the BSSD linear combination requires a reference satellite, which can be selected from any of the GPS, Galileo, and BeiDou systems. In this paper three BSSD scenarios are tested; each considers a reference satellite from a different GNSS constellation. Natural Resources Canada’s GPSPace PPP software is modified to enable a combined GPS, Galileo, and BeiDou PPP solution and to handle the newly introduced biases. A total of four data sets collected at four different IGS stations are processed to verify the developed PPP model. Precise satellite orbit and clock products from the International GNSS Service Multi-GNSS Experiment (IGS-MGEX) network are used to correct the GPS, Galileo, and BeiDou measurements in the post-processing PPP mode. A real-time PPP solution is also obtained, which is referred to as RT-PPP in the sequel, through the use of the IGS real-time service (RTS) for satellite orbit and clock corrections. However, only GPS and Galileo observations are used for the RT-PPP solution, as the RTS-IGS satellite products are not presently available for BeiDou system. All post-processed and real-time PPP solutions are compared with the traditional un-differenced GPS-only counterparts. It is shown that combining the GPS, Galileo, and BeiDou observations in the post-processing mode improves the PPP convergence time by 25% compared with the GPS-only counterpart, regardless of the linear combination used. The use of BSSD linear combination improves the precision of the estimated positioning parameters by about 25% in comparison with the GPS-only PPP solution. Additionally, the solution convergence time is reduced to 10 minutes for the BSSD model, which represents about 50% reduction, in comparison with the GPS-only PPP solution. The GNSS RT-PPP solution, on the other hand, shows a similar convergence time and precision to the GPS-only counterpart. PMID:27240376

Precise Point Positioning Using Triple GNSS Constellations in Various Modes.

PubMed

Afifi, Akram; El-Rabbany, Ahmed

2016-05-28

This paper introduces a new dual-frequency precise point positioning (PPP) model, which combines the observations from three different global navigation satellite system (GNSS) constellations, namely GPS, Galileo, and BeiDou. Combining measurements from different GNSS systems introduces additional biases, including inter-system bias and hardware delays, which require rigorous modelling. Our model is based on the un-differenced and between-satellite single-difference (BSSD) linear combinations. BSSD linear combination cancels out some receiver-related biases, including receiver clock error and non-zero initial phase bias of the receiver oscillator. Forming the BSSD linear combination requires a reference satellite, which can be selected from any of the GPS, Galileo, and BeiDou systems. In this paper three BSSD scenarios are tested; each considers a reference satellite from a different GNSS constellation. Natural Resources Canada's GPSPace PPP software is modified to enable a combined GPS, Galileo, and BeiDou PPP solution and to handle the newly introduced biases. A total of four data sets collected at four different IGS stations are processed to verify the developed PPP model. Precise satellite orbit and clock products from the International GNSS Service Multi-GNSS Experiment (IGS-MGEX) network are used to correct the GPS, Galileo, and BeiDou measurements in the post-processing PPP mode. A real-time PPP solution is also obtained, which is referred to as RT-PPP in the sequel, through the use of the IGS real-time service (RTS) for satellite orbit and clock corrections. However, only GPS and Galileo observations are used for the RT-PPP solution, as the RTS-IGS satellite products are not presently available for BeiDou system. All post-processed and real-time PPP solutions are compared with the traditional un-differenced GPS-only counterparts. It is shown that combining the GPS, Galileo, and BeiDou observations in the post-processing mode improves the PPP convergence time by 25% compared with the GPS-only counterpart, regardless of the linear combination used. The use of BSSD linear combination improves the precision of the estimated positioning parameters by about 25% in comparison with the GPS-only PPP solution. Additionally, the solution convergence time is reduced to 10 minutes for the BSSD model, which represents about 50% reduction, in comparison with the GPS-only PPP solution. The GNSS RT-PPP solution, on the other hand, shows a similar convergence time and precision to the GPS-only counterpart.

Geometrical accuracy of metallic objects produced with additive or subtractive manufacturing: A comparative in vitro study.

PubMed

Braian, Michael; Jönsson, David; Kevci, Mir; Wennerberg, Ann

2018-07-01

To evaluate the accuracy and precision of objects produced by additive manufacturing systems (AM) for use in dentistry and to compare with subtractive manufacturing systems (SM). Ten specimens of two geometrical objects were produced by five different AM machines and one SM machine. Object A mimics an inlay-shaped object, while object B imitates a four-unit bridge model. All the objects were sorted into different measurement dimensions (x, y, z), linear distances, angles and corner radius. None of the additive manufacturing or subtractive manufacturing groups presented a perfect match to the CAD file with regard to all parameters included in the present study. Considering linear measurements, the precision for subtractive manufacturing group was consistent in all axes for object A, presenting results of <0.050mm. The additive manufacturing groups had consistent precision in the x-axis and y-axis but not in the z-axis. With regard to corner radius measurements, the SM group had the best overall accuracy and precision for both objects A and B when compared to the AM groups. Within the limitations of this in vitro study, the conclusion can be made that subtractive manufacturing presented overall precision on all measurements below 0.050mm. The AM machines also presented fairly good precision, <0.150mm, on all axes except for the z-axis. Knowledge regarding accuracy and precision for different production techniques utilized in dentistry is of great clinical importance. The dental community has moved from casting to milling and additive techniques are now being implemented. Thus all these production techniques need to be tested, compared and validated. Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.

Third party EPID with IGRT capability retrofitted onto an existing medical linear accelerator

PubMed Central

Odero, DO; Shimm, DS

2009-01-01

Radiation therapy requires precision to avoid unintended irradiation of normal organs. Electronic Portal Imaging Devices (EPIDs), can help with precise patient positioning for accurate treatment. EPIDs are now bundled with new linear accelerators, or they can be purchased from the Linac manufacturer for retrofit. Retrofitting a third party EPID to a linear accelerator can pose challenges. The authors describe a relatively inexpensive third party CCD camera-based EPID manufactured by TheraView (Cablon Medical B.V.), installed onto a Siemens Primus linear accelerator, and integrated with a Lantis record and verify system, an Oldelft simulator with Digital Therapy Imaging (DTI) unit, and a Philips ADAC Pinnacle treatment planning system (TPS). This system integrates well with existing equipment and its software can process DICOM images from other sources. The system provides a complete imaging system that eliminates the need for separate software for portal image viewing, interpretation, analysis, archiving, image guided radiation therapy and other image management applications. It can also be accessed remotely via safe VPN tunnels. TheraView EPID retrofit therefore presents an example of a less expensive alternative to linear accelerator manufacturers’ proprietary EPIDs suitable for implementation in third world countries radiation therapy departments which are often faced with limited financial resources. PMID:21611056

Third party EPID with IGRT capability retrofitted onto an existing medical linear accelerator.

PubMed

Odero, D O; Shimm, D S

2009-07-01

Radiation therapy requires precision to avoid unintended irradiation of normal organs. Electronic Portal Imaging Devices (EPIDs), can help with precise patient positioning for accurate treatment. EPIDs are now bundled with new linear accelerators, or they can be purchased from the Linac manufacturer for retrofit. Retrofitting a third party EPID to a linear accelerator can pose challenges. The authors describe a relatively inexpensive third party CCD camera-based EPID manufactured by TheraView (Cablon Medical B.V.), installed onto a Siemens Primus linear accelerator, and integrated with a Lantis record and verify system, an Oldelft simulator with Digital Therapy Imaging (DTI) unit, and a Philips ADAC Pinnacle treatment planning system (TPS). This system integrates well with existing equipment and its software can process DICOM images from other sources. The system provides a complete imaging system that eliminates the need for separate software for portal image viewing, interpretation, analysis, archiving, image guided radiation therapy and other image management applications. It can also be accessed remotely via safe VPN tunnels. TheraView EPID retrofit therefore presents an example of a less expensive alternative to linear accelerator manufacturers' proprietary EPIDs suitable for implementation in third world countries radiation therapy departments which are often faced with limited financial resources.

Precision thermometry and the quantum speed limit

NASA Astrophysics Data System (ADS)

Campbell, Steve; Genoni, Marco G.; Deffner, Sebastian

2018-04-01

We assess precision thermometry for an arbitrary single quantum system. For a d-dimensional harmonic system we show that the gap sets a single temperature that can be optimally estimated. Furthermore, we establish a simple linear relationship between the gap and this temperature, and show that the precision exhibits a quadratic relationship. We extend our analysis to explore systems with arbitrary spectra, showing that exploiting anharmonicity and degeneracy can greatly enhance the precision of thermometry. Finally, we critically assess the dynamical features of two thermometry protocols for a two level system. By calculating the quantum speed limit we find that, despite the gap fixing a preferred temperature to probe, there is no evidence of this emerging in the dynamical features.

Image guided IMRT dosimetry using anatomy specific MOSFET configurations

PubMed Central

Norrlinger, Bern; Heaton, Robert; Islam, Mohammad

2008-01-01

We have investigated the feasibility of using a set of multiple MOSFETs in conjunction with the mobileMOSFET wireless dosimetry system, to perform a comprehensive and efficient quality assurance (QA) of IMRT plans. Anatomy specific MOSFET configurations incorporating 5 MOSFETs have been developed for a specially designed IMRT dosimetry phantom. Kilovoltage cone beam computed tomography (kV CBCT) imaging was used to increase the positional precision and accuracy of the detectors and phantom, and so minimize dosimetric uncertainties in high dose gradient regions. The effectiveness of the MOSFET based dose measurements was evaluated by comparing the corresponding doses measured by an ion chamber. For 20 head and neck IMRT plans the agreement between the MOSFET and ionization chamber dose measurements was found to be within −0.26±0.88% and 0.06±1.94% (1σ) for measurement points in the high dose and low dose respectively. A precision of 1 mm in detector positioning was achieved by using the X‐Ray Volume Imaging (XVI) kV CBCT system available with the Elekta Synergy Linear Accelerator. Using the anatomy specific MOSFET configurations, simultaneous measurements were made at five strategically located points covering high dose and low dose regions. The agreement between measurements and calculated doses by the treatment planning system for head and neck and prostate IMRT plans was found to be within 0.47±2.45%. The results indicate that a cylindrical phantom incorporating multiple MOSFET detectors arranged in an anatomy specific configuration, in conjunction with image guidance, can be utilized to perform a comprehensive and efficient quality assurance of IMRT plans. PACS number: 87.55.Qr

Design of Feedforward Controller to Reduce Force Ripple for Linear Motor using Halbach Magnet Array with T Shape Magnet

NASA Astrophysics Data System (ADS)

Kim, Moojong; Kim, Jinyoung; Lee, Moon G.

Recently, in micro/nano fabrication equipments, linear motors are widely used as an actuator to position workpiece, machining tool and measurement head. To control them faster and more precise, the motor should have high actuating force and small force ripple. High actuating force enable us to more workpiece with high acceleration. Eventually, it may provide higher throughput. Force ripple gives detrimental effect on the precision and tracking performance of the equipments. In order to accomplish more precise motion, it is important to make lower the force ripple. Force ripple is categorized into cogging and mutual ripple. First is dependent on the shape of magnets and/or core. The second is not dependent on them but dependent on current commutation. In this work, coreless mover i.e. coil winding is applied to the linear motor to avoid the cogging ripple. Therefore, the mutual ripple is only considered to be minimized. Ideal Halbach magnet array has continuously varying magnetization. The THMA (Halbach magnet array with T shape magnets) is proposed to approximate the ideal one. The THMA can not produce ideal sinusoidal flux, therefore, the linear motor with THMA and sinusoidal commutation of current generates the mutual force ripple. In this paper, in order to compensate mutual force ripple by feedforward(FF) controller, we calculate the optimized commutation of input current. The ripple is lower than 1.17% of actuating force if the commutation current agree with the magnetic flux from THMA. The performance of feedforward(FF) controller is verified by experiment.

In vivo inhibition of circulating tumor cells by two apoptosis-promoting circular aptamers with enhanced specificity.

PubMed

Dong, Haiyan; Han, Longyu; Wang, Jie; Xie, Jingjing; Gao, Yu; Xie, Fangwei; Jia, Lee

2018-05-07

Circulating tumor cells (CTCs) are known as the root cause of cancer metastasis that accounts for 90% of cancer death. Owing to the rarity of blood CTCs and their microenvironmental complexity, the existing biotechnology could not precisely capture and apoptosize CTCs in vivo for cancer metastasis prevention. Here, we designed two double strand circular aptamers aimed to simultaneously target MUC1 and HER2 surface biomarkers on mesenchymal cancer cells. The circular aptamers are composed of a capture arm for binding and seizing CTCs and a circular body for resisting degradation by exonucleases. We conjugated the two circular aptamers onto dendrimer PAMAM G4.5 (dcAp1-G-dcAp2), and the conjugate entity showed both significantly-enhanced biostability in serum for days compared with their linear counterparts and capture specificity in RBC (1:10 8 ) compared with their single circular aptamers. dcAp1-G-dcAp2 apoptosized the targeted cells and inhibited their bioenergetic activities significantly by lowing △Ψm, ATP and lactate productions while increasing ROS production. dcAp1-G-dcAp2 captured CTCs in mice in vivo and in patient blood. This study lays the foundation for developing multiple biostable circular aptamers and conjugating them together to precisely capture and apoptosize mesenchymal CTCs in vivo. Copyright © 2018 Elsevier B.V. All rights reserved.

Estimating economic thresholds for site-specific weed control using manual weed counts and sensor technology: an example based on three winter wheat trials.

PubMed

Keller, Martina; Gutjahr, Christoph; Möhring, Jens; Weis, Martin; Sökefeld, Markus; Gerhards, Roland

2014-02-01

Precision experimental design uses the natural heterogeneity of agricultural fields and combines sensor technology with linear mixed models to estimate the effect of weeds, soil properties and herbicide on yield. These estimates can be used to derive economic thresholds. Three field trials are presented using the precision experimental design in winter wheat. Weed densities were determined by manual sampling and bi-spectral cameras, yield and soil properties were mapped. Galium aparine, other broad-leaved weeds and Alopecurus myosuroides reduced yield by 17.5, 1.2 and 12.4 kg ha(-1) plant(-1)  m(2) in one trial. The determined thresholds for site-specific weed control with independently applied herbicides were 4, 48 and 12 plants m(-2), respectively. Spring drought reduced yield effects of weeds considerably in one trial, since water became yield limiting. A negative herbicide effect on the crop was negligible, except in one trial, in which the herbicide mixture tended to reduce yield by 0.6 t ha(-1). Bi-spectral cameras for weed counting were of limited use and still need improvement. Nevertheless, large weed patches were correctly identified. The current paper presents a new approach to conducting field trials and deriving decision rules for weed control in farmers' fields. © 2013 Society of Chemical Industry.

A refined methodology for modeling volume quantification performance in CT

NASA Astrophysics Data System (ADS)

Chen, Baiyu; Wilson, Joshua; Samei, Ehsan

2014-03-01

The utility of CT lung nodule volume quantification technique depends on the precision of the quantification. To enable the evaluation of quantification precision, we previously developed a mathematical model that related precision to image resolution and noise properties in uniform backgrounds in terms of an estimability index (e'). The e' was shown to predict empirical precision across 54 imaging and reconstruction protocols, but with different correlation qualities for FBP and iterative reconstruction (IR) due to the non-linearity of IR impacted by anatomical structure. To better account for the non-linearity of IR, this study aimed to refine the noise characterization of the model in the presence of textured backgrounds. Repeated scans of an anthropomorphic lung phantom were acquired. Subtracted images were used to measure the image quantum noise, which was then used to adjust the noise component of the e' calculation measured from a uniform region. In addition to the model refinement, the validation of the model was further extended to 2 nodule sizes (5 and 10 mm) and 2 segmentation algorithms. Results showed that the magnitude of IR's quantum noise was significantly higher in structured backgrounds than in uniform backgrounds (ASiR, 30-50%; MBIR, 100-200%). With the refined model, the correlation between e' values and empirical precision no longer depended on reconstruction algorithm. In conclusion, the model with refined noise characterization relfected the nonlinearity of iterative reconstruction in structured background, and further showed successful prediction of quantification precision across a variety of nodule sizes, dose levels, slice thickness, reconstruction algorithms, and segmentation software.

Linear Collider Physics Resource Book for Snowmass 2001 - Part 3: Studies of Exotic and Standard Model Physics

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

Abe, T.; et al.

This Resource Book reviews the physics opportunities of a next-generation e+e- linear collider and discusses options for the experimental program. Part 3 reviews the possible experiments on that can be done at a linear collider on strongly coupled electroweak symmetry breaking, exotic particles, and extra dimensions, and on the top quark, QCD, and two-photon physics. It also discusses the improved precision electroweak measurements that this collider will make available.

Characterizations of linear sufficient statistics

NASA Technical Reports Server (NTRS)

Peters, B. C., Jr.; Reoner, R.; Decell, H. P., Jr.

1977-01-01

A surjective bounded linear operator T from a Banach space X to a Banach space Y must be a sufficient statistic for a dominated family of probability measures defined on the Borel sets of X. These results were applied, so that they characterize linear sufficient statistics for families of the exponential type, including as special cases the Wishart and multivariate normal distributions. The latter result was used to establish precisely which procedures for sampling from a normal population had the property that the sample mean was a sufficient statistic.

Lexan Linear Shaped Charge Holder with Magnets and Backing Plate

NASA Technical Reports Server (NTRS)

Maples, Matthew W.; Dutton, Maureen L.; Hacker, Scott C.; Dean, Richard J.; Kidd, Nicholas; Long, Chris; Hicks, Robert C.

2013-01-01

A method was developed for cutting a fabric structural member in an inflatable module, without damaging the internal structure of the module, using linear shaped charge. Lexan and magnets are used in a charge holder to precisely position the linear shaped charge over the desired cut area. Two types of charge holders have been designed, each with its own backing plate. One holder cuts fabric straps in the vertical configuration, and the other charge holder cuts fabric straps in the horizontal configuration.

An in-house assay for BK polyomavirus quantification using the Abbott m2000 RealTime system.

PubMed

Muldrew, Kenneth L; Lovett, Jennie L

2013-11-01

BK polyomavirus (BKPyV) quantification is useful for monitoring renal transplant patient response to therapy. The Abbott m2000 RealTime System employed by some clinical laboratories to perform US Food and Drug Administration-approved assays can also be used to develop in-house assays such as the one presented here. This study aimed to validate an in-house quantitative real-time PCR assay targeting the BKPyV major capsid VP1 gene for assessment of viral load using the Abbott m2000 RealTime System. BKPyV load was measured in 95 urine and plasma samples previously tested for BKPyV by one of three laboratories (46 BKPyV-positive samples consisting of 35 plasma and 11 urine samples; 49 samples negative for BKPyV consisting of 47 plasma and two urine samples). Two additional plasma specimens from the College of American Pathologists proficiency testing survey were also analysed. Precision studies were performed by diluting a high-viral-titre patient sample into BKPyV-negative pooled plasma to create high-positive (6.16 log10 copies ml(-1)) and low-positive (3.16 log10 copies ml(-1)) samples. For precision studies of inter-assay variability, a high-positive (7.0 log10 copies ml(-1)) and a low-positive (3.0 log10 copies ml(-1)) sample were measured in 20 separate runs. The assay's limit of quantification and limit of detection were 2.70 and 2.25 log10 copies ml(-1), respectively. The assay was linear from 2.70 to 9.26 log10 copies ml(-1). Of the 48 known positives, 43 were detected as positive, with three reported by the reference laboratory as values lower than the limit of detection. Two known positives at 3.27 and 3.80 log10 copies ml(-1) tested negative by the m2000 BKPyV assay. Of the 49 known negative samples, 48 were negative by the m2000 BKPyV load assay, with one sample confirmed positive by a reference laboratory. Qualitative analysis prior to discrepancy testing demonstrated a sensitivity of 89.58 % and a specificity of 97.96 %. Precision studies demonstrated inter-assay coefficients of variation of 0.63 % (high positive) and 4.38 % (low positive). Genotyping was performed on 22 patient samples, of which 21 (95.45 %) were type I and one (4.55 %) was type II. In conclusion, the m2000 BKPyV viral load assay sensitivity, specificity, linear range, precision and cost effectiveness make it an attractive methodology for clinical laboratories using the Abbott m2000 RealTime System.

A novel high sensitivity HPLC assay for topiramate, using 4-chloro-7-nitrobenzofurazan as pre-column fluorescence derivatizing agent.

PubMed

Bahrami, Gholamreza; Mohammadi, Bahareh

2007-05-01

A new, sensitive and simple high-performance liquid chromatographic method for analysis of topiramate, an antiepileptic agent, using 4-chloro-7-nitrobenzofurazan as pre-column derivatization agent is described. Following liquid-liquid extraction of topiramate and an internal standard (amlodipine) from human serum, derivatization of the drugs was performed by the labeling agent in the presence of dichloromethane, methanol, acetonitrile and borate buffer (0.05 M; pH 10.6). A mixture of sodium phosphate buffer (0.05 M; pH 2.4): methanol (35:65 v/v) was eluted as mobile phase and chromatographic separation was achieved using a Shimpack CLC-C18 (150 x 4.6 mm) column. In this method the limit of quantification of 0.01 microg/mL was obtained and the procedure was validated over the concentration range of 0.01 to 12.8 microg/mL. No interferences were found from commonly co-administrated antiepileptic drugs including phenytoin, phenobarbital carbamazepine, lamotrigine, zonisamide, primidone, gabapentin, vigabatrin, and ethosuximide. The analysis performance was carried-out in terms of specificity, sensitivity, linearity, precision, accuracy and stability and the method was shown to be accurate, with intra-day and inter-day accuracy from -3.4 to 10% and precise, with intra-day and inter-day precision from 1.1 to 18%.

Precision of a CAD/CAM-engineered surgical template based on a facebow for orthognathic surgery: an experiment with a rapid prototyping maxillary model.

PubMed

Lee, Jae-Won; Lim, Se-Ho; Kim, Moon-Key; Kang, Sang-Hoon

2015-12-01

We examined the precision of a computer-aided design/computer-aided manufacturing-engineered, manufactured, facebow-based surgical guide template (facebow wafer) by comparing it with a bite splint-type orthognathic computer-aided design/computer-aided manufacturing-engineered surgical guide template (bite wafer). We used 24 rapid prototyping (RP) models of the craniofacial skeleton with maxillary deformities. Twelve RP models each were used for the facebow wafer group and the bite wafer group (experimental group). Experimental maxillary orthognathic surgery was performed on the RP models of both groups. Errors were evaluated through comparisons with surgical simulations. We measured the minimum distances from 3 planes of reference to determine the vertical, lateral, and anteroposterior errors at specific measurement points. The measured errors were compared between experimental groups using a t test. There were significant intergroup differences in the lateral error when we compared the absolute values of the 3-D linear distance, as well as vertical, lateral, and anteroposterior errors between experimental groups. The bite wafer method exhibited little lateral error overall and little error in the anterior tooth region. The facebow wafer method exhibited very little vertical error in the posterior molar region. The clinical precision of the facebow wafer method did not significantly exceed that of the bite wafer method. Copyright © 2015 Elsevier Inc. All rights reserved.

Determination of lipophilic marine toxins in mussels. Quantification and confirmation criteria using high resolution mass spectrometry.

PubMed

Domènech, Albert; Cortés-Francisco, Nuria; Palacios, Oscar; Franco, José M; Riobó, Pilar; Llerena, José J; Vichi, Stefania; Caixach, Josep

2014-02-07

A multitoxin method has been developed for quantification and confirmation of lipophilic marine biotoxins in mussels by liquid chromatography coupled to high resolution mass spectrometry (HRMS), using an Orbitrap-Exactive HCD mass spectrometer. Okadaic acid (OA), yessotoxin, azaspiracid-1, gymnodimine, 13-desmethyl spirolide C, pectenotoxin-2 and Brevetoxin B were analyzed as representative compounds of each lipophilic toxin group. HRMS identification and confirmation criteria were established. Fragment and isotope ions and ion ratios were studied and evaluated for confirmation purpose. In depth characterization of full scan and fragmentation spectrum of the main toxins were carried out. Accuracy (trueness and precision), linearity, calibration curve check, limit of quantification (LOQ) and specificity were the parameters established for the method validation. The validation was performed at 0.5 times the current European Union permitted levels. The method performed very well for the parameters investigated. The trueness, expressed as recovery, ranged from 80% to 94%, the precision, expressed as intralaboratory reproducibility, ranged from 5% to 22% and the LOQs range from 0.9 to 4.8pg on column. Uncertainty of the method was also estimated for OA, using a certified reference material. A top-down approach considering two main contributions: those arising from the trueness studies and those coming from the precision's determination, was used. An overall expanded uncertainty of 38% was obtained. Copyright © 2014 Elsevier B.V. All rights reserved.

High Performance Thin layer Chromatography: Densitometry Method for Determination of Rubraxanthone in the Stem Bark Extract of Garcinia cowa Roxb.

PubMed

Hamidi, Dachriyanus; Aulia, Hilyatul; Susanti, Meri

2017-01-01

Garcinia cowa is a medicinal plant widely grown in Southeast Asia and tropical countries. Various parts of this plant have been used in traditional folk medicine. The bark, latex, and root have been used as an antipyretic agent, while fruit and leaves have been used as an expectorant, for indigestion and improvement of blood circulation. This study aims to determine the concentration of rubraxanthone found in ethyl acetate extract of the stem bark of G. cowa by the high-performance thin-layer chromatography (HPTLC). HPTLC method was performed on precoated silica gel G 60 F254 plates using an HPTLC system with a developed mobile-phase system of chloroform: ethyl acetate: methanol: formic acid (86:6:3:5). A volume of 5 μL of standard and sample solutions was applied to the chromatographic plates. The plates were developed in saturated mode of twin trough chamber at room temperature. The method was validated based on linearity, accuracy, precision, limit of detection (LOD), limit of quantification (LOQ), and specificity. The spots were observed at ultraviolet 243 nm. The linearity of rubraxanthone was obtained between 52.5 and 157.5 ppm/spot. The LOD and LOQ were found to be 4.03 and 13.42 ppm/spot, respectively. The proposed method showed good linearity, precision, accuracy, and high sensitivity. Therefore, it may be applied for the quantification of rubraxanthone in ethyl acetate extract of the stem bark of G. cowa . High performance thin layer chromatography (HPTLC) method provides rapid qualitative and quantitative estimation of rubraxanthone as a marker com¬pound in G. cowa extract used for commercial productRubraxanthone found in ethyl acetate extracts of G. cowa was successfully quantified using HPTLC method. Abbreviations Used : TLC: Thin-layer chromatography, HPTLC: High-performance thin-layer chromatography, LOD: Limit of detection, LOQ: Limit of quantification, ICH: International Conference on Harmonization.

Simultaneous Quantification of Gymnemic Acid as Gymnemagenin and Charantin as β-Sitosterol Using Validated HPTLC Densitometric Method.

PubMed

Ahamad, Javed; Amin, Saima; Mir, Showkat R

2015-08-01

Gymnemic acid and charantin are well-established antidiabetic phytosterols found in Gymnema sylvestre and Momordica charantia, respectively. The fact that these plants are often used together in antidiabetic poly-herbal formulations lured us to develop an HPTLC densitometric method for the simultaneous quantification of their bioactive compounds. Indirect estimation of gymnemic acid as gymnemagenin and charantin as β-sitosterol after hydrolysis has been proposed. Aluminum-backed silica gel 60 F254 plates (20 × 10 cm) were used as stationary phase and toluene-ethyl acetate-methanol-formic acid (60 : 20 : 15 : 5, v/v) as mobile phase. Developed chromatogram was scanned at 550 nm after derivatization with modified vanillin-sulfuric acid reagent. Regression analysis of the calibration data showed an excellent linear relationship between peak area versus concentration of the analytes. Linearity was found to be in the range of 500-2,500 and 100-500 ng/band for gymnemagenin and β-sitosterol, respectively. The suitability of the developed HPTLC method for simultaneous estimation of analytes was established by validating it as per the ICH guidelines. The limits of detection and quantification for gymnemagenin were found to be ≈60 and ≈190 ng/band, and those for β-sitosterol ≈30 and ≈90 ng/band, respectively. The developed method was found to be linear (r(2) = 0.9987 and 0.9943), precise (relative standard deviation <1.5 and <2% for intra- and interday precision) and accurate (mean recovery ranged between 98.43-101.44 and 98.68-100.20%) for gymnemagenin and β-sitosterol, respectively. The proposed method was also found specific and robust for quantification of both the analytes and was successfully applied to herbal drugs and in-house herbal formulation without any interference. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Quantifying Isoniazid Levels in Small Hair Samples: A Novel Method for Assessing Adherence during the Treatment of Latent and Active Tuberculosis

PubMed Central

Gerona, Roy; Wen, Anita; Chin, Aaron T.; Koss, Catherine A.; Bacchetti, Peter; Metcalfe, John; Gandhi, Monica

2016-01-01

Background Tuberculosis (TB) is the leading cause of death from an infectious pathogen worldwide and the most prevalent opportunistic infection in people living with HIV. Isoniazid preventive therapy (IPT) reduces the incidence of active TB and reduces morbidity and mortality in HIV-infected patients independently of antiretroviral therapy. However, treatment of latent or active TB is lengthy and inter-patient variability in pharmacokinetics and adherence common. Current methods of assessing adherence to TB treatment using drug levels in plasma or urine assess short-term exposure and pose logistical challenges. Drug concentrations in hair assess long-term exposure and have demonstrated pharmacodynamic relevance in HIV. Methods A large hair sample from a patient with active TB was obtained for assay development. Methods to pulverize hair and extract isoniazid were optimized and then the drug detected by liquid chromatography/ tandem mass spectrometry (LC/MS-MS). The method was validated for specificity, accuracy, precision, recovery, linearity and stability to establish the assay’s suitability for therapeutic drug monitoring (TDM). Hair samples from patients on directly-observe isoniazid-based latent or active TB therapy from the San Francisco Department of Public Health TB clinic were then tested. Results Our LC/MS-MS-based assay detected isoniazid in quantities as low as 0.02ng/mg using 10–25 strands hair. Concentrations in spiked samples demonstrated linearity from 0.05–50ng/mg. Assay precision and accuracy for spiked quality-control samples were high, with an overall recovery rate of 79.5%. In 18 patients with latent or active TB on treatment, isoniazid was detected across a wide linear dynamic range. Conclusions An LC-MS/MS-based assay to quantify isoniazid levels in hair with performance characteristics suitable for TDM was developed and validated. Hair concentrations of isoniazid assess long-term exposure and may be useful for monitoring adherence to latent or active TB treatment in the setting of HIV. PMID:27191185

In vivo dosimetry with optically stimulated luminescent dosimeters for conformal and intensity-modulated radiation therapy: A 2-year multicenter cohort study.

