Shock compression modeling of metallic single crystals: comparison of finite difference, steady wave, and analytical solutions

DOE PAGES

Lloyd, Jeffrey T.; Clayton, John D.; Austin, Ryan A.; ...

2015-07-10

Background: The shock response of metallic single crystals can be captured using a micro-mechanical description of the thermoelastic-viscoplastic material response; however, using a such a description within the context of traditional numerical methods may introduce a physical artifacts. Advantages and disadvantages of complex material descriptions, in particular the viscoplastic response, must be framed within approximations introduced by numerical methods. Methods: Three methods of modeling the shock response of metallic single crystals are summarized: finite difference simulations, steady wave simulations, and algebraic solutions of the Rankine-Hugoniot jump conditions. For the former two numerical techniques, a dislocation density based framework describes themore » rate- and temperature-dependent shear strength on each slip system. For the latter analytical technique, a simple (two-parameter) rate- and temperature-independent linear hardening description is necessarily invoked to enable simultaneous solution of the governing equations. For all models, the same nonlinear thermoelastic energy potential incorporating elastic constants of up to order 3 is applied. Results: Solutions are compared for plate impact of highly symmetric orientations (all three methods) and low symmetry orientations (numerical methods only) of aluminum single crystals shocked to 5 GPa (weak shock regime) and 25 GPa (overdriven regime). Conclusions: For weak shocks, results of the two numerical methods are very similar, regardless of crystallographic orientation. For strong shocks, artificial viscosity affects the finite difference solution, and effects of transverse waves for the lower symmetry orientations not captured by the steady wave method become important. The analytical solution, which can only be applied to highly symmetric orientations, provides reasonable accuracy with regards to prediction of most variables in the final shocked state but, by construction, does not provide insight into the shock structure afforded by the numerical methods.« less

Simultaneous analysis of multiple classes of antimicrobials in environmental water samples using SPE coupled with UHPLC-ESI-MS/MS and isotope dilution.

PubMed

Tran, Ngoc Han; Chen, Hongjie; Do, Thanh Van; Reinhard, Martin; Ngo, Huu Hao; He, Yiliang; Gin, Karina Yew-Hoong

2016-10-01

A robust and sensitive analytical method was developed for the simultaneous analysis of 21 target antimicrobials in different environmental water samples. Both single SPE and tandem SPE cartridge systems were investigated to simultaneously extract multiple classes of antimicrobials. Experimental results showed that good extraction efficiencies (84.5-105.6%) were observed for the vast majority of the target analytes when extraction was performed using the tandem SPE cartridge (SB+HR-X) system under an extraction pH of 3.0. HPLC-MS/MS parameters were optimized for simultaneous analysis of all the target analytes in a single injection. Quantification of target antimicrobials in water samples was accomplished using 15 isotopically labeled internal standards (ILISs), which allowed the efficient compensation of the losses of target analytes during sample preparation and correction of matrix effects during UHPLC-MS/MS as well as instrument fluctuations in MS/MS signal intensity. Method quantification limit (MQL) for most target analytes based on SPE was below 5ng/L for surface waters, 10ng/L for treated wastewater effluents, and 15ng/L for raw wastewater. The method was successfully applied to detect and quantify the occurrence of the target analytes in raw influent, treated effluent and surface water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Analytical and molecular dynamics studies on the impact loading of single-layered graphene sheet by fullerene

NASA Astrophysics Data System (ADS)

Hosseini-Hashemi, Shahrokh; Sepahi-Boroujeni, Amin; Sepahi-Boroujeni, Saeid

2018-04-01

Normal impact performance of a system including a fullerene molecule and a single-layered graphene sheet is studied in the present paper. Firstly, through a mathematical approach, a new contact law is derived to describe the overall non-bonding interaction forces of the "hollow indenter-target" system. Preliminary verifications show that the derived contact law gives a reliable picture of force field of the system which is in good agreements with the results of molecular dynamics (MD) simulations. Afterwards, equation of the transversal motion of graphene sheet is utilized on the basis of both the nonlocal theory of elasticity and the assumptions of classical plate theory. Then, to derive dynamic behavior of the system, a set including the proposed contact law and the equations of motion of both graphene sheet and fullerene molecule is solved numerically. In order to evaluate outcomes of this method, the problem is modeled by MD simulation. Despite intrinsic differences between analytical and MD methods as well as various errors arise due to transient nature of the problem, acceptable agreements are established between analytical and MD outcomes. As a result, the proposed analytical method can be reliably used to address similar impact problems. Furthermore, it is found that a single-layered graphene sheet is capable of trapping fullerenes approaching with low velocities. Otherwise, in case of rebound, the sheet effectively absorbs predominant portion of fullerene energy.

Single-cell MALDI-MS as an analytical tool for studying intrapopulation metabolic heterogeneity of unicellular organisms.

PubMed

Amantonico, Andrea; Urban, Pawel L; Fagerer, Stephan R; Balabin, Roman M; Zenobi, Renato

2010-09-01

Heterogeneity is a characteristic feature of all populations of living organisms. Here we make an attempt to validate a single-cell mass spectrometric method for detection of changes in metabolite levels occurring in populations of unicellular organisms. Selected metabolites involved in central metabolism (ADP, ATP, GTP, and UDP-Glucose) could readily be detected in single cells of Closterium acerosum by means of negative-mode matrix-assisted laser desorption/ionization (MALDI) mass spectrometry (MS). The analytical capabilities of this approach were characterized using standard compounds. The method was then used to study populations of individual cells with different levels of the chosen metabolites. With principal component analysis and support vector machine algorithms, it was possible to achieve a clear separation of individual C. acerosum cells in different metabolic states. This study demonstrates the suitability of mass spectrometric analysis of metabolites in single cells to measure cell-population heterogeneity.

Documentation of spreadsheets for the analysis of aquifer-test and slug-test data

USGS Publications Warehouse

Halford, Keith J.; Kuniansky, Eve L.

2002-01-01

Several spreadsheets have been developed for the analysis of aquifer-test and slug-test data. Each spreadsheet incorporates analytical solution(s) of the partial differential equation for ground-water flow to a well for a specific type of condition or aquifer. The derivations of the analytical solutions were previously published. Thus, this report abbreviates the theoretical discussion, but includes practical information about each method and the important assumptions for the applications of each method. These spreadsheets were written in Microsoft Excel 9.0 (use of trade names does not constitute endorsement by the USGS). Storage properties should not be estimated with many of the spreadsheets because most are for analyzing single-well tests. Estimation of storage properties from single-well tests is generally discouraged because single-well tests are affected by wellbore storage and by well construction. These non-ideal effects frequently cause estimates of storage to be erroneous by orders of magnitude. Additionally, single-well tests are not sensitive to aquifer-storage properties. Single-well tests include all slug tests (Bouwer and Rice Method, Cooper, Bredehoeft, Papadopulos Method, and van der Kamp Method), the Cooper-Jacob straight-line Method, Theis recovery-data analysis, Jacob-Lohman method for flowing wells in a confined aquifer, and the step-drawdown test. Multi-well test spreadsheets included in this report are; Hantush-Jacob Leaky Aquifer Method and Distance-Drawdown Methods. The distance-drawdown method is an equilibrium or steady-state method, thus storage cannot be estimated.

A technique for setting analytical thresholds in massively parallel sequencing-based forensic DNA analysis

PubMed Central

2017-01-01

Amplicon (targeted) sequencing by massively parallel sequencing (PCR-MPS) is a potential method for use in forensic DNA analyses. In this application, PCR-MPS may supplement or replace other instrumental analysis methods such as capillary electrophoresis and Sanger sequencing for STR and mitochondrial DNA typing, respectively. PCR-MPS also may enable the expansion of forensic DNA analysis methods to include new marker systems such as single nucleotide polymorphisms (SNPs) and insertion/deletions (indels) that currently are assayable using various instrumental analysis methods including microarray and quantitative PCR. Acceptance of PCR-MPS as a forensic method will depend in part upon developing protocols and criteria that define the limitations of a method, including a defensible analytical threshold or method detection limit. This paper describes an approach to establish objective analytical thresholds suitable for multiplexed PCR-MPS methods. A definition is proposed for PCR-MPS method background noise, and an analytical threshold based on background noise is described. PMID:28542338

A technique for setting analytical thresholds in massively parallel sequencing-based forensic DNA analysis.