PubMed

Riegel, Adam C; Chen, Yu; Kapur, Ajay; Apicello, Laura; Kuruvilla, Abraham; Rea, Anthony J; Jamshidi, Abolghassem; Potters, Louis

Optically stimulated luminescent dosimeters (OSLDs) are utilized for in vivo dosimetry (IVD) of modern radiation therapy techniques such as intensity modulated radiation therapy (IMRT) and volumetric modulated arc therapy (VMAT). Dosimetric precision achieved with conventional techniques may not be attainable. In this work, we measured accuracy and precision for a large sample of clinical OSLD-based IVD measurements. Weekly IVD measurements were collected from 4 linear accelerators for 2 years and were expressed as percent differences from planned doses. After outlier analysis, 10,224 measurements were grouped in the following way: overall, modality (photons, electrons), treatment technique (3-dimensional [3D] conformal, field-in-field intensity modulation, inverse-planned IMRT, and VMAT), placement location (gantry angle, cardinality, and central axis positioning), and anatomical site (prostate, breast, head and neck, pelvis, lung, rectum and anus, brain, abdomen, esophagus, and bladder). Distributions were modeled via a Gaussian function. Fitting was performed with least squares, and goodness-of-fit was assessed with the coefficient of determination. Model means (μ) and standard deviations (σ) were calculated. Sample means and variances were compared for statistical significance by analysis of variance and the Levene tests (α = 0.05). Overall, μ ± σ was 0.3 ± 10.3%. Precision for electron measurements (6.9%) was significantly better than for photons (10.5%). Precision varied significantly among treatment techniques (P < .0001) with field-in-field lowest (σ = 7.2%) and IMRT and VMAT highest (σ = 11.9% and 13.4%, respectively). Treatment site models with goodness-of-fit greater than 0.90 (6 of 10) yielded accuracy within ±3%, except for head and neck (μ = -3.7%). Precision varied with treatment site (range, 7.3%-13.0%), with breast and head and neck yielding the best and worst precision, respectively. Placement on the central axis of cardinal gantry angles yielded more precise results (σ = 8.5%) compared with other locations (range, 10.5%-11.4%). Accuracy of ±3% was achievable. Precision ranged from 6.9% to 13.4% depending on modality, technique, and treatment site. Simple, standardized locations may improve IVD precision. These findings may aid development of patient-specific tolerances for OSLD-based IVD. Copyright © 2016 American Society for Radiation Oncology. Published by Elsevier Inc. All rights reserved.

Evaluation of a Commercial Glycoprotein Enzyme-Linked Immunosorbent Assay for Measuring Vaccine Immunity to Varicella

PubMed Central

Kim, Yun Hwa; Hwang, Ji Young; Shim, Hye Min; Lee, Eunsil; Park, Songyong

2014-01-01

Purpose To evaluate a recently marketed commercial glycoprotein enzyme-linked immunosorbent assay (gpEIA) kit, the VaccZyme™ VZV gpEIA, for measuring the immunity of varicella-vaccinated children. Materials and Methods We investigated the accuracy and reproducibility of the VaccZyme™ VZV gpEIA kit for the detection of antibodies to VZV. We also examined the sensitivity, specificity, and correlation between antibody titers calculated with gpEIA versus fluorescent antibody to membrane antigen (FAMA) by using sera of 349 children, ranging from 1 to 6 years old. Results VaccZyme™ VZV gpEIA gave precise and reproducible intra- and inter-assay results. FAMA and gpEIA titers showed a linear correlation (Pearson correlation coefficient=0.987). The sensitivity and specificity of the VaccZyme™ gpEIA was 31.4% and 100%, respectively, when the guidelines of the gpEIA (<100 mIU/mL) and FAMA 1:4 were adopted as cutoff values. However, the maximum sensitivity and specificity were 88.9% and 95.1%, respectively, with the highest correlation (κ=0.840), if the cutoff values were set with gpEIA at 49.7 mIU/mL and FAMA 1:16. Conclusion These results demonstrate that the VaccZyme™ VZV gpEIA kit gave precise and reproducible data for measuring antibody titer after varicella vaccination. The results also showed that the antibody titer calculated with the VaccZyme™ gpEIA kit strongly correlated with the FAMA titer. However, cutoff values should be re-optimized for the evaluation of vaccine immunity. PMID:24532518

High Precision Piezoelectric Linear Motors for Operations at Cryogenic Temperatures and Vacuum

NASA Technical Reports Server (NTRS)

Wong, D.; Carman, G.; Stam, M.; Bar-Cohen, Y.; Sen, A.; Henry, P.; Bearman, G.; Moacanin, J.

1995-01-01

The use of an electromechanical device for optically positioning a mirror system during the pre-project phase of the Pluto Fast Flyby mission was evaluated at JPL. The device under consideration was a piezoelectric driven linear motor functionally dependent upon a time varying electric field which induces displacements ranging from submicrons to millimeters with positioning accuracy within nanometers.

Measuring Anxiety in Visually-Impaired People: A Comparison between the Linear and the Nonlinear IRT Approaches

ERIC Educational Resources Information Center

Ferrando, Pere J.; Pallero, Rafael; Anguiano-Carrasco, Cristina

2013-01-01

The present study has two main interests. First, some pending issues about the psychometric properties of the CTAC (an anxiety questionnaire for blind and visually-impaired people) are assessed using item response theory (IRT). Second, the linear model is compared to the graded response model (GRM) in terms of measurement precision, sensitivity…

On the Linear Relation between the Mean and the Standard Deviation of a Response Time Distribution

ERIC Educational Resources Information Center

Wagenmakers, Eric-Jan; Brown, Scott

2007-01-01

Although it is generally accepted that the spread of a response time (RT) distribution increases with the mean, the precise nature of this relation remains relatively unexplored. The authors show that in several descriptive RT distributions, the standard deviation increases linearly with the mean. Results from a wide range of tasks from different…

BLAS- BASIC LINEAR ALGEBRA SUBPROGRAMS

NASA Technical Reports Server (NTRS)

Krogh, F. T.

1994-01-01

The Basic Linear Algebra Subprogram (BLAS) library is a collection of FORTRAN callable routines for employing standard techniques in performing the basic operations of numerical linear algebra. The BLAS library was developed to provide a portable and efficient source of basic operations for designers of programs involving linear algebraic computations. The subprograms available in the library cover the operations of dot product, multiplication of a scalar and a vector, vector plus a scalar times a vector, Givens transformation, modified Givens transformation, copy, swap, Euclidean norm, sum of magnitudes, and location of the largest magnitude element. Since these subprograms are to be used in an ANSI FORTRAN context, the cases of single precision, double precision, and complex data are provided for. All of the subprograms have been thoroughly tested and produce consistent results even when transported from machine to machine. BLAS contains Assembler versions and FORTRAN test code for any of the following compilers: Lahey F77L, Microsoft FORTRAN, or IBM Professional FORTRAN. It requires the Microsoft Macro Assembler and a math co-processor. The PC implementation allows individual arrays of over 64K. The BLAS library was developed in 1979. The PC version was made available in 1986 and updated in 1988.

Analysis of friction and instability by the centre manifold theory for a non-linear sprag-slip model

NASA Astrophysics Data System (ADS)

Sinou, J.-J.; Thouverez, F.; Jezequel, L.

2003-08-01

This paper presents the research devoted to the study of instability phenomena in non-linear model with a constant brake friction coefficient. Indeed, the impact of unstable oscillations can be catastrophic. It can cause vehicle control problems and component degradation. Accordingly, complex stability analysis is required. This paper outlines stability analysis and centre manifold approach for studying instability problems. To put it more precisely, one considers brake vibrations and more specifically heavy trucks judder where the dynamic characteristics of the whole front axle assembly is concerned, even if the source of judder is located in the brake system. The modelling introduces the sprag-slip mechanism based on dynamic coupling due to buttressing. The non-linearity is expressed as a polynomial with quadratic and cubic terms. This model does not require the use of brake negative coefficient, in order to predict the instability phenomena. Finally, the centre manifold approach is used to obtain equations for the limit cycle amplitudes. The centre manifold theory allows the reduction of the number of equations of the original system in order to obtain a simplified system, without loosing the dynamics of the original system as well as the contributions of non-linear terms. The goal is the study of the stability analysis and the validation of the centre manifold approach for a complex non-linear model by comparing results obtained by solving the full system and by using the centre manifold approach. The brake friction coefficient is used as an unfolding parameter of the fundamental Hopf bifurcation point.

An improved triangulation laser rangefinder using a custom CMOS HDR linear image sensor

NASA Astrophysics Data System (ADS)

Liscombe, Michael

3-D triangulation laser rangefinders are used in many modern applications, from terrain mapping to biometric identification. Although a wide variety of designs have been proposed, laser speckle noise still provides a fundamental limitation on range accuracy. These works propose a new triangulation laser rangefinder designed specifically to mitigate the effects of laser speckle noise. The proposed rangefinder uses a precision linear translator to laterally reposition the imaging system (e.g., image sensor and imaging lens). For a given spatial location of the laser spot, capturing N spatially uncorrelated laser spot profiles is shown to improve range accuracy by a factor of N . This technique has many advantages over past speckle-reduction technologies, such as a fixed system cost and form factor, and the ability to virtually eliminate laser speckle noise. These advantages are made possible through spatial diversity and come at the cost of increased acquisition time. The rangefinder makes use of the ICFYKWG1 linear image sensor, a custom CMOS sensor developed at the Vision Sensor Laboratory (York University). Tests are performed on the image sensor's innovative high dynamic range technology to determine its effects on range accuracy. As expected, experimental results have shown that the sensor provides a trade-off between dynamic range and range accuracy.

Fabrication Technologies of the High Gradient Accelerator Structures at 100MV/M Range

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

Wang, Juwen; /SLAC; Lewandowski, James

A CERN-SLAC-KEK collaboration on high gradient X-band structure research has been established in order to demonstrate the feasibility of the CLIC baseline design for the main linac stably operating at more than 100 MV/m loaded accelerating gradient. Several prototype CLIC structures were successfully fabricated and high power tested. They operated at 105 MV/m with a breakdown rate that meets the CLIC linear collider specifications of < 5 x 10{sup -7}/pulse/m. This paper summarizes the fabrication technologies including the mechanical design, precision machining, chemical cleaning, diffusion bonding as well as vacuum baking and all related assembly technologies. Also, the tolerances control,more » tuning and RF characterization will be discussed.« less

[The development and validation of the methods for the quantitative determination of sibutramine derivatives in dietary supplements].

PubMed

Stern, K I; Malkova, T L

The objective of the present study was the development and validation of sibutramine demethylated derivatives, desmethyl sibutramine and didesmethyl sibutramine. Gas-liquid chromatography with the flame ionization detector was used for the quantitative determination of the above substances in dietary supplements. The conditions for the chromatographic determination of the analytes in the presence of the reference standard, methyl stearate, were proposed allowing to achieve the efficient separation. The method has the necessary sensitivity, specificity, linearity, accuracy, and precision (on the intra-day and inter-day basis) which suggests its good validation characteristics. The proposed method can be employed in the analytical laboratories for the quantitative determination of sibutramine derivatives in biologically active dietary supplements.

Fast BIA-amperometric determination of isoniazid in tablets.

PubMed

Quintino, Maria S M; Angnes, Lúcio

2006-09-26

This paper proposes a new, fast and precise method to analyze isoniazid based on the electrochemical oxidation of the analyte at a glassy carbon electrode in 0.1M NaOH. The quantification was performed utilizing amperometry associated with batch injection analysis (BIA) technique. Fast sequential analysis (60 determinations h(-1)) in an unusually wide linear dynamic range (from 2.5 x 10(-8) to 1.0 x 10(-3)M), with high sensitivity and low limits of detection (4.1 x 10(-9)M) and quantification (1.4 x 10(-8)M), was achieved. Such characteristics allied to a good repeatability of the current responses (relative standard deviation of 0.79% for 30 measurements), were explored for the specific determination of isoniazid in isoniazid-rifampin tablet.

Validation of analytical methods in GMP: the disposable Fast Read 102® device, an alternative practical approach for cell counting.

PubMed

Gunetti, Monica; Castiglia, Sara; Rustichelli, Deborah; Mareschi, Katia; Sanavio, Fiorella; Muraro, Michela; Signorino, Elena; Castello, Laura; Ferrero, Ivana; Fagioli, Franca

2012-05-31

The quality and safety of advanced therapy products must be maintained throughout their production and quality control cycle to ensure their final use in patients. We validated the cell count method according to the International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use and European Pharmacopoeia, considering the tests' accuracy, precision, repeatability, linearity and range. As the cell count is a potency test, we checked accuracy, precision, and linearity, according to ICH Q2. Briefly our experimental approach was first to evaluate the accuracy of Fast Read 102® compared to the Bürker chamber. Once the accuracy of the alternative method was demonstrated, we checked the precision and linearity test only using Fast Read 102®. The data were statistically analyzed by average, standard deviation and coefficient of variation percentages inter and intra operator. All the tests performed met the established acceptance criteria of a coefficient of variation of less than ten percent. For the cell count, the precision reached by each operator had a coefficient of variation of less than ten percent (total cells) and under five percent (viable cells). The best range of dilution, to obtain a slope line value very similar to 1, was between 1:8 and 1:128. Our data demonstrated that the Fast Read 102® count method is accurate, precise and ensures the linearity of the results obtained in a range of cell dilution. Under our standard method procedures, this assay may thus be considered a good quality control method for the cell count as a batch release quality control test. Moreover, the Fast Read 102® chamber is a plastic, disposable device that allows a number of samples to be counted in the same chamber. Last but not least, it overcomes the problem of chamber washing after use and so allows a cell count in a clean environment such as that in a Cell Factory. In a good manufacturing practice setting the disposable cell counting devices will allow a single use of the count chamber they can then be thrown away, thus avoiding the waste disposal of vital dye (e.g. Trypan Blue) or lysing solution (e.g. Tuerk solution).

Validation of analytical methods in GMP: the disposable Fast Read 102® device, an alternative practical approach for cell counting

PubMed Central

2012-01-01

Background The quality and safety of advanced therapy products must be maintained throughout their production and quality control cycle to ensure their final use in patients. We validated the cell count method according to the International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use and European Pharmacopoeia, considering the tests’ accuracy, precision, repeatability, linearity and range. Methods As the cell count is a potency test, we checked accuracy, precision, and linearity, according to ICH Q2. Briefly our experimental approach was first to evaluate the accuracy of Fast Read 102® compared to the Bürker chamber. Once the accuracy of the alternative method was demonstrated, we checked the precision and linearity test only using Fast Read 102®. The data were statistically analyzed by average, standard deviation and coefficient of variation percentages inter and intra operator. Results All the tests performed met the established acceptance criteria of a coefficient of variation of less than ten percent. For the cell count, the precision reached by each operator had a coefficient of variation of less than ten percent (total cells) and under five percent (viable cells). The best range of dilution, to obtain a slope line value very similar to 1, was between 1:8 and 1:128. Conclusions Our data demonstrated that the Fast Read 102® count method is accurate, precise and ensures the linearity of the results obtained in a range of cell dilution. Under our standard method procedures, this assay may thus be considered a good quality control method for the cell count as a batch release quality control test. Moreover, the Fast Read 102® chamber is a plastic, disposable device that allows a number of samples to be counted in the same chamber. Last but not least, it overcomes the problem of chamber washing after use and so allows a cell count in a clean environment such as that in a Cell Factory. In a good manufacturing practice setting the disposable cell counting devices will allow a single use of the count chamber they can then be thrown away, thus avoiding the waste disposal of vital dye (e.g. Trypan Blue) or lysing solution (e.g. Tuerk solution). PMID:22650233

Clinical Evaluation of the BD FACSPresto™ Near-Patient CD4 Counter in Kenya

PubMed Central

Angira, Francis; Akoth, Benta; Omolo, Paul; Opollo, Valarie; Bornheimer, Scott; Judge, Kevin; Tilahun, Henok; Lu, Beverly; Omana-Zapata, Imelda; Zeh, Clement

2016-01-01

Background The BD FACSPresto™ Near-Patient CD4 Counter was developed to expand HIV/AIDS management in resource-limited settings. It measures absolute CD4 counts (AbsCD4), percent CD4 (%CD4), and hemoglobin (Hb) from a single drop of capillary or venous blood in approximately 23 minutes, with throughput of 10 samples per hour. We assessed the performance of the BD FACSPresto system, evaluating accuracy, stability, linearity, precision, and reference intervals using capillary and venous blood at KEMRI/CDC HIV-research laboratory, Kisumu, Kenya, and precision and linearity at BD Biosciences, California, USA. Methods For accuracy, venous samples were tested using the BD FACSCalibur™ instrument with BD Tritest™ CD3/CD4/CD45 reagent, BD Trucount™ tubes, and BD Multiset™ software for AbsCD4 and %CD4, and the Sysmex™ KX-21N for Hb. Stability studies evaluated duration of staining (18–120-minute incubation), and effects of venous blood storage <6–24 hours post-draw. A normal cohort was tested for reference intervals. Precision covered multiple days, operators, and instruments. Linearity required mixing two pools of samples, to obtain evenly spaced concentrations for AbsCD4, total lymphocytes, and Hb. Results AbsCD4 and %CD4 venous/capillary (N = 189/ N = 162) accuracy results gave Deming regression slopes within 0.97–1.03 and R2 ≥0.96. For Hb, Deming regression results were R2 ≥0.94 and slope ≥0.94 for both venous and capillary samples. Stability varied within 10% 2 hours after staining and for venous blood stored less than 24 hours. Reference intervals results showed that gender—but not age—differences were statistically significant (p<0.05). Precision results had <3.5% coefficient of variation for AbsCD4, %CD4, and Hb, except for low AbsCD4 samples (<6.8%). Linearity was 42–4,897 cells/μL for AbsCD4, 182–11,704 cells/μL for total lymphocytes, and 2–24 g/dL for Hb. Conclusions The BD FACSPresto system provides accurate, precise clinical results for capillary or venous blood samples and is suitable for near-patient CD4 testing. Trial Registration ClinicalTrials.gov NCT02396355 PMID:27483008

Linear CCD attitude measurement system based on the identification of the auxiliary array CCD

NASA Astrophysics Data System (ADS)

Hu, Yinghui; Yuan, Feng; Li, Kai; Wang, Yan

2015-10-01

Object to the high precision flying target attitude measurement issues of a large space and large field of view, comparing existing measurement methods, the idea is proposed of using two array CCD to assist in identifying the three linear CCD with multi-cooperative target attitude measurement system, and to address the existing nonlinear system errors and calibration parameters and more problems with nine linear CCD spectroscopic test system of too complicated constraints among camera position caused by excessive. The mathematical model of binocular vision and three linear CCD test system are established, co-spot composition triangle utilize three red LED position light, three points' coordinates are given in advance by Cooperate Measuring Machine, the red LED in the composition of the three sides of a triangle adds three blue LED light points as an auxiliary, so that array CCD is easier to identify three red LED light points, and linear CCD camera is installed of a red filter to filter out the blue LED light points while reducing stray light. Using array CCD to measure the spot, identifying and calculating the spatial coordinates solutions of red LED light points, while utilizing linear CCD to measure three red LED spot for solving linear CCD test system, which can be drawn from 27 solution. Measured with array CCD coordinates auxiliary linear CCD has achieved spot identification, and has solved the difficult problems of multi-objective linear CCD identification. Unique combination of linear CCD imaging features, linear CCD special cylindrical lens system is developed using telecentric optical design, the energy center of the spot position in the depth range of convergence in the direction is perpendicular to the optical axis of the small changes ensuring highprecision image quality, and the entire test system improves spatial object attitude measurement speed and precision.

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

PubMed

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

2018-04-01

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

Development of an ion-pair HPLC method for investigation of energy charge changes in cerebral ischemia of mice and hypoxia of Neuro-2a cell line.

PubMed

Chen, Yunyun; Xing, Dongming; Wang, Wei; Ding, Yi; Du, Lijun

2007-06-01

The determination of adenine nucleotides and energy charge (EC) has great importance in the characterization of cerebral ischemic injury and post-ischemic recovery. An IP-HPLC method was developed for the quantification of AMP, ADP, ATP and EC in cerebral ischemia and hypoxia of the Neuro-2a cell line. The chromatographic conditions were: a Zorbax SB-C18 reversed-phase column; mobile phase 100 mM KH(2)PO(4), 1 mM tetrabutylammonium hydroxide, and 2.5% acetonitrile, brought to pH 7.0 with potassium hydroxide (4 M), filtered through a 0.45 microm Millipore filter and degassed prior to use. The flow-rate was 1.0 mL/min. The injection volume was 20 microL. Detection was performed at a wavelength of 254 nm under a constant temperature (27 +/- 1 degrees C). The method was validated by means of linearity, using calibration curves constructed with five concentration levels of each compound. The limit of detection was also determined. The system precision was calculated as the coefficient of variation for five injections for each compound tested. Cerebral tissue was homogenized (4 degrees C) in 1 mL of an ice-cold 6% trichloroacetic acid that contained ATPase inhibitor and obtained good recovery (>90%). The results show that the described method for the determination of adenine nucleotides by HPLC has good linearity, limit of detection, precision and specificity, and is simple and rapid to perform. Copyright 2007 John Wiley & Sons, Ltd.

Development of an improved sample preparation platform for acidic endogenous hormones in plant tissues using electromembrane extraction.

PubMed

Suh, Joon Hyuk; Han, Sang Beom; Wang, Yu

2018-02-02

Despite their importance in pivotal signaling pathways due to trace quantities and complex matrices, the analysis of plant hormones is a challenge. Here, to improve this issue, we present an electromembrane extraction technology combined with liquid chromatography-tandem mass spectrometry for determination of acidic plant hormones including jasmonic acid, abscisic acid, salicylic acid, benzoic acid, gibberellic acid and gibberellin A 4 in plant tissues. Factors influencing extraction efficiency, such as voltage, extraction time and stirring rate were optimized using a design of experiments. Analytical performance was evaluated in terms of specificity, linearity, limit of quantification, precision, accuracy, recovery and repeatability. The results showed good linearity (r 2  > 0.995), precision and acceptable accuracy. The limit of quantification ranged from 0.1 to 10 ng mL -1 , and the recoveries were 34.6-50.3%. The developed method was applied in citrus leaf samples, showing better clean-up efficiency, as well as higher sensitivity compared to a previous method using liquid-liquid extraction. Organic solvent consumption was minimized during the process, making it an appealing method. More noteworthy, electromembrane extraction has been scarcely applied to plant tissues, and this is the first time that major plant hormones were extracted using this technology, with high sensitivity and selectivity. Taken together, this work gives not only a novel sample preparation platform using an electric field for plant hormones, but also a good example of extracting complex plant tissues in a simple and effective way. Copyright © 2017 Elsevier B.V. All rights reserved.

Comparison of UV spectrophotometry and high performance liquid chromatography methods for the determination of repaglinide in tablets.

PubMed

Dhole, Seema M; Khedekar, Pramod B; Amnerkar, Nikhil D

2012-07-01

Repaglinide is a miglitinide class of antidiabetic drug used for the treatment of type 2 diabetes mellitus. A fast and reliable method for the determination of repaglinide was highly desirable to support formulation screening and quality control. UV spectrophotometric and reversed-phase high performance liquid chromatography (RP-HPLC) methods were developed for determination of repaglinide in the tablet dosage form. The UV spectrum recorded between 200 400 nm using methanol as solvent and the wavelength 241 nm was selected for the determination of repaglinide. RP-HPLC analysis was carried out using Agilent TC-C18 (2) column and mobile phase composed of methanol and water (80:20 v/v, pH adjusted to 3.5 with orthophosphoric acid) at a flow rate of 1.0 ml/min. Parameters such as linearity, precision, accuracy, recovery, specificity and ruggedness are studied as reported in the International Conference on Harmonization (ICH) guidelines. The developed methods illustrated excellent linearity (r(2) > 0.999) in the concentration range of 5-30 μg/ml and 5-50 μg/ml for UV spectrophotometric and HPLC methods, respectively. Precision (%R.S.D < 1.50) and mean recoveries were found in the range of 99.63-100.45% for UV spectrophotometric method and 99.71-100.25% for HPLC method which shows accuracy of the methods. The developed methods were found to be reliable, simple, fast, accurate and successfully used for the quality control of repaglinide as a bulk drug and in pharmaceutical formulations.

Comparison of UV spectrophotometry and high performance liquid chromatography methods for the determination of repaglinide in tablets

PubMed Central

Dhole, Seema M.; Khedekar, Pramod B.; Amnerkar, Nikhil D.

2012-01-01

Background: Repaglinide is a miglitinide class of antidiabetic drug used for the treatment of type 2 diabetes mellitus. A fast and reliable method for the determination of repaglinide was highly desirable to support formulation screening and quality control. Objective: UV spectrophotometric and reversed-phase high performance liquid chromatography (RP-HPLC) methods were developed for determination of repaglinide in the tablet dosage form. Materials and Methods: The UV spectrum recorded between 200 400 nm using methanol as solvent and the wavelength 241 nm was selected for the determination of repaglinide. RP-HPLC analysis was carried out using Agilent TC-C18 (2) column and mobile phase composed of methanol and water (80:20 v/v, pH adjusted to 3.5 with orthophosphoric acid) at a flow rate of 1.0 ml/min. Parameters such as linearity, precision, accuracy, recovery, specificity and ruggedness are studied as reported in the International Conference on Harmonization (ICH) guidelines. Results: The developed methods illustrated excellent linearity (r2 > 0.999) in the concentration range of 5-30 μg/ml and 5-50 μg/ml for UV spectrophotometric and HPLC methods, respectively. Precision (%R.S.D < 1.50) and mean recoveries were found in the range of 99.63-100.45% for UV spectrophotometric method and 99.71-100.25% for HPLC method which shows accuracy of the methods. Conclusion: The developed methods were found to be reliable, simple, fast, accurate and successfully used for the quality control of repaglinide as a bulk drug and in pharmaceutical formulations. PMID:23781481

Validated spectrophotometric methods for determination of sodium valproate based on charge transfer complexation reactions.

PubMed

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

2016-02-15

This work presents the development, validation and application of four simple and direct spectrophotometric methods for determination of sodium valproate (VP) through charge transfer complexation reactions. The first method is based on the reaction of the drug with p-chloranilic acid (p-CA) in acetone to give a purple colored product with maximum absorbance at 524nm. The second method depends on the reaction of VP with dichlone (DC) in dimethylformamide forming a reddish orange product measured at 490nm. The third method is based upon the interaction of VP and picric acid (PA) in chloroform resulting in the formation of a yellow complex measured at 415nm. The fourth method involves the formation of a yellow complex peaking at 361nm upon the reaction of the drug with iodine in chloroform. Experimental conditions affecting the color development were studied and optimized. Stoichiometry of the reactions was determined. The proposed spectrophotometric procedures were effectively validated with respect to linearity, ranges, precision, accuracy, specificity, robustness, detection and quantification limits. Calibration curves of the formed color products with p-CA, DC, PA and iodine showed good linear relationships over the concentration ranges 24-144, 40-200, 2-20 and 1-8μg/mL respectively. The proposed methods were successfully applied to the assay of sodium valproate in tablets and oral solution dosage forms with good accuracy and precision. Assay results were statistically compared to a reference pharmacopoeial HPLC method where no significant differences were observed between the proposed methods and reference method. Copyright © 2015 Elsevier B.V. All rights reserved.

Validated spectrophotometric methods for determination of sodium valproate based on charge transfer complexation reactions

NASA Astrophysics Data System (ADS)

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

2016-02-01

This work presents the development, validation and application of four simple and direct spectrophotometric methods for determination of sodium valproate (VP) through charge transfer complexation reactions. The first method is based on the reaction of the drug with p-chloranilic acid (p-CA) in acetone to give a purple colored product with maximum absorbance at 524 nm. The second method depends on the reaction of VP with dichlone (DC) in dimethylformamide forming a reddish orange product measured at 490 nm. The third method is based upon the interaction of VP and picric acid (PA) in chloroform resulting in the formation of a yellow complex measured at 415 nm. The fourth method involves the formation of a yellow complex peaking at 361 nm upon the reaction of the drug with iodine in chloroform. Experimental conditions affecting the color development were studied and optimized. Stoichiometry of the reactions was determined. The proposed spectrophotometric procedures were effectively validated with respect to linearity, ranges, precision, accuracy, specificity, robustness, detection and quantification limits. Calibration curves of the formed color products with p-CA, DC, PA and iodine showed good linear relationships over the concentration ranges 24-144, 40-200, 2-20 and 1-8 μg/mL respectively. The proposed methods were successfully applied to the assay of sodium valproate in tablets and oral solution dosage forms with good accuracy and precision. Assay results were statistically compared to a reference pharmacopoeial HPLC method where no significant differences were observed between the proposed methods and reference method.

Sources of variability in satellite-derived estimates of Phytoplankton production in the eastern tropical Pacific

NASA Astrophysics Data System (ADS)

Banse, Karl; Yong, Marina

1990-05-01

As a proxy for satellite (coastal zone color scanner) observations and concurrent measurements of primary production rates, data from 138 stations occupied seasonally during 1967-1968 in the offshore, eastern tropical Pacific were analyzed in terms of six temporal groups and four current regimes. In multiple linear regressions on column production Pt, we found that simulated satellite pigment is generally weakly correlated, but sometimes not correlated with Pt, and that incident irradiance, sea surface temperature, nitrate, transparency, and depths of mixed layer or nitracline assume little or no importance. After a proxy for the light-saturated chlorophyll-specific photosynthetic rate pmax is added, the coefficient of determination (r2) ranges from 0.55 to 0.91 (median of 0.85) for the 10 cases. In stepwise multiple linear regressions the pmax proxy is the best predictor for Pt. Pt can be calculated fairly accurately (on the average, within 10-20%) from satellite pigment, the 10% light depth, and station values (but not from regional or seasonal means) of the pmax proxy; for individual stations the precision is 35-84% (median of 57% for the 10 groupings; p = 0.05) of the means of observed values. At present, pmax cannot be estimated from space; in the data set it is not even highly correlated with irradiance, temperature, and nitrate at depth of occurrence. Therefore extant models for calculating Pt in this tropical ocean have inherent limits of accuracy as well as of precision owing to ignorance about a physiological parameter.

Comparison of the efficacy of three PubMed search filters in finding randomized controlled trials to answer clinical questions.

PubMed

Yousefi-Nooraie, Reza; Irani, Shirin; Mortaz-Hedjri, Soroush; Shakiba, Behnam

2013-10-01

The aim of this study was to compare the performance of three search methods in the retrieval of relevant clinical trials from PubMed to answer specific clinical questions. Included studies of a sample of 100 Cochrane reviews which recorded in PubMed were considered as the reference standard. The search queries were formulated based on the systematic review titles. Precision, recall and number of retrieved records for limiting the results to clinical trial publication type, and using sensitive and specific clinical queries filters were compared. The number of keywords, presence of specific names of intervention and syndrome in the search keywords were used in a model to predict the recalls and precisions. The Clinical queries-sensitive search strategy retrieved the largest number of records (33) and had the highest recall (41.6%) and lowest precision (4.8%). The presence of specific intervention name was the only significant predictor of all recalls and precisions (P = 0.016). The recall and precision of combination of simple clinical search queries and methodological search filters to find clinical trials in various subjects were considerably low. The limit field strategy yielded in higher precision and fewer retrieved records and approximately similar recall, compared with the clinical queries-sensitive strategy. Presence of specific intervention name in the search keywords increased both recall and precision. © 2010 John Wiley & Sons Ltd.

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

PubMed

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

2017-08-20

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

On the reliability of computed chaotic solutions of non-linear differential equations

NASA Astrophysics Data System (ADS)

Liao, Shijun

2009-08-01

A new concept, namely the critical predictable time Tc, is introduced to give a more precise description of computed chaotic solutions of non-linear differential equations: it is suggested that computed chaotic solutions are unreliable and doubtable when t > Tc. This provides us a strategy to detect reliable solution from a given computed result. In this way, the computational phenomena, such as computational chaos (CC), computational periodicity (CP) and computational prediction uncertainty, which are mainly based on long-term properties of computed time-series, can be completely avoided. Using this concept, the famous conclusion `accurate long-term prediction of chaos is impossible' should be replaced by a more precise conclusion that `accurate prediction of chaos beyond the critical predictable time Tc is impossible'. So, this concept also provides us a timescale to determine whether or not a particular time is long enough for a given non-linear dynamic system. Besides, the influence of data inaccuracy and various numerical schemes on the critical predictable time is investigated in details by using symbolic computation software as a tool. A reliable chaotic solution of Lorenz equation in a rather large interval 0 <= t < 1200 non-dimensional Lorenz time units is obtained for the first time. It is found that the precision of the initial condition and the computed data at each time step, which is mathematically necessary to get such a reliable chaotic solution in such a long time, is so high that it is physically impossible due to the Heisenberg uncertainty principle in quantum physics. This, however, provides us a so-called `precision paradox of chaos', which suggests that the prediction uncertainty of chaos is physically unavoidable, and that even the macroscopical phenomena might be essentially stochastic and thus could be described by probability more economically.

Computing Generalized Matrix Inverse on Spiking Neural Substrate

PubMed Central

Shukla, Rohit; Khoram, Soroosh; Jorgensen, Erik; Li, Jing; Lipasti, Mikko; Wright, Stephen

2018-01-01

Emerging neural hardware substrates, such as IBM's TrueNorth Neurosynaptic System, can provide an appealing platform for deploying numerical algorithms. For example, a recurrent Hopfield neural network can be used to find the Moore-Penrose generalized inverse of a matrix, thus enabling a broad class of linear optimizations to be solved efficiently, at low energy cost. However, deploying numerical algorithms on hardware platforms that severely limit the range and precision of representation for numeric quantities can be quite challenging. This paper discusses these challenges and proposes a rigorous mathematical framework for reasoning about range and precision on such substrates. The paper derives techniques for normalizing inputs and properly quantizing synaptic weights originating from arbitrary systems of linear equations, so that solvers for those systems can be implemented in a provably correct manner on hardware-constrained neural substrates. The analytical model is empirically validated on the IBM TrueNorth platform, and results show that the guarantees provided by the framework for range and precision hold under experimental conditions. Experiments with optical flow demonstrate the energy benefits of deploying a reduced-precision and energy-efficient generalized matrix inverse engine on the IBM TrueNorth platform, reflecting 10× to 100× improvement over FPGA and ARM core baselines. PMID:29593483

27 CFR 30.25 - Use of precision specific gravity hydrometers.

Code of Federal Regulations, 2010 CFR

2010-04-01

... gravity hydrometers. 30.25 Section 30.25 Alcohol, Tobacco Products and Firearms ALCOHOL AND TOBACCO TAX... precision specific gravity hydrometers. The provisions of § 30.23 respecting the care, handling, and use of... specific gravity hydrometers. Specific gravity hydrometers shall be read to the nearest subdivision...

27 CFR 30.25 - Use of precision specific gravity hydrometers.

Code of Federal Regulations, 2012 CFR

2012-04-01

... gravity hydrometers. 30.25 Section 30.25 Alcohol, Tobacco Products and Firearms ALCOHOL AND TOBACCO TAX... precision specific gravity hydrometers. The provisions of § 30.23 respecting the care, handling, and use of... specific gravity hydrometers. Specific gravity hydrometers shall be read to the nearest subdivision...

27 CFR 30.25 - Use of precision specific gravity hydrometers.

Code of Federal Regulations, 2011 CFR

2011-04-01

... gravity hydrometers. 30.25 Section 30.25 Alcohol, Tobacco Products and Firearms ALCOHOL AND TOBACCO TAX... precision specific gravity hydrometers. The provisions of § 30.23 respecting the care, handling, and use of... specific gravity hydrometers. Specific gravity hydrometers shall be read to the nearest subdivision...

27 CFR 30.25 - Use of precision specific gravity hydrometers.

Code of Federal Regulations, 2013 CFR

2013-04-01

... gravity hydrometers. 30.25 Section 30.25 Alcohol, Tobacco Products and Firearms ALCOHOL AND TOBACCO TAX... precision specific gravity hydrometers. The provisions of § 30.23 respecting the care, handling, and use of... specific gravity hydrometers. Specific gravity hydrometers shall be read to the nearest subdivision...

27 CFR 30.25 - Use of precision specific gravity hydrometers.

Code of Federal Regulations, 2014 CFR

2014-04-01

... gravity hydrometers. 30.25 Section 30.25 Alcohol, Tobacco Products and Firearms ALCOHOL AND TOBACCO TAX... precision specific gravity hydrometers. The provisions of § 30.23 respecting the care, handling, and use of... specific gravity hydrometers. Specific gravity hydrometers shall be read to the nearest subdivision...

Manipulation of ultracold Rb atoms using a single linearly chirped laser pulse.

PubMed

Collins, T A; Malinovskaya, S A

2012-06-15

At ultracold temperatures, atoms are free from thermal motion, which makes them ideal objects of investigations aiming to advance high-precision spectroscopy, metrology, quantum computation, producing Bose condensates, etc. The quantum state of ultracold atoms may be created and manipulated by making use of quantum control methods employing low-intensity pulses. We theoretically investigate population dynamics of ultracold Rb vapor induced by nanosecond linearly chirped pulses having kW/cm2 beam intensity and show a possibility of controllable population transfer between hyperfine (HpF) levels of 5(2)/S(1/2) state through Raman transitions. Satisfying the one-photon resonance condition with the lowest of the HpF states of 5(2)/P(1/2) or 5(2)/P(3/2) state allows us to enter the adiabatic region of population transfer at very low field intensities, such that corresponding Rabi frequencies are less than or equal to the HpF splitting. This methodology provides a robust way to create a specifically designed superposition state in Rb in the basis of HpF levels and perform state manipulation controllable on the picosecond-to-nanosecond time scale.

Scattering matrix approach to the dissociative recombination of HCO{sup +} and N{sub 2}H{sup +}

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

Fonseca dos Santos, S.; Douguet, N.; Orel, A. E.

We present a theoretical study of the indirect dissociative recombination of linear polyatomic ions at low collisional energies. The approach is based on the computation of the scattering matrix just above the ionization threshold and enables the explicit determination of all diabatic electronic couplings responsible for dissociative recombination. In addition, we use the multi-channel quantum-defect theory to demonstrate the precision of the scattering matrix by reproducing accurately ab initio Rydberg state energies of the neutral molecule. We consider the molecular ions N{sub 2}H{sup +} and HCO{sup +} as benchmark systems of astrophysical interest and improve former theoretical studies, which hadmore » repeatedly produced smaller cross sections than experimentally measured. Specifically, we demonstrate the crucial role of the previously overlooked stretching modes for linear polyatomic ions with large permanent dipole moment. The theoretical cross sections for both ions agree well with experimental data over a wide energy range. Finally, we consider the potential role of the HOC{sup +} isomer in the experimental cross sections of HCO{sup +} at energies below 10 meV.« less

State preparation and detector effects in quantum measurements of rotation with circular polarization-entangled photons and photon counting

NASA Astrophysics Data System (ADS)

Cen, Longzhu; Zhang, Zijing; Zhang, Jiandong; Li, Shuo; Sun, Yifei; Yan, Linyu; Zhao, Yuan; Wang, Feng

2017-11-01

Circular polarization-entangled photons can be used to obtain an enhancement of the precision in a rotation measurement. In this paper, the method of entanglement transformation is used to produce NOON states in circular polarization from a readily generated linear polarization-entangled photon source. Detection of N -fold coincidences serves as the postselection and N -fold superoscillating fringes are obtained simultaneously. A parity strategy and conditional probabilistic statistics contribute to a better fringe, saturating the angle sensitivity to the Heisenberg limit. The impact of imperfect state preparation and detection is discussed both separately and jointly. For the separated case, the influence of each system imperfection is pronounced. For the joint case, the feasibility region for surpassing the standard quantum limit is given. Our work pushes the state preparation of circular polarization-entangled photons to the same level as that in the case of linear polarization. It is also confirmed that entanglement can be transformed into different frames for specific applications, serving as a useful scheme for using entangled sources.

Development and validation of an HPLC method to quantify camptothecin in polymeric nanocapsule suspensions.

PubMed

Granada, Andréa; Murakami, Fabio S; Sartori, Tatiane; Lemos-Senna, Elenara; Silva, Marcos A S

2008-01-01

A simple, rapid, and sensitive reversed-phase column high-performance liquid chromatographic method was developed and validated to quantify camptothecin (CPT) in polymeric nanocapsule suspensions. The chromatographic separation was performed on a Supelcosil LC-18 column (15 cm x 4.6 mm id, 5 microm) using a mobile phase consisting of methanol-10 mM KH2PO4 (60 + 40, v/v; pH 2.8) at a flow rate of 1.0 mL/min and ultraviolet detection at 254 nm. The calibration graph was linear from 0.5 to 3.0 microg/mL with a correlation coefficient of 0.9979, and the limit of quantitation was 0.35 microg/mL. The assay recovery ranged from 97.3 to 105.0%. The intraday and interday relative standard deviation values were < 5.0%. The validation results confirmed that the developed method is specific, linear, accurate, and precise for its intended use. The current method was successfully applied to the evaluation of CPT entrapment efficiency and drug content in polymeric nanocapsule suspensions during the early stage of formulation development.

Development and validation of a liquid chromatography-isotope dilution tandem mass spectrometry for determination of olanzapine in human plasma and its application to bioavailability study.

PubMed

Zhang, Meng-Qi; Jia, Jing-Ying; Lu, Chuan; Liu, Gang-Yi; Yu, Cheng-Yin; Gui, Yu-Zhou; Liu, Yun; Liu, Yan-Mei; Wang, Wei; Li, Shui-Jun; Yu, Chen

2010-06-01

A simple, reliable and sensitive liquid chromatography-isotope dilution mass spectrometry (LC-ID/MS) was developed and validated for quantification of olanzapine in human plasma. Plasma samples (50 microL) were extracted with tert-butyl methyl ether and isotope-labeled internal standard (olanzapine-D3) was used. The chromatographic separation was performed on XBridge Shield RP 18 (100 mm x 2.1 mm, 3.5 microm, Waters). An isocratic program was used at a flow rate of 0.4 m x min(-1) with mobile phase consisting of acetonitrile and ammonium buffer (pH 8). The protonated ions of analytes were detected in positive ionization by multiple reactions monitoring (MRM) mode. The plasma method, with a lower limit of quantification (LLOQ) of 0.1 ng x mL(-1), demonstrated good linearity over a range of 0.1 - 30 ng x mL(-1) of olanzapine. Specificity, linearity, accuracy, precision, recovery, matrix effect and stability were evaluated during method validation. The validated method was successfully applied to analyzing human plasma samples in bioavailability study.

Validation of a CD1b tetramer assay for studies of human mycobacterial infection or vaccination.

PubMed

Layton, Erik D; Yu, Krystle K Q; Smith, Malisa T; Scriba, Thomas J; De Rosa, Stephen C; Seshadri, Chetan

2018-07-01

CD1 tetramers loaded with lipid antigens facilitate the identification of rare lipid-antigen specific T cells present in human blood and tissue. Because CD1 proteins are structurally non-polymorphic, these tetramers can be applied to genetically diverse human populations, unlike MHC-I and MHC-II tetramers. However, there are no standardized assays to quantify and characterize lipid antigen-specific T cells present within clinical samples. We incorporated CD1b tetramers loaded with the mycobacterial lipid glucose monomycolate (GMM) into a multi-parameter flow cytometry assay. Using a GMM-specific T-cell line, we demonstrate that the assay is linear, reproducible, repeatable, precise, accurate, and has a limit of detection of approximately 0.007%. Having formally validated this assay, we performed a cross-sectional study of healthy U.S. controls and South African adolescents with and without latent tuberculosis infection (LTBI). We show that GMM-specific T cells are specifically detected in South African subjects with LTBI and not in U.S. healthy controls. This assay can be expanded to include additional tetramers or phenotypic markers to characterize GMM-specific T cells in studies of mycobacterial infection, disease, or vaccination. Copyright © 2018 Elsevier B.V. All rights reserved.

Multiplexed lateral flow biosensors: Technological advances for radically improving point-of-care diagnoses.

PubMed

Li, Jia; Macdonald, Joanne

2016-09-15

Lateral flow biosensors are a leading technology in point-of-care diagnostics due to their simplicity, rapidness and low cost. Their primacy in this arena continues through technological breakthroughs such as multiplexing: the detection of more than one biomarker in a single assay. Multiplexing capacity is critical for improving diagnostic efficiency, enhancing the diagnostic precision for specific diseases and reducing diagnostic cost. Here we review, for the first time, the various types and strategies employed for creating multiplexed lateral flow biosensors. These are classified into four main categories in terms of specific application or multiplexing level, namely linear, parameter, spatial and conceptual. We describe the practical applications and implications for each approach and compare their advantages and disadvantages. Importantly, multiplexing is still subject to limitations of the traditional lateral flow biosensor, such as sensitivity and specificity. However, by pushing the limitations of the traditional medium into the multiplex arena, several technological breakthroughs are emerging with novel solutions that further expand the utility of lateral flow biosensing for point-of-care applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Design and Analysis of a Compact Precision Positioning Platform Integrating Strain Gauges and the Piezoactuator

PubMed Central

Huang, Hu; Zhao, Hongwei; Yang, Zhaojun; Fan, Zunqiang; Wan, Shunguang; Shi, Chengli; Ma, Zhichao

2012-01-01

Miniaturization precision positioning platforms are needed for in situ nanomechanical test applications. This paper proposes a compact precision positioning platform integrating strain gauges and the piezoactuator. Effects of geometric parameters of two parallel plates on Von Mises stress distribution as well as static and dynamic characteristics of the platform were studied by the finite element method. Results of the calibration experiment indicate that the strain gauge sensor has good linearity and its sensitivity is about 0.0468 mV/μm. A closed-loop control system was established to solve the problem of nonlinearity of the platform. Experimental results demonstrate that for the displacement control process, both the displacement increasing portion and the decreasing portion have good linearity, verifying that the control system is available. The developed platform has a compact structure but can realize displacement measurement with the embedded strain gauges, which is useful for the closed-loop control and structure miniaturization of piezo devices. It has potential applications in nanoindentation and nanoscratch tests, especially in the field of in situ nanomechanical testing which requires compact structures. PMID:23012566

Design and implementation of a novel rotary micropositioning system driven by linear voice coil motor.

PubMed

Xu, Qingsong

2013-05-01

Limited-angle rotary micropositioning stages are required in precision engineering applications where an ultrahigh-precision rotational motion within a restricted range is needed. This paper presents the design, fabrication, and control of a compliant rotary micropositioning stage dedicated to the said applications. To tackle the challenge of achieving both a large rotational range and a compact size, a new idea of multi-stage compound radial flexure is proposed. A compact rotary stage is devised to deliver an over 10° rotational range while possessing a negligible magnitude of center shift. The stage is driven by a linear voice coil motor and its output motion is measured by laser displacement sensors. Analytical models are derived to facilitate the parametric design, which is validated by conducting finite element analysis. The actuation and sensing issues are addressed to guarantee the stage performance. A prototype is fabricated and a proportional-integral-derivative control is implemented to achieve a precise positioning. Experimental results demonstrate a resolution of 2 μrad over 10° rotational range as well as a low level of center shift of the rotary micropositioning system.

Bit Grooming: Statistically accurate precision-preserving quantization with compression, evaluated in the netCDF operators (NCO, v4.4.8+)

DOE PAGES

Zender, Charles S.

2016-09-19

Geoscientific models and measurements generate false precision (scientifically meaningless data bits) that wastes storage space. False precision can mislead (by implying noise is signal) and be scientifically pointless, especially for measurements. By contrast, lossy compression can be both economical (save space) and heuristic (clarify data limitations) without compromising the scientific integrity of data. Data quantization can thus be appropriate regardless of whether space limitations are a concern. We introduce, implement, and characterize a new lossy compression scheme suitable for IEEE floating-point data. Our new Bit Grooming algorithm alternately shaves (to zero) and sets (to one) the least significant bits ofmore » consecutive values to preserve a desired precision. This is a symmetric, two-sided variant of an algorithm sometimes called Bit Shaving that quantizes values solely by zeroing bits. Our variation eliminates the artificial low bias produced by always zeroing bits, and makes Bit Grooming more suitable for arrays and multi-dimensional fields whose mean statistics are important. Bit Grooming relies on standard lossless compression to achieve the actual reduction in storage space, so we tested Bit Grooming by applying the DEFLATE compression algorithm to bit-groomed and full-precision climate data stored in netCDF3, netCDF4, HDF4, and HDF5 formats. Bit Grooming reduces the storage space required by initially uncompressed and compressed climate data by 25–80 and 5–65 %, respectively, for single-precision values (the most common case for climate data) quantized to retain 1–5 decimal digits of precision. The potential reduction is greater for double-precision datasets. When used aggressively (i.e., preserving only 1–2 digits), Bit Grooming produces storage reductions comparable to other quantization techniques such as Linear Packing. Unlike Linear Packing, whose guaranteed precision rapidly degrades within the relatively narrow dynamic range of values that it can compress, Bit Grooming guarantees the specified precision throughout the full floating-point range. Data quantization by Bit Grooming is irreversible (i.e., lossy) yet transparent, meaning that no extra processing is required by data users/readers. Hence Bit Grooming can easily reduce data storage volume without sacrificing scientific precision or imposing extra burdens on users.« less

The Effect of Test and Examinee Characteristics on the Occurrence of Aberrant Response Patterns in a Computerized Adaptive Test

ERIC Educational Resources Information Center

Rizavi, Saba; Hariharan, Swaminathan

2001-01-01

The advantages that computer adaptive testing offers over linear tests have been well documented. The Computer Adaptive Test (CAT) design is more efficient than the Linear test design as fewer items are needed to estimate an examinee's proficiency to a desired level of precision. In the ideal situation, a CAT will result in examinees answering…

High Bandwidth Rotary Fast Tool Servos and a Hybrid Rotary/Linear Electromagnetic Actuator

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

Montesanti, Richard Clement

2005-09-01

This thesis describes the development of two high bandwidth short-stroke rotary fast tool servos and the hybrid rotary/linear electromagnetic actuator developed for one of them. Design insights, trade-o® methodologies, and analytical tools are developed for precision mechanical systems, power and signal electronic systems, control systems, normal-stress electromagnetic actuators, and the dynamics of the combined systems.

New Steering Strategies for the USNO Master Clocks

DTIC Science & Technology

1999-12-01

1992. P. Koppang and R. Leland , “Linear quadratic stochastic control of atomic hydrogen masers,” IEEE Trans. Ultrason., Ferroelect., Freq. Contr...vol. 46, pp. 517-522, May 1999. P. Koppang and R. Leland , “Steering of frequency standards by the use of linear quadratic gaussian control theory...3lst Annual Precise Time and Time Interval (PTTI) Meeting NEWSTEERINGSTRATEGIESFOR THEUSNOMASTERCLOCKS Paul A. Koppang Datum, Inc. Beverly, MA

Smartphone application for mechanical quality assurance of medical linear accelerators

NASA Astrophysics Data System (ADS)

Kim, Hwiyoung; Lee, Hyunseok; In Park, Jong; Choi, Chang Heon; Park, So-Yeon; Kim, Hee Jung; Kim, Young Suk; Ye, Sung-Joon

2017-06-01

Mechanical quality assurance (QA) of medical linear accelerators consists of time-consuming and human-error-prone procedures. We developed a smartphone application system for mechanical QA. The system consists of two smartphones: one attached to a gantry for obtaining real-time information on the mechanical parameters of the medical linear accelerator, and another displaying real-time information via a Bluetooth connection with the former. Motion sensors embedded in the smartphone were used to measure gantry and collimator rotations. Images taken by the smartphone’s high-resolution camera were processed to evaluate accuracies of jaw-positioning, crosshair centering and source-to-surface distance (SSD). The application was developed using Android software development kit and OpenCV library. The accuracy and precision of the system was validated against an optical rotation stage and digital calipers, prior to routine QA measurements of five medical linear accelerators. The system accuracy and precision in measuring angles and lengths were determined to be 0.05  ±  0.05° and 0.25  ±  0.14 mm, respectively. The mean absolute errors (MAEs) in QA measurements of gantry and collimator rotation were 0.05  ±  0.04° and 0.05  ±  0.04°, respectively. The MAE in QA measurements of light field was 0.39  ±  0.36 mm. The MAEs in QA measurements of crosshair centering and SSD were 0.40  ±  0.35 mm and 0.41  ±  0.32 mm, respectively. In conclusion, most routine mechanical QA procedures could be performed using the smartphone application system with improved precision and within a shorter time-frame, while eliminating potential human errors.

Smartphone application for mechanical quality assurance of medical linear accelerators.

PubMed

Kim, Hwiyoung; Lee, Hyunseok; Park, Jong In; Choi, Chang Heon; Park, So-Yeon; Kim, Hee Jung; Kim, Young Suk; Ye, Sung-Joon

2017-06-07

Mechanical quality assurance (QA) of medical linear accelerators consists of time-consuming and human-error-prone procedures. We developed a smartphone application system for mechanical QA. The system consists of two smartphones: one attached to a gantry for obtaining real-time information on the mechanical parameters of the medical linear accelerator, and another displaying real-time information via a Bluetooth connection with the former. Motion sensors embedded in the smartphone were used to measure gantry and collimator rotations. Images taken by the smartphone's high-resolution camera were processed to evaluate accuracies of jaw-positioning, crosshair centering and source-to-surface distance (SSD). The application was developed using Android software development kit and OpenCV library. The accuracy and precision of the system was validated against an optical rotation stage and digital calipers, prior to routine QA measurements of five medical linear accelerators. The system accuracy and precision in measuring angles and lengths were determined to be 0.05  ±  0.05° and 0.25  ±  0.14 mm, respectively. The mean absolute errors (MAEs) in QA measurements of gantry and collimator rotation were 0.05  ±  0.04° and 0.05  ±  0.04°, respectively. The MAE in QA measurements of light field was 0.39  ±  0.36 mm. The MAEs in QA measurements of crosshair centering and SSD were 0.40  ±  0.35 mm and 0.41  ±  0.32 mm, respectively. In conclusion, most routine mechanical QA procedures could be performed using the smartphone application system with improved precision and within a shorter time-frame, while eliminating potential human errors.

Linear FMCW Laser Radar for Precision Range and Vector Velocity Measurements

NASA Technical Reports Server (NTRS)

Pierrottet, Diego; Amzajerdian, Farzin; Petway, Larry; Barnes, Bruce; Lockhard, George; Rubio, Manuel

2008-01-01

An all fiber linear frequency modulated continuous wave (FMCW) coherent laser radar system is under development with a goal to aide NASA s new Space Exploration initiative for manned and robotic missions to the Moon and Mars. By employing a combination of optical heterodyne and linear frequency modulation techniques and utilizing state-of-the-art fiber optic technologies, highly efficient, compact and reliable laser radar suitable for operation in a space environment is being developed. Linear FMCW lidar has the capability of high-resolution range measurements, and when configured into a multi-channel receiver system it has the capability of obtaining high precision horizontal and vertical velocity measurements. Precision range and vector velocity data are beneficial to navigating planetary landing pods to the preselected site and achieving autonomous, safe soft-landing. The all-fiber coherent laser radar has several important advantages over more conventional pulsed laser altimeters or range finders. One of the advantages of the coherent laser radar is its ability to measure directly the platform velocity by extracting the Doppler shift generated from the motion, as opposed to time of flight range finders where terrain features such as hills, cliffs, or slopes add error to the velocity measurement. Doppler measurements are about two orders of magnitude more accurate than the velocity estimates obtained by pulsed laser altimeters. In addition, most of the components of the device are efficient and reliable commercial off-the-shelf fiber optic telecommunication components. This paper discusses the design and performance of a second-generation brassboard system under development at NASA Langley Research Center as part of the Autonomous Landing and Hazard Avoidance (ALHAT) project.

Precision-feeding dairy heifers a high rumen-degradable protein diet with different proportions of dietary fiber and forage-to-concentrate ratios.

PubMed

Lascano, G J; Koch, L E; Heinrichs, A J

2016-09-01

The objective of this experiment was to determine the effects of feeding a high-rumen-degradable protein (RDP) diet when dietary fiber content is manipulated within differing forage-to-concentrate ratio (F:C) on nutrient utilization of precision-fed dairy heifers. Six cannulated Holstein heifers (486.98±15.07kg of body weight) were randomly assigned to 2 F:C, low- (45% forage; LF) and high-forage (90% forage; HF) diets and to a fiber proportion sequence [33% grass hay and wheat straw (HS), 67% corn silage (CS; low fiber); 50% HS, 50% CS (medium fiber); and 67% HS, 33% CS (high fiber)] within forage proportion administered according to a split-plot, 3×3 Latin square design (16-d periods). Heifers fed LF had greater apparent total-tract organic matter digestibility coefficients (dC), neutral detergent fiber, and cellulose than those fed LC diets. Substituting CS with HS resulted in a linear reduction in dry matter, organic matter, and cellulose dC. Nitrogen dC was not different between F:C or with increasing proportions of HS in diets, but N retention tended to decrease linearly as HS was increased in the diets. Predicted microbial protein flow to the duodenum decreased linearly with HS addition and protozoa numbers HS interacted linearly, exhibiting a decrease as HS increased for LF, whereas no effects were observed for HF. Blood urea N increased linearly as HS was incorporated. The LF-fed heifers had a greater ruminal volatile fatty acids concentration. We noted a tendency for a greater dry matter, and a significantly higher liquid fraction turnover rate for HF diets. There was a linear numerical increase in the liquid and solid fraction turnover rate as fiber was added to the diets. Rumen fermentation parameters and fractional passages (solid and liquid) rates support the reduction in dC, N retention, and microbial protein synthesis observed as more dietary fiber is added to the rations of dairy heifers precision-fed a constant proportion of rumen-degradable protein. Copyright © 2016 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Manufacturing plastic injection optical molds

NASA Astrophysics Data System (ADS)

Bourque, David

2008-08-01

ABCO Tool & Die, Inc. is a mold manufacturer specializing in the manufacturing of plastic injection molds for molded optical parts. The purpose of this presentation is to explain the concepts and procedures required to build a mold that produces precision optical parts. Optical molds can produce a variety of molded parts ranging from safety eyewear to sophisticated military lens parts, which must meet precise optical specifications. The manufacturing of these molds begins with the design engineering of precision optical components. The mold design and the related optical inserts are determined based upon the specific optical criteria and optical surface geometry. The mold manufacturing techniques will be based upon the optical surface geometry requirements and specific details. Manufacturing processes used will be specific to prescribed geometrical surface requirements of the molded part. The combined efforts result in a robust optical mold which can produce molded parts that meet the most precise optical specifications.

Linear modeling of steady-state behavioral dynamics.

PubMed Central

Palya, William L; Walter, Donald; Kessel, Robert; Lucke, Robert

2002-01-01

The observed steady-state behavioral dynamics supported by unsignaled periods of reinforcement within repeating 2,000-s trials were modeled with a linear transfer function. These experiments employed improved schedule forms and analytical methods to improve the precision of the measured transfer function, compared to previous work. The refinements include both the use of multiple reinforcement periods that improve spectral coverage and averaging of independently determined transfer functions. A linear analysis was then used to predict behavior observed for three different test schedules. The fidelity of these predictions was determined. PMID:11831782

Impact of beam-beam effects on precision luminosity measurements at the ILC

NASA Astrophysics Data System (ADS)

Rimbault, C.; Bambade, P.; Mönig, K.; Schulte, D.

2007-09-01

In this paper, the impact of beam-beam effects on the precision luminosity measurement at the International Linear Collider is investigated quantitatively for the first time. GUINEA-PIG, a beam-beam interaction simulation tool, is adapted to treat the space charge effects affecting the Bhabha events used in this measurement. The biases due to the resulting changes in kinematics are evaluated for different center-of-mass energies and beam parameters.

Biotransformation of lignan glycoside to its aglycone by Woodfordia fruticosa flowers: quantification of compounds using a validated HPTLC method.

PubMed

Mishra, Shikha; Aeri, Vidhu

2017-12-01

Saraca asoca Linn. (Caesalpiniaceae) is an important traditional remedy for gynaecological disorders and it contains lyoniside, an aryl tetralin lignan glycoside. The aglycone of lyoniside, lyoniresinol possesses structural similarity to enterolignan precursors which are established phytoestrogens. This work illustrates biotransformation of lyoniside to lyoniresinol using Woodfordia fruticosa Kurz. (Lythraceae) flowers and simultaneous quantification of lyoniside and lyoniresinol using a validated HPTLC method. The aqueous extract prepared from S. asoca bark was fermented using W. fruticosa flowers. The substrate and fermented product both were simultaneously analyzed using solvent system:toluene:ethyl acetate:formic acid (4:3:0.4) at 254 nm. The method was validated for specificity, accuracy, precision, linearity, sensitivity and robustness as per ICH guidelines. The substrate showed the presence of lyoniside, however, it decreased as the fermentation proceeded. On 3rd day, lyoniresinol starts appearing in the medium. In 8 days duration most of the lyoniside converted to lyoniresinol. The developed method was specific for lyoniside and lyoniresinol. Lyoniside and lyoniresinol showed linearity in the range of 250-3000 and 500-2500 ng. The method was accurate as resulted in 99.84% and 99.83% recovery, respectively, for lyoniside and lyoniresinol. Aryl tetralin lignan glycoside, lyoniside was successfully transformed into lyoniresinol using W. fruticosa flowers and their contents were simultaneously analyzed using developed validated HPTLC method.

Validated method for determination of bromopride in human plasma by liquid chromatography--electrospray tandem mass spectrometry: application to the bioequivalence study.

PubMed

Nazare, P; Massaroti, P; Duarte, L F; Campos, D R; Marchioretto, M A M; Bernasconi, G; Calafatti, S; Barros, F A P; Meurer, E C; Pedrazzoli, J; Moraes, L A B

2005-09-01

A simple, sensitive and specific liquid chromatography-tandem mass spectrometry method for the quantification of bromopride I in human plasma is presented. Sample preparation consisted of the addition of procainamide II as the internal standard, liquid-liquid extraction in alkaline conditions using hexane-ethyl acetate (1 : 1, v/v) as the extracting solvent, followed by centrifugation, evaporation of the solvent and sample reconstitution in acetonitrile. Both I and II (internal standard, IS) were analyzed using a C18 column and the mobile-phase acetonitrile-water (formic acid 0.1%). The eluted compounds were monitored using electrospray tandem mass spectrometry. The analyses were carried out by multiple reaction monitoring (MRM) using the parent-to-daughter combinations of m/z 344.20 > 271.00 and m/z 236.30 > 163.10. The areas of peaks from analyte and IS were used for quantification of I. The achieved limit of quantification was 1.0 ng/ml and the assay exhibited a linear dynamic range of 1-100.0 ng/ml and gave a correlation coefficient (r) of 0.995 or better. Validation results on linearity, specificity, accuracy, precision and stability, as well as application to the analysis of samples taken up to 24 h after oral administration of 10 mg of I in healthy volunteers demonstrated the applicability to bioequivalence studies.