PubMed

Young, Brian; King, Jonathan L; Budowle, Bruce; Armogida, Luigi

2017-01-01

Amplicon (targeted) sequencing by massively parallel sequencing (PCR-MPS) is a potential method for use in forensic DNA analyses. In this application, PCR-MPS may supplement or replace other instrumental analysis methods such as capillary electrophoresis and Sanger sequencing for STR and mitochondrial DNA typing, respectively. PCR-MPS also may enable the expansion of forensic DNA analysis methods to include new marker systems such as single nucleotide polymorphisms (SNPs) and insertion/deletions (indels) that currently are assayable using various instrumental analysis methods including microarray and quantitative PCR. Acceptance of PCR-MPS as a forensic method will depend in part upon developing protocols and criteria that define the limitations of a method, including a defensible analytical threshold or method detection limit. This paper describes an approach to establish objective analytical thresholds suitable for multiplexed PCR-MPS methods. A definition is proposed for PCR-MPS method background noise, and an analytical threshold based on background noise is described.

SSD for R: A Comprehensive Statistical Package to Analyze Single-System Data

ERIC Educational Resources Information Center

Auerbach, Charles; Schudrich, Wendy Zeitlin

2013-01-01

The need for statistical analysis in single-subject designs presents a challenge, as analytical methods that are applied to group comparison studies are often not appropriate in single-subject research. "SSD for R" is a robust set of statistical functions with wide applicability to single-subject research. It is a comprehensive package…

Simultaneous quantitative analysis of main components in linderae reflexae radix with one single marker.

PubMed

Wang, Li-Li; Zhang, Yun-Bin; Sun, Xiao-Ya; Chen, Sui-Qing

2016-05-08

Establish a quantitative analysis of multi-components by the single marker (QAMS) method for quality evaluation and validate its feasibilities by the simultaneous quantitative assay of four main components in Linderae Reflexae Radix. Four main components of pinostrobin, pinosylvin, pinocembrin, and 3,5-dihydroxy-2-(1- p -mentheneyl)- trans -stilbene were selected as analytes to evaluate the quality by RP-HPLC coupled with a UV-detector. The method was evaluated by a comparison of the quantitative results between the external standard method and QAMS with a different HPLC system. The results showed that no significant differences were found in the quantitative results of the four contents of Linderae Reflexae Radix determined by the external standard method and QAMS (RSD <3%). The contents of four analytes (pinosylvin, pinocembrin, pinostrobin, and Reflexanbene I) in Linderae Reflexae Radix were determined by the single marker of pinosylvin. This fingerprint was the spectra determined by Shimadzu LC-20AT and Waters e2695 HPLC that were equipped with three different columns.

Sampling and analysis for radon-222 dissolved in ground water and surface water

USGS Publications Warehouse

DeWayne, Cecil L.; Gesell, T.F.

1992-01-01

Radon-222 is a naturally occurring radioactive gas in the uranium-238 decay series that has traditionally been called, simply, radon. The lung cancer risks associated with the inhalation of radon decay products have been well documented by epidemiological studies on populations of uranium miners. The realization that radon is a public health hazard has raised the need for sampling and analytical guidelines for field personnel. Several sampling and analytical methods are being used to document radon concentrations in ground water and surface water worldwide but no convenient, single set of guidelines is available. Three different sampling and analytical methods - bubbler, liquid scintillation, and field screening - are discussed in this paper. The bubbler and liquid scintillation methods have high accuracy and precision, and small analytical method detection limits of 0.2 and 10 pCi/l (picocuries per liter), respectively. The field screening method generally is used as a qualitative reconnaissance tool.

Empirical evaluation of meta-analytic approaches for nutrient and health outcome dose-response data

USDA-ARS?s Scientific Manuscript database

The objective of this study is to empirically compare alternative meta-analytic methods for combining dose-response data from epidemiological studies. We identified meta-analyses of epidemiological studies that analyzed the association between a single nutrient and a dichotomous outcome. For each to...

Nine-analyte detection using an array-based biosensor

NASA Technical Reports Server (NTRS)

Taitt, Chris Rowe; Anderson, George P.; Lingerfelt, Brian M.; Feldstein, s. Mark. J.; Ligler, Frances S.

2002-01-01

A fluorescence-based multianalyte immunosensor has been developed for simultaneous analysis of multiple samples. While the standard 6 x 6 format of the array sensor has been used to analyze six samples for six different analytes, this same format has the potential to allow a single sample to be tested for 36 different agents. The method described herein demonstrates proof of principle that the number of analytes detectable using a single array can be increased simply by using complementary mixtures of capture and tracer antibodies. Mixtures were optimized to allow detection of closely related analytes without significant cross-reactivity. Following this facile modification of patterning and assay procedures, the following nine targets could be detected in a single 3 x 3 array: Staphylococcal enterotoxin B, ricin, cholera toxin, Bacillus anthracis Sterne, Bacillus globigii, Francisella tularensis LVS, Yersiniapestis F1 antigen, MS2 coliphage, and Salmonella typhimurium. This work maximizes the efficiency and utility of the described array technology, increasing only reagent usage and cost; production and fabrication costs are not affected.

Process-Hardened, Multi-Analyte Sensor for Characterizing Rocket Plume Constituents

NASA Technical Reports Server (NTRS)

Goswami, Kisholoy

2011-01-01

A multi-analyte sensor was developed that enables simultaneous detection of rocket engine combustion-product molecules in a launch-vehicle ground test stand. The sensor was developed using a pin-printing method by incorporating multiple sensor elements on a single chip. It demonstrated accurate and sensitive detection of analytes such as carbon dioxide, carbon monoxide, kerosene, isopropanol, and ethylene from a single measurement. The use of pin-printing technology enables high-volume fabrication of the sensor chip, which will ultimately eliminate the need for individual sensor calibration since many identical sensors are made in one batch. Tests were performed using a single-sensor chip attached to a fiber-optic bundle. The use of a fiber bundle allows placement of the opto-electronic readout device at a place remote from the test stand. The sensors are rugged for operation in harsh environments.

Analytical and Numerical Results for an Adhesively Bonded Joint Subjected to Pure Bending

NASA Technical Reports Server (NTRS)

Smeltzer, Stanley S., III; Lundgren, Eric

2006-01-01

A one-dimensional, semi-analytical methodology that was previously developed for evaluating adhesively bonded joints composed of anisotropic adherends and adhesives that exhibit inelastic material behavior is further verified in the present paper. A summary of the first-order differential equations and applied joint loading used to determine the adhesive response from the methodology are also presented. The method was previously verified against a variety of single-lap joint configurations from the literature that subjected the joints to cases of axial tension and pure bending. Using the same joint configuration and applied bending load presented in a study by Yang, the finite element analysis software ABAQUS was used to further verify the semi-analytical method. Linear static ABAQUS results are presented for two models, one with a coarse and one with a fine element meshing, that were used to verify convergence of the finite element analyses. Close agreement between the finite element results and the semi-analytical methodology were determined for both the shear and normal stress responses of the adhesive bondline. Thus, the semi-analytical methodology was successfully verified using the ABAQUS finite element software and a single-lap joint configuration subjected to pure bending.

A method of mounting multiple otoliths for beam-based microchemical analyses

USGS Publications Warehouse

Donohoe, C.J.; Zimmerman, C.E.

2010-01-01

Beam-based analytical methods are widely used to measure the concentrations of elements and isotopes in otoliths. These methods usually require that otoliths be individually mounted and prepared to properly expose the desired growth region to the analytical beam. Most analytical instruments, such as LA-ICPMS and ion and electron microprobes, have sample holders that will accept only one to six slides or mounts at a time. We describe a method of mounting otoliths that allows for easy transfer of many otoliths to a single mount after they have been prepared. Such an approach increases the number of otoliths that can be analyzed in a single session by reducing the need open the sample chamber to exchange slides-a particularly time consuming step on instruments that operate under vacuum. For ion and electron microprobes, the method also greatly reduces the number of slides that must be coated with an electrical conductor prior to analysis. In this method, a narrow strip of cover glass is first glued at one end to a standard microscope slide. The otolith is then mounted in thermoplastic resin on the opposite, free end of the strip. The otolith can then be ground and flipped, if needed, by reheating the mounting medium. After otolith preparation is complete, the cover glass is cut with a scribe to free the otolith and up to 20 small otoliths can be arranged on a single petrographic slide. ?? 2010 The Author(s).

HEATED PURGE AND TRAP METHOD DEVELOPMENT AND TESTING

EPA Science Inventory

The goal of the research was to develop a heated purge and trap method that could be used in conjunction with SW-846 method 8240 for the analysis of volatile, water soluble Appendix VIII analytes. The developed method was validated according to a partial single laboratory method ...

Nondestructive assessment of single-span timber bridges using a vibration- based method

Treesearch

Xiping Wang; James P. Wacker; Angus M. Morison; John W. Forsman; John R. Erickson; Robert J. Ross

2005-01-01

This paper describes an effort to develop a global dynamic testing technique for evaluating the overall stiffness of timber bridge superstructures. A forced vibration method was used to measure the natural frequency of single-span timber bridges in the laboratory and field. An analytical model based on simple beam theory was proposed to represent the relationship...