Measuring Solar Coronal Magnetism during the Total Solar Eclipse of 2017

NASA Astrophysics Data System (ADS)

Gibson, K. L.; Tomczyk, S.

2017-12-01

The total solar eclipse on August 21, 2017 provided a notable opportunity to measure the solar corona at specific emission wavelengths to gain information about coronal magnetic fields. Solar magnetic fields are intimately related to the generation of space weather and its effects on the earth, and the infrared imaging and polarization information collected on coronal emission lines here will enhance the scientific value of several other ongoing experiments, as well as benefit the astrophysics and upper atmosphere communities. Coronal measurements were collected during the 2 minute and 24 second totality period from Casper Mountain, WY. Computer-controlled telescopes automatically inserted four different narrow band pass filters to capture images in the visible range on a 4D PolCam, and in the infrared range on the FLIR 8501c camera. Each band pass filter selects a specific wavelength range that corresponds to a known coronal emission line possessing magnetic sensitivity. The 4D PolCam incorporated a novel grid of linear polarizers precisely aligned with the micron scale pixels. This allowed for direct measurement of the degree of linear polarization in a very small instrument with no external moving parts as is typically required. The FLIR offers short exposure times to freeze motion and output accurate thermal measurements. This allowed a new observation of the sun's corona using thermo infrared technology.

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

PubMed

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

2016-11-01

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

Analytical procedure for the determination of Ethyl Lauroyl Arginate (LAE) to assess the kinetics and specific migration from a new antimicrobial active food packaging.

PubMed

Pezo, Davinson; Navascués, Beatriz; Salafranca, Jesús; Nerín, Cristina

2012-10-01

Ethyl Lauroyl Arginate (LAE) is a cationic tensoactive compound, soluble in water, with a wide activity spectrum against moulds and bacteria. LAE has been incorporated as antimicrobial agent into packaging materials for food contact and these materials require to comply with the specific migration criteria. In this paper, one analytical procedure has been developed and optimized for the analysis of LAE in food simulants after the migrations tests. It consists of the formation of an ionic pair between LAE and the inorganic complex Co(SCN)(4)(2-) in aqueous solution, followed by a liquid-liquid extraction in a suitable organic solvent and further UV-Vis absorbance measurement. In order to evaluate possible interferences, the ionic pair has been also analyzed by high performance liquid chromatography with UV-Vis detection. Both procedures provided similar analytical characteristics, with linear ranges from 1.10 to 25.00 mg kg(-1), linearity higher than 0.9886, limits of detection and quantification of 0.33 and 1.10 mg kg(-1), respectively, accuracy better than 1% as relative error and precision better than 3.6% expressed as RSD. Optimization of analytical techniques, thermal and chemical stability of LAE, as well as migration kinetics of LAE from experimental active packaging are reported and discussed. Copyright © 2012 Elsevier B.V. All rights reserved.

Use of Linear Prediction Uncertainty Analysis to Guide Conditioning of Models Simulating Surface-Water/Groundwater Interactions

NASA Astrophysics Data System (ADS)

Hughes, J. D.; White, J.; Doherty, J.

2011-12-01

Linear prediction uncertainty analysis in a Bayesian framework was applied to guide the conditioning of an integrated surface water/groundwater model that will be used to predict the effects of groundwater withdrawals on surface-water and groundwater flows. Linear prediction uncertainty analysis is an effective approach for identifying (1) raw and processed data most effective for model conditioning prior to inversion, (2) specific observations and periods of time critically sensitive to specific predictions, and (3) additional observation data that would reduce model uncertainty relative to specific predictions. We present results for a two-dimensional groundwater model of a 2,186 km2 area of the Biscayne aquifer in south Florida implicitly coupled to a surface-water routing model of the actively managed canal system. The model domain includes 5 municipal well fields withdrawing more than 1 Mm3/day and 17 operable surface-water control structures that control freshwater releases from the Everglades and freshwater discharges to Biscayne Bay. More than 10 years of daily observation data from 35 groundwater wells and 24 surface water gages are available to condition model parameters. A dense parameterization was used to fully characterize the contribution of the inversion null space to predictive uncertainty and included bias-correction parameters. This approach allows better resolution of the boundary between the inversion null space and solution space. Bias-correction parameters (e.g., rainfall, potential evapotranspiration, and structure flow multipliers) absorb information that is present in structural noise that may otherwise contaminate the estimation of more physically-based model parameters. This allows greater precision in predictions that are entirely solution-space dependent, and reduces the propensity for bias in predictions that are not. Results show that application of this analysis is an effective means of identifying those surface-water and groundwater data, both raw and processed, that minimize predictive uncertainty, while simultaneously identifying the maximum solution-space dimensionality of the inverse problem supported by the data.

T-Slide Linear Actuators

NASA Technical Reports Server (NTRS)

Vranish, John

2009-01-01

T-slide linear actuators use gear bearing differential epicyclical transmissions (GBDETs) to directly drive a linear rack, which, in turn, performs the actuation. Conventional systems use a rotary power source in conjunction with a nut and screw to provide linear motion. Non-back-drive properties of GBDETs make the new actuator more direct and simpler. Versions of this approach will serve as a long-stroke, ultra-precision, position actuator for NASA science instruments, and as a rugged, linear actuator for NASA deployment duties. The T slide can operate effectively in the presence of side forces and torques. Versions of the actuator can perform ultra-precision positioning. A basic T-slide actuator is a long-stroke, rack-and-pinion linear actuator that, typically, consists of a T-slide, several idlers, a transmission to drive the slide (powered by an electric motor) and a housing that holds the entire assembly. The actuator is driven by gear action on its top surface, and is guided and constrained by gear-bearing idlers on its other two parallel surfaces. The geometry, implemented with gear-bearing technology, is particularly effective. An electronic motor operating through a GBDET can directly drive the T slide against large loads, as a rack and pinion linear actuator, with no break and no danger of back driving. The actuator drives the slide into position and stops. The slide holes position with power off and no brake, regardless of load. With the T slide configuration, this GBDET has an entire T-gear surface on which to operate. The GB idlers coupling the other two T slide parallel surfaces to their housing counterpart surfaces provide constraints in five degrees-of-freedom and rolling friction in the direction of actuation. Multiple GB idlers provide roller bearing strength sufficient to support efficient, rolling friction movement, even in the presence of large, resisting forces. T-slide actuators can be controlled using the combination of an off-the-shelf, electric servomotor, a motor angle resolution sensor (typically an encoder or resolver), and microprocessor-based intelligent software. In applications requiring precision positioning, it may be necessary to add strain gauges to the T-slide housing. Existing sensory- interactive motion control art will work for T slides. For open-loop positioning, a stepping motor emulation technique can be used.

Precision control of multiple quantum cascade lasers for calibration systems

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

Taubman, Matthew S., E-mail: Matthew.Taubman@pnnl.gov; Myers, Tanya L.; Pratt, Richard M.

We present a precision, 1-A, digitally interfaced current controller for quantum cascade lasers, with demonstrated temperature coefficients for continuous and 40-kHz full-depth square-wave modulated operation, of 1–2 ppm/ °C and 15 ppm/ °C, respectively. High precision digital to analog converters (DACs) together with an ultra-precision voltage reference produce highly stable, precision voltages, which are selected by a multiplexer (MUX) chip to set output currents via a linear current regulator. The controller is operated in conjunction with a power multiplexing unit, allowing one of three lasers to be driven by the controller, while ensuring protection of controller and all lasers during operation, standby,more » and switching. Simple ASCII commands sent over a USB connection to a microprocessor located in the current controller operate both the controller (via the DACs and MUX chip) and the power multiplexer.« less

Precision digital control systems

NASA Astrophysics Data System (ADS)

Vyskub, V. G.; Rozov, B. S.; Savelev, V. I.

This book is concerned with the characteristics of digital control systems of great accuracy. A classification of such systems is considered along with aspects of stabilization, programmable control applications, digital tracking systems and servomechanisms, and precision systems for the control of a scanning laser beam. Other topics explored are related to systems of proportional control, linear devices and methods for increasing precision, approaches for further decreasing the response time in the case of high-speed operation, possibilities for the implementation of a logical control law, and methods for the study of precision digital control systems. A description is presented of precision automatic control systems which make use of electronic computers, taking into account the existing possibilities for an employment of computers in automatic control systems, approaches and studies required for including a computer in such control systems, and an analysis of the structure of automatic control systems with computers. Attention is also given to functional blocks in the considered systems.

High precision locating control system based on VCM for Talbot lithography

NASA Astrophysics Data System (ADS)

Yao, Jingwei; Zhao, Lixin; Deng, Qian; Hu, Song

2016-10-01

Aiming at the high precision and efficiency requirements of Z-direction locating in Talbot lithography, a control system based on Voice Coil Motor (VCM) was designed. In this paper, we built a math model of VCM and its moving characteristic was analyzed. A double-closed loop control strategy including position loop and current loop were accomplished. The current loop was implemented by driver, in order to achieve the rapid follow of the system current. The position loop was completed by the digital signal processor (DSP) and the position feedback was achieved by high precision linear scales. Feed forward control and position feedback Proportion Integration Differentiation (PID) control were applied in order to compensate for dynamic lag and improve the response speed of the system. And the high precision and efficiency of the system were verified by simulation and experiments. The results demonstrated that the performance of Z-direction gantry was obviously improved, having high precision, quick responses, strong real-time and easily to expend for higher precision.

The development of a novel high-precision major depressive disorder screening system using transient autonomic responses induced by dual mental tasks.

PubMed

Matsui, Takemi; Shinba, Toshikazu; Sun, Guanghao

2018-02-01

12.6% of major depressive disorder (MDD) patients have suicide intent, while it has been reported that 43% of patients did not consult their doctors for MDD, automated MDD screening is eagerly anticipated. Recently, in order to achieve automated screening of MDD, biomarkers such as multiplex DNA methylation profiles or physiological method using near infra-red spectroscopy (NIRS) have been studied, however, they require inspection using 96-well DNA ELIZA kit after blood sampling or significant cost. Using a single-lead electrocardiography (ECG), we developed a high-precision MDD screening system using transient autonomic responses induced by dual mental tasks. We developed a novel high precision MDD screening system which is composed of a single-lead ECG monitor, analogue to digital (AD) converter and a personal computer with measurement and analysis program written by LabView programming language. The system discriminates MDD patients from normal subjects using heat rate variability (HRV)-derived transient autonomic responses induced by dual mental tasks, i.e. verbal fluency task and random number generation task, via linear discriminant analysis (LDA) adopting HRV-related predictor variables (hear rate (HR), high frequency (HF), low frequency (LF)/HF). The proposed system was tested for 12 MDD patients (32 ± 15 years) under antidepressant treatment from Shizuoka Saiseikai General Hospital outpatient unit and 30 normal volunteers (37 ± 17 years) from Tokyo Metropolitan University. The proposed system achieved 100% sensitivity and 100% specificity in classifying 42 examinees into 12 MDD patients and 30 normal subjects. The proposed system appears promising for future HRV-based high-precision and low-cost screening of MDDs using only single-lead ECG.

Evaluation of consumer monitors to measure particulate matter.

PubMed

Sousan, Sinan; Koehler, Kirsten; Hallett, Laura; Peters, Thomas M

2017-05-01

Recently, inexpensive (<$300) consumer aerosol monitors (CAMs) targeted for use in homes have become available. We evaluated the accuracy, bias, and precision of three CAMs (Foobot from Airoxlab, Speck from Carnegie Mellon University, and AirBeam from HabitatMap) for measuring mass concentrations in occupational settings. In a laboratory study, PM 2.5 measured with the CAMs and a medium-cost aerosol photometer (personal DataRAM 1500, Thermo Scientific) were compared to that from reference instruments for three aerosols (salt, welding fume, and Arizona road dust, ARD) at concentrations up to 8500 μg/m 3 . Three of each type of CAM were included to estimate precision. Compared to reference instruments, mass concentrations measured with the Foobot (r-value = 0.99) and medium-cost photometer (r-value = 0.99) show strong correlation, whereas those from the Speck (r-value range 0.88 - 0.99) and AirBeam (0.7 - 0.96) were less correlated. The Foobot bias was (-12%) for ARD and measurements were similar to the medium-cost instrument. Foobot bias was (< -46%) for salt and welding fume aerosols. Speck bias was at 18% salt for ARD and -86% for welding fume. AirBeam bias was (-36%) for salt and (-83%) for welding fume. All three photometers had a bias (< -82%) for welding fume. Precision was excellent for the Foobot (coefficient of variation range: 5% to 8%) and AirBeam (2% to 9%), but poorer for the Speck (8% to 25%). These findings suggest that the Foobot, with a linear response to different aerosol types and good precision, can provide reasonable estimates of PM 2.5 in the workplace after site-specific calibration to account for particle size and composition.

Development and validation of a stability-indicating LC method for the assay of lodenafil carbonate in tablets.

PubMed

Codevilla, Cristiane Franco; Lemos, Alice Machado; Delgado, Leila Schreiner; Rolim, Clarice Madalena Bueno; Adams, Andréa Inês Horn; Bergold, Ana Maria

2011-08-01

A stability-indicating liquid chromatographic method has been developed for the quantitative determination of lodenafil carbonate in tablets. The method employs a Synergi Fusion C18 column (250 × 4.6 mm, i.d., 4 μm particle size), with mobile phase consisting of a mixture of methanol-acetic acid 0.1% pH 4.0 (65:35, v/v) and UV detection at 290 nm, using a photodiode array detector. A linear response (r = 0.9999) was observed in the range of 10-80 μg/mL. The method showed good recoveries (average 100.3%) and also intra and inter-day precision (RSD < 2.0%). Validation parameters as specificity and robustness were also determined. Specificity analysis showed that no impurities or degradation products were co-eluting with the lodenafil carbonate peak. The method was found to be stability-indicating and due to its simplicity and accuracy can be applied for routine quality control analysis of lodenafil carbonate in tablets.

Novel Spectrofluorimetric Method for the Determination of Perindopril Erbumine Based on Fluorescence Quenching of Rhodamine B.

PubMed

Fael, Hanan; Sakur, Amir Al-Haj

2015-11-01

A novel, simple and specific spectrofluorimetric method was developed and validated for the determination of perindopril erbumine (PDE). The method is based on the fluorescence quenching of Rhodamine B upon adding perindopril erbumine. The quenched fluorescence was monitored at 578 nm after excitation at 500 nm. The optimization of the reaction conditions such as the solvent, reagent concentration, and reaction time were investigated. Under the optimum conditions, the fluorescence quenching was linear over a concentration range of 1.0-6.0 μg/mL. The proposed method was fully validated and successfully applied to the analysis of perindopril erbumine in pure form and tablets. Statistical comparison of the results obtained by the developed and reference methods revealed no significant differences between the methods compared in terms of accuracy and precision. The method was shown to be highly specific in the presence of indapamide, a diuretic that is commonly combined with perindopril erbumine. The mechanism of rhodamine B quenching was also discussed.

Simultaneous determination of five systemic azoles in plasma by high-performance liquid chromatography with ultraviolet detection.

PubMed

Gordien, Jean-Baptiste; Pigneux, Arnaud; Vigouroux, Stephane; Tabrizi, Reza; Accoceberry, Isabelle; Bernadou, Jean-Marc; Rouault, Audrey; Saux, Marie-Claude; Breilh, Dominique

2009-12-05

A simple, specific and automatable HPLC assay was developed for a simultaneous determination of systemic azoles (fluconazole, posaconazole, voriconazole, itraconazole and its metabolite hydroxyl-itraconazole, and ketoconazole) in plasma. The major advantage of this assay was sample preparation by a fully automatable solid phase extraction with Varian Plexa cartridges. C6-phenyl column was used for chromatographic separation, and UV detection was set at a wavelength of 260 nm. Linezolid was used as an internal standard. The assay was specific and linear over the concentration range of 0.05 to 40 microg/ml excepted for fluconazole which was between 0.05 and 100 microg/ml, and itraconazole between 0.1 and 40 microg/ml. Validation data for accuracy and precision for intra- and inter-day were good and satisfied FDA's guidance: CV between 0.24% and 11.66% and accuracy between 93.8% and 108.7% for all molecules. This assay was applied to therapeutic drug monitoring on patients hospitalized in intensive care and onco-hematologic units.

Quantitative imaging biomarkers: Effect of sample size and bias on confidence interval coverage.

PubMed

Obuchowski, Nancy A; Bullen, Jennifer

2017-01-01

Introduction Quantitative imaging biomarkers (QIBs) are being increasingly used in medical practice and clinical trials. An essential first step in the adoption of a quantitative imaging biomarker is the characterization of its technical performance, i.e. precision and bias, through one or more performance studies. Then, given the technical performance, a confidence interval for a new patient's true biomarker value can be constructed. Estimating bias and precision can be problematic because rarely are both estimated in the same study, precision studies are usually quite small, and bias cannot be measured when there is no reference standard. Methods A Monte Carlo simulation study was conducted to assess factors affecting nominal coverage of confidence intervals for a new patient's quantitative imaging biomarker measurement and for change in the quantitative imaging biomarker over time. Factors considered include sample size for estimating bias and precision, effect of fixed and non-proportional bias, clustered data, and absence of a reference standard. Results Technical performance studies of a quantitative imaging biomarker should include at least 35 test-retest subjects to estimate precision and 65 cases to estimate bias. Confidence intervals for a new patient's quantitative imaging biomarker measurement constructed under the no-bias assumption provide nominal coverage as long as the fixed bias is <12%. For confidence intervals of the true change over time, linearity must hold and the slope of the regression of the measurements vs. true values should be between 0.95 and 1.05. The regression slope can be assessed adequately as long as fixed multiples of the measurand can be generated. Even small non-proportional bias greatly reduces confidence interval coverage. Multiple lesions in the same subject can be treated as independent when estimating precision. Conclusion Technical performance studies of quantitative imaging biomarkers require moderate sample sizes in order to provide robust estimates of bias and precision for constructing confidence intervals for new patients. Assumptions of linearity and non-proportional bias should be assessed thoroughly.

Method validation for control determination of mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry.

PubMed

Torres, Daiane Placido; Martins-Teixeira, Maristela Braga; Cadore, Solange; Queiroz, Helena Müller

2015-01-01

A method for the determination of total mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry (TDA AAS) has been validated following international foodstuff protocols in order to fulfill the Brazilian National Residue Control Plan. The experimental parameters have been previously studied and optimized according to specific legislation on validation and inorganic contaminants in foodstuff. Linearity, sensitivity, specificity, detection and quantification limits, precision (repeatability and within-laboratory reproducibility), robustness as well as accuracy of the method have been evaluated. Linearity of response was satisfactory for the two range concentrations available on the TDA AAS equipment, between approximately 25.0 and 200.0 μg kg(-1) (square regression) and 250.0 and 2000.0 μg kg(-1) (linear regression) of mercury. The residues for both ranges were homoscedastic and independent, with normal distribution. Correlation coefficients obtained for these ranges were higher than 0.995. Limits of quantification (LOQ) and of detection of the method (LDM), based on signal standard deviation (SD) for a low-in-mercury sample, were 3.0 and 1.0 μg kg(-1), respectively. Repeatability of the method was better than 4%. Within-laboratory reproducibility achieved a relative SD better than 6%. Robustness of the current method was evaluated and pointed sample mass as a significant factor. Accuracy (assessed as the analyte recovery) was calculated on basis of the repeatability, and ranged from 89% to 99%. The obtained results showed the suitability of the present method for direct mercury measurement in fresh fish and shrimp samples and the importance of monitoring the analysis conditions for food control purposes. Additionally, the competence of this method was recognized by accreditation under the standard ISO/IEC 17025.

Accelerated Microstructure Imaging via Convex Optimization (AMICO) from diffusion MRI data.

PubMed

Daducci, Alessandro; Canales-Rodríguez, Erick J; Zhang, Hui; Dyrby, Tim B; Alexander, Daniel C; Thiran, Jean-Philippe

2015-01-15

Microstructure imaging from diffusion magnetic resonance (MR) data represents an invaluable tool to study non-invasively the morphology of tissues and to provide a biological insight into their microstructural organization. In recent years, a variety of biophysical models have been proposed to associate particular patterns observed in the measured signal with specific microstructural properties of the neuronal tissue, such as axon diameter and fiber density. Despite very appealing results showing that the estimated microstructure indices agree very well with histological examinations, existing techniques require computationally very expensive non-linear procedures to fit the models to the data which, in practice, demand the use of powerful computer clusters for large-scale applications. In this work, we present a general framework for Accelerated Microstructure Imaging via Convex Optimization (AMICO) and show how to re-formulate this class of techniques as convenient linear systems which, then, can be efficiently solved using very fast algorithms. We demonstrate this linearization of the fitting problem for two specific models, i.e. ActiveAx and NODDI, providing a very attractive alternative for parameter estimation in those techniques; however, the AMICO framework is general and flexible enough to work also for the wider space of microstructure imaging methods. Results demonstrate that AMICO represents an effective means to accelerate the fit of existing techniques drastically (up to four orders of magnitude faster) while preserving accuracy and precision in the estimated model parameters (correlation above 0.9). We believe that the availability of such ultrafast algorithms will help to accelerate the spread of microstructure imaging to larger cohorts of patients and to study a wider spectrum of neurological disorders. Copyright © 2014 The Authors. Published by Elsevier Inc. All rights reserved.

Intensity-Modulated Radiation Therapy (IMRT)

MedlinePlus

... specialized training in the field of radiation oncology physics, ensures the linear accelerator delivers the precise radiation ... critical normal structures, as well as the patient's health. Typically, patients are scheduled for IMRT sessions five ...

Multi-objective optimization in quantum parameter estimation

NASA Astrophysics Data System (ADS)

Gong, BeiLi; Cui, Wei

2018-04-01

We investigate quantum parameter estimation based on linear and Kerr-type nonlinear controls in an open quantum system, and consider the dissipation rate as an unknown parameter. We show that while the precision of parameter estimation is improved, it usually introduces a significant deformation to the system state. Moreover, we propose a multi-objective model to optimize the two conflicting objectives: (1) maximizing the Fisher information, improving the parameter estimation precision, and (2) minimizing the deformation of the system state, which maintains its fidelity. Finally, simulations of a simplified ɛ-constrained model demonstrate the feasibility of the Hamiltonian control in improving the precision of the quantum parameter estimation.

Lawrence Livermore National Laboratory ULTRA-350 Test Bed

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

Hopkins, D J; Wulff, T A; Carlisle, K

2001-04-10

LLNL has many in-house designed high precision machine tools. Some of these tools include the Large Optics Diamond Turning Machine (LODTM) [1], Diamond Turning Machine No.3 (DTM-3) and two Precision Engineering Research Lathes (PERL-1 and PERL-11). These machines have accuracy in the sub-micron range and in most cases position resolution in the couple of nanometers range. All of these machines are built with similar underlying technologies. The machines use capstan drive technology, laser interferometer position feedback, tachometer velocity feedback, permanent magnet (PM) brush motors and analog velocity and position loop servo compensation [2]. The machine controller does not perform anymore » servo compensation it simply computes the differences between the commanded position and the actual position (the following error) and sends this to a D/A for the analog servo position loop. LLNL is designing a new high precision diamond turning machine. The machine is called the ULTRA 350 [3]. In contrast to many of the proven technologies discussed above, the plan for the new machine is to use brushless linear motors, high precision linear scales, machine controller motor commutation and digital servo compensation for the velocity and position loops. Although none of these technologies are new and have been in use in industry, applications of these technologies to high precision diamond turning is limited. To minimize the risks of these technologies in the new machine design, LLNL has established a test bed to evaluate these technologies for application in high precision diamond turning. The test bed is primarily composed of commercially available components. This includes the slide with opposed hydrostatic bearings, the oil system, the brushless PM linear motor, the two-phase input three-phase output linear motor amplifier and the system controller. The linear scales are not yet commercially available but use a common electronic output format. As of this writing, the final verdict for the use of these technologies is still out but the first part of the work has been completed with promising results. The goal of this part of the work was to close a servo position loop around a slide incorporating these technologies and to measure the performance. This paper discusses the tests that were setup for system evaluation and the results of the measurements made. Some very promising results include; slide positioning to nanometer level and slow speed slide direction reversal at less than 100nm/min with no observed discontinuities. This is very important for machine contouring in diamond turning. As a point of reference, at 100 nm/min it would take the slide almost 7 years to complete the full designed travel of 350 mm. This speed has been demonstrated without the use of a velocity sensor. The velocity is derived from the position sensor. With what has been learned on the test bed, the paper finishes with a brief comparison of the old and new technologies. The emphasis of this comparison will be on the servo performance as illustrated with bode plot diagrams.« less

Lawrence Livermore National Laboratory ULTRA-350 Test Bed

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

Hopkins, D J; Wulff, T A; Carlisle, K

2001-04-10

LLNL has many in-house designed high precision machine tools. Some of these tools include the Large Optics Diamond Turning Machine (LODTM) [1], Diamond Turning Machine No.3 (DTM-3) and two Precision Engineering Research Lathes (PERL-I and PERL-II). These machines have accuracy in the sub-micron range and in most cases position resolution in the couple of nanometers range. All of these machines are built with similar underlying technologies. The machines use capstan drive technology, laser interferometer position feedback, tachometer velocity feedback, permanent magnet (PM) brush motors and analog velocity and position loop servo compensation [2]. The machine controller does not perform anymore » servo compensation it simply computes the differences between the commanded position and the actual position (the following error) and sends this to a D/A for the analog servo position loop. LLNL is designing a new high precision diamond turning machine. The machine is called the ULTRA 350 [3]. In contrast to many of the proven technologies discussed above, the plan for the new machine is to use brushless linear motors, high precision linear scales, machine controller motor commutation and digital servo compensation for the velocity and position loops. Although none of these technologies are new and have been in use in industry, applications of these technologies to high precision diamond turning is limited. To minimize the risks of these technologies in the new machine design, LLNL has established a test bed to evaluate these technologies for application in high precision diamond turning. The test bed is primarily composed of commercially available components. This includes the slide with opposed hydrostatic bearings, the oil system, the brushless PM linear motor, the two-phase input three-phase output linear motor amplifier and the system controller. The linear scales are not yet commercially available but use a common electronic output format. As of this writing, the final verdict for the use of these technologies is still out but the first part of the work has been completed with promising results. The goal of this part of the work was to close a servo position loop around a slide incorporating these technologies and to measure the performance. This paper discusses the tests that were setup for system evaluation and the results of the measurements made. Some very promising results include; slide positioning to nanometer level and slow speed slide direction reversal at less than 100nm/min with no observed discontinuities. This is very important for machine contouring in diamond turning. As a point of reference, at 100 nm/min it would take the slide almost 7 years to complete the full designed travel of 350 mm. This speed has been demonstrated without the use of a velocity sensor. The velocity is derived from the position sensor. With what has been learned on the test bed, the paper finishes with a brief comparison of the old and new technologies. The emphasis of this comparison will be on the servo performance as illustrated with bode plot diagrams.« 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.

Novel spectrophotometric determination of chloramphenicol and dexamethasone in the presence of non labeled interfering substances using univariate methods and multivariate regression model updating

NASA Astrophysics Data System (ADS)

Hegazy, Maha A.; Lotfy, Hayam M.; Rezk, Mamdouh R.; Omran, Yasmin Rostom

2015-04-01

Smart and novel spectrophotometric and chemometric methods have been developed and validated for the simultaneous determination of a binary mixture of chloramphenicol (CPL) and dexamethasone sodium phosphate (DSP) in presence of interfering substances without prior separation. The first method depends upon derivative subtraction coupled with constant multiplication. The second one is ratio difference method at optimum wavelengths which were selected after applying derivative transformation method via multiplying by a decoding spectrum in order to cancel the contribution of non labeled interfering substances. The third method relies on partial least squares with regression model updating. They are so simple that they do not require any preliminary separation steps. Accuracy, precision and linearity ranges of these methods were determined. Moreover, specificity was assessed by analyzing synthetic mixtures of both drugs. The proposed methods were successfully applied for analysis of both drugs in their pharmaceutical formulation. The obtained results have been statistically compared to that of an official spectrophotometric method to give a conclusion that there is no significant difference between the proposed methods and the official ones with respect to accuracy and precision.

Determination of ketamine and its main metabolites by liquid chromatography coupled to tandem mass spectrometry in pig plasma: Comparison of extraction methods.

PubMed

Ramiole, Cindy; D'Hayer, Benoit; Boudy, Vincent; Legagneux, Josette; Fonsart, Julien; Houzé, Pascal

2017-11-30

A rapid, sensitive and specific liquid chromatography coupled to tandem mass spectrometry method was developed for the simultaneous quantification pig plasma of ketamine and its two principal metabolites, norketamine and dehydronorketamine. Three extraction procoles were assessed including acetonitrile precipitation, Oase™ microplate extraction, and liquid-liquid extraction. Oase™ microplate extraction induced no significant matrix effect, important signal/noise ratio and good recoveries, ranging from 82 to 87% for the considered compounds. Using this extraction procedure, the assay was linear in the dynamic range 10-3000ng/mL (R 2 >0.99) regardless of the analytes. Intra- and inter-day accuracies were less than 12% for all compounds and intra- and inter-day precisions expressed as RSD were within <9.9%. Samples were stable in different storage conditions. High ketamine, norketamine and dehydronorketamine concentrations up to 15,000ng/mL can be determined with good precision using appropriate sample dilution. The assay was successfully applied to pig plasma samples to determine the pharmacokinetics of ketamine and the consecutive metabolites after buccal administration of a 4mg/kg ketamine base solutions. Copyright © 2017 Elsevier B.V. All rights reserved.

Optima XE Single Wafer High Energy Ion Implanter

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

Satoh, Shu; Ferrara, Joseph; Bell, Edward

2008-11-03

The Optima XE is the first production worthy single wafer high energy implanter. The new system combines a state-of-art single wafer endstation capable of throughputs in excess of 400 wafers/hour with a production-proven RF linear accelerator technology. Axcelis has been evolving and refining RF Linac technology since the introduction of the NV1000 in 1986. The Optima XE provides production worthy beam currents up to energies of 1.2 MeV for P{sup +}, 2.9 MeV for P{sup ++}, and 1.5 MeV for B{sup +}. Energies as low as 10 keV and tilt angles as high as 45 degrees are also available., allowingmore » the implanter to be used for a wide variety of traditional medium current implants to ensure high equipment utilization. The single wafer endstation provides precise implant angle control across wafer and wafer to wafer. In addition, Optima XE's unique dose control system allows compensation of photoresist outgassing effects without relying on traditional pressure-based methods. We describe the specific features, angle control and dosimetry of the Optima XE and their applications in addressing the ever-tightening demands for more precise process controls and higher productivity.« less

Quantitative determination and validation of octreotide acetate using 1 H-NMR spectroscopy with internal standard method.