An Analytical Method To Compute Comet Cloud Formation Efficiency And Its Application

NASA Astrophysics Data System (ADS)

Brasser, Ramon; Duncan, M. J.

2007-07-01

A quick analytical method is presented for calculating comet cloud formation efficiency in the case of a single planet or multiple-planet system for planets that are not too eccentric (e_p < 0.2). A method to calculate the fraction of comets that stay under the control of each planet is also presented. The location of the planet(s) in mass-semi-major axis space to form a comet cloud is constrained based on the conditions developed by Tremaine (1993) together with estimates of the likelihood of passing comets between planets; and, in the case of a single, eccentric planet, the additional constraint that it is, by itself, able to accelerate material to lower values of Tisserand parameter within the age of the stellar system without sweeping up the majority of the material beforehand. For a single planet, it turns out the efficiency is mainly a function of planetary mass and semi-major axis of the planet and density of the stellar environment. The theory has been applied to some extrasolar systems and compared to numerical simulations for both these systems and the Solar system, as well as a diffusion scheme based on the energy kick distribution of Everhart (1968). Results agree well with analytical predictions.

Reviews of Single Subject Research Designs: Applications to Special Education and School Psychology

ERIC Educational Resources Information Center

Nevin, Ann I., Ed.

2004-01-01

The authors of this collection of research reviews studied how single subject research designs might be a useful method to apply as part of being accountable to clients. The single subject research studies were evaluated in accordance with the following criteria: Was the study applied, behavioral, reliable, analytic, effective, and generalizable?…

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of selected carbamate pesticides in water by high-performance liquid chromatography

USGS Publications Warehouse

Werner, S.L.; Johnson, S.M.

1994-01-01

As part of its primary responsibility concerning water as a national resource, the U.S. Geological Survey collects and analyzes samples of ground water and surface water to determine water quality. This report describes the method used since June 1987 to determine selected total-recoverable carbamate pesticides present in water samples. High- performance liquid chromatography is used to separate N-methyl carbamates, N-methyl carbamoyloximes, and an N-phenyl carbamate which have been extracted from water and concentrated in dichloromethane. Analytes, surrogate compounds, and reference compounds are eluted from the analytical column within 25 minutes. Two modes of analyte detection are used: (1) a photodiode-array detector measures and records ultraviolet-absorbance profiles, and (2) a fluorescence detector measures and records fluorescence from an analyte derivative produced when analyte hydrolysis is combined with chemical derivatization. Analytes are identified and confirmed in a three-stage process by use of chromatographic retention time, ultraviolet (UV) spectral comparison, and derivatization/fluorescence detection. Quantitative results are based on the integration of single-wavelength UV-absorbance chromatograms and on comparison with calibration curves derived from external analyte standards that are run with samples as part of an instrumental analytical sequence. Estimated method detection limits vary for each analyte, depending on the sample matrix conditions, and range from 0.5 microgram per liter to as low as 0.01 microgram per liter. Reporting levels for all analytes have been set at 0.5 microgram per liter for this method. Corrections on the basis of percentage recoveries of analytes spiked into distilled water are not applied to values calculated for analyte concentration in samples. These values for analyte concentrations instead indicate the quantities recovered by the method from a particular sample matrix.

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

PubMed

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

2015-01-15

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

On the calculation of resonances by analytic continuation of eigenvalues from the stabilization graph

NASA Astrophysics Data System (ADS)

Haritan, Idan; Moiseyev, Nimrod

2017-07-01

Resonances play a major role in a large variety of fields in physics and chemistry. Accordingly, there is a growing interest in methods designed to calculate them. Recently, Landau et al. proposed a new approach to analytically dilate a single eigenvalue from the stabilization graph into the complex plane. This approach, termed Resonances Via Padé (RVP), utilizes the Padé approximant and is based on a unique analysis of the stabilization graph. Yet, analytic continuation of eigenvalues from the stabilization graph into the complex plane is not a new idea. In 1975, Jordan suggested an analytic continuation method based on the branch point structure of the stabilization graph. The method was later modified by McCurdy and McNutt, and it is still being used today. We refer to this method as the Truncated Characteristic Polynomial (TCP) method. In this manuscript, we perform an in-depth comparison between the RVP and the TCP methods. We demonstrate that while both methods are important and complementary, the advantage of one method over the other is problem-dependent. Illustrative examples are provided in the manuscript.

A simple and fast method for computing the relativistic Compton Scattering Kernel for radiative transfer

NASA Technical Reports Server (NTRS)

Kershaw, David S.; Prasad, Manoj K.; Beason, J. Douglas

1986-01-01

The Klein-Nishina differential cross section averaged over a relativistic Maxwellian electron distribution is analytically reduced to a single integral, which can then be rapidly evaluated in a variety of ways. A particularly fast method for numerically computing this single integral is presented. This is, to the authors' knowledge, the first correct computation of the Compton scattering kernel.

Molecular counting of membrane receptor subunits with single-molecule localization microscopy

NASA Astrophysics Data System (ADS)

Krüger, Carmen; Fricke, Franziska; Karathanasis, Christos; Dietz, Marina S.; Malkusch, Sebastian; Hummer, Gerhard; Heilemann, Mike

2017-02-01

We report on quantitative single-molecule localization microscopy, a method that next to super-resolved images of cellular structures provides information on protein copy numbers in protein clusters. This approach is based on the analysis of blinking cycles of single fluorophores, and on a model-free description of the distribution of the number of blinking events. We describe the experimental and analytical procedures, present cellular data of plasma membrane proteins and discuss the applicability of this method.

Empirical Evaluation of Meta-Analytic Approaches for Nutrient and Health Outcome Dose-Response Data

ERIC Educational Resources Information Center

Yu, Winifred W.; Schmid, Christopher H.; Lichtenstein, Alice H.; Lau, Joseph; Trikalinos, Thomas A.

2013-01-01

The objective of this study is to empirically compare alternative meta-analytic methods for combining dose-response data from epidemiological studies. We identified meta-analyses of epidemiological studies that analyzed the association between a single nutrient and a dichotomous outcome. For each topic, we performed meta-analyses of odds ratios…

Group specific internal standard technology (GSIST) for simultaneous identification and quantification of small molecules

DOEpatents

Adamec, Jiri; Yang, Wen-Chu; Regnier, Fred E

2014-01-14

Reagents and methods are provided that permit simultaneous analysis of multiple diverse small molecule analytes present in a complex mixture. Samples are labeled with chemically identical but isotopically distince forms of the labeling reagent, and analyzed using mass spectrometry. A single reagent simultaneously derivatizes multiple small molecule analytes having different reactive functional groups.

An analytical method of estimating turbine performance

NASA Technical Reports Server (NTRS)

Kochendorfer, Fred D; Nettles, J Cary

1949-01-01

A method is developed by which the performance of a turbine over a range of operating conditions can be analytically estimated from the blade angles and flow areas. In order to use the method, certain coefficients that determine the weight flow and the friction losses must be approximated. The method is used to calculate the performance of the single-stage turbine of a commercial aircraft gas-turbine engine and the calculated performance is compared with the performance indicated by experimental data. For the turbine of the typical example, the assumed pressure losses and the tuning angles give a calculated performance that represents the trends of the experimental performance with reasonable accuracy. The exact agreement between analytical performance and experimental performance is contingent upon the proper selection of a blading-loss parameter.

Analysis of multiple mycotoxins in food.

PubMed

Hajslova, Jana; Zachariasova, Milena; Cajka, Tomas

2011-01-01

Mycotoxins are secondary metabolites of microscopic filamentous fungi. With regard to the widespread distribution of fungi in the environment, mycotoxins are considered to be one of the most important natural contaminants in foods and feeds. To protect consumers' health and reduce economic losses, surveillance and control of mycotoxins in food and feed has become a major objective for producers, regulatory authorities, and researchers worldwide. In this context, availability of reliable analytical methods applicable for this purpose is essential. Since the variety of chemical structures of mycotoxins makes impossible to use one single technique for their analysis, a vast number of analytical methods has been developed and validated. Both a large variability of food matrices and growing demands for a fast, cost-saving and accurate determination of multiple mycotoxins by a single method outline new challenges for analytical research. This strong effort is facilitated by technical developments in mass spectrometry allowing decreasing the influence of matrix effects in spite of omitting sample clean-up step. The current state-of-the-art together with future trends is presented in this chapter. Attention is focused mainly on instrumental method; advances in biosensors and other screening bioanalytical approaches enabling analysis of multiple mycotoxins are not discussed in detail.

Generalized model of electromigration with 1:1 (analyte:selector) complexation stoichiometry: part I. Theory.