PubMed

Yu, Chen; Zhang, Qian; Xu, Peng-Yao; Bai, Yin; Shen, Wen-Bin; Di, Bin; Su, Meng-Xiang

2018-01-01

Quantitative nuclear magnetic resonance (qNMR) is a well-established technique in quantitative analysis. We presented a validated 1 H-qNMR method for assay of octreotide acetate, a kind of cyclic octopeptide. Deuterium oxide was used to remove the undesired exchangeable peaks, which was referred to as proton exchange, in order to make the quantitative signals isolated in the crowded spectrum of the peptide and ensure precise quantitative analysis. Gemcitabine hydrochloride was chosen as the suitable internal standard. Experimental conditions, including relaxation delay time, the numbers of scans, and pulse angle, were optimized first. Then method validation was carried out in terms of selectivity, stability, linearity, precision, and robustness. The assay result was compared with that by means of high performance liquid chromatography, which is provided by Chinese Pharmacopoeia. The statistical F test, Student's t test, and nonparametric test at 95% confidence level indicate that there was no significant difference between these two methods. qNMR is a simple and accurate quantitative tool with no need for specific corresponding reference standards. It has the potential of the quantitative analysis of other peptide drugs and standardization of the corresponding reference standards. Copyright © 2017 John Wiley & Sons, Ltd.

Determination of residual cell culture media components by MEKC.

PubMed

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

2009-11-01

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

A validated HPLC determination of the flavone aglycone diosmetin in human plasma.

PubMed

Kanaze, Feras Imad; Bounartzi, Melpomeni I; Niopas, Ioannis

2004-12-01

Diosmetin, 3',5,7-trihydroxy-4'-methoxy flavone, is the aglycone of the flavonoid glycoside diosmin that occurs naturally in foods of plant origin. Diosmin exhibits antioxidant and anti-inflammatory activities, improves venous tone and it is used for the treatment of chronic venous insufficiency. Diosmin is hydrolyzed by enzymes of intestinal micro flora before absorption of its aglycone diosmetin. A specific, sensitive, precise, accurate and robust HPLC assay for the determination of diosmetin in human plasma was developed and validated. Diosmetin and the internal standard 7-ethoxycoumarin were isolated from plasma by liquid-liquid extraction and separated on a C8 reversed-phase column with methanol-water-acetic acid (55:43:2, v/v/v) as the mobile phase at 43 degrees C. Peaks were monitored at 344 nm. The method was linear in the 10-300 ng/mL concentration range (r > 0.999). Recovery for diosmetin and internal standard was greater than 89.7 and 86.8%, respectively. Intra-day and inter-day precision for diosmetin ranged from 1.6 to 4.6 and from 2.2 to 5.3%, respectively, and accuracy was better than 97.9%. Copyright 2004 John Wiley & Sons, Ltd.

Validation of four different spectrophotometric methods for simultaneous determination of Domperidone and Ranitidine in bulk and pharmaceutical formulation.

PubMed

Abdel-Ghany, Maha F; Abdel-Aziz, Omar; Mohammed, Yomna Y

2015-01-01

Four simple, specific, accurate and precise spectrophotometric methods were developed and validated for simultaneous determination of Domperidone (DP) and Ranitidine Hydrochloride (RT) in bulk powder and pharmaceutical formulation. The first method was simultaneous ratio subtraction (SRS), the second was ratio subtraction (RS) coupled with zero order spectrophotometry (D(0)), the third was first derivative of the ratio spectra ((1)DD) and the fourth method was mean centering of ratio spectra (MCR). The calibration curve is linear over the concentration range of 0.5-5 and 1-45 μg mL(-1) for DP and RT, respectively. The proposed spectrophotometric methods can analyze both drugs without any prior separation steps. The selectivity of the adopted methods was tested by analyzing synthetic mixtures of the investigated drugs, also in their pharmaceutical formulation. The suggested methods were validated according to International Conference of Harmonization (ICH) guidelines and the results revealed that; they were precise and reproducible. All the obtained results were statistically compared with those of the reported method, where there was no significant difference. Copyright © 2015 Elsevier B.V. All rights reserved.

Quantitative analysis of pork and chicken products by droplet digital PCR.

PubMed

Cai, Yicun; Li, Xiang; Lv, Rong; Yang, Jielin; Li, Jian; He, Yuping; Pan, Liangwen

2014-01-01

In this project, a highly precise quantitative method based on the digital polymerase chain reaction (dPCR) technique was developed to determine the weight of pork and chicken in meat products. Real-time quantitative polymerase chain reaction (qPCR) is currently used for quantitative molecular analysis of the presence of species-specific DNAs in meat products. However, it is limited in amplification efficiency and relies on standard curves based Ct values, detecting and quantifying low copy number target DNA, as in some complex mixture meat products. By using the dPCR method, we find the relationships between the raw meat weight and DNA weight and between the DNA weight and DNA copy number were both close to linear. This enabled us to establish formulae to calculate the raw meat weight based on the DNA copy number. The accuracy and applicability of this method were tested and verified using samples of pork and chicken powder mixed in known proportions. Quantitative analysis indicated that dPCR is highly precise in quantifying pork and chicken in meat products and therefore has the potential to be used in routine analysis by government regulators and quality control departments of commercial food and feed enterprises.

Determination of Bosentan in Pharmaceutical Preparations by Linear Sweep, Square Wave and Differential Pulse Voltammetry Methods

PubMed Central

Atila, Alptug; Yilmaz, Bilal

2015-01-01

In this study, simple, fast and reliable cyclic voltammetry (CV), linear sweep voltammetry (LSV), square wave voltammetry (SWV) and differential pulse voltammetry (DPV) methods were developed and validated for determination of bosentan in pharmaceutical preparations. The proposed methods were based on electrochemical oxidation of bosentan at platinum electrode in acetonitrile solution containing 0.1 M TBACIO4. The well-defined oxidation peak was observed at 1.21 V. The calibration curves were linear for bosentan at the concentration range of 5-40 µg/mL for LSV and 5-35 µg/mL for SWV and DPV methods, respectively. Intra- and inter-day precision values for bosentan were less than 4.92, and accuracy (relative error) was better than 6.29%. The mean recovery of bosentan was 100.7% for pharmaceutical preparations. No interference was found from two tablet excipients at the selected assay conditions. Developed methods in this study are accurate, precise and can be easily applied to Tracleer and Diamond tablets as pharmaceutical preparation. PMID:25901151

Development and Validation of High Performance Liquid Chromatography Method for Determination Atorvastatin in Tablet

NASA Astrophysics Data System (ADS)

Yugatama, A.; Rohmani, S.; Dewangga, A.

2018-03-01

Atorvastatin is the primary choice for dyslipidemia treatment. Due to patent expiration of atorvastatin, the pharmaceutical industry makes copy of the drug. Therefore, the development methods for tablet quality tests involving atorvastatin concentration on tablets needs to be performed. The purpose of this research was to develop and validate the simple atorvastatin tablet analytical method by HPLC. HPLC system used in this experiment consisted of column Cosmosil C18 (150 x 4,6 mm, 5 µm) as the stationary reverse phase chomatography, a mixture of methanol-water at pH 3 (80:20 v/v) as the mobile phase, flow rate of 1 mL/min, and UV detector at wavelength of 245 nm. Validation methods were including: selectivity, linearity, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ). The results of this study indicate that the developed method had good validation including selectivity, linearity, accuracy, precision, LOD, and LOQ for analysis of atorvastatin tablet content. LOD and LOQ were 0.2 and 0.7 ng/mL, and the linearity range were 20 - 120 ng/mL.

Determination of bosentan in pharmaceutical preparations by linear sweep, square wave and differential pulse voltammetry methods.

PubMed

Atila, Alptug; Yilmaz, Bilal

2015-01-01

In this study, simple, fast and reliable cyclic voltammetry (CV), linear sweep voltammetry (LSV), square wave voltammetry (SWV) and differential pulse voltammetry (DPV) methods were developed and validated for determination of bosentan in pharmaceutical preparations. The proposed methods were based on electrochemical oxidation of bosentan at platinum electrode in acetonitrile solution containing 0.1 M TBACIO4. The well-defined oxidation peak was observed at 1.21 V. The calibration curves were linear for bosentan at the concentration range of 5-40 µg/mL for LSV and 5-35 µg/mL for SWV and DPV methods, respectively. Intra- and inter-day precision values for bosentan were less than 4.92, and accuracy (relative error) was better than 6.29%. The mean recovery of bosentan was 100.7% for pharmaceutical preparations. No interference was found from two tablet excipients at the selected assay conditions. Developed methods in this study are accurate, precise and can be easily applied to Tracleer and Diamond tablets as pharmaceutical preparation.

Issues in the digital implementation of control compensators. Ph.D. Thesis

NASA Technical Reports Server (NTRS)

Moroney, P.

1979-01-01

Techniques developed for the finite-precision implementation of digital filters were used, adapted, and extended for digital feedback compensators, with particular emphasis on steady state, linear-quadratic-Gaussian compensators. Topics covered include: (1) the linear-quadratic-Gaussian problem; (2) compensator structures; (3) architectural issues: serialism, parallelism, and pipelining; (4) finite wordlength effects: quantization noise, quantizing the coefficients, and limit cycles; and (5) the optimization of structures.

Arbitrary nonlinearity is sufficient to represent all functions by neural networks - A theorem

NASA Technical Reports Server (NTRS)

Kreinovich, Vladik YA.

1991-01-01

It is proved that if we have neurons implementing arbitrary linear functions and a neuron implementing one (arbitrary but smooth) nonlinear function g(x), then for every continuous function f(x sub 1,..., x sub m) of arbitrarily many variables, and for arbitrary e above 0, we can construct a network that consists of g-neurons and linear neurons, and computes f with precision e.

Propagating synchrony in feed-forward networks

PubMed Central

Jahnke, Sven; Memmesheimer, Raoul-Martin; Timme, Marc

2013-01-01

Coordinated patterns of precisely timed action potentials (spikes) emerge in a variety of neural circuits but their dynamical origin is still not well understood. One hypothesis states that synchronous activity propagating through feed-forward chains of groups of neurons (synfire chains) may dynamically generate such spike patterns. Additionally, synfire chains offer the possibility to enable reliable signal transmission. So far, mostly densely connected chains, often with all-to-all connectivity between groups, have been theoretically and computationally studied. Yet, such prominent feed-forward structures have not been observed experimentally. Here we analytically and numerically investigate under which conditions diluted feed-forward chains may exhibit synchrony propagation. In addition to conventional linear input summation, we study the impact of non-linear, non-additive summation accounting for the effect of fast dendritic spikes. The non-linearities promote synchronous inputs to generate precisely timed spikes. We identify how non-additive coupling relaxes the conditions on connectivity such that it enables synchrony propagation at connectivities substantially lower than required for linearly coupled chains. Although the analytical treatment is based on a simple leaky integrate-and-fire neuron model, we show how to generalize our methods to biologically more detailed neuron models and verify our results by numerical simulations with, e.g., Hodgkin Huxley type neurons. PMID:24298251

Using High-Precision Specific Gravity Measurements to Study Minerals in Undergraduate Geoscience Courses

ERIC Educational Resources Information Center

Brandriss, Mark E.

2010-01-01

This article describes ways to incorporate high-precision measurements of the specific gravities of minerals into undergraduate courses in mineralogy and physical geology. Most traditional undergraduate laboratory methods of measuring specific gravity are suitable only for unusually large samples, which severely limits their usefulness for student…

The Lumipulse G HBsAg-Quant assay for screening and quantification of the hepatitis B surface antigen.

PubMed

Yang, Ruifeng; Song, Guangjun; Guan, Wenli; Wang, Qian; Liu, Yan; Wei, Lai

2016-02-01

Qualitative HBsAg assay is used to screen HBV infection for decades. The utility of quantitative assay is also rejuvenated recently. We aimed to evaluate and compare the performance of a novel ultra-sensitive and quantitative assay, the Lumipulse assay, with the Architect and Elecsys assays. As screening methods, specificity was compared using 2043 consecutive clinical routine samples. As quantitative assays, precision and accuracy were assessed. Sera from 112 treatment-naïve chronic hepatitis B patients, four patients undergoing antiviral therapy and one patient with acute infection were tested to compare the correlations. Samples with concurrent HBsAg/anti-HBs were also quantified. The Lumipulse assay precisely quantified ultra-low level of HBsAg (0.004 IU/mL). It identified additional 0.98% (20/2043) clinical samples with trance amount of HBsAg. Three assays displayed excellent linear correlations irrespective of genotypes and S-gene mutations (R(2)>0.95, P<0.0001), while minor quantitative biases existed. The Lumipulse assay did not yield higher HBsAg concentrations in samples with concomitant anti-HBs. Compared with other assays, the Lumipulse assay is sensitive and specific for detecting HBsAg. The interpretation of the extremely low-level results, however, is challenging. Quantitative HBsAg results by different assays are highly correlated, but they should be interpreted interchangeably only after conversion to eliminate the biases. Copyright © 2015 Elsevier B.V. All rights reserved.

3D printing PLGA: a quantitative examination of the effects of polymer composition and printing parameters on print resolution

PubMed Central

Guo, Ting; Holzberg, Timothy R; Lim, Casey G; Gao, Feng; Gargava, Ankit; Trachtenberg, Jordan E; Mikos, Antonios G; Fisher, John P

2018-01-01

In the past few decades, 3D printing has played a significant role in fabricating scaffolds with consistent, complex structure that meet patient-specific needs in future clinical applications. Although many studies have contributed to this emerging field of additive manufacturing, which includes material development and computer-aided scaffold design, current quantitative analyses do not correlate material properties, printing parameters, and printing outcomes to a great extent. A model that correlates these properties has tremendous potential to standardize 3D printing for tissue engineering and biomaterial science. In this study, we printed poly(lactic-co-glycolic acid) (PLGA) utilizing a direct melt extrusion technique without additional ingredients. We investigated PLGA with various lactic acid: glycolic acid (LA:GA) molecular weight ratios and end caps to demonstrate the dependence of the extrusion process on the polymer composition. Micro-computed tomography was then used to evaluate printed scaffolds containing different LA:GA ratios, composed of different fiber patterns, and processed under different printing conditions. We built a statistical model to reveal the correlation and predominant factors that determine printing precision. Our model showed a strong linear relationship between the actual and predicted precision under different combinations of printing conditions and material compositions. This quantitative examination establishes a significant foreground to 3D print biomaterials following a systematic fabrication procedure. Additionally, our proposed statistical models can be applied to couple specific biomaterials and 3D printing applications for patient implants with particular requirements. PMID:28244880

3D printing PLGA: a quantitative examination of the effects of polymer composition and printing parameters on print resolution.

PubMed

Guo, Ting; Holzberg, Timothy R; Lim, Casey G; Gao, Feng; Gargava, Ankit; Trachtenberg, Jordan E; Mikos, Antonios G; Fisher, John P

2017-04-12

In the past few decades, 3D printing has played a significant role in fabricating scaffolds with consistent, complex structure that meet patient-specific needs in future clinical applications. Although many studies have contributed to this emerging field of additive manufacturing, which includes material development and computer-aided scaffold design, current quantitative analyses do not correlate material properties, printing parameters, and printing outcomes to a great extent. A model that correlates these properties has tremendous potential to standardize 3D printing for tissue engineering and biomaterial science. In this study, we printed poly(lactic-co-glycolic acid) (PLGA) utilizing a direct melt extrusion technique without additional ingredients. We investigated PLGA with various lactic acid:glycolic acid (LA:GA) molecular weight ratios and end caps to demonstrate the dependence of the extrusion process on the polymer composition. Micro-computed tomography was then used to evaluate printed scaffolds containing different LA:GA ratios, composed of different fiber patterns, and processed under different printing conditions. We built a statistical model to reveal the correlation and predominant factors that determine printing precision. Our model showed a strong linear relationship between the actual and predicted precision under different combinations of printing conditions and material compositions. This quantitative examination establishes a significant foreground to 3D print biomaterials following a systematic fabrication procedure. Additionally, our proposed statistical models can be applied to couple specific biomaterials and 3D printing applications for patient implants with particular requirements.

Analysis of anabolic steroids in human hair using LC-MS/MS.

PubMed

Deshmukh, Nawed; Hussain, Iltaf; Barker, James; Petroczi, Andrea; Naughton, Declan P

2010-10-01

New highly sensitive, specific, reliable, reproducible and robust LC-MS/MS methods were developed to detect the anabolic steroids, nandrolone and stanozolol, in human hair for the first time. Hair samples from 180 participants (108 males, 72 females, 62% athletes) were screened using ELISA which revealed 16 athletes as positive for stanozolol and 3 for nandrolone. Positive samples were confirmed on LC-MS/MS in selective reaction monitoring (SRM) mode. The assays for stanozolol and nandrolone showed good linearity in the range 1-400pg/mg and 5-400pg/mg, respectively. The methods were validated for LLOD, interday precision, intraday precision, specificity, extraction recovery and accuracy. The assays were capable of detecting 0.5pg stanozolol and 3.0pg nandrolone per mg of hair, when approximately 20mg of hair were processed. Analysis using LC-MS/MS confirmed 11 athletes' positive for stanozolol (5.0pg/mg to 86.3pg/mg) and 1 for nandrolone (14.0pg/mg) thus avoiding false results from ELISA screening. The results obtained demonstrate the application of these hair analysis methods to detect both steroids at low concentrations, hence reducing the amount of hair required significantly. The new methods complement urinalysis or blood testing and facilitate improved doping testing regimes. Hair analysis benefits from non-invasiveness, negligible risk of infection and facile sample storage and collection, whilst reducing risks of tampering and cross-contamination. Owing to the wide detection window, this approach may also offer an alternative approach for out-of-competition testing.

Determination of 25-OH-PPD in rat plasma by high-performance liquid chromatography-mass spectrometry and its application in rat pharmacokinetic studies.

PubMed

Zhang, Xiangrong; Zhang, Dan; Xu, Jinghua; Gu, Jingkai; Zhao, Yuqing

2007-10-15

A sensitive and specific liquid chromatography/tandem mass spectrometry (LC/MS/MS) method was developed for the investigation of the pharmacokinetics of 20(R)-dammarane-3beta,12beta,20,25-tetrol (25-OH-PPD) in rat. Ginsenoside Rh(2) was employed as an internal standard. The plasma samples were pretreated by liquid-liquid extraction and analyzed using LC/MS/MS with an electrospray ionization interface. The mobile phase consisted of methanol-acetonitrile-10 mmol/l aqueous ammonium acetate (42.5:42.5:15, v:v:v), which was pumped at 0.4 ml/min. The analytical column (50 mm x 2.1 mm i.d.) was packed with Venusil XBP C8 material (3.5 microm). The standard curve was linear from 10 to 3000 ng/ml. The assay was specific, accurate (accuracy between -1.19 and 2.57% for all quality control samples), precise and reproducible (within- and between-day precisions measured as relative standard deviation were <5% and <7%, respectively). 25-OH-PPD in rat plasma was stable over three freeze-thaw cycles and at ambient temperatures for 6h. The method had a lower limit of quantitation of 10 ng/ml, which offered a satisfactory sensitivity for the determination of (25-OH-PPD) in plasma. This quantitation method was successfully applied to pharmacokinetic studies of 25-OH-PPD after both an oral and an intravenous administration to rats and the absolute bioavailability is 64.8+/-14.3%.

Determination of some phenolic compounds in red wine by RP-HPLC: method development and validation.

PubMed

Burin, Vívian Maria; Arcari, Stefany Grützmann; Costa, Léa Luzia Freitas; Bordignon-Luiz, Marilde T

2011-09-01

A methodology employing reversed-phase high-performance liquid chromatography (RP-HPLC) was developed and validated for simultaneous determination of five phenolic compounds in red wine. The chromatographic separation was carried out in a C(18) column with water acidify with acetic acid (pH 2.6) (solvent A) and 20% solvent A and 80% acetonitrile (solvent B) as the mobile phase. The validation parameters included: selectivity, linearity, range, limits of detection and quantitation, precision and accuracy, using an internal standard. All calibration curves were linear (R(2) > 0.999) within the range, and good precision (RSD < 2.6%) and recovery (80-120%) was obtained for all compounds. This method was applied to quantify phenolics in red wine samples from Santa Catarina State, Brazil, and good separation peaks for phenolic compounds in these wines were observed.

HPTLC Determination of Artemisinin and Its Derivatives in Bulk and Pharmaceutical Dosage

NASA Astrophysics Data System (ADS)

Agarwal, Suraj P.; Ahuja, Shipra

A simple, selective, accurate, and precise high-performance thin-layer chromatographic (HPTLC) method has been established and validated for the analysis of artemisinin and its derivatives (artesunate, artemether, and arteether) in the bulk drugs and formulations. The artemisinin, artesunate, artemether, and arteether were separated on aluminum-backed silica gel 60 F254 plates with toluene:ethyl acetate (10:1), toluene: ethyl acetate: acetic acid (2:8:0.2), toluene:butanol (10:1), and toluene:dichloro methane (0.5:10) mobile phase, respectively. The linear detector response for concentrations between 100 and 600 ng/spot showed good linear relationship with r value 0.9967, 0.9989, 0.9981 and 0.9989 for artemisinin, artesunate, artemether, and arteether, respectively. Statistical analysis proves that the method is precise, accurate, and reproducible and hence can be employed for the routine analysis.

Performance characteristics of two bioassays and high-performance liquid chromatography for determination of flucytosine in serum.

PubMed Central

St-Germain, G; Lapierre, S; Tessier, D

1989-01-01

We compared the accuracy and precision of two microbiological methods and one high-pressure liquid chromatography (HPLC) procedure used to measure the concentrations of flucytosine in serum. On the basis of an analysis of six standards, all methods were judged reliable within acceptable limits for clinical use. With the biological methods, a slight loss of linearity was observed in the 75- to 100-micrograms/ml range. Compared with the bioassays, the HPLC method did not present linearity problems and was more precise and accurate in the critical zone of 100 micrograms/ml. On average, results obtained with patient sera containing 50 to 100 micrograms of flucytosine per ml were 10.6% higher with the HPLC method than with the bioassays. Standards for the biological assays may be prepared in serum or water. PMID:2802566

[Simultaneous determination of five active constitutents in Xiaochaihu Tang by HPLC].

PubMed

Liu, Qingchun; Zhao, Junning; Yan, Liangchun; Yi, Jinhai; Song, Jun

2010-03-01

To establish a HPLC-PDA method for the determination of baicalin, wogonoside, baicalein, wogonin and glycyrrhizic acid in Xiaochaihu Tang. A Symmetry Shield RP18 (4.6 mm x 250 mm, 5.0 microm) was used with a mobile phase of acetonitrile-0.01% H3PO4 in gradient elution. The detection wavelength was 251 nm,the flow rate was 0.45 mL x min(-1) and the column temperature was maintained at 30 degrees C. The accuracy, precision, sensitivity, specificity and linearity of this method met the requirements. The contents of the five effective fractions were determined simultaneously. The method is rapid,simple and accurate and it can be suitable for the determination of baicalin, wogonoside, baicalein, wogonin and glycyrrhizic acid in Xiaochaihu Tang simultaneously.

Representations of time coordinates in FITS. Time and relative dimension in space

NASA Astrophysics Data System (ADS)

Rots, Arnold H.; Bunclark, Peter S.; Calabretta, Mark R.; Allen, Steven L.; Manchester, Richard N.; Thompson, William T.

2015-02-01

Context. In a series of three previous papers, formulation and specifics of the representation of world coordinate transformations in FITS data have been presented. This fourth paper deals with encoding time. Aims: Time on all scales and precisions known in astronomical datasets is to be described in an unambiguous, complete, and self-consistent manner. Methods: Employing the well-established World Coordinate System (WCS) framework, and maintaining compatibility with the FITS conventions that are currently in use to specify time, the standard is extended to describe rigorously the time coordinate. Results: World coordinate functions are defined for temporal axes sampled linearly and as specified by a lookup table. The resulting standard is consistent with the existing FITS WCS standards and specifies a metadata set that achieves the aims enunciated above.

Optimization and Validation of the TZM-bl Assay for Standardized Assessments of Neutralizing Antibodies Against HIV-1

PubMed Central

Sarzotti-Kelsoe, Marcella; Bailer, Robert T; Turk, Ellen; Lin, Chen-li; Bilska, Miroslawa; Greene, Kelli M.; Gao, Hongmei; Todd, Christopher A.; Ozaki, Daniel A.; Seaman, Michael S.; Mascola, John R.; Montefiori, David C.

2014-01-01

The TZM-bl assay measures antibody-mediated neutralization of HIV-1 as a function of reductions in HIV-1 Tat-regulated firefly luciferase (Luc) reporter gene expression after a single round of infection with Env-pseudotyped viruses. This assay has become the main endpoint neutralization assay used for the assessment of preclinical and clinical trial samples by a growing number of laboratories worldwide. Here we present the results of the formal optimization and validation of the TZM-bl assay, performed in compliance with Good Clinical Laboratory Practice (GCLP) guidelines. The assay was evaluated for specificity, accuracy, precision, limits of detection and quantitation, linearity, range and robustness. The validated manual TZM-bl assay was also adapted, optimized and qualified to an automated 384-well format. PMID:24291345

Improving the sensitivity and specificity of a bioanalytical assay for the measurement of certolizumab pegol.

PubMed

Smeraglia, John; Silva, John-Paul; Jones, Kieran

2017-08-01

In order to evaluate placental transfer of certolizumab pegol (CZP), a more sensitive and selective bioanalytical assay was required to accurately measure low CZP concentrations in infant and umbilical cord blood. Results & methodology: A new electrochemiluminescence immunoassay was developed to measure CZP levels in human plasma. Validation experiments demonstrated improved selectivity (no matrix interference observed) and a detection range of 0.032-5.0 μg/ml. Accuracy and precision met acceptance criteria (mean total error ≤20.8%). Dilution linearity and sample stability were acceptable and sufficient to support the method. The electrochemiluminescence immunoassay was validated for measuring low CZP concentrations in human plasma. The method demonstrated a more than tenfold increase in sensitivity compared with previous assays, and improved selectivity for intact CZP.

Spectroscopic characterization and quantitative determination of atorvastatin calcium impurities by novel HPLC method

NASA Astrophysics Data System (ADS)

Gupta, Lokesh Kumar

2012-11-01

Seven process related impurities were identified by LC-MS in the atorvastatin calcium drug substance. These impurities were identified by LC-MS. The structure of impurities was confirmed by modern spectroscopic techniques like 1H NMR and IR and physicochemical studies conducted by using synthesized authentic reference compounds. The synthesized reference samples of the impurity compounds were used for the quantitative HPLC determination. These impurities were detected by newly developed gradient, reverse phase high performance liquid chromatographic (HPLC) method. The system suitability of HPLC analysis established the validity of the separation. The analytical method was validated according to International Conference of Harmonization (ICH) with respect to specificity, precision, accuracy, linearity, robustness and stability of analytical solutions to demonstrate the power of newly developed HPLC method.

Multi-center evaluation of analytical performance of the Beckman Coulter AU5822 chemistry analyzer.

PubMed

Zimmerman, M K; Friesen, L R; Nice, A; Vollmer, P A; Dockery, E A; Rankin, J D; Zmuda, K; Wong, S H

2015-09-01

Our three academic institutions, Indiana University, Northwestern Memorial Hospital, and Wake Forest, were among the first in the United States to implement the Beckman Coulter AU5822 series chemistry analyzers. We undertook this post-hoc multi-center study by merging our data to determine performance characteristics and the impact of methodology changes on analyte measurement. We independently completed performance validation studies including precision, linearity/analytical measurement range, method comparison, and reference range verification. Complete data sets were available from at least one institution for 66 analytes with the following groups: 51 from all three institutions, and 15 from 1 or 2 institutions for a total sample size of 12,064. Precision was similar among institutions. Coefficients of variation (CV) were <10% for 97%. Analytes with CVs >10% included direct bilirubin and digoxin. All analytes exhibited linearity over the analytical measurement range. Method comparison data showed slopes between 0.900-1.100 for 87.9% of the analytes. Slopes for amylase, tobramycin and urine amylase were <0.8; the slope for lipase was >1.5, due to known methodology or standardization differences. Consequently, reference ranges of amylase, urine amylase and lipase required only minor or no modification. The four AU5822 analyzers independently evaluated at three sites showed consistent precision, linearity, and correlation results. Since installations, the test results had been well received by clinicians from all three institutions. Copyright © 2015. Published by Elsevier Inc.

Can you trust the parametric standard errors in nonlinear least squares? Yes, with provisos.

PubMed

Tellinghuisen, Joel

2018-04-01

Questions about the reliability of parametric standard errors (SEs) from nonlinear least squares (LS) algorithms have led to a general mistrust of these precision estimators that is often unwarranted. The importance of non-Gaussian parameter distributions is illustrated by converting linear models to nonlinear by substituting e A , ln A, and 1/A for a linear parameter a. Monte Carlo (MC) simulations characterize parameter distributions in more complex cases, including when data have varying uncertainty and should be weighted, but weights are neglected. This situation leads to loss of precision and erroneous parametric SEs, as is illustrated for the Lineweaver-Burk analysis of enzyme kinetics data and the analysis of isothermal titration calorimetry data. Non-Gaussian parameter distributions are generally asymmetric and biased. However, when the parametric SE is <10% of the magnitude of the parameter, both the bias and the asymmetry can usually be ignored. Sometimes nonlinear estimators can be redefined to give more normal distributions and better convergence properties. Variable data uncertainty, or heteroscedasticity, can sometimes be handled by data transforms but more generally requires weighted LS, which in turn require knowledge of the data variance. Parametric SEs are rigorously correct in linear LS under the usual assumptions, and are a trustworthy approximation in nonlinear LS provided they are sufficiently small - a condition favored by the abundant, precise data routinely collected in many modern instrumental methods. Copyright © 2018 Elsevier B.V. All rights reserved.

Analytical parameters of the microplate-based ORAC-pyrogallol red assay.

PubMed

Ortiz, Rocío; Antilén, Mónica; Speisky, Hernán; Aliaga, Margarita E; López-Alarcón, Camilo

2011-01-01

The analytical parameters of the microplate-based oxygen radicals absorbance capacity (ORAC) method using pyrogallol red (PGR) as probe (ORAC-PGR) are presented. In addition, the antioxidant capacity of commercial beverages, such as wines, fruit juices, and iced teas, is estimated. A good linearity of the area under the curve (AUC) versus Trolox concentration plots was obtained [AUC = (845 +/- 110) + (23 +/- 2) [Trolox, microM], R = 0.9961, n = 19]. QC experiments showed better precision and accuracy at the highest Trolox concentration (40 microM) with RSD and REC (recuperation) values of 1.7 and 101.0%, respectively. When red wine was used as sample, the method also showed good linearity [AUC = (787 +/- 77) + (690 +/- 60) [red wine, microL/mL]; R = 0.9926, n = 17], precision and accuracy with RSD values from 1.4 to 8.3%, and REC values that ranged from 89.7 to 103.8%. Additivity assays using solutions containing gallic acid and Trolox (or red wine) showed an additive protection of PGR given by the samples. Red wines showed higher ORAC-PGR values than white wines, while the ORAC-PGR index of fruit juices and iced teas presented a great variability, ranging from 0.6 to 21.6 mM of Trolox equivalents. This variability was also observed for juices of the same fruit, showing the influence of the brand on the ORAC-PGR index. The ORAC-PGR methodology can be applied in a microplate reader with good linearity, precision, and accuracy.