PubMed

Dubský, Pavel; Müllerová, Ludmila; Dvořák, Martin; Gaš, Bohuslav

2015-03-06

The model of electromigration of a multivalent weak acidic/basic/amphoteric analyte that undergoes complexation with a mixture of selectors is introduced. The model provides an extension of the series of models starting with the single-selector model without dissociation by Wren and Rowe in 1992, continuing with the monovalent weak analyte/single-selector model by Rawjee, Williams and Vigh in 1993 and that by Lelièvre in 1994, and ending with the multi-selector overall model without dissociation developed by our group in 2008. The new multivalent analyte multi-selector model shows that the effective mobility of the analyte obeys the original Wren and Row's formula. The overall complexation constant, mobility of the free analyte and mobility of complex can be measured and used in a standard way. The mathematical expressions for the overall parameters are provided. We further demonstrate mathematically that the pH dependent parameters for weak analytes can be simply used as an input into the multi-selector overall model and, in reverse, the multi-selector overall parameters can serve as an input into the pH-dependent models for the weak analytes. These findings can greatly simplify the rationale method development in analytical electrophoresis, specifically enantioseparations. Copyright © 2015 Elsevier B.V. All rights reserved.

One-calibrant kinetic calibration for on-site water sampling with solid-phase microextraction.

PubMed

Ouyang, Gangfeng; Cui, Shufen; Qin, Zhipei; Pawliszyn, Janusz

2009-07-15

The existing solid-phase microextraction (SPME) kinetic calibration technique, using the desorption of the preloaded standards to calibrate the extraction of the analytes, requires that the physicochemical properties of the standard should be similar to those of the analyte, which limited the application of the technique. In this study, a new method, termed the one-calibrant kinetic calibration technique, which can use the desorption of a single standard to calibrate all extracted analytes, was proposed. The theoretical considerations were validated by passive water sampling in laboratory and rapid water sampling in the field. To mimic the variety of the environment, such as temperature, turbulence, and the concentration of the analytes, the flow-through system for the generation of standard aqueous polycyclic aromatic hydrocarbons (PAHs) solution was modified. The experimental results of the passive samplings in the flow-through system illustrated that the effect of the environmental variables was successfully compensated with the kinetic calibration technique, and all extracted analytes can be calibrated through the desorption of a single calibrant. On-site water sampling with rotated SPME fibers also illustrated the feasibility of the new technique for rapid on-site sampling of hydrophobic organic pollutants in water. This technique will accelerate the application of the kinetic calibration method and also will be useful for other microextraction techniques.

Development and application of accurate analytical models for single active electron potentials

NASA Astrophysics Data System (ADS)

Miller, Michelle; Jaron-Becker, Agnieszka; Becker, Andreas

2015-05-01

The single active electron (SAE) approximation is a theoretical model frequently employed to study scenarios in which inner-shell electrons may productively be treated as frozen spectators to a physical process of interest, and accurate analytical approximations for these potentials are sought as a useful simulation tool. Density function theory is often used to construct a SAE potential, requiring that a further approximation for the exchange correlation functional be enacted. In this study, we employ the Krieger, Li, and Iafrate (KLI) modification to the optimized-effective-potential (OEP) method to reduce the complexity of the problem to the straightforward solution of a system of linear equations through simple arguments regarding the behavior of the exchange-correlation potential in regions where a single orbital dominates. We employ this method for the solution of atomic and molecular potentials, and use the resultant curve to devise a systematic construction for highly accurate and useful analytical approximations for several systems. Supported by the U.S. Department of Energy (Grant No. DE-FG02-09ER16103), and the U.S. National Science Foundation (Graduate Research Fellowship, Grants No. PHY-1125844 and No. PHY-1068706).

A Semi-Analytical Method for Determining the Energy Release Rate of Cracks in Adhesively-Bonded Single-Lap Composite Joints

NASA Technical Reports Server (NTRS)

Yang, Charles; Sun, Wenjun; Tomblin, John S.; Smeltzer, Stanley S., III

2007-01-01

A semi-analytical method for determining the strain energy release rate due to a prescribed interface crack in an adhesively-bonded, single-lap composite joint subjected to axial tension is presented. The field equations in terms of displacements within the joint are formulated by using first-order shear deformable, laminated plate theory together with kinematic relations and force equilibrium conditions. The stress distributions for the adherends and adhesive are determined after the appropriate boundary and loading conditions are applied and the equations for the field displacements are solved. Based on the adhesive stress distributions, the forces at the crack tip are obtained and the strain energy release rate of the crack is determined by using the virtual crack closure technique (VCCT). Additionally, the test specimen geometry from both the ASTM D3165 and D1002 test standards are utilized during the derivation of the field equations in order to correlate analytical models with future test results. The system of second-order differential field equations is solved to provide the adherend and adhesive stress response using the symbolic computation tool, Maple 9. Finite element analyses using J-integral as well as VCCT were performed to verify the developed analytical model. The finite element analyses were conducted using the commercial finite element analysis software ABAQUS. The results determined using the analytical method correlated well with the results from the finite element analyses.

Medio-lateral Knee Fluency in Anterior Cruciate Ligament-Injured Athletes During Dynamic Movement Trials

PubMed Central

Panos, Joseph A.; Hoffman, Joshua T.; Wordeman, Samuel C.; Hewett, Timothy E.

2016-01-01

Background Correction of neuromuscular impairments after anterior cruciate ligament injury is vital to successful return to sport. Frontal plane knee control during landing is a common measure of lower-extremity neuromuscular control and asymmetries in neuromuscular control of the knee can predispose injured athletes to additional injury and associated morbidities. Therefore, this study investigated the effects of anterior cruciate ligament injury on knee biomechanics during landing. Methods Two-dimensional frontal plane video of single leg drop, cross over drop, and drop vertical jump dynamic movement trials was analyzed for twenty injured and reconstructed athletes. The position of the knee joint center was tracked in ImageJ software for 500 milliseconds after landing to calculate medio-lateral knee motion velocities and determine normal fluency, the number of times per second knee velocity changed direction. The inverse of this calculation, analytical fluency, was used to associate larger numerical values with fluent movement. Findings Analytical fluency was decreased in involved limbs for single leg drop trials (P=0.0018). Importantly, analytical fluency for single leg drop differed compared to cross over drop trials for involved (P<0.001), but not uninvolved limbs (P=0.5029). For involved limbs, analytical fluency values exhibited a stepwise trend in relative magnitudes. Interpretation Decreased analytical fluency in involved limbs is consistent with previous studies. Fluency asymmetries observed during single leg drop tasks may be indicative of abhorrent landing strategies in the involved limb. Analytical fluency differences in unilateral tasks for injured limbs may represent neuromuscular impairment as a result of injury. PMID:26895446

How Much Can We Learn from a Single Chromatographic Experiment? A Bayesian Perspective.

PubMed

Wiczling, Paweł; Kaliszan, Roman

2016-01-05

In this work, we proposed and investigated a Bayesian inference procedure to find the desired chromatographic conditions based on known analyte properties (lipophilicity, pKa, and polar surface area) using one preliminary experiment. A previously developed nonlinear mixed effect model was used to specify the prior information about a new analyte with known physicochemical properties. Further, the prior (no preliminary data) and posterior predictive distribution (prior + one experiment) were determined sequentially to search towards the desired separation. The following isocratic high-performance reversed-phase liquid chromatographic conditions were sought: (1) retention time of a single analyte within the range of 4-6 min and (2) baseline separation of two analytes with retention times within the range of 4-10 min. The empirical posterior Bayesian distribution of parameters was estimated using the "slice sampling" Markov Chain Monte Carlo (MCMC) algorithm implemented in Matlab. The simulations with artificial analytes and experimental data of ketoprofen and papaverine were used to test the proposed methodology. The simulation experiment showed that for a single and two randomly selected analytes, there is 97% and 74% probability of obtaining a successful chromatogram using none or one preliminary experiment. The desired separation for ketoprofen and papaverine was established based on a single experiment. It was confirmed that the search for a desired separation rarely requires a large number of chromatographic analyses at least for a simple optimization problem. The proposed Bayesian-based optimization scheme is a powerful method of finding a desired chromatographic separation based on a small number of preliminary experiments.

Solid-phase microfibers based on polyethylene glycol modified single-walled carbon nanotubes for the determination of chlorinated organic carriers in textiles.

PubMed

Zhang, Wei-Ya; Sun, Yin; Wang, Cheng-Ming; Wu, Cai-Ying

2011-09-01

Based on polyethylene glycol modified single-walled carbon nanotubes, a novel sol-gel fiber coating was prepared and applied to the headspace microextraction of chlorinated organic carriers (COCs) in textiles by gas chromatography-electron capture detection. The preparation of polyethylene glycol modified single-walled carbon nanotubes and the sol-gel fiber coating process was stated and confirmed by infrared spectra, Raman spectroscopy, and scanning electron microscopy. Several parameters affecting headspace microextraction, including extraction temperature, extraction time, salting-out effect, and desorption time, were optimized by detecting 11 COCs in simulative sweat samples. Compared with the commercial solid-phase microextraction fibers, the sol-gel polyethylene glycol modified single-walled carbon nanotubes fiber showed higher extraction efficiency, better thermal stability, and longer life span. The method detection limits for COCs were in the range from 0.02 to 7.5 ng L(-1) (S/N = 3). The linearity of the developed method varied from 0.001 to 50 μg L(-1) for all analytes, with coefficients of correlation greater than 0.974. The developed method was successfully applied to the analysis of trace COCs in textiles, the recoveries of the analytes indicated that the developed method was considerably useful for the determination of COCs in ecological textile samples.

Single-Case Experimental Designs: A Systematic Review of Published Research and Current Standards

PubMed Central

Smith, Justin D.

2013-01-01

This article systematically reviews the research design and methodological characteristics of single-case experimental design (SCED) research published in peer-reviewed journals between 2000 and 2010. SCEDs provide researchers with a flexible and viable alternative to group designs with large sample sizes. However, methodological challenges have precluded widespread implementation and acceptance of the SCED as a viable complementary methodology to the predominant group design. This article includes a description of the research design, measurement, and analysis domains distinctive to the SCED; a discussion of the results within the framework of contemporary standards and guidelines in the field; and a presentation of updated benchmarks for key characteristics (e.g., baseline sampling, method of analysis), and overall, it provides researchers and reviewers with a resource for conducting and evaluating SCED research. The results of the systematic review of 409 studies suggest that recently published SCED research is largely in accordance with contemporary criteria for experimental quality. Analytic method emerged as an area of discord. Comparison of the findings of this review with historical estimates of the use of statistical analysis indicates an upward trend, but visual analysis remains the most common analytic method and also garners the most support amongst those entities providing SCED standards. Although consensus exists along key dimensions of single-case research design and researchers appear to be practicing within these parameters, there remains a need for further evaluation of assessment and sampling techniques and data analytic methods. PMID:22845874

U/Th dating by SHRIMP RG ion-microprobe mass spectrometry using single ion-exchange beads

NASA Astrophysics Data System (ADS)

Bischoff, James L.; Wooden, Joe; Murphy, Fred; Williams, Ross W.

2005-04-01

We present a new analytical method for U-series isotopes using the SHRIMP RG (Sensitive High mass Resolution Ion MicroProbe) mass spectrometer that utilizes the preconcentration of the U-series isotopes from a sample onto a single ion-exchange bead. Ion-microprobe mass spectrometry is capable of producing Th ionization efficiencies in excess of 2%. Analytical precision is typically better than alpha spectroscopy, but not as good as thermal ionization mass spectroscopy (TIMS) and inductively coupled plasma multicollector mass spectrometry (ICP-MS). Like TIMS and ICP-MS the method allows analysis of small samples sizes, but also adds the advantage of rapidity of analysis. A major advantage of ion-microprobe analysis is that U and Th isotopes are analyzed in the same bead, simplifying the process of chemical separation. Analytical time on the instrument is ˜60 min per sample, and a single instrument-loading can accommodate 15-20 samples to be analyzed in a 24-h day. An additional advantage is that the method allows multiple reanalyses of the same bead and that samples can be archived for reanalysis at a later time. Because the ion beam excavates a pit only a few μm deep, the mount can later be repolished and reanalyzed numerous times. The method described of preconcentrating a low concentration sample onto a small conductive substrate to allow ion-microprobe mass spectrometry is potentially applicable to many other systems.

U/Th dating by SHRIMP RG ion-microprobe mass spectrometry using single ion-exchange beads

USGS Publications Warehouse

Bischoff, J.L.; Wooden, J.; Murphy, F.; Williams, Ross W.

2005-01-01

We present a new analytical method for U-series isotopes using the SHRIMP RG (Sensitive High mass Resolution Ion MicroProbe) mass spectrometer that utilizes the preconcentration of the U-series isotopes from a sample onto a single ion-exchange bead. Ion-microprobe mass spectrometry is capable of producing Th ionization efficiencies in excess of 2%. Analytical precision is typically better than alpha spectroscopy, but not as good as thermal ionization mass spectroscopy (TIMS) and inductively coupled plasma multicollector mass spectrometry (ICP-MS). Like TIMS and ICP-MS the method allows analysis of small samples sizes, but also adds the advantage of rapidity of analysis. A major advantage of ion-microprobe analysis is that U and Th isotopes are analyzed in the same bead, simplifying the process of chemical separation. Analytical time on the instrument is ???60 min per sample, and a single instrument-loading can accommodate 15-20 samples to be analyzed in a 24-h day. An additional advantage is that the method allows multiple reanalyses of the same bead and that samples can be archived for reanalysis at a later time. Because the ion beam excavates a pit only a few ??m deep, the mount can later be repolished and reanalyzed numerous times. The method described of preconcentrating a low concentration sample onto a small conductive substrate to allow ion-microprobe mass spectrometry is potentially applicable to many other systems. Copyright ?? 2005 Elsevier Ltd.

Screening Methods for Metal-Containing Nanoparticles in Water

EPA Science Inventory

Screening-level analysis of water for metal-containing nanoparticles is achieved with single particle-inductively coupled plasma mass spectrometry (SP-ICPMS). This method measures both the concentration of nanoparticles containing an analyte metal and the mass of the metal in eac...

Single Cell Proteomics in Biomedicine: High-dimensional Data Acquisition, Visualization and Analysis

PubMed Central

Su, Yapeng; Shi, Qihui; Wei, Wei

2017-01-01

New insights on cellular heterogeneity in the last decade provoke the development of a variety of single cell omics tools at a lightning pace. The resultant high-dimensional single cell data generated by these tools require new theoretical approaches and analytical algorithms for effective visualization and interpretation. In this review, we briefly survey the state-of-the-art single cell proteomic tools with a particular focus on data acquisition and quantification, followed by an elaboration of a number of statistical and computational approaches developed to date for dissecting the high-dimensional single cell data. The underlying assumptions, unique features and limitations of the analytical methods with the designated biological questions they seek to answer will be discussed. Particular attention will be given to those information theoretical approaches that are anchored in a set of first principles of physics and can yield detailed (and often surprising) predictions. PMID:28128880

Replica Analysis for Portfolio Optimization with Single-Factor Model

NASA Astrophysics Data System (ADS)

Shinzato, Takashi

2017-06-01

In this paper, we use replica analysis to investigate the influence of correlation among the return rates of assets on the solution of the portfolio optimization problem. We consider the behavior of an optimal solution for the case where the return rate is described with a single-factor model and compare the findings obtained from our proposed methods with correlated return rates with those obtained with independent return rates. We then analytically assess the increase in the investment risk when correlation is included. Furthermore, we also compare our approach with analytical procedures for minimizing the investment risk from operations research.

An analytical method to compute comet cloud formation efficiency and its application

NASA Astrophysics Data System (ADS)

Brasser, Ramon; Duncan, Martin J.

2008-01-01

A quick analytical method is presented for calculating comet cloud formation efficiency in the case of a single planet or multiple-planet system for planets that are not too eccentric ( e p ≲ 0.3). A method to calculate the fraction of comets that stay under the control of each planet is also presented, as well as a way to determine the efficiency in different star cluster environments. The location of the planet(s) in mass-semi-major axis space to form a comet cloud is constrained based on the conditions developed by Tremaine (1993) together with estimates of the likelyhood of passing comets between planets; and, in the case of a single, eccentric planet, the additional constraint that it is, by itself, able to accelerate material to relative encounter velocity U ~ 0.4 within the age of the stellar system without sweeping up the majority of the material beforehand. For a single planet, it turns out the efficiency is mainly a function of planetary mass and semi-major axis of the planet and density of the stellar environment. The theory has been applied to some extrasolar systems and compared to numerical simulations for both these systems and the Solar System, as well as a diffusion scheme based on the energy kick distribution of Everhart (Astron J 73:1039 1052, 1968). The analytic results are in good agreement with the simulations.

Detection, characterization and quantification of inorganic engineered nanomaterials: A review of techniques and methodological approaches for the analysis of complex samples.