Linear and volumetric dimensional changes of injection-molded PMMA denture base resins.

PubMed

El Bahra, Shadi; Ludwig, Klaus; Samran, Abdulaziz; Freitag-Wolf, Sandra; Kern, Matthias

2013-11-01

The aim of this study was to evaluate the linear and volumetric dimensional changes of six denture base resins processed by their corresponding injection-molding systems at 3 time intervals of water storage. Two heat-curing (SR Ivocap Hi Impact and Lucitone 199) and four auto-curing (IvoBase Hybrid, IvoBase Hi Impact, PalaXpress, and Futura Gen) acrylic resins were used with their specific injection-molding technique to fabricate 6 specimens of each material. Linear and volumetric dimensional changes were determined by means of a digital caliper and an electronic hydrostatic balance, respectively, after water storage of 1, 30, or 90 days. Means and standard deviations of linear and volumetric dimensional changes were calculated in percentage (%). Statistical analysis was done using Student's and Welch's t tests with Bonferroni-Holm correction for multiple comparisons (α=0.05). Statistically significant differences in linear dimensional changes between resins were demonstrated at all three time intervals of water immersion (p≤0.05), with exception of the following comparisons which showed no significant difference: IvoBase Hi Impact/SR Ivocap Hi Impact and PalaXpress/Lucitone 199 after 1 day, Futura Gen/PalaXpress and PalaXpress/Lucitone 199 after 30 days, and IvoBase Hybrid/IvoBase Hi Impact after 90 days. Also, statistically significant differences in volumetric dimensional changes between resins were found at all three time intervals of water immersion (p≤0.05), with exception of the comparison between PalaXpress and Futura Gen. Denture base resins (IvoBase Hybrid and IvoBase Hi Impact) processed by the new injection-molding system (IvoBase), revealed superior dimensional precision. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Biomotor structures in elite female handball players.

PubMed

Katić, Ratko; Cavala, Marijana; Srhoj, Vatromir

2007-09-01

In order to identify biomotor structures in elite female handball players, factor structures of morphological characteristics and basic motor abilities of elite female handball players (N = 53) were determined first, followed by determination of relations between the morphological-motor space factors obtained and the set of criterion variables evaluating situation motor abilities in handball. Factor analysis of 14 morphological measures produced three morphological factors, i.e. factor of absolute voluminosity (mesoendomorph), factor of longitudinal skeleton dimensionality, and factor of transverse hand dimensionality. Factor analysis of 15 motor variables yielded five basic motor dimensions, i.e. factor of agility, factor of jumping explosive strength, factor of throwing explosive strength, factor of movement frequency rate, and factor of running explosive strength (sprint). Four significant canonic correlations, i.e. linear combinations, explained the correlation between the set of eight latent variables of the morphological and basic motor space and five variables of situation motoricity. First canonic linear combination is based on the positive effect of the factors of agility/coordination on the ability of fast movement without ball. Second linear combination is based on the effect of jumping explosive strength and transverse hand dimensionality on ball manipulation, throw precision, and speed of movement with ball. Third linear combination is based on the running explosive strength determination by the speed of movement with ball, whereas fourth combination is determined by throwing and jumping explosive strength, and agility on ball pass. The results obtained were consistent with the model of selection in female handball proposed (Srhoj et al., 2006), showing the speed of movement without ball and the ability of ball manipulation to be the predominant specific abilities, as indicated by the first and second linear combination.

High precision triangular waveform generator

DOEpatents

Mueller, Theodore R.

1983-01-01

An ultra-linear ramp generator having separately programmable ascending and descending ramp rates and voltages is provided. Two constant current sources provide the ramp through an integrator. Switching of the current at current source inputs rather than at the integrator input eliminates switching transients and contributes to the waveform precision. The triangular waveforms produced by the waveform generator are characterized by accurate reproduction and low drift over periods of several hours. The ascending and descending slopes are independently selectable.

High-precision triangular-waveform generator

DOEpatents

Mueller, T.R.

1981-11-14

An ultra-linear ramp generator having separately programmable ascending and decending ramp rates and voltages is provided. Two constant current sources provide the ramp through an integrator. Switching of the current at current source inputs rather than at the integrator input eliminates switching transients and contributes to the waveform precision. The triangular waveforms produced by the waveform generator are characterized by accurate reproduction and low drift over periods of several hours. The ascending and descending slopes are independently selectable.

Spectrophotometric simultaneous determination of Rabeprazole Sodium and Itopride Hydrochloride in capsule dosage form

NASA Astrophysics Data System (ADS)

Sabnis, Shweta S.; Dhavale, Nilesh D.; Jadhav, Vijay. Y.; Gandhi, Santosh V.

2008-03-01

A new simple, economical, rapid, precise and accurate method for simultaneous determination of rabeprazole sodium and itopride hydrochloride in capsule dosage form has been developed. The method is based on ratio spectra derivative spectrophotometry. The amplitudes in the first derivative of the corresponding ratio spectra at 231 nm (minima) and 260 nm were selected to determine rabeprazole sodium and itopride hydrochloride, respectively. The method was validated with respect to linearity, precision and accuracy.

Spectrophotometric simultaneous determination of rabeprazole sodium and itopride hydrochloride in capsule dosage form.

PubMed

Sabnis, Shweta S; Dhavale, Nilesh D; Jadhav, Vijay Y; Gandhi, Santosh V

2008-03-01

A new simple, economical, rapid, precise and accurate method for simultaneous determination of rabeprazole sodium and itopride hydrochloride in capsule dosage form has been developed. The method is based on ratio spectra derivative spectrophotometry. The amplitudes in the first derivative of the corresponding ratio spectra at 231nm (minima) and 260nm were selected to determine rabeprazole sodium and itopride hydrochloride, respectively. The method was validated with respect to linearity, precision and accuracy.

Communication: Analysing kinetic transition networks for rare events.

PubMed

Stevenson, Jacob D; Wales, David J

2014-07-28

The graph transformation approach is a recently proposed method for computing mean first passage times, rates, and committor probabilities for kinetic transition networks. Here we compare the performance to existing linear algebra methods, focusing on large, sparse networks. We show that graph transformation provides a much more robust framework, succeeding when numerical precision issues cause the other methods to fail completely. These are precisely the situations that correspond to rare event dynamics for which the graph transformation was introduced.

A comparative study of smart spectrophotometric methods for simultaneous determination of sitagliptin phosphate and metformin hydrochloride in their binary mixture.

PubMed

Lotfy, Hayam M; Mohamed, Dalia; Mowaka, Shereen

2015-01-01

Simple, specific, accurate and precise spectrophotometric methods were developed and validated for the simultaneous determination of the oral antidiabetic drugs; sitagliptin phosphate (STG) and metformin hydrochloride (MET) in combined pharmaceutical formulations. Three methods were manipulating ratio spectra namely; ratio difference (RD), ratio subtraction (RS) and a novel approach of induced amplitude modulation (IAM) methods. The first two methods were used for determination of STG, while MET was directly determined by measuring its absorbance at λmax 232 nm. However, (IAM) was used for the simultaneous determination of both drugs. Moreover, another three methods were developed based on derivative spectroscopy followed by mathematical manipulation steps namely; amplitude factor (P-factor), amplitude subtraction (AS) and modified amplitude subtraction (MAS). In addition, in this work the novel sample enrichment technique named spectrum addition was adopted. The proposed spectrophotometric methods did not require any preliminary separation step. The accuracy, precision and linearity ranges of the proposed methods were determined. The selectivity of the developed methods was investigated by analyzing laboratory prepared mixtures of the drugs and their combined pharmaceutical formulations. Standard deviation values were less than 1.5 in the assay of raw materials and tablets. The obtained results were statistically compared to that of a reported spectrophotometric method. The statistical comparison showed that there was no significant difference between the proposed methods and the reported one regarding both accuracy and precision. Copyright © 2015 Elsevier B.V. All rights reserved.

A small, linear, piezoelectric ultrasonic cryomotor

NASA Astrophysics Data System (ADS)

Dong, Shuxiang; Yan, Li; Wang, Naigang; Viehland, Dwight; Jiang, Xiaoning; Rehrig, Paul; Hackenberger, Wes

2005-01-01

A small, linear-type, piezoelectric ultrasonic cryomotor has been developed for precision positioning at extremely low temperatures (⩾-200°C). This cryomotor consists of a pair of Pb(Mg1/3Nb2/3)O3-PbTiO3 single crystal stacks, which are piezoelectrically excited into the rotating third-bending mode of the cryomotor stator's center, which in turn drives a contacted slider into linear motion via frictional forces. The performance characteristics achieved by the cryomotor are: (i) a maximum linear speed of >50mm /s; (ii) a stroke of >10mm; (iii) a driving force of >0.2N; (iv) a response time of ˜29ms; and (v) a step resolution of ˜20nm.

Determination of enantiomeric vigabatrin by derivatization with diacetyl-l-tartaric anhydride followed by ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry.

PubMed

Zhao, Jing; Shin, Yujin; Jin, Yan; Jeong, Kyung Min; Lee, Jeongmi

2017-01-01

Vigabatrin, one of the most widely used antiepileptic drugs, is marketed and administered as a racemic mixture, while only S-enantiomer is therapeutically effective. In the present study, diacetyl-l-tartaric acid anhydride was used as an inexpensive and effective chiral derivatization reagent to produce tartaric acid monoester derivatives of vigabatrin enantiomers that could be readily resolved by reversed phase chromatography. Derivatization conditions were statistically optimized by response surface methodology, resulting in an optimal reaction temperature of 44°C and an optimal reaction time of 30min. The derivatized diastereomers of vigabatrin and internal standard (gabapentin) were analyzed using ultra-high performance liquid chromatography coupled to quadrupole-time-of-flight mass spectrometry. For this analysis, an Agilent ZORBAX Rapid Resolution High Definition Eclipse Plus C18 column (100mm×2.1mm, 1.8μm) was employed for chromatographic separation using 10mM ammonium formate (pH 3.0) and methanol as mobile phase at a flow rate of 0.2mLmin -1 . The established method was validated in terms of specificity, linearity, precision, accuracy, dilution integrity, recovery, matrix effect, stability, and incurred sample reanalysis. It was linear over a range of 0.25-100.0mgL -1 for both S- and R-enantiomers (R 2 ≥0.9987 for both). Intra- and inter-day precisions and accuracies were within acceptable ranges. The method was successfully applied to determine the levels of vigabatrin enantiomers in mouse serum after administration of vigabatrin racemate. Copyright © 2016 Elsevier B.V. All rights reserved.

Stability-indicating HPLC Method for Simultaneous Determination of Terbutaline Sulphate, Bromhexine Hydrochloride and Guaifenesin

PubMed Central

Porel, A.; Haty, Sanjukta; Kundu, A.

2011-01-01

The aim of the present study was the development and subsequent validation of a simple, precise and stability-indicating reversed phase HPLC method for the simultaneous determination of guaifenesin, terbutaline sulphate and bromhexine hydrochloride in the presence of their potential impurities in a single run. The photolytic as well as hydrolytic impurities were detected as 3,5-dihydroxybenzoic acid, 3,5-dihydroxybenzaldehyde, 1-(3,5-dihydroxyphenyl)-2-[(1,1-dimethylethyl) amino]-ethanone from terbutaline, 2-methoxyphenol and an unknown impurity identified as (2RS)-3-(2-hydroxyphenoxy)-propane-1,2-diol from guaifenesin. The chromatographic separation of all the three active components and their impurities was achieved on Wakosil II column, using phosphate buffer (pH 3.0) and acetonitrile as mobile phase which was delivered initially in the ratio of 80:20 (v/v) for 18 min, then changed to 60:40 (v/v) for next 12 min, and finally equilibrated back to 80:20 (v/v) for 10 min. Other HPLC parameters were: Flow rate at 1.0 ml/min, detection wavelengths 248 and 280 nm, injection volume 10 μl. The calibration graphs plotted with five concentrations of each component were linear with a regression coefficient R2 >0.9999. The limit of detection and limit of quantitation were estimated for all the five impurities. The established method was then validated for linearity, precision, accuracy, and specificity and demonstrated to be applicable to the determination of the active ingredients in commercial and model cough syrup. No interference from the formulation excipients was observed. These results suggest that this LC method can be used for the determination of multiple active ingredients and their impurities in a cough and cold syrup. PMID:22131621

Stability-indicating HPLC Method for Simultaneous Determination of Terbutaline Sulphate, Bromhexine Hydrochloride and Guaifenesin.

PubMed

Porel, A; Haty, Sanjukta; Kundu, A

2011-01-01

The aim of the present study was the development and subsequent validation of a simple, precise and stability-indicating reversed phase HPLC method for the simultaneous determination of guaifenesin, terbutaline sulphate and bromhexine hydrochloride in the presence of their potential impurities in a single run. The photolytic as well as hydrolytic impurities were detected as 3,5-dihydroxybenzoic acid, 3,5-dihydroxybenzaldehyde, 1-(3,5-dihydroxyphenyl)-2-[(1,1-dimethylethyl) amino]-ethanone from terbutaline, 2-methoxyphenol and an unknown impurity identified as (2RS)-3-(2-hydroxyphenoxy)-propane-1,2-diol from guaifenesin. The chromatographic separation of all the three active components and their impurities was achieved on Wakosil II column, using phosphate buffer (pH 3.0) and acetonitrile as mobile phase which was delivered initially in the ratio of 80:20 (v/v) for 18 min, then changed to 60:40 (v/v) for next 12 min, and finally equilibrated back to 80:20 (v/v) for 10 min. Other HPLC parameters were: Flow rate at 1.0 ml/min, detection wavelengths 248 and 280 nm, injection volume 10 μl. The calibration graphs plotted with five concentrations of each component were linear with a regression coefficient R(2) >0.9999. The limit of detection and limit of quantitation were estimated for all the five impurities. The established method was then validated for linearity, precision, accuracy, and specificity and demonstrated to be applicable to the determination of the active ingredients in commercial and model cough syrup. No interference from the formulation excipients was observed. These results suggest that this LC method can be used for the determination of multiple active ingredients and their impurities in a cough and cold syrup.

Development of an HPLC method for determination of metabolic compounds in myocardial tissue.

PubMed

Volonté, M G; Yuln, G; Quiroga, P; Consolini, A E

2004-05-28

The determination of adenine nucleotides and creatine compounds has great importance in the characterization of ischemic myocardial injury and post-ischemic recovery. It was developed by an HPLC method for the quantification of creatine (Cr), creatine phosphate (CrP), hypoxanthine (HX), AMP, adenosine (Ad), ADP and ATP in isolated perfused rat hearts. The chromatographic conditions were: RP 18 column; mobile phase composed by KH(2)PO(4) (215 mM), tetrabutylammonium hydrogen sulfate (2.3mM), acetonitrile (4%) and KOH (1M 0.4%); flow rate 1 ml min(-1); temperature 25 degrees C; injection volume 20 microl; detection at 220 nm and height peak (HP) as the integration parameter. The method was validated by means of linearity and sensitivity evaluations, using calibration curves done with five concentration levels of each compound. The limits of quantification (LOQ) were also determined. The system precision was calculated as the coefficient of variation for five injections for each compound tested. The purity of the peaks was established using enzymatic peak shift analysis with hexokinase and creatine kinase and also comparing HP at various wavelengths. Frozen hearts were homogenized with a mechanical homogenizer for 3 min at 0 degrees C added with 5 ml of 0.4N HCLO(4). After precipitation with 0.8 ml of 2M KOH the extract was shaked for 2 min and later centrifuged at 0 degrees C for 10 min. The supernatant was kept on ice, filtrated and injected into the HPLC system. The results show that the method for the determination of Cr, CrP, HX, AMP, Ad, ADP and ATP by HPLC here described has good linearity, LOQ, precision, specificity and is simple and rapid to perform.

Simultaneous determination of chromones and coumarins in Radix Saposhnikoviae by high performance liquid chromatography with diode array and tandem mass detectors.

PubMed

Kim, Min Kyung; Yang, Dong-Hyug; Jung, Mihye; Jung, Eun Ha; Eom, Han Young; Suh, Joon Hyuk; Min, Jung Won; Kim, Unyong; Min, Hyeyoung; Kim, Jinwoong; Han, Sang Beom

2011-09-16

Methods using high performance liquid chromatography with diode array detection (HPLC-DAD) and tandem mass spectrometry (HPLC-MS/MS) were developed and validated for the simultaneous determination of 5 chromones and 6 coumarins: prim-O-glucosylcimifugin (1), cimifugin (2), nodakenin (3), 4'-O-β-d-glucosyl-5-O-methylvisamminol (4), sec-O-glucosylhamaudol (5), psoralen (6), bergapten (7), imperatorin (8), phellopterin (9), 3'-O-angeloylhamaudol (10) and anomalin (11), in Radix Saposhnikoviae. The separation conditions for HPLC-DAD were optimized using an Ascentis Express C18 (4.6 mm×100 mm, 2.7 μm particle size) fused-core column. The mobile phase was composed of 10% aqueous acetonitrile (A) and 90% acetonitrile (B) and the elution was performed under a gradient mode at a flow rate of 1.0 mL/min. The detection wavelength was set at 300 nm. The HPLC-DAD method yielded a base line separation of the 11 components in 50% methanol extract of Radix Saposhnikoviae with no interfering peaks detected. The HPLC-DAD method was validated in terms of linearity, accuracy and precision (intra- and inter-day), limit of quantification (LOQ), recovery, and robustness. Specific determination of the 11 components was also accomplished by a triple quadrupole tandem mass spectrometer equipped with an electrospray ionization (ESI) source. This HPLC-MS/MS method was also validated by determining the linearity, limit of quantification, accuracy, and precision. Quantification of the 11 components in 51 commercial Radix Saposhnikoviae samples was successfully performed using the developed HPLC-DAD method. The identity, batch-to-batch consistency, and authenticity of Radix Saposhnikoviae were successfully monitored by the proposed HPLC-DAD and HPLC-MS/MS methods. Copyright © 2011 Elsevier B.V. All rights reserved.

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

PubMed

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

2011-11-01

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

Comparison of two indices of exposure to polycyclic aromatic hydrocarbons in a retrospective aluminium smelter cohort.

PubMed

Friesen, Melissa C; Demers, Paul A; Spinelli, John J; Lorenzi, Maria F; Le, Nhu D

2007-04-01

The association between coal tar-derived substances, a complex mixture of polycyclic aromatic hydrocarbons, and cancer is well established. However, the specific aetiological agents are unknown. To compare the dose-response relationships for two common measures of coal tar-derived substances, benzene-soluble material (BSM) and benzo(a)pyrene (BaP), and to evaluate which among these is more strongly related to the health outcomes. The study population consisted of 6423 men with > or =3 years of work experience at an aluminium smelter (1954-97). Three health outcomes identified from national mortality and cancer databases were evaluated: incidence of bladder cancer (n = 90), incidence of lung cancer (n = 147) and mortality due to acute myocardial infarction (AMI, n = 184). The shape, magnitude and precision of the dose-response relationships and cumulative exposure levels for BSM and BaP were evaluated. Two model structures were assessed, where 1n(relative risk) increased with cumulative exposure (log-linear model) or with log-transformed cumulative exposure (log-log model). The BaP and BSM cumulative exposure metrics were highly correlated (r = 0.94). The increase in model precision using BaP over BSM was 14% for bladder cancer and 5% for lung cancer; no difference was observed for AMI. The log-linear BaP model provided the best fit for bladder cancer. The log-log dose-response models, where risk of disease plateaus at high exposure levels, were the best-fitting models for lung cancer and AMI. BaP and BSM were both strongly associated with bladder and lung cancer and modestly associated with AMI. Similar conclusions regarding the associations could be made regardless of the exposure metric.

Stability-indicating methods for the determination of piretanide in presence of the alkaline induced degradates.

PubMed

Youssef, Nadia F

2005-10-04

Stability-indicating high performance liquid chromatography (HPLC), thin-layer chromatography (TLC) and first-derivative of ratio spectra (1DD) methods are developed for the determination of piretanide in presence of its alkaline induced degradates. HPLC method depends on separation of piretanide from its degradates on mu-Bondapak C18 column using methanol:water:acetic acid (70:30:1, v/v/v) as a mobile phase at flow rate 1.0 ml/min and UV detector at 275 nm. TLC densitometic method is based on the difference in Rf-values between the intact drug and its degradates on thin-layer silica gel. Iso-propanol:ammonia 33% (8:2, v/v) was used as a developing mobile phase and the chromatogram was scanned at 275 nm. The derivative of ratio spectra method (1DD) depends on the measurement of the absorbance at 288 nm in the first-derivative of ratio spectra for the determination of the cited drug in the presence of its degradates. Calibration graphs of the three suggested methods are linear in the concentration ranges 0.02-0.3 microg/20 microl, 0.5-10 microg/spot and 5-50 microg/ml, with mean percentage recovery 99.27+/-0.52, 99,17+/-1.01 and 99.65+/-1.01%, respectively. The three proposed methods were successfully applied for the determination of piretanide in bulk powder, laboratory-prepared mixtures and pharmaceutical dosage form with good accuracy and precision. The results were statistically analyzed and compared with those obtained by the official method. Validation of the method was determined with favourable specificity, linearity, precision, and accuracy was assessed by applying the standard addition technique.

Clinical performance evaluation of total protein measurement by digital refractometry and characterization of non-protein solute interferences.

PubMed

Hunsaker, Joshua J H; Wyness, Sara P; Snow, Taylor M; Genzen, Jonathan R

2016-12-01

Refractometric methods to measure total protein (TP) in serum and plasma specimens have been replaced by automated biuret methods in virtually all routine clinical testing. A subset of laboratories, however, still report using refractometry to measure TP in conjunction with serum protein electrophoresis. The objective of this study was therefore to conduct a modern performance evaluation of a digital refractometer for TP measurement. Performance evaluation of a MISCO Palm Abbe™ digital refractometer was conducted through device familiarization, carryover, precision, accuracy, linearity, analytical sensitivity, analytical specificity, and reference interval verification. Comparison assays included a manual refractometer and an automated biuret assay. Carryover risk was eliminated using a demineralized distilled water (ddH 2 O) wash step. Precision studies demonstrated overall imprecision of 2.2% CV (low TP pool) and 0.5% CV (high TP pool). Accuracy studies demonstrated correlation to both manual refractometry and the biuret method. An overall positive bias (+5.0%) was observed versus the biuret method. On average, outlier specimens had an increased triglyceride concentration. Linearity was verified using mixed dilutions of: a) low and high concentration patient pools, or b) albumin-spiked ddH 2 O and high concentration patient pool. Decreased recovery was observed using ddH 2 O dilutions at low TP concentrations. Significant interference was detected at high concentrations of glucose (>267 mg/dL) and triglycerides (>580 mg/dL). Current laboratory reference intervals for TP were verified. Performance characteristics of this digital refractometer were validated in a clinical laboratory setting. Biuret method remains the preferred assay for TP measurement in routine clinical analyses.

Stability-indicating assay of repaglinide in bulk and optimized nanoemulsion by validated high performance thin layer chromatography technique.

PubMed

Akhtar, Juber; Fareed, Sheeba; Aqil, Mohd

2013-07-01

A sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic (HPTLC) method for analysis of repaglinide both as a bulk drug and in nanoemulsion formulation was developed and validated. The method employed TLC aluminum plates precoated with silica gel 60F-254 as the stationary phase. The solvent system consisted of chloroform/methanol/ammonia/glacial acetic acid (7.5:1.5:0.9:0.1, v/v/v/v). This system was found to give compact spots for repaglinide (R f value of 0.38 ± 0.02). Repaglinide was subjected to acid and alkali hydrolysis, oxidation, photodegradation and dry heat treatment. Also, the degraded products were well separated from the pure drug. Densitometric analysis of repaglinide was carried out in the absorbance mode at 240 nm. The linear regression data for the calibration plots showed good linear relationship with r (2)= 0.998 ± 0.032 in the concentration range of 50-800 ng. The method was validated for precision, accuracy as recovery, robustness and specificity. The limits of detection and quantitation were 0.023 and 0.069 ng per spot, respectively. The drug undergoes degradation under acidic and basic conditions, oxidation and dry heat treatment. All the peaks of the degraded product were resolved from the standard drug with significantly different R f values. Statistical analysis proves that the method is reproducible and selective for the estimation of the said drug. As the method could effectively separate the drug from its degradation products, it can be employed as a stability-indicating one. Moreover, the proposed HPTLC method was utilized to investigate the degradation kinetics in 1M NaOH.

Development of validated stability indicating assay method for simultaneous estimation of metformin hydrochloride and vildagliptin by RP-HPLC.

PubMed

Satheeshkumar, N; Pradeepkumar, M; Shanthikumar, S; Rao, V J

2014-03-01

A simple, precise and stability-indicating HPLC method was developed and validated for the simultaneous determination of metformin hydrochloride (MET) and vildagliptin (VLG) in pharmaceutical dosage forms. The method involves use of easily available inexpensive laboratory reagents. The separation was achieved on Grace Cyano column (250 mm×4.6 mm) 5 µm with isocratic flow. The mobile phase was pumped at a flow rate of 1.0 mL/min, consisted of 25 mM ammonium bicarbonate buffer and acetonitrile (65:35, v/v). The UV detection was carried out at 207 nm. A linear response was observed over the concentration range of 25-125 µg/mL for MET and 50-250 µg/mL for VLG respectively. Limit of detection and limit of quantification for MET were 0.36 µg/mL and 1.22 µg/mL, and for VLG were 0.75 µg/mL and 2.51 µg/mL respectively. The method was successfully validated in accordance to ICH guidelines acceptance criteria for specificity, linearity, accuracy, precision, robustness, and system suitability. Individual drugs (MET and VLG) were exposed to thermal, photolytic, hydrolytic and oxidative stress conditions. The resultant stressed samples were analyzed by the proposed method. The method gave high resolution among the degradation products and the analytes. The peak purity of analyte peak in the stressed samples was confirmed by photo diode array detector. The proposed method was successfully applied for the quantitative analysis of MET and VLG in tablet dosage form, which will help to improve quality control and contribute to stability studies of pharmaceutical tablets containing these drugs. © Georg Thieme Verlag KG Stuttgart · New York.

Liquid chromatography/tandem mass spectrometry method for simultaneous determination of cocaine and its metabolite (-)ecgonine methyl ester in human acidified stabilized plasma samples.

PubMed

Liu, Yongzhen; Zheng, Bo; Strafford, Stephanie; Orugunty, Ravi; Sullivan, Michael; Gus, Jeffrey; Heidbreder, Christian; Fudala, Paul J; Nasser, Azmi

2014-06-15

Two simple, sensitive and rapid liquid chromatography/electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) methods (low range and high range) were developed and validated for the quantification of cocaine and its metabolite (-)ecgonine methyl ester (EME) in human acidified stabilized plasma samples. In the low range assay, cocaine and the internal standard, cocaine-D3, were extracted using a single step liquid-liquid extraction from human acidified stabilized plasma. For the high range assay, human acidified stabilized plasma containing cocaine, EME, and the internal standards, cocaine-D3 and EME-D3, was mixed with acetonitrile, and the protein precipitate was separated by centrifugation. Both cocaine and EME extracted from both assays were separated on a HILIC column and detected in positive ion mode using multiple reaction monitoring (MRM). Both methods were validated and the specificity, linearity, lower limit of quantitation (LLOQ), precision, accuracy, recoveries and stability were determined. The linear range for the low range assay was 0.01-5ng/mL for cocaine; in the high range assay values were 5-1000ng/mL for cocaine and 1-200ng/mL for EME. The correlation coefficient (R(2)) values for both assays were 0.993 or greater. The precision and accuracy for intra-day and inter-day were better than 13.0%. The recovery was above 85% and matrix effects were low with the matrix factor ranging from 0.817 to 1.10 for both analytes in both assays. The validated methods were successfully used to quantify the plasma concentrations of cocaine and EME in clinical pharmacokinetic and pharmacodynamic studies. Copyright © 2014 Elsevier B.V. All rights reserved.

Development of a high-throughput detection system for HIV-1 using real-time NASBA based on molecular beacons

NASA Astrophysics Data System (ADS)

van Beuningen, Rinie; Marras, Salvatore A.; Kramer, Fred R.; Oosterlaken, Tom; Weusten, Jos; Borst, G.; van de Wiel, Paul

2001-04-01

HIV-1 viral load assays require accuracy and sensitivity at low RNA levels with the capability to detect all subtypes. Furthermore, the assay should be easy to perform and fast to be useful for routine diagnostics. In order to meet these demands we have combined isothermal NASBA amplification with molecular beacon probes for real-time detection and quantitation of HIV-1 RNA. Quantitation is based on co-amplification of the HIV-1 RNA in the clinical sample and a synthetic calibrator RNA which is amplified by the same primer set but detected with a differently labeled molecular beacon. The entire procedure is simple and analysis of 48 samples requires less than 1» hours with minimal hands-on time. A fluorescent plate reader is used for real-time detection and isothermal amplification. The linearity and precision of the assay was determined with the VQC HIV-1 type B standard of the Central Laboratory of the Dutch Red Cross Blood Banks, The Netherlands. Sensitivity was shown to be 50 copies per ml (cps/ml). The average assay precision was 0,19 log10 over a range of 100-300,000 cps/ml tested at nine concentrations. The linearity of dilution series of 15 cultured HIV-1 gag clades A-H was shown. The specificity was 100% on non HIV-1 samples HIV-2, HTLV-1 and HTLV-2. The assay robustness in terms of valid results was 99%. In conclusion, the new real-time NASBA assay meets state-of-the-art HIV-1 viral load performance requirements combined with a high level of user convenience.

Novel AC Servo Rotating and Linear Composite Driving Device for Plastic Forming Equipment

NASA Astrophysics Data System (ADS)

Liang, Jin-Tao; Zhao, Sheng-Dun; Li, Yong-Yi; Zhu, Mu-Zhi

2017-07-01

The existing plastic forming equipment are mostly driven by traditional AC motors with long transmission chains, low efficiency, large size, low precision and poor dynamic response are the common disadvantages. In order to realize high performance forming processes, the driving device should be improved, especially for complicated processing motions. Based on electric servo direct drive technology, a novel AC servo rotating and linear composite driving device is proposed, which features implementing both spindle rotation and feed motion without transmission, so that compact structure and precise control can be achieved. Flux switching topology is employed in the rotating drive component for strong robustness, and fractional slot is employed in the linear direct drive component for large force capability. Then the mechanical structure for compositing rotation and linear motion is designed. A device prototype is manufactured, machining of each component and the whole assembly are presented respectively. Commercial servo amplifiers are utilized to construct the control system of the proposed device. To validate the effectiveness of the proposed composite driving device, experimental study on the dynamic test benches are conducted. The results indicate that the output torque can attain to 420 N·m and the dynamic tracking errors are less than about 0.3 rad in the rotating drive. the dynamic tracking errors are less than about 1.6 mm in the linear feed. The proposed research provides a method to construct high efficiency and accuracy direct driving device in plastic forming equipment.