PubMed

Laborda, Francisco; Bolea, Eduardo; Cepriá, Gemma; Gómez, María T; Jiménez, María S; Pérez-Arantegui, Josefina; Castillo, Juan R

2016-01-21

The increasing demand of analytical information related to inorganic engineered nanomaterials requires the adaptation of existing techniques and methods, or the development of new ones. The challenge for the analytical sciences has been to consider the nanoparticles as a new sort of analytes, involving both chemical (composition, mass and number concentration) and physical information (e.g. size, shape, aggregation). Moreover, information about the species derived from the nanoparticles themselves and their transformations must also be supplied. Whereas techniques commonly used for nanoparticle characterization, such as light scattering techniques, show serious limitations when applied to complex samples, other well-established techniques, like electron microscopy and atomic spectrometry, can provide useful information in most cases. Furthermore, separation techniques, including flow field flow fractionation, capillary electrophoresis and hydrodynamic chromatography, are moving to the nano domain, mostly hyphenated to inductively coupled plasma mass spectrometry as element specific detector. Emerging techniques based on the detection of single nanoparticles by using ICP-MS, but also coulometry, are in their way to gain a position. Chemical sensors selective to nanoparticles are in their early stages, but they are very promising considering their portability and simplicity. Although the field is in continuous evolution, at this moment it is moving from proofs-of-concept in simple matrices to methods dealing with matrices of higher complexity and relevant analyte concentrations. To achieve this goal, sample preparation methods are essential to manage such complex situations. Apart from size fractionation methods, matrix digestion, extraction and concentration methods capable of preserving the nature of the nanoparticles are being developed. This review presents and discusses the state-of-the-art analytical techniques and sample preparation methods suitable for dealing with complex samples. Single- and multi-method approaches applied to solve the nanometrological challenges posed by a variety of stakeholders are also presented. Copyright © 2015 Elsevier B.V. All rights reserved.

Single excitation-emission fluorescence spectrum (EEF) for determination of cetane improver in diesel fuel.

PubMed

Insausti, Matías; Fernández Band, Beatriz S

2015-04-05

A highly sensitive spectrofluorimetric method has been developed for the determination of 2-ethylhexyl nitrate in diesel fuel. Usually, this compound is used as an additive in order to improve cetane number. The analytical method consists in building the chemometric model as a first step. Then, it is possible to quantify the analyte with only recording a single excitation-emission fluorescence spectrum (EEF), whose data are introduced in the chemometric model above mentioned. Another important characteristic of this method is that the fuel sample was used without any pre-treatment for EEF. This work provides an interest improvement to fluorescence techniques using the rapid and easily applicable EEF approach to analyze such complex matrices. Exploding EEF was the key to a successful determination, obtaining a detection limit of 0.00434% (v/v) and a limit of quantification of 0.01446% (v/v). Copyright © 2015 Elsevier B.V. All rights reserved.

Interlaboratory comparability, bias, and precision for four laboratories measuring constituents in precipitation, November 1982-August 1983

USGS Publications Warehouse

Brooks, M.H.; Schroder, L.J.; Malo, B.A.

1985-01-01

Four laboratories were evaluated in their analysis of identical natural and simulated precipitation water samples. Interlaboratory comparability was evaluated using analysis of variance coupled with Duncan 's multiple range test, and linear-regression models describing the relations between individual laboratory analytical results for natural precipitation samples. Results of the statistical analyses indicate that certain pairs of laboratories produce different results when analyzing identical samples. Analyte bias for each laboratory was examined using analysis of variance coupled with Duncan 's multiple range test on data produced by the laboratories from the analysis of identical simulated precipitation samples. Bias for a given analyte produced by a single laboratory has been indicated when the laboratory mean for that analyte is shown to be significantly different from the mean for the most-probable analyte concentrations in the simulated precipitation samples. Ion-chromatographic methods for the determination of chloride, nitrate, and sulfate have been compared with the colorimetric methods that were also in use during the study period. Comparisons were made using analysis of variance coupled with Duncan 's multiple range test for means produced by the two methods. Analyte precision for each laboratory has been estimated by calculating a pooled variance for each analyte. Analyte estimated precisions have been compared using F-tests and differences in analyte precisions for laboratory pairs have been reported. (USGS)

DAPNe with micro-capillary separatory chemistry-coupled to MALDI-MS for the analysis of polar and non-polar lipid metabolism in one cell

NASA Astrophysics Data System (ADS)

Hamilton, Jason S.; Aguilar, Roberto; Petros, Robby A.; Verbeck, Guido F.

2017-05-01

The cellular metabolome is considered to be a representation of cellular phenotype and cellular response to changes to internal or external events. Methods to expand the coverage of the expansive physiochemical properties that makeup the metabolome currently utilize multi-step extractions and chromatographic separations prior to chemical detection, leading to lengthy analysis times. In this study, a single-step procedure for the extraction and separation of a sample using a micro-capillary as a separatory funnel to achieve analyte partitioning within an organic/aqueous immiscible solvent system is described. The separated analytes are then spotted for MALDI-MS imaging and distribution ratios are calculated. Initially, the method is applied to standard mixtures for proof of partitioning. The extraction of an individual cell is non-reproducible; therefore, a broad chemical analysis of metabolites is necessary and will be illustrated with the one-cell analysis of a single Snu-5 gastric cancer cell taken from a cellular suspension. The method presented here shows a broad partitioning dynamic range as a single-step method for lipid analysis demonstrating a decrease in ion suppression often present in MALDI analysis of lipids.

Single-step transesterification with simultaneous concentration and stable isotope analysis of fatty acid methyl esters by gas chromatography-combustion-isotope ratio mass spectrometry.

PubMed

Panetta, Robert J; Jahren, A Hope

2011-05-30

Gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS) is increasingly applied to food and metabolic studies for stable isotope analysis (δ(13) C), with the quantification of analyte concentration often obtained via a second alternative method. We describe a rapid direct transesterification of triacylglycerides (TAGs) for fatty acid methyl ester (FAME) analysis by GC-C-IRMS demonstrating robust simultaneous quantification of amount of analyte (mean r(2) =0.99, accuracy ±2% for 37 FAMEs) and δ(13) C (±0.13‰) in a single analytical run. The maximum FAME yield and optimal δ(13) C values are obtained by derivatizing with 10% (v/v) acetyl chloride in methanol for 1 h, while lower levels of acetyl chloride and shorter reaction times skewed the δ(13) C values by as much as 0.80‰. A Bland-Altman evaluation of the GC-C-IRMS measurements resulted in excellent agreement for pure oils (±0.08‰) and oils extracted from French fries (±0.49‰), demonstrating reliable simultaneous quantification of FAME concentration and δ(13) C values. Thus, we conclude that for studies requiring both the quantification of analyte and δ(13) C data, such as authentication or metabolic flux studies, GC-C-IRMS can be used as the sole analytical method. Copyright © 2011 John Wiley & Sons, Ltd.

Development and validation of a multi-analyte method for the regulatory control of carotenoids used as feed additives in fish and poultry feed.

PubMed

Vincent, Ursula; Serano, Federica; von Holst, Christoph

2017-08-01

Carotenoids are used in animal nutrition mainly as sensory additives that favourably affect the colour of fish, birds and food of animal origin. Various analytical methods exist for their quantification in compound feed, reflecting the different physico-chemical characteristics of the carotenoid and the corresponding feed additives. They may be natural products or specific formulations containing the target carotenoids produced by chemical synthesis. In this study a multi-analyte method was developed that can be applied to the determination of all 10 carotenoids currently authorised within the European Union for compound feedingstuffs. The method functions regardless of whether the carotenoids have been added to the compound feed via natural products or specific formulations. It is comprised of three steps: (1) digestion of the feed sample with an enzyme; (2) pressurised liquid extraction; and (3) quantification of the analytes by reversed-phase HPLC coupled to a photodiode array detector in the visible range. The method was single-laboratory validated for poultry and fish feed covering a mass fraction range of the target analyte from 2.5 to 300 mg kg - 1 . The following method performance characteristics were obtained: the recovery rate varied from 82% to 129% and precision expressed as the relative standard deviation of intermediate precision varied from 1.6% to 15%. Based on the acceptable performance obtained in the validation study, the multi-analyte method is considered fit for the intended purpose.

Evaluation of a multiclass, multiresidue liquid chromatography-tandem mass spectrometry method for analysis of 120 veterinary drugs in bovine kidney

USDA-ARS?s Scientific Manuscript database

Traditionally, regulatory monitoring of veterinary drug residues in food animal tissues involves the use of several single-class methods to cover a wide analytical scope. Multiclass, multiresidue methods of analysis tend to provide greater overall laboratory efficiency than the use of multiple meth...

Single Molecule Detection in Living Biological Cells using Carbon Nanotube Optical Probes

NASA Astrophysics Data System (ADS)

Strano, Michael

2009-03-01

Nanoscale sensing elements offer promise for single molecule analyte detection in physically or biologically constrained environments. Molecular adsorption can be amplified via modulation of sharp singularities in the electronic density of states that arise from 1D quantum confinement [1]. Single-walled carbon nanotubes (SWNT), as single molecule optical sensors [2-3], offer unique advantages such as photostable near-infrared (n-IR) emission for prolonged detection through biological media, single-molecule sensitivity and, nearly orthogonal optical modes for signal transduction that can be used to identify distinct classes of analytes. Selective binding to the SWNT surface is difficult to engineer [4]. In this lecture, we will briefly review the immerging field of fluorescent diagnostics using band gap emission from SWNT. In recent work, we demonstrate that even a single pair of SWNT provides at least four optical modes that can be modulated to uniquely fingerprint chemical agents by the degree to which they alter either the emission band intensity or wavelength. We validate this identification method in vitro by demonstrating detection and identification of six genotoxic analytes, including chemotherapeutic drugs and reactive oxygen species (ROS), which are spectroscopically differentiated into four distinct classes. We also demonstrate single-molecule sensitivity in detecting hydrogen peroxide, one of the most common genotoxins and an important cellular signal. Finally, we employ our sensing and fingerprinting method of these analytes in real time within live 3T3 cells, demonstrating the first multiplexed optical detection from a nanoscale biosensor and the first label-free tool to optically discriminate between genotoxins. We will also discuss our recent efforts to fabricate biomedical sensors for real time detection of glucose and other important physiologically relevant analytes in-vivo. The response of embedded SWNT in a swellable hydrogel construct to osmotic pressure gradients will be discussed, as well as its potential as a unique transduction mechanism for a new class of implantable sensors. [4pt] [1] Saito, R., Dresselhaus, G. & Dresselhaus, M. S. Physical Properties of Carbon Nanotubes (Imperial College Press, London, 1998). [0pt] [2] Barone, P. W., Baik, S., Heller, D. A. & Strano, M. S. Near-Infrared Optical Sensors Based on Single-Walled Carbon Nanotubes. Nature Materials 4, 86-92 (2005). [0pt] [3] Jeng, E. S., Moll, A. E., Roy, A. C., Gastala, J. B. & Strano, M. S. Detection of DNA hybridization using the near infrared band-gap fluorescence of single-walled carbon nanotubes. Nano Letters 6, 371-375 (2006). [0pt] [4] Heller, D. A. et al. Optical detection of DNA conformational polymorphism on single-walled carbon nanotubes. Science 311, 508-511 (2006).

Solid-phase microextraction fiber development for sampling and analysis of volatile organohalogen compounds in air.

PubMed

Attari, Seyed Ghavameddin; Bahrami, Abdolrahman; Shahna, Farshid Ghorbani; Heidari, Mahmoud

2014-01-01

A green, environmental friendly and sensitive method for determination of volatile organohalogen compounds was described in this paper. The method is based on a homemade sol-gel single-walled carbon nanotube/silica composite coated solid-phase microextraction to develop for sampling and analysis of Carbon tetrachloride, Benzotrichloride, Chloromethyl methyl ether and Trichloroethylene in air. Application of this method was investigated under different laboratory conditions. Predetermined concentrations of each analytes were prepared in a home-made standard chamber and the influences of experimental parameters such as temperature, humidity, extraction time, storage time, desorption temperature, desorption time and the sorbent performance were investigated. Under optimal conditions, the use of single-walled carbon nanotube/silica composite fiber showed good performance, high sensitive and fast sampling of volatile organohalogen compounds from air. For linearity test the regression correlation coefficient was more than 98% for analyte of interest and linear dynamic range for the proposed fiber and the applied Gas Chromatography-Flame Ionization Detector technique was from 1 to 100 ngmL(-1). Method detection limits ranged between 0.09 to 0.2 ngmL(-1) and method quantification limits were between 0.25 and 0.7 ngmL(-1). Single-walled carbon nanotube/silica composite fiber was highly reproducible, relative standard deviations were between 4.3 to 11.7 percent.

Analytical Bistatic k Space Images Compared to Experimental Swept Frequency EAR Images

NASA Technical Reports Server (NTRS)

Shaeffer, John; Cooper, Brett; Hom, Kam

2004-01-01

A case study of flat plate scattering images obtained by the analytical bistatic k space and experimental swept frequency ISAR methods is presented. The key advantage of the bistatic k space image is that a single excitation is required, i.e., one frequency I one angle. This means that prediction approaches such as MOM only need to compute one solution at a single frequency. Bistatic image Fourier transform data are obtained by computing the scattered field at various bistatic positions about the body in k space. Experimental image Fourier transform data are obtained from the measured response to a bandwidth of frequencies over a target rotation range.

Approaching the Limit in Atomic Spectrochemical Analysis.

ERIC Educational Resources Information Center

Hieftje, Gary M.

1982-01-01

To assess the ability of current analytical methods to approach the single-atom detection level, theoretical and experimentally determined detection levels are presented for several chemical elements. A comparison of these methods shows that the most sensitive atomic spectrochemical technique currently available is based on emission from…

Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory - Determination of Moderate-Use Pesticides and Selected Degradates in Water by C-18 Solid-Phase Extraction and Gas Chromatography/Mass Spectrometry

USGS Publications Warehouse

Sandstrom, Mark W.; Stroppel, Max E.; Foreman, William T.; Schroeder, Michael P.

2001-01-01

A method for the isolation and analysis of 21 parent pesticides and 20 pesticide degradates in natural-water samples is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase-extraction columns that contain octadecyl-bonded porous silica to extract the analytes. The columns are dried by using nitrogen gas, and adsorbed analytes are eluted with ethyl acetate. Extracted analytes are determined by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring of three characteristic ions. The upper concentration limit is 2 micrograms per liter (?g/L) for most analytes. Single-operator method detection limits in reagent-water samples range from 0.00 1 to 0.057 ?g/L. Validation data also are presented for 14 parent pesticides and 20 degradates that were determined to have greater bias or variability, or shorter holding times than the other compounds. The estimated maximum holding time for analytes in pesticide-grade water before extraction was 4 days. The estimated maximum holding time for analytes after extraction on the dry solid-phase-extraction columns was 7 days. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time. The method complements existing U.S. Geological Survey Method O-1126-95 (NWQL Schedules 2001 and 2010) by using identical sample preparation and comparable instrument analytical conditions so that sample extracts can be analyzed by either method to expand the range of analytes determined from one water sample.

Simultaneous Determination of Parathion, Malathion, Diazinon, and Pirimiphos Methyl in Dried Medicinal Plants Using Solid-Phase Microextraction Fibre Coated with Single-Walled Carbon Nanotubes

PubMed Central

Ahmadkhaniha, Reza; Samadi, Nasrin; Salimi, Mona; Sarkhail, Parisa; Rastkari, Noushin

2012-01-01

A reliable and sensitive headspace solid-phase microextraction gas chromatography-mass spectrometry method for simultaneous determination of different organophosphorus pesticides in dried medicinal plant samples is described. The analytes were extracted by single-walled carbon nanotubes as a new solid-phase microextraction adsorbent. The developed method showed good performance. For diazinon and pirimiphos methyl calibration, curves were linear (r 2 ≥ 0.993) over the concentration ranges from 1.5 to 300 ng g−1, and the limit of detection at signal-to-noise ratio of 3 was 0.3 ng g−1. For parathion and malathion, the linear range and limit of detection were 2.5–300 (r 2 ≥ 0.991) and 0.5 ng g−1, respectively. In addition, a comparative study between the single-walled carbon nanotubes and a commercial polydimethylsiloxane fibre for the determination of target analytes was carried out. Single-walled carbon nanotubes fibre showed higher extraction capacity, better thermal stability (over 350°C), and longer lifespan (over 250 times) than the commercial polydimethylsiloxane fibre. The developed method was successfully applied to determine target organophosphorus pesticides in real samples. PMID:22645439

Predictive Analytical Model for Isolator Shock-Train Location in a Mach 2.2 Direct-Connect Supersonic Combustion Tunnel

NASA Astrophysics Data System (ADS)

Lingren, Joe; Vanstone, Leon; Hashemi, Kelley; Gogineni, Sivaram; Donbar, Jeffrey; Akella, Maruthi; Clemens, Noel

2016-11-01

This study develops an analytical model for predicting the leading shock of a shock-train in the constant area isolator section in a Mach 2.2 direct-connect scramjet simulation tunnel. The effective geometry of the isolator is assumed to be a weakly converging duct owing to boundary-layer growth. For some given pressure rise across the isolator, quasi-1D equations relating to isentropic or normal shock flows can be used to predict the normal shock location in the isolator. The surface pressure distribution through the isolator was measured during experiments and both the actual and predicted locations can be calculated. Three methods of finding the shock-train location are examined, one based on the measured pressure rise, one using a non-physics-based control model, and one using the physics-based analytical model. It is shown that the analytical model performs better than the non-physics-based model in all cases. The analytic model is less accurate than the pressure threshold method but requires significantly less information to compute. In contrast to other methods for predicting shock-train location, this method is relatively accurate and requires as little as a single pressure measurement. This makes this method potentially useful for unstart control applications.