High-Affinity Recombinant Antibody Fragments (Fabs) Can Be Applied in Peptide Enrichment Immuno-MRM Assays

PubMed Central

2015-01-01

High-affinity antibodies binding to linear peptides in solution are a prerequisite for performing immuno-MRM, an emerging technology for protein quantitation with high precision and specificity using peptide immunoaffinity enrichment coupled to stable isotope dilution and targeted mass spectrometry. Recombinant antibodies can be generated from appropriate libraries in high-throughput in an automated laboratory and thus may offer advantages over conventional monoclonal antibodies. However, recombinant antibodies are typically obtained as fragments (Fab or scFv) expressed from E. coli, and it is not known whether these antibody formats are compatible with the established protocols and whether the affinities necessary for immunocapture of small linear peptides can be achieved with this technology. Hence, we performed a feasibility study to ask: (a) whether it is feasible to isolate high-affinity Fabs to small linear antigens and (b) whether it is feasible to incorporate antibody fragments into robust, quantitative immuno-MRM assays. We describe successful isolation of high-affinity Fab fragments against short (tryptic) peptides from a human combinatorial Fab library. We analytically characterize three immuno-MRM assays using recombinant Fabs, full-length IgGs constructed from these Fabs, or traditional monoclonals. We show that the antibody fragments show similar performance compared with traditional mouse- or rabbit-derived monoclonal antibodies. The data establish feasibility of isolating and incorporating high-affinity Fabs into peptide immuno-MRM assays. PMID:24568200

High-affinity recombinant antibody fragments (Fabs) can be applied in peptide enrichment immuno-MRM assays.

PubMed

Whiteaker, Jeffrey R; Zhao, Lei; Frisch, Christian; Ylera, Francisco; Harth, Stefan; Knappik, Achim; Paulovich, Amanda G

2014-04-04

High-affinity antibodies binding to linear peptides in solution are a prerequisite for performing immuno-MRM, an emerging technology for protein quantitation with high precision and specificity using peptide immunoaffinity enrichment coupled to stable isotope dilution and targeted mass spectrometry. Recombinant antibodies can be generated from appropriate libraries in high-throughput in an automated laboratory and thus may offer advantages over conventional monoclonal antibodies. However, recombinant antibodies are typically obtained as fragments (Fab or scFv) expressed from E. coli, and it is not known whether these antibody formats are compatible with the established protocols and whether the affinities necessary for immunocapture of small linear peptides can be achieved with this technology. Hence, we performed a feasibility study to ask: (a) whether it is feasible to isolate high-affinity Fabs to small linear antigens and (b) whether it is feasible to incorporate antibody fragments into robust, quantitative immuno-MRM assays. We describe successful isolation of high-affinity Fab fragments against short (tryptic) peptides from a human combinatorial Fab library. We analytically characterize three immuno-MRM assays using recombinant Fabs, full-length IgGs constructed from these Fabs, or traditional monoclonals. We show that the antibody fragments show similar performance compared with traditional mouse- or rabbit-derived monoclonal antibodies. The data establish feasibility of isolating and incorporating high-affinity Fabs into peptide immuno-MRM assays.

Validating the applicability of the GUM procedure

NASA Astrophysics Data System (ADS)

Cox, Maurice G.; Harris, Peter M.

2014-08-01

This paper is directed at practitioners seeking a degree of assurance in the quality of the results of an uncertainty evaluation when using the procedure in the Guide to the Expression of Uncertainty in Measurement (GUM) (JCGM 100 : 2008). Such assurance is required in adhering to general standards such as International Standard ISO/IEC 17025 or other sector-specific standards. We investigate the extent to which such assurance can be given. For many practical cases, a measurement result incorporating an evaluated uncertainty that is correct to one significant decimal digit would be acceptable. Any quantification of the numerical precision of an uncertainty statement is naturally relative to the adequacy of the measurement model and the knowledge used of the quantities in that model. For general univariate and multivariate measurement models, we emphasize the use of a Monte Carlo method, as recommended in GUM Supplements 1 and 2. One use of this method is as a benchmark in terms of which measurement results provided by the GUM can be assessed in any particular instance. We mainly consider measurement models that are linear in the input quantities, or have been linearized and the linearization process is deemed to be adequate. When the probability distributions for those quantities are independent, we indicate the use of other approaches such as convolution methods based on the fast Fourier transform and, particularly, Chebyshev polynomials as benchmarks.

Development of Bonded Joint Technology for a Rigidizable-Inflatable Deployable Truss

NASA Technical Reports Server (NTRS)

Smeltzer, Stanley S., III

2006-01-01

Microwave and Synthetic Aperture Radar antenna systems have been developed as instrument systems using truss structures as their primary support and deployment mechanism for over a decade. NASA Langley Research Center has been investigating fabrication, modular assembly, and deployment methods of lightweight rigidizable/inflatable linear truss structures during that time for large spacecraft systems. The primary goal of the research at Langley Research Center is to advance these existing state-of-the-art joining and deployment concepts to achieve prototype system performance in a relevant space environment. During 2005, the development, fabrication, and testing of a 6.7 meter multi-bay, deployable linear truss was conducted at Langley Research Center to demonstrate functional and precision metrics of a rigidizable/inflatable truss structure. The present paper is intended to summarize aspects of bonded joint technology developed for the 6.7 meter deployable linear truss structure while providing a brief overview of the entire truss fabrication, assembly, and deployment methodology. A description of the basic joint design, surface preparation investigations, and experimental joint testing of component joint test articles will be described. Specifically, the performance of two room temperature adhesives were investigated to obtain qualitative data related to tube folding testing and quantitative data related to tensile shear strength testing. It was determined from the testing that a polyurethane-based adhesive best met the rigidizable/inflatable truss project requirements.

Number games, magnitude representation, and basic number skills in preschoolers.

PubMed

Whyte, Jemma Catherine; Bull, Rebecca

2008-03-01

The effect of 3 intervention board games (linear number, linear color, and nonlinear number) on young children's (mean age = 3.8 years) counting abilities, number naming, magnitude comprehension, accuracy in number-to-position estimation tasks, and best-fit numerical magnitude representations was examined. Pre- and posttest performance was compared following four 25-min intervention sessions. The linear number board game significantly improved children's performance in all posttest measures and facilitated a shift from a logarithmic to a linear representation of numerical magnitude, emphasizing the importance of spatial cues in estimation. Exposure to the number card games involving nonsymbolic magnitude judgments and association of symbolic and nonsymbolic quantities, but without any linear spatial cues, improved some aspects of children's basic number skills but not numerical estimation precision.

Networked dynamical systems with linear coupling: synchronisation patterns, coherence and other behaviours.

PubMed

Judd, Kevin

2013-12-01

Many physical and biochemical systems are well modelled as a network of identical non-linear dynamical elements with linear coupling between them. An important question is how network structure affects chaotic dynamics, for example, by patterns of synchronisation and coherence. It is shown that small networks can be characterised precisely into patterns of exact synchronisation and large networks characterised by partial synchronisation at the local and global scale. Exact synchronisation modes are explained using tools of symmetry groups and invariance, and partial synchronisation is explained by finite-time shadowing of exact synchronisation modes.

Linear algebraic theory of partial coherence: discrete fields and measures of partial coherence.

PubMed

Ozaktas, Haldun M; Yüksel, Serdar; Kutay, M Alper

2002-08-01

A linear algebraic theory of partial coherence is presented that allows precise mathematical definitions of concepts such as coherence and incoherence. This not only provides new perspectives and insights but also allows us to employ the conceptual and algebraic tools of linear algebra in applications. We define several scalar measures of the degree of partial coherence of an optical field that are zero for full incoherence and unity for full coherence. The mathematical definitions are related to our physical understanding of the corresponding concepts by considering them in the context of Young's experiment.

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

Yu, Dae Jung; Lee, Dong-Hun; Kim, Kihong

We study theoretically the linear mode conversion between electromagnetic waves and Langmuir waves in warm, stratified, and unmagnetized plasmas, using a numerically precise calculation based on the invariant imbedding method. We verify that the principle of reciprocity for the forward and backward mode conversion coefficients holds precisely regardless of temperature. We also find that the temperature dependence of the mode conversion coefficient is substantially stronger than that previously reported. Depending on the wave frequency and the incident angle, the mode conversion coefficient is found to increase or decrease with the increase of temperature.

Development and validation of dissolution study of sustained release dextromethorphan hydrobromide tablets.

PubMed

Rajan, Sekar; Colaco, Socorrina; Ramesh, N; Meyyanathan, Subramania Nainar; Elango, K

2014-02-01

This study describes the development and validation of dissolution tests for sustained release Dextromethorphan hydrobromide tablets using an HPLC method. Chromatographic separation was achieved on a C18 column utilizing 0.5% triethylamine (pH 7.5) and acetonitrile in the ratio of 50:50. The detection wavelength was 280 nm. The method was validated and response was found to be linear in the drug concentration range of 10-80 microg mL(-1). The suitable conditions were clearly decided after testing sink conditions, dissolution medium and agitation intensity. The most excellent dissolution conditions tested, for the Dextromethorphan hydrobromide was applied to appraise the dissolution profiles. The method was validated and response was found to be linear in the drug concentration range of 10-80 microg mL(-1). The method was established to have sufficient intermediate precision as similar separation was achieved on another instrument handled by different operators. Mean Recovery was 101.82%. Intra precisions for three different concentrations were 1.23, 1.10 0.72 and 1.57, 1.69, 0.95 and inter run precisions were % RSD 0.83, 1.36 and 1.57%, respectively. The method was successfully applied for dissolution study of the developed Dextromethorphan hydrobromide tablets.

Higgs physics at the CLIC electron-positron linear collider.

PubMed

Abramowicz, H; Abusleme, A; Afanaciev, K; Alipour Tehrani, N; Balázs, C; Benhammou, Y; Benoit, M; Bilki, B; Blaising, J-J; Boland, M J; Boronat, M; Borysov, O; Božović-Jelisavčić, I; Buckland, M; Bugiel, S; Burrows, P N; Charles, T K; Daniluk, W; Dannheim, D; Dasgupta, R; Demarteau, M; Díaz Gutierrez, M A; Eigen, G; Elsener, K; Felzmann, U; Firlej, M; Firu, E; Fiutowski, T; Fuster, J; Gabriel, M; Gaede, F; García, I; Ghenescu, V; Goldstein, J; Green, S; Grefe, C; Hauschild, M; Hawkes, C; Hynds, D; Idzik, M; Kačarević, G; Kalinowski, J; Kananov, S; Klempt, W; Kopec, M; Krawczyk, M; Krupa, B; Kucharczyk, M; Kulis, S; Laštovička, T; Lesiak, T; Levy, A; Levy, I; Linssen, L; Lukić, S; Maier, A A; Makarenko, V; Marshall, J S; Martin, V J; Mei, K; Milutinović-Dumbelović, G; Moroń, J; Moszczyński, A; Moya, D; Münker, R M; Münnich, A; Neagu, A T; Nikiforou, N; Nikolopoulos, K; Nürnberg, A; Pandurović, M; Pawlik, B; Perez Codina, E; Peric, I; Petric, M; Pitters, F; Poss, S G; Preda, T; Protopopescu, D; Rassool, R; Redford, S; Repond, J; Robson, A; Roloff, P; Ros, E; Rosenblat, O; Ruiz-Jimeno, A; Sailer, A; Schlatter, D; Schulte, D; Shumeiko, N; Sicking, E; Simon, F; Simoniello, R; Sopicki, P; Stapnes, S; Ström, R; Strube, J; Świentek, K P; Szalay, M; Tesař, M; Thomson, M A; Trenado, J; Uggerhøj, U I; van der Kolk, N; van der Kraaij, E; Vicente Barreto Pinto, M; Vila, I; Vogel Gonzalez, M; Vos, M; Vossebeld, J; Watson, M; Watson, N; Weber, M A; Weerts, H; Wells, J D; Weuste, L; Winter, A; Wojtoń, T; Xia, L; Xu, B; Żarnecki, A F; Zawiejski, L; Zgura, I-S

2017-01-01

The Compact Linear Collider (CLIC) is an option for a future [Formula: see text] collider operating at centre-of-mass energies up to [Formula: see text], providing sensitivity to a wide range of new physics phenomena and precision physics measurements at the energy frontier. This paper is the first comprehensive presentation of the Higgs physics reach of CLIC operating at three energy stages: [Formula: see text], 1.4 and [Formula: see text]. The initial stage of operation allows the study of Higgs boson production in Higgsstrahlung ([Formula: see text]) and [Formula: see text]-fusion ([Formula: see text]), resulting in precise measurements of the production cross sections, the Higgs total decay width [Formula: see text], and model-independent determinations of the Higgs couplings. Operation at [Formula: see text] provides high-statistics samples of Higgs bosons produced through [Formula: see text]-fusion, enabling tight constraints on the Higgs boson couplings. Studies of the rarer processes [Formula: see text] and [Formula: see text] allow measurements of the top Yukawa coupling and the Higgs boson self-coupling. This paper presents detailed studies of the precision achievable with Higgs measurements at CLIC and describes the interpretation of these measurements in a global fit.

Multiparameter Estimation in Networked Quantum Sensors

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

Proctor, Timothy J.; Knott, Paul A.; Dunningham, Jacob A.

We introduce a general model for a network of quantum sensors, and we use this model to consider the question: When can entanglement between the sensors, and/or global measurements, enhance the precision with which the network can measure a set of unknown parameters? We rigorously answer this question by presenting precise theorems proving that for a broad class of problems there is, at most, a very limited intrinsic advantage to using entangled states or global measurements. Moreover, for many estimation problems separable states and local measurements are optimal, and can achieve the ultimate quantum limit on the estimation uncertainty. Thismore » immediately implies that there are broad conditions under which simultaneous estimation of multiple parameters cannot outperform individual, independent estimations. Our results apply to any situation in which spatially localized sensors are unitarily encoded with independent parameters, such as when estimating multiple linear or non-linear optical phase shifts in quantum imaging, or when mapping out the spatial profile of an unknown magnetic field. We conclude by showing that entangling the sensors can enhance the estimation precision when the parameters of interest are global properties of the entire network.« less

Precision controlled atomic resolution scanning transmission electron microscopy using spiral scan pathways

NASA Astrophysics Data System (ADS)

Sang, Xiahan; Lupini, Andrew R.; Ding, Jilai; Kalinin, Sergei V.; Jesse, Stephen; Unocic, Raymond R.

2017-03-01

Atomic-resolution imaging in an aberration-corrected scanning transmission electron microscope (STEM) can enable direct correlation between atomic structure and materials functionality. The fast and precise control of the STEM probe is, however, challenging because the true beam location deviates from the assigned location depending on the properties of the deflectors. To reduce these deviations, i.e. image distortions, we use spiral scanning paths, allowing precise control of a sub-Å sized electron probe within an aberration-corrected STEM. Although spiral scanning avoids the sudden changes in the beam location (fly-back distortion) present in conventional raster scans, it is not distortion-free. “Archimedean” spirals, with a constant angular frequency within each scan, are used to determine the characteristic response at different frequencies. We then show that such characteristic functions can be used to correct image distortions present in more complicated constant linear velocity spirals, where the frequency varies within each scan. Through the combined application of constant linear velocity scanning and beam path corrections, spiral scan images are shown to exhibit less scan distortion than conventional raster scan images. The methodology presented here will be useful for in situ STEM imaging at higher temporal resolution and for imaging beam sensitive materials.

Precision controlled atomic resolution scanning transmission electron microscopy using spiral scan pathways.

PubMed

Sang, Xiahan; Lupini, Andrew R; Ding, Jilai; Kalinin, Sergei V; Jesse, Stephen; Unocic, Raymond R

2017-03-08

Atomic-resolution imaging in an aberration-corrected scanning transmission electron microscope (STEM) can enable direct correlation between atomic structure and materials functionality. The fast and precise control of the STEM probe is, however, challenging because the true beam location deviates from the assigned location depending on the properties of the deflectors. To reduce these deviations, i.e. image distortions, we use spiral scanning paths, allowing precise control of a sub-Å sized electron probe within an aberration-corrected STEM. Although spiral scanning avoids the sudden changes in the beam location (fly-back distortion) present in conventional raster scans, it is not distortion-free. "Archimedean" spirals, with a constant angular frequency within each scan, are used to determine the characteristic response at different frequencies. We then show that such characteristic functions can be used to correct image distortions present in more complicated constant linear velocity spirals, where the frequency varies within each scan. Through the combined application of constant linear velocity scanning and beam path corrections, spiral scan images are shown to exhibit less scan distortion than conventional raster scan images. The methodology presented here will be useful for in situ STEM imaging at higher temporal resolution and for imaging beam sensitive materials.

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

PubMed

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

2008-01-01

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

Multiparameter Estimation in Networked Quantum Sensors

DOE PAGES

Proctor, Timothy J.; Knott, Paul A.; Dunningham, Jacob A.

2018-02-21

We introduce a general model for a network of quantum sensors, and we use this model to consider the question: When can entanglement between the sensors, and/or global measurements, enhance the precision with which the network can measure a set of unknown parameters? We rigorously answer this question by presenting precise theorems proving that for a broad class of problems there is, at most, a very limited intrinsic advantage to using entangled states or global measurements. Moreover, for many estimation problems separable states and local measurements are optimal, and can achieve the ultimate quantum limit on the estimation uncertainty. Thismore » immediately implies that there are broad conditions under which simultaneous estimation of multiple parameters cannot outperform individual, independent estimations. Our results apply to any situation in which spatially localized sensors are unitarily encoded with independent parameters, such as when estimating multiple linear or non-linear optical phase shifts in quantum imaging, or when mapping out the spatial profile of an unknown magnetic field. We conclude by showing that entangling the sensors can enhance the estimation precision when the parameters of interest are global properties of the entire network.« less

Linear accelerator: a reproducible, efficacious and cost effective alternative for blood irradiation.

PubMed

Shastry, Shamee; Ramya, B; Ninan, Jefy; Srinidhi, G C; Bhat, Sudha S; Fernandes, Donald J

2013-12-01

The dedicated devices for blood irradiation are available only at a few centers in developing countries thus the irradiation remains a service with limited availability due to prohibitive cost. To implement a blood irradiation program at our center using linear accelerator. The study is performed detailing the specific operational and quality assurance measures employed in providing a blood component-irradiation service at tertiary care hospital. X-rays generated from linear accelerator were used to irradiate the blood components. To facilitate and standardize the blood component irradiation, a blood irradiator box was designed and fabricated in acrylic. Using Elekta Precise Linear Accelerator, a dose of 25 Gy was delivered at the centre of the irradiation box. Standardization was done using five units of blood obtained from healthy voluntary blood donors. Each unit was divided to two parts. One aliquot was subjected to irradiation. Biochemical and hematological parameters were analyzed on various days of storage. Cost incurred was analyzed. Progressive increase in plasma hemoglobin, potassium and lactate dehydrogenase was noted in the irradiated units but all the parameters were within the acceptable range indicating the suitability of the product for transfusion. The irradiation process was completed in less than 30 min. Validation of the radiation dose done using TLD showed less than ± 3% variation. This study shows that that the blood component irradiation is within the scope of most of the hospitals in developing countries even in the absence of dedicated blood irradiators at affordable cost. Copyright © 2013 Elsevier Ltd. All rights reserved.

High Performance Liquid Chromatography-Diode Array Detector Method for the Simultaneous Determination of Five Compounds in the Pulp and Seed of Sea Buckthorn.

PubMed

Zhao, Lu; Wen, E; Upur, Halmuart; Tian, Shuge

2017-01-01

Sea buckthorn ( Hippophae rhamnoides L.) as a traditional Chinese medicinal plant has various uses in Xinjiang. A reversed-phase rapid-resolution liquid-chromatography method with diode array detector was developed for simultaneous determination of protocatechuic acid, rutin, quercetin, kaempferol, and isorhamnetin in the pulp and seed of sea buckthorn, a widely used traditional Chinese medicine for promoting metabolism and treating scurvy and other diseases. Compounds were separated on an Agilent ZORBAX SB-C18 column (4.6 mm × 250 mm, 5 μm; USA) with gradient elution using methanol and 0.4% phosphoric acid (v/v) at 1.0 mL/min. Detection wavelength was set at 280 nm. The fruits of wild sea buckthorn were collected from Wushi County in Aksu, Xinjiang Province. The RSD of precision test of the five compounds were in the range of 0.60-2.22%, and the average recoveries ranged from 97.36% to 101.19%. Good linearity between specific chromatographic peak and component qualities were observed in the investigated ranges for all the analytes ( R 2 > 0.9997). The proposed method was successfully applied to determine the levels of five active components in sea buckthorn samples from Aksu in Xinjiang. The proposed method is simple, fast, sensitive, accurate, and suitable for quantitative assessment of the pulp and seed of sea buckthorn. Quantitative analysis method of protocatechuic acid, rutin, quercetin, kaempferol, and isorhamnetin in the extract of sea buckthorn pulp and seed is developed by high-performance liquid chromatography (HPLC) diode array detection.This method is simple and accurate; has strong specificity, good precision, and high recovery rate; and provides a reliable basis for further development of the substances in the pulp and seed of sea buckthorn.The method is widely used for content determination of active ingredients or physiologically active components in traditional Chinese medicine and its preparation Abbreviation used: PR: protocatechuic acid, RU: rutin, QU: quercetin, KA: kaempferol, IS: isorhamnetin, HPLC: high-performance liquid chromatography, HPLC-DAD: high performance liquid chromatographydiode array detector, LOD: linearity and limit of detection, LOQ: limit of quantitation, RSD: relative standard deviation.

Engineering and agronomy aspects of a long-term precision agriculture field experiment

USDA-ARS?s Scientific Manuscript database

Much research has been conducted on specific precision agriculture tools and implementation strategies, but little has been reported on long-term evaluation of integrated precision agriculture field experiments. In 2004 our research team developed and initiated a multi-faceted “precision agriculture...

High-performance Thin-layer Chromatography Method Development, Validation, and Simultaneous Quantification of Four Compounds Identified in Standardized Extracts of Orthosiphon stamineus.

PubMed

Hashim, Suzana; Beh, Hooi Kheng; Hamil, Mohamad Shahrul Ridzuan; Ismail, Zhari; Majid, Amin Malik Shah Abdul

2016-01-01

Orthosiphon stamineus is a medicinal herb widely grown in Southeast Asia and tropical countries. It has been used traditionally as a diuretic, abdominal pain, kidney and bladder inflammation, gout, and hypertension. This study aims to develop and validate the high-performance thin layer chromatography (HPTLC) method for quantification of rosmarinic acid (RA), 3'-hydroxy-5,6,7,4'-tetramethoxyflavone (TMF), sinensitin (SIN) and eupatorin (EUP) found in ethanol, 50% ethanol and water extract of O. stamineus leaves. HPTLC method was conducted using an HPTLC system with a developed mobile phase system of toluene: ethyl acetate: formic acid (3:7:0.1) performed on precoated silica gel 60 F254 TLC plates. The method was validated based on linearity, accuracy, precision, limit of detection, limit of quantification (LOQ), and specificity, respectively. The detection of spots was observed at ultraviolet 254 nm and 366 nm. The linearity of RA, TMF, SIN, and EUP were obtained between 10 and 100 ng/spot with high correlation coefficient value (R 2 ) of more than 0.986. The limit of detection was found to be 122.47 ± 3.95 (RA), 43.38 ± 0.79 (SIN), 17.26 ± 1.16 (TMF), and 46.80 ± 1.33 ng/spot (EUP), respectively. Whereas the LOQ was found to be 376.44 ± 6.70 (RA), 131.45 ± 2.39 (SIN), 52.30 ± 2.01 (TMF), and 141.82 ± 1.58 ng/spot (EUP), respectively. The proposed method showed good linearity, precision, accuracy, and high sensitivity. Hence, it may be applied in a routine quantification of RA, SIN, TMF, and EUP found in ethanol, 50% of ethanol and water extract of O. stamineus leaves. HPTLC method provides rapid estimation of the marker compound for routine quality control analysis.The established HPTLC method is rapid for qualitative and quantitative fingerprinting of Orthosiphon stamineus extract used for commercial product.Four identified markers (RA, SIN, EUP and TMF) found in three a different type of O. stamineus extracts specifically ethanol, 50% ethanol and water extract were successfully quantified using HPTLC method. Abbreviations Used : HPTLC: High-performance thin layer chromatography; RA: Rosmarinic acid; TMF: 3'-hydroxy-5,6,7,4'-tetramethoxyflavone; SIN: Sinensitin; EUP: Eupatorin; E: Ethanol; EW: 50% ethanol; W: Water; BK: Batu Kurau; KB: Kepala Batas; S: Sik; CJ: Changkat Jering; SB: Sungai Buloh.

Clinical performance of the LCx HCV RNA quantitative assay.

PubMed

Bertuzis, Rasa; Hardie, Alison; Hottentraeger, Barbara; Izopet, Jacques; Jilg, Wolfgang; Kaesdorf, Barbara; Leckie, Gregor; Leete, Jean; Perrin, Luc; Qiu, Chunfu; Ran, Iris; Schneider, George; Simmonds, Peter; Robinson, John

2005-02-01

This study was conducted to assess the performance of the Abbott laboratories LCx HCV RNA Quantitative Assay (LCx assay) in the clinical setting. Four clinical laboratories measured LCx assay precision, specificity, and linearity. In addition, a method comparison was conducted between the LCx assay and the Roche HCV Amplicor Monitor, version 2.0 (Roche Monitor 2.0) and the Bayer VERSANT HCV RNA 3.0 Assay (Bayer bDNA 3.0) quantitative assays. For precision, the observed LCx assay intra-assay standard deviation (S.D.) was 0.060-0.117 log IU/ml, the inter-assay S.D. was 0.083-0.133 log IU/ml, the inter-lot S.D. was 0.105-0.177 log IU/ml, the inter-site S.D. was 0.099-0.190 log IU/ml, and the total S.D. was 0.113-0.190 log IU/ml. The specificity of the LCx assay was 99.4% (542/545; 95% CI, 98.4-99.9%). For linearity, the mean pooled LCx assay results were linear (r=0.994) over the range of the panel (2.54-5.15 log IU/ml). A method comparison demonstrated a correlation coefficient of 0.881 between the LCx assay and Roche Monitor 2.0, 0.872 between the LCx assay and Bayer bDNA 3.0, and 0.870 between Roche Monitor 2.0 and Bayer bDNA 3.0. The mean LCx assay result was 0.04 log IU/ml (95% CI, -0.08, 0.01) lower than the mean Roche Monitor 2.0 result, but 0.57 log IU/ml (95% CI, 0.53, 0.61) higher than the mean Bayer bDNA 3.0 result. The mean Roche Monitor 2.0 result was 0.60 log IU/ml (95% CI, 0.56, 0.65) higher than the mean Bayer bDNA 3.0 result. The LCx assay quantitated genotypes 1-4 with statistical equivalency. The vast majority (98.9%, 278/281) of paired LCx assay-Roche Monitor 2.0 specimen results were within 1 log IU/ml. Similarly, 86.6% (240/277) of paired LCx assay and Bayer bDNA 3.0 specimen results were within 1 log, as were 85.6% (237/277) of paired Roche Monitor 2.0 and Bayer specimen results. These data demonstrate that the LCx assay may be used for quantitation of HCV RNA in HCV-infected individuals.

Deficits in Coordinative Bimanual Timing Precision in Children with Specific Language Impairment

ERIC Educational Resources Information Center

Vuolo, Janet; Goffman, Lisa; Zelaznik, Howard N.

2017-01-01

Purpose: Our objective was to delineate components of motor performance in specific language impairment (SLI); specifically, whether deficits in timing precision in one effector (unimanual tapping) and in two effectors (bimanual clapping) are observed in young children with SLI. Method: Twenty-seven 4- to 5-year-old children with SLI and 21…

Recombine Endostatin With Neoadjuvant Chemotherapy Followed by Concurrent Chemoradiation in Advanced Nasopharynx Cancer

ClinicalTrials.gov

2013-03-11

1、Enough Cases; 2、Elekta Precise 1343 Digital Control Electron Linear Accelerator; Can Undertake Nasopharyngeal Carcinoma Specimens in the Materia，; Image Department of Nose Pharynx Ministry MRI Dynamic Testing,

Propagation and stability characteristics of a 500-m-long laser-based fiducial line for high-precision alignment of long-distance linear accelerators.

PubMed

Suwada, Tsuyoshi; Satoh, Masanori; Telada, Souichi; Minoshima, Kaoru

2013-09-01

A laser-based alignment system with a He-Ne laser has been newly developed in order to precisely align accelerator units at the KEKB injector linac. The laser beam was first implemented as a 500-m-long fiducial straight line for alignment measurements. We experimentally investigated the propagation and stability characteristics of the laser beam passing through laser pipes in vacuum. The pointing stability at the last fiducial point was successfully obtained with the transverse displacements of ±40 μm level in one standard deviation by applying a feedback control. This pointing stability corresponds to an angle of ±0.08 μrad. This report contains a detailed description of the experimental investigation for the propagation and stability characteristics of the laser beam in the laser-based alignment system for long-distance linear accelerators.

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

PubMed

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

2016-01-01

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

Propagation and stability characteristics of a 500-m-long laser-based fiducial line for high-precision alignment of long-distance linear accelerators

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

Suwada, Tsuyoshi; Satoh, Masanori; Telada, Souichi

2013-09-15

A laser-based alignment system with a He-Ne laser has been newly developed in order to precisely align accelerator units at the KEKB injector linac. The laser beam was first implemented as a 500-m-long fiducial straight line for alignment measurements. We experimentally investigated the propagation and stability characteristics of the laser beam passing through laser pipes in vacuum. The pointing stability at the last fiducial point was successfully obtained with the transverse displacements of ±40 μm level in one standard deviation by applying a feedback control. This pointing stability corresponds to an angle of ±0.08 μrad. This report contains a detailedmore » description of the experimental investigation for the propagation and stability characteristics of the laser beam in the laser-based alignment system for long-distance linear accelerators.« less

Aircraft MSS data registration and vegetation classification of wetland change detection

USGS Publications Warehouse

Christensen, E.J.; Jensen, J.R.; Ramsey, Elijah W.; Mackey, H.E.

1988-01-01

Portions of the Savannah River floodplain swamp were evaluated for vegetation change using high resolution (5a??6 m) aircraft multispectral scanner (MSS) data. Image distortion from aircraft movement prevented precise image-to-image registration in some areas. However, when small scenes were used (200-250 ha), a first-order linear transformation provided registration accuracies of less than or equal to one pixel. A larger area was registered using a piecewise linear method. Five major wetland classes were identified and evaluated for change. Phenological differences and the variable distribution of vegetation limited wetland type discrimination. Using unsupervised methods and ground-collected vegetation data, overall classification accuracies ranged from 84 per cent to 87 per cent for each scene. Results suggest that high-resolution aircraft MSS data can be precisely registered, if small areas are used, and that wetland vegetation change can be accurately detected and monitored.

Accuracy of Intraoral Digital Impressions for Whole Upper Jaws, Including Full Dentitions and Palatal Soft Tissues.

PubMed

Gan, Ning; Xiong, Yaoyang; Jiao, Ting

2016-01-01

Intraoral digital impressions have been stated to meet the clinical requirements for some teeth-supported restorations, though fewer evidences were proposed for larger scanning range. The aim of this study was to compare the accuracy (trueness and precision) of intraoral digital impressions for whole upper jaws, including the full dentitions and palatal soft tissues, as well as to determine the effect of different palatal vault height or arch width on accuracy of intraoral digital impressions. Thirty-two volunteers were divided into three groups according to the palatal vault height or arch width. Each volunteer received three scans with TRIOS intraoral scanner and one conventional impression of whole upper jaw. Three-dimensional (3D) images digitized from conventional gypsum casts by a laboratory scanner were chose as the reference models. All datasets were imported to a specific software program for 3D analysis by "best fit alignment" and "3D compare" process. Color-coded deviation maps showed qualitative visualization of the deviations. For the digital impressions for palatal soft tissues, trueness was (130.54±33.95)μm and precision was (55.26±11.21)μm. For the digital impressions for upper full dentitions, trueness was (80.01±17.78)μm and precision was (59.52±11.29)μm. Larger deviations were found between intraoral digital impressions and conventional impressions in the areas of palatal soft tissues than that in the areas of full dentitions (p<0.001). Precision of digital impressions for palatal soft tissues was slightly better than that for full dentitions (p = 0.049). There was no significant effect of palatal vault height on accuracy of digital impressions for palatal soft tissues (p>0.05), but arch width was found to have a significant effect on precision of intraoral digital impressions for full dentitions (p = 0.016). A linear correlation was found between arch width and precision of digital impressions for whole upper jaws (r = 0.326, p = 0.034 for palatal soft tissues and r = 0.485, p = 0.002 for full dentitions). It was feasible to use the intraoral scanner to obtain digital impressions for whole upper jaws. Wider dental arch contributed to lower precision of an intraoral digital impression. It should be confirmed in further studies that whether accuracy of digital impressions for whole upper jaws is clinically acceptable.

A farm-level precision land management framework based on integer programming

PubMed Central

Li, Qi; Hu, Guiping; Jubery, Talukder Zaki; Ganapathysubramanian, Baskar

2017-01-01

Farmland management involves several planning and decision making tasks including seed selection and irrigation management. A farm-level precision farmland management model based on mixed integer linear programming is proposed in this study. Optimal decisions are designed for pre-season planning of crops and irrigation water allocation. The model captures the effect of size and shape of decision scale as well as special irrigation patterns. The authors illustrate the model with a case study on a farm in the state of California in the U.S. and show the model can capture the impact of precision farm management on profitability. The results show that threefold increase of annual net profit for farmers could be achieved by carefully choosing irrigation and seed selection. Although farmers could increase profits by applying precision management to seed or irrigation alone, profit increase is more significant if farmers apply precision management on seed and irrigation simultaneously. The proposed model can also serve as a risk analysis tool for farmers facing seasonal irrigation water limits as well as a quantitative tool to explore the impact of precision agriculture. PMID:28346499

Bit-Grooming: Shave Your Bits with Razor-sharp Precision

NASA Astrophysics Data System (ADS)

Zender, C. S.; Silver, J.

2017-12-01

Lossless compression can reduce climate data storage by 30-40%. Further reduction requires lossy compression that also reduces precision. Fortunately, geoscientific models and measurements generate false precision (scientifically meaningless data bits) that can be eliminated without sacrificing scientifically meaningful data. We introduce Bit Grooming, a lossy compression algorithm that removes the bloat due to false-precision, those bits and bytes beyond the meaningful precision of the data.Bit Grooming is statistically unbiased, applies to all floating point numbers, and is easy to use. Bit-Grooming reduces geoscience data storage requirements by 40-80%. We compared Bit Grooming to competitors Linear Packing, Layer Packing, and GRIB2/JPEG2000. The other compression methods have the edge in terms of compression, but Bit Grooming is the most accurate and certainly the most usable and portable.Bit Grooming provides flexible and well-balanced solutions to the trade-offs among compression, accuracy, and usability required by lossy compression. Geoscientists could reduce their long term storage costs, and show leadership in the elimination of false precision, by adopting Bit Grooming.

Influence of Waveform Characteristics on LiDAR Ranging Accuracy and Precision

PubMed Central

Yang, Bingwei; Xie, Xinhao; Li, Duan

2018-01-01

Time of flight (TOF) based light detection and ranging (LiDAR) is a technology for calculating distance between start/stop signals of time of flight. In lab-built LiDAR, two ranging systems for measuring flying time between start/stop signals include time-to-digital converter (TDC) that counts time between trigger signals and analog-to-digital converter (ADC) that processes the sampled start/stop pulses waveform for time estimation. We study the influence of waveform characteristics on range accuracy and precision of two kinds of ranging system. Comparing waveform based ranging (WR) with analog discrete return system based ranging (AR), a peak detection method (WR-PK) shows the best ranging performance because of less execution time, high ranging accuracy, and stable precision. Based on a novel statistic mathematical method maximal information coefficient (MIC), WR-PK precision has a high linear relationship with the received pulse width standard deviation. Thus keeping the received pulse width of measuring a constant distance as stable as possible can improve ranging precision. PMID:29642639

High-precision radius automatic measurement using laser differential confocal technology

NASA Astrophysics Data System (ADS)

Jiang, Hongwei; Zhao, Weiqian; Yang, Jiamiao; Guo, Yongkui; Xiao, Yang

2015-02-01

A high precision radius automatic measurement method using laser differential confocal technology is proposed. Based on the property of an axial intensity curve that the null point precisely corresponds to the focus of the objective and the bipolar property, the method uses the composite PID (proportional-integral-derivative) control to ensure the steady movement of the motor for process of quick-trigger scanning, and uses least-squares linear fitting to obtain the position of the cat-eye and confocal positions, then calculates the radius of curvature of lens. By setting the number of measure times, precision auto-repeat measurement of the radius of curvature is achieved. The experiment indicates that the method has the measurement accuracy of better than 2 ppm, and the measuring repeatability is better than 0.05 μm. In comparison with the existing manual-single measurement, this method has a high measurement precision, a strong environment anti-interference capability, a better measuring repeatability which is only tenth of former's.

Fabrication of micro-lens array on convex surface by meaning of micro-milling

NASA Astrophysics Data System (ADS)

Zhang, Peng; Du, Yunlong; Wang, Bo; Shan, Debin

2014-08-01

In order to develop the application of the micro-milling technology, and to fabricate ultra-precision optical surface with complex microstructure, in this paper, the primary experimental research on micro-milling complex microstructure array is carried out. A complex microstructure array surface with vary parameters is designed, and the mathematic model of the surface is set up and simulated. For the fabrication of the designed microstructure array surface, a micro three-axis ultra-precision milling machine tool is developed, aerostatic guideway drove directly by linear motor is adopted in order to guarantee the enough stiffness of the machine, and novel numerical control strategy with linear encoders of 5nm resolution used as the feedback of the control system is employed to ensure the extremely high motion control accuracy. With the help of CAD/CAM technology, convex micro lens array on convex spherical surface with different scales on material of polyvinyl chloride (PVC) and pure copper is fabricated using micro tungsten carbide ball end milling tool based on the ultra-precision micro-milling machine. Excellent nanometer-level micro-movement performance of the axis is proved by motion control experiment. The fabrication is nearly as the same as the design, the characteristic scale of the microstructure is less than 200μm and the accuracy is better than 1μm. It prove that ultra-precision micro-milling technology based on micro ultra-precision machine tool is a suitable and optional method for micro manufacture of microstructure array surface on different kinds of materials, and with the development of micro milling cutter, ultraprecision micro-milling complex microstructure surface will be achieved in future.

Validation of a method for quantitation of the clopidogrel active metabolite, clopidogrel, clopidogrel carboxylic acid, and 2-oxo-clopidogrel in feline plasma.

PubMed

Lyngby, Janne G; Court, Michael H; Lee, Pamela M

2017-08-01

The clopidogrel active metabolite (CAM) is unstable and challenging to quantitate. The objective was to validate a new method for stabilization and quantitation of CAM, clopidogrel, and the inactive metabolites clopidogrel carboxylic acid and 2-oxo-clopiodgrel in feline plasma. Two healthy cats administered clopidogrel to demonstrate assay in vivo utility. Stabilization of CAM was achieved by adding 2-bromo-3'methoxyacetophenone to blood tubes to form a derivatized CAM (CAM-D). Method validation included evaluation of calibration curve linearity, accuracy, and precision; within and between assay precision and accuracy; and compound stability using spiked blank feline plasma. Analytes were measured by high performance liquid chromatography with tandem mass spectrometry. In vivo utility was demonstrated by a pharmacokinetic study of cats given a single oral dose of 18.75mg clopidogrel. The 2-oxo-clopidogrel metabolite was unstable. Clopidogrel, CAM-D, and clopidogrel carboxylic acid appear stable for 1 week at room temperature and 9 months at -80°C. Standard curves showed linearity for CAM-D, clopidogrel, and clopidogrel carboxylic acid (r > 0.99). Between assay accuracy and precision was ≤2.6% and ≤7.1% for CAM-D and ≤17.9% and ≤11.3% for clopidogrel and clopidogrel carboxylic acid. Within assay precision for all three compounds was ≤7%. All three compounds were detected in plasma from healthy cats receiving clopidogrel. This methodology is accurate and precise for simultaneous quantitation of CAM-D, clopidogrel, and clopidogrel carboxylic acid in feline plasma but not 2-oxo-clopidogrel. Validation of this assay is the first step to more fully understanding the use of clopidogrel in cats. Copyright © 2017 Elsevier B.V. All rights reserved.

Defining a stem cell hierarchy in the intestine: markers, caveats and controversies

PubMed Central

Smith, Nicholas R.; Gallagher, Alexandra C.

2016-01-01

Abstract The past decade has appreciated rapid advance in identifying the once elusive intestinal stem cell (ISC) populations that fuel the continual renewal of the epithelial layer. This advance was largely driven by identification of novel stem cell marker genes, revealing the existence of quiescent, slowly‐ and active‐cycling ISC populations. However, a critical barrier for translating this knowledge to human health and disease remains elucidating the functional interplay between diverse stem cell populations. Currently, the precise hierarchical and regulatory relationships between these ISC populations are under intense scrutiny. The classical theory of a linear hierarchy, where quiescent and slowly‐cycling stem cells self‐renew but replenish an active‐cycling population, is well established in other rapidly renewing tissues such as the haematopoietic system. Efforts to definitively establish a similar stem cell hierarchy within the intestinal epithelium have yielded conflicting results, been difficult to interpret, and suggest non‐conventional alternatives to a linear hierarchy. While these new and potentially paradigm‐shifting discoveries are intriguing, the field will require development of a number of critical tools, including highly specific stem cell marker genes along with more rigorous experimental methodologies, to delineate the complex cellular relationships within this dynamic organ system. PMID:26864260

LC/MS/MS quantitation assay for pharmacokinetics of naringenin and double peaks phenomenon in rats plasma.

PubMed

Ma, Yan; Li, Peibo; Chen, Dawei; Fang, Tiezheng; Li, Haitian; Su, Weiwei

2006-01-13

A highly sensitive and specific electrospray ionization (ESI) liquid chromatography-tandem mass spectrometry (LC/MS/MS) method for quantitation of naringenin (NAR) and an explanation for the double peaks phenomenon was developed and validated. NAR was extracted from rat plasma and tissues along with the internal standard (IS), hesperidin, with ethyl acetate. The analytes were analyzed in the multiple-reaction-monitoring (MRM) mode as the precursor/product ion pair of m/z 273.4/151.3 for NAR and m/z 611.5/303.3 for the IS. The assay was linear over the concentration range of 5-2500 ng/mL. The lower limit quantification was 5 ng/mL, available for plasma pharmacokinetics of NAR in rats. Accuracy in within- and between-run precisions showed good reproducibility. When NAR was administered orally, only little and predominantly its glucuronidation were into circulation in the plasma. There existed double peaks phenomenon in plasma concentration-time curve leading to the relatively slow elimination of NAR in plasma. The results showed that there was a linear relationship between the AUC of total NAR and dosages. And the double peaks are mainly due to enterohepatic circulation.

Trace Level Determination of Mesityl Oxide and Diacetone Alcohol in Atazanavir Sulfate Drug Substance by a Gas Chromatography Method.

PubMed

Raju, K V S N; Pavan Kumar, K S R; Siva Krishna, N; Madhava Reddy, P; Sreenivas, N; Kumar Sharma, Hemant; Himabindu, G; Annapurna, N

2016-01-01

A capillary gas chromatography method with a short run time, using a flame ionization detector, has been developed for the quantitative determination of trace level analysis of mesityl oxide and diacetone alcohol in the atazanavir sulfate drug substance. The chromatographic method was achieved on a fused silica capillary column coated with 5% diphenyl and 95% dimethyl polysiloxane stationary phase (Rtx-5, 30 m x 0.53 mm x 5.0 µm). The run time was 20 min employing programmed temperature with a split mode (1:5) and was validated for specificity, sensitivity, precision, linearity, and accuracy. The detection and quantitation limits obtained for mesityl oxide and diacetone alcohol were 5 µg/g and 10 µg/g, respectively, for both of the analytes. The method was found to be linear in the range between 10 µg/g and 150 µg/g with a correlation coefficient greater than 0.999, and the average recoveries obtained in atazanavir sulfate were between 102.0% and 103.7%, respectively, for mesityl oxide and diacetone alcohol. The developed method was found to be robust and rugged. The detailed experimental results are discussed in this research paper.

Development and validation of a fast RP-HPLC method for determination of methotrexate entrapment efficiency in polymeric nanocapsules.

PubMed

Sartori, Tatiane; Seigi Murakami, Fabio; Pinheiro Cruz, Ariane; Machado de Campos, Angela

2008-07-01

A rapid and effective isocratic chromatographic procedure is successfully developed to determinate methotrexate (MTX) entrapment efficiency (EE) in polymeric nanocapsules using reversed-phase high-performance liquid chromatography. The method employed a RP-C(18) Shimadzu Shim-pack CLC-ODS (150 mm x 4.6 mm, 5 microm) column with mobile phase constituted by a mixture of water-acetonitrile-tetrahydrofuran (65:30:5 v/v/v; pH 3.0) at a flow rate of 0.8 mL/min. The eluate is monitored with a UV detector set at 313 nm. The parameters used in the validation process are: linearity, specificity, precision, accuracy, and limit of quantitation (LOQ). The linearity is evaluated by a calibration curve in the concentration range of 10-50 microg/mL and presented a correlation coefficient of 0.9998. The polymers (PLA or PLA-PEG), oil, and surfactants used in the nanocapsule formulation did not interfere with analysis and the recovery was quantitative. The intra and inter-day assay relative standard deviation were less than 0.72%. Results are satisfactory, and the method proved to be adequate for the determination of methotrexate in nanocapsules formulations.

Relationship between tribology and optics in thin films of mechanically oriented nanocrystals.

PubMed

Wong, Liana; Hu, Chunhua; Paradise, Ruthanne; Zhu, Zina; Shtukenberg, Alexander; Kahr, Bart

2012-07-25

Many crystalline dyes, when rubbed unidirectionally with cotton on glass slides, can be organized as thin films of highly aligned nanocrystals. Commonly, the linear birefringence and linear dichroism of these films resemble the optical properties of single crystals, indicating precisely oriented particles. Of 186 colored compounds, 122 showed sharp extinction and 50 were distinctly linearly dichroic. Of the latter 50 compounds, 88% were more optically dense when linearly polarized light was aligned with the rubbing axis. The mechanical properties of crystals that underlie the nonstatistical correlation between tribological processes and the direction of electron oscillations in absorption bands are discussed. The features that give rise to the orientation of dye crystallites naturally extend to colorless molecular crystals.

A linearly frequency-swept high-speed-rate multi-wavelength laser for optical coherence tomography

NASA Astrophysics Data System (ADS)

Wang, Qiyu; Wang, Zhaoying; Yuan, Quan; Ma, Rui; Du, Tao; Yang, Tianxin

2017-02-01

We proposed and demonstrated a linearly frequency-swept multi-wavelength laser source for optical coherence tomography (OCT) eliminating the need of wavenumber space resampling in the postprocessing progress. The source consists of a multi-wavelength fiber laser source (MFS) and an optical sweeping loop. In this novel laser source, an equally spaced multi-wavelength laser is swept simultaneously by a certain step each time in the frequency domain in the optical sweeping loop. The sweeping step is determined by radio frequency (RF) signal which can be precisely controlled. Thus the sweeping behavior strictly maintains a linear relationship between time and frequency. We experimentally achieved linear time-frequency sweeping at a sweeping rate of 400 kHz with our laser source.

Axial calibration methods of piezoelectric load sharing dynamometer

NASA Astrophysics Data System (ADS)

Zhang, Jun; Chang, Qingbing; Ren, Zongjin; Shao, Jun; Wang, Xinlei; Tian, Yu

2018-06-01

The relationship between input and output of load sharing dynamometer is seriously non-linear in different loading points of a plane, so it's significant for accutately measuring force to precisely calibrate the non-linear relationship. In this paper, firstly, based on piezoelectric load sharing dynamometer, calibration experiments of different loading points are performed in a plane. And then load sharing testing system is respectively calibrated based on BP algorithm and ELM (Extreme Learning Machine) algorithm. Finally, the results show that the calibration result of ELM is better than BP for calibrating the non-linear relationship between input and output of loading sharing dynamometer in the different loading points of a plane, which verifies that ELM algorithm is feasible in solving force non-linear measurement problem.

Physics with e{sup +}e{sup -} Linear Colliders

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

Barklow, Timothy L

2003-05-05

We describe the physics potential of e{sup +}e{sup -} linear colliders in this report. These machines are planned to operate in the first phase at a center-of-mass energy of 500 GeV, before being scaled up to about 1 TeV. In the second phase of the operation, a final energy of about 2 TeV is expected. The machines will allow us to perform precision tests of the heavy particles in the Standard Model, the top quark and the electroweak bosons. They are ideal facilities for exploring the properties of Higgs particles, in particular in the intermediate mass range. New vector bosonsmore » and novel matter particles in extended gauge theories can be searched for and studied thoroughly. The machines provide unique opportunities for the discovery of particles in supersymmetric extensions of the Standard Model, the spectrum of Higgs particles, the supersymmetric partners of the electroweak gauge and Higgs bosons, and of the matter particles. High precision analyses of their properties and interactions will allow for extrapolations to energy scales close to the Planck scale where gravity becomes significant. In alternative scenarios, like compositeness models, novel matter particles and interactions can be discovered and investigated in the energy range above the existing colliders up to the TeV scale. Whatever scenario is realized in Nature, the discovery potential of e{sup +}e{sup -} linear colliders and the high-precision with which the properties of particles and their interactions can be analyzed, define an exciting physics programme complementary to hadron machines.« less

Macroeconomic effects on mortality revealed by panel analysis with nonlinear trends.

PubMed

Ionides, Edward L; Wang, Zhen; Tapia Granados, José A

2013-10-03

Many investigations have used panel methods to study the relationships between fluctuations in economic activity and mortality. A broad consensus has emerged on the overall procyclical nature of mortality: perhaps counter-intuitively, mortality typically rises above its trend during expansions. This consensus has been tarnished by inconsistent reports on the specific age groups and mortality causes involved. We show that these inconsistencies result, in part, from the trend specifications used in previous panel models. Standard econometric panel analysis involves fitting regression models using ordinary least squares, employing standard errors which are robust to temporal autocorrelation. The model specifications include a fixed effect, and possibly a linear trend, for each time series in the panel. We propose alternative methodology based on nonlinear detrending. Applying our methodology on data for the 50 US states from 1980 to 2006, we obtain more precise and consistent results than previous studies. We find procyclical mortality in all age groups. We find clear procyclical mortality due to respiratory disease and traffic injuries. Predominantly procyclical cardiovascular disease mortality and countercyclical suicide are subject to substantial state-to-state variation. Neither cancer nor homicide have significant macroeconomic association.

Macroeconomic effects on mortality revealed by panel analysis with nonlinear trends

PubMed Central

Ionides, Edward L.; Wang, Zhen; Tapia Granados, José A.

2013-01-01

Many investigations have used panel methods to study the relationships between fluctuations in economic activity and mortality. A broad consensus has emerged on the overall procyclical nature of mortality: perhaps counter-intuitively, mortality typically rises above its trend during expansions. This consensus has been tarnished by inconsistent reports on the specific age groups and mortality causes involved. We show that these inconsistencies result, in part, from the trend specifications used in previous panel models. Standard econometric panel analysis involves fitting regression models using ordinary least squares, employing standard errors which are robust to temporal autocorrelation. The model specifications include a fixed effect, and possibly a linear trend, for each time series in the panel. We propose alternative methodology based on nonlinear detrending. Applying our methodology on data for the 50 US states from 1980 to 2006, we obtain more precise and consistent results than previous studies. We find procyclical mortality in all age groups. We find clear procyclical mortality due to respiratory disease and traffic injuries. Predominantly procyclical cardiovascular disease mortality and countercyclical suicide are subject to substantial state-to-state variation. Neither cancer nor homicide have significant macroeconomic association. PMID:24587843

Spatial and temporal Brook Trout density dynamics: Implications for conservation, management, and monitoring

USGS Publications Warehouse

Wagner, Tyler; Jefferson T. Deweber,; Jason Detar,; Kristine, David; John A. Sweka,

2014-01-01

Many potential stressors to aquatic environments operate over large spatial scales, prompting the need to assess and monitor both site-specific and regional dynamics of fish populations. We used hierarchical Bayesian models to evaluate the spatial and temporal variability in density and capture probability of age-1 and older Brook Trout Salvelinus fontinalis from three-pass removal data collected at 291 sites over a 37-year time period (1975–2011) in Pennsylvania streams. There was high between-year variability in density, with annual posterior means ranging from 2.1 to 10.2 fish/100 m2; however, there was no significant long-term linear trend. Brook Trout density was positively correlated with elevation and negatively correlated with percent developed land use in the network catchment. Probability of capture did not vary substantially across sites or years but was negatively correlated with mean stream width. Because of the low spatiotemporal variation in capture probability and a strong correlation between first-pass CPUE (catch/min) and three-pass removal density estimates, the use of an abundance index based on first-pass CPUE could represent a cost-effective alternative to conducting multiple-pass removal sampling for some Brook Trout monitoring and assessment objectives. Single-pass indices may be particularly relevant for monitoring objectives that do not require precise site-specific estimates, such as regional monitoring programs that are designed to detect long-term linear trends in density.

HPTLC and Spectrophotometric Estimation of Febuxostat and Diclofenac Potassium in Their Combined Tablets.

PubMed

El-Yazbi, Fawzi A; Amin, Omayma A; El-Kimary, Eman I; Khamis, Essam F; Younis, Sameh E

2016-08-01

An accurate, precise, rapid, specific and economic high-performance thin-layer chromatographic (HPTLC) method has been developed for the simultaneous quantitative determination of febuxostat (FEB) and diclofenac potassium (DIC). The chromatographic separation was performed on precoated silica gel 60 GF254 plates with chloroform-methanol 7:3 (v/v) as the mobile phase. The developed plates were scanned and quantified at 289 nm. Experimental conditions including band size, mobile phase composition and chamber-saturation time were critically studied, and the optimum conditions were selected. A satisfactory resolution (Rs = 2.67) with RF 0.48 and 0.69 and high sensitivity with limits of detection of 4 and 7 ng/band for FEB and DIC, respectively, were obtained. In addition, derivative ratio and ratio difference spectrophotometric methods were established for the analysis of such a mixture. All methods were validated as per the ICH guidelines. In the HPTLC method, the calibration plots were linear between 0.01-0.55 and 0.02-0.60 µg/band, for FEB and DIC, respectively. For the spectrophotometric methods, the calibration graphs were linear between 2-14 and 4-18 µg/mL for FEB and DIC, respectively. The simplicity and specificity of the proposed methods suggest their application in quality control analysis of FEB and DIC in their raw materials and tablets. A comparison of the proposed methods with the existing methods is presented. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

A strategy for simultaneous determination of fatty acid composition, fatty acid position, and position-specific isotope contents in triacylglycerol matrices by 13C-NMR.

PubMed

Merchak, Noelle; Silvestre, Virginie; Loquet, Denis; Rizk, Toufic; Akoka, Serge; Bejjani, Joseph

2017-01-01

Triacylglycerols, which are quasi-universal components of food matrices, consist of complex mixtures of molecules. Their site-specific 13 C content, their fatty acid profile, and their position on the glycerol moiety may significantly vary with the geographical, botanical, or animal origin of the sample. Such variables are valuable tracers for food authentication issues. The main objective of this work was to develop a new method based on a rapid and precise 13 C-NMR spectroscopy (using a polarization transfer technique) coupled with multivariate linear regression analyses in order to quantify the whole set of individual fatty acids within triacylglycerols. In this respect, olive oil samples were analyzed by means of both adiabatic 13 C-INEPT sequence and gas chromatography (GC). For each fatty acid within the studied matrix and for squalene as well, a multivariate prediction model was constructed using the deconvoluted peak areas of 13 C-INEPT spectra as predictors, and the data obtained by GC as response variables. This 13 C-NMR-based strategy, tested on olive oil, could serve as an alternative to the gas chromatographic quantification of individual fatty acids in other matrices, while providing additional compositional and isotopic information. Graphical abstract A strategy based on the multivariate linear regression of variables obtained by a rapid 13 C-NMR technique was developed for the quantification of individual fatty acids within triacylglycerol matrices. The conceived strategy was tested on olive oil.

Practical controller design for ultra-precision positioning of stages with a pneumatic artificial muscle actuator

NASA Astrophysics Data System (ADS)

Tang, T. F.; Chong, S. H.

2017-06-01

This paper presents a practical controller design method for ultra-precision positioning of pneumatic artificial muscle actuator stages. Pneumatic artificial muscle (PAM) actuators are safe to use and have numerous advantages which have brought these actuators to wide applications. However, PAM exhibits strong non-linear characteristics, and these limitations lead to low controllability and limit its application. In practice, the non-linear characteristics of PAM mechanism are difficult to be precisely modeled, and time consuming to model them accurately. The purpose of the present study is to clarify a practical controller design method that emphasizes a simple design procedure that does not acquire plants parameters modeling, and yet is able to demonstrate ultra-precision positioning performance for a PAM driven stage. The practical control approach adopts continuous motion nominal characteristic trajectory following (CM NCTF) control as the feedback controller. The constructed PAM driven stage is in low damping characteristic and causes severe residual vibration that deteriorates motion accuracy of the system. Therefore, the idea to increase the damping characteristic by having an acceleration feedback compensation to the plant has been proposed. The effectiveness of the proposed controller was verified experimentally and compared with a classical PI controller in point-to-point motion. The experiment results proved that the CM NCTF controller demonstrates better positioning performance in smaller motion error than the PI controller. Overall, the CM NCTF controller has successfully to reduce motion error to 3µm, which is 88.7% smaller than the PI controller.

Accuracy and precision of polyurethane dental arch models fabricated using a three-dimensional subtractive rapid prototyping method with an intraoral scanning technique.

PubMed

Kim, Jae-Hong; Kim, Ki-Baek; Kim, Woong-Chul; Kim, Ji-Hwan; Kim, Hae-Young

2014-03-01

This study aimed to evaluate the accuracy and precision of polyurethane (PUT) dental arch models fabricated using a three-dimensional (3D) subtractive rapid prototyping (RP) method with an intraoral scanning technique by comparing linear measurements obtained from PUT models and conventional plaster models. Ten plaster models were duplicated using a selected standard master model and conventional impression, and 10 PUT models were duplicated using the 3D subtractive RP technique with an oral scanner. Six linear measurements were evaluated in terms of x, y, and z-axes using a non-contact white light scanner. Accuracy was assessed using mean differences between two measurements, and precision was examined using four quantitative methods and the Bland-Altman graphical method. Repeatability was evaluated in terms of intra-examiner variability, and reproducibility was assessed in terms of inter-examiner and inter-method variability. The mean difference between plaster models and PUT models ranged from 0.07 mm to 0.33 mm. Relative measurement errors ranged from 2.2% to 7.6% and intraclass correlation coefficients ranged from 0.93 to 0.96, when comparing plaster models and PUT models. The Bland-Altman plot showed good agreement. The accuracy and precision of PUT dental models for evaluating the performance of oral scanner and subtractive RP technology was acceptable. Because of the recent improvements in block material and computerized numeric control milling machines, the subtractive RP method may be a good choice for dental arch models.

Similarity of scattering rates in metals showing T-linear resistivity.

PubMed

Bruin, J A N; Sakai, H; Perry, R S; Mackenzie, A P

2013-02-15

Many exotic compounds, such as cuprate superconductors and heavy fermion materials, exhibit a linear in temperature (T) resistivity, the origin of which is not well understood. We found that the resistivity of the quantum critical metal Sr(3)Ru(2)O(7) is also T-linear at the critical magnetic field of 7.9 T. Using the precise existing data for the Fermi surface topography and quasiparticle velocities of Sr(3)Ru(2)O(7), we show that in the region of the T-linear resistivity, the scattering rate per kelvin is well approximated by the ratio of the Boltzmann constant to the Planck constant divided by 2π. Extending the analysis to a number of other materials reveals similar results in the T-linear region, in spite of large differences in the microscopic origins of the scattering.

LINEAR AND NONLINEAR CORRECTIONS IN THE RHIC INTERACTION REGIONS.

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

PILAT,F.; CAMERON,P.; PTITSYN,V.

2002-06-02

A method has been developed to measure operationally the linear and non-linear effects of the interaction region triplets, that gives access to the multipole content through the action kick, by applying closed orbit bumps and analysing tune and orbit shifts. This technique has been extensively tested and used during the RHIC operations in 2001. Measurements were taken at 3 different interaction regions and for different focusing at the interaction point. Non-linear effects up to the dodecapole have been measured as well as the effects of linear, sextupolar and octupolar corrections. An analysis package for the data processing has been developedmore » that through a precise fit of the experimental tune shift data (measured by a phase lock loop technique to better than 10{sup -5} resolution) determines the multipole content of an IR triplet.« less

Quantum algorithms for Gibbs sampling and hitting-time estimation

DOE PAGES

Chowdhury, Anirban Narayan; Somma, Rolando D.

2017-02-01

In this paper, we present quantum algorithms for solving two problems regarding stochastic processes. The first algorithm prepares the thermal Gibbs state of a quantum system and runs in time almost linear in √Nβ/Ζ and polynomial in log(1/ϵ), where N is the Hilbert space dimension, β is the inverse temperature, Ζ is the partition function, and ϵ is the desired precision of the output state. Our quantum algorithm exponentially improves the dependence on 1/ϵ and quadratically improves the dependence on β of known quantum algorithms for this problem. The second algorithm estimates the hitting time of a Markov chain. Formore » a sparse stochastic matrix Ρ, it runs in time almost linear in 1/(ϵΔ 3/2), where ϵ is the absolute precision in the estimation and Δ is a parameter determined by Ρ, and whose inverse is an upper bound of the hitting time. Our quantum algorithm quadratically improves the dependence on 1/ϵ and 1/Δ of the analog classical algorithm for hitting-time estimation. Finally, both algorithms use tools recently developed in the context of Hamiltonian simulation, spectral gap amplification, and solving linear systems of equations.« less