An efficient formulation and implementation of the analytic energy gradient method to the single and double excitation coupled-cluster wave function - Application to Cl2O2

NASA Technical Reports Server (NTRS)

Rendell, Alistair P.; Lee, Timothy J.

1991-01-01

The analytic energy gradient for the single and double excitation coupled-cluster (CCSD) wave function has been reformulated and implemented in a new set of programs. The reformulated set of gradient equations have a smaller computational cost than any previously published. The iterative solution of the linear equations and the construction of the effective density matrices are fully vectorized, being based on matrix multiplications. The new method has been used to investigate the Cl2O2 molecule, which has recently been postulated as an important intermediate in the destruction of ozone in the stratosphere. In addition to reporting computational timings, the CCSD equilibrium geometries, harmonic vibrational frequencies, infrared intensities, and relative energetics of three isomers of Cl2O2 are presented.

Quantitative Method for Simultaneous Analysis of Acetaminophen and 6 Metabolites.

PubMed

Lammers, Laureen A; Achterbergh, Roos; Pistorius, Marcel C M; Romijn, Johannes A; Mathôt, Ron A A

2017-04-01

Hepatotoxicity after ingestion of high-dose acetaminophen [N-acetyl-para-aminophenol (APAP)] is caused by the metabolites of the drug. To gain more insight into factors influencing susceptibility to APAP hepatotoxicity, quantification of APAP and metabolites is important. A few methods have been developed to simultaneously quantify APAP and its most important metabolites. However, these methods require a comprehensive sample preparation and long run times. The aim of this study was to develop and validate a simplified, but sensitive method for the simultaneous quantification of acetaminophen, the main metabolites acetaminophen glucuronide and acetaminophen sulfate, and 4 Cytochrome P450-mediated metabolites by using liquid chromatography with mass spectrometric (LC-MS) detection. The method was developed and validated for the human plasma, and it entailed a single method for sample preparation, enabling quick processing of the samples followed by an LC-MS method with a chromatographic run time of 9 minutes. The method was validated for selectivity, linearity, accuracy, imprecision, dilution integrity, recovery, process efficiency, ionization efficiency, and carryover effect. The method showed good selectivity without matrix interferences. For all analytes, the mean process efficiency was >86%, and the mean ionization efficiency was >94%. Furthermore, the accuracy was between 90.3% and 112% for all analytes, and the within- and between-run imprecision were <20% for the lower limit of quantification and <14.3% for the middle level and upper limit of quantification. The method presented here enables the simultaneous quantification of APAP and 6 of its metabolites. It is less time consuming than previously reported methods because it requires only a single and simple method for the sample preparation followed by an LC-MS method with a short run time. Therefore, this analytical method provides a useful method for both clinical and research purposes.

Implementation of radiation shielding calculation methods. Volume 2: Seminar/Workshop notes

NASA Technical Reports Server (NTRS)

Capo, M. A.; Disney, R. K.

1971-01-01

Detailed descriptions are presented of the input data for each of the MSFC computer codes applied to the analysis of a realistic nuclear propelled vehicle. The analytical techniques employed include cross section data, preparation, one and two dimensional discrete ordinates transport, point kernel, and single scatter methods.

Single cell proteomics in biomedicine: High-dimensional data acquisition, visualization, and analysis.

PubMed

Su, Yapeng; Shi, Qihui; Wei, Wei

2017-02-01

New insights on cellular heterogeneity in the last decade provoke the development of a variety of single cell omics tools at a lightning pace. The resultant high-dimensional single cell data generated by these tools require new theoretical approaches and analytical algorithms for effective visualization and interpretation. In this review, we briefly survey the state-of-the-art single cell proteomic tools with a particular focus on data acquisition and quantification, followed by an elaboration of a number of statistical and computational approaches developed to date for dissecting the high-dimensional single cell data. The underlying assumptions, unique features, and limitations of the analytical methods with the designated biological questions they seek to answer will be discussed. Particular attention will be given to those information theoretical approaches that are anchored in a set of first principles of physics and can yield detailed (and often surprising) predictions. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Enantioselective determination of representative profens in wastewater by a single-step sample treatment and chiral liquid chromatography-tandem mass spectrometry.

PubMed

Caballo, C; Sicilia, M D; Rubio, S

2015-03-01

This manuscript describes, for the first time, the simultaneous enantioselective determination of ibuprofen, naproxen and ketoprofen in wastewater based on liquid chromatography tandem mass spectrometry (LC-MS/MS). The method uses a single-step sample treatment based on microextraction with a supramolecular solvent made up of hexagonal inverted aggregates of decanoic acid, formed in situ in the wastewater sample through a spontaneous self-assembly process. Microextraction of profens was optimized and the analytical method validated. Isotopically labeled internal standards were used to compensate for both matrix interferences and recoveries. Apparent recoveries for the six enantiomers in influent and effluent wastewater samples were in the interval 97-103%. Low method detection limits (MDLs) were obtained (0.5-1.2 ng L(-1)) as a result of the high concentration factors achieved in the microextraction process (i.e. actual concentration factors 469-736). No analyte derivatization or evaporation of extracts, as it is required with GC-MS, was necessary. Relative standard deviations for enantiomers in wastewater were always below 8%. The method was applied to the determination of the concentrations and enantiomeric fractions of the targeted analytes in influents and effluents from three wastewater treatment plants. All the values found for profen enantiomers were consistent with those previously reported and confirmed again the suitability of using the enantiomeric fraction of ibuprofen as an indicator of the discharge of untreated or poorly treated wastewaters. Both the analytical and operational features of this method make it applicable to the assessment of the enantiomeric fate of profens in the environment. Copyright © 2014 Elsevier B.V. All rights reserved.

Environmental and human monitoring of Americium-241 utilizing extraction chromatography and alpha-spectrometry.

PubMed

Goldstein, S J; Hensley, C A; Armenta, C E; Peters, R J

1997-03-01

Recent developments in extraction chromatography have simplified the separation of americium from complex matrices in preparation for alpha-spectroscopy relative to traditional methods. Here we present results of procedures developed/adapted for water, air, and bioassay samples with less than 1 g of inorganic residue. Prior analytical methods required the use of a complex, multistage procedure for separation of americium from these matrices. The newer, simplified procedure requires only a single 2 mL extraction chromatographic separation for isolation of Am and lanthanides from other components of the sample. This method has been implemented on an extensive variety of "real" environmental and bioassay samples from the Los Alamos area, and consistently reliable and accurate results with appropriate detection limits have been obtained. The new method increases analytical throughput by a factor of approximately 2 and decreases environmental hazards from acid and mixed-waste generation relative to the prior technique. Analytical accuracy, reproducibility, and reliability are also significantly improved over the more complex and laborious method used previously.

Single-laboratory validation of a saponification method for the determination of four polycyclic aromatic hydrocarbons in edible oils by HPLC-fluorescence detection.

PubMed

Akdoğan, Abdullah; Buttinger, Gerhard; Wenzl, Thomas

2016-01-01

An analytical method is reported for the determination of four polycyclic aromatic hydrocarbons (benzo[a]pyrene (BaP), benz[a]anthracene (BaA), benzo[b]fluoranthene (BbF) and chrysene (CHR)) in edible oils (sesame, maize, sunflower and olive oil) by high-performance liquid chromatography. Sample preparation is based on three steps including saponification, liquid-liquid partitioning and, finally, clean-up by solid phase extraction on 2 g of silica. Guidance on single-laboratory validation of the proposed analysis method was taken from the second edition of the Eurachem guide on method validation. The lower level of the working range of the method was determined by the limits of quantification of the individual analytes, and the upper level was equal to 5.0 µg kg(-1). The limits of detection and quantification of the four PAHs ranged from 0.06 to 0.12 µg kg(-1) and from 0.13 to 0.24 µg kg(-1). Recoveries of more than 84.8% were achieved for all four PAHs at two concentration levels (2.5 and 5.0 µg kg(-1)), and expanded relative measurement uncertainties were below 20%. The performance of the validated method was in all aspects compliant with provisions set in European Union legislation for the performance of analytical methods employed in the official control of food. The applicability of the method to routine samples was evaluated based on a limited number of commercial edible oil samples.

Achieving optimal SERS through enhanced experimental design

PubMed Central

Fisk, Heidi; Westley, Chloe; Turner, Nicholas J.

2016-01-01

One of the current limitations surrounding surface‐enhanced Raman scattering (SERS) is the perceived lack of reproducibility. SERS is indeed challenging, and for analyte detection, it is vital that the analyte interacts with the metal surface. However, as this is analyte dependent, there is not a single set of SERS conditions that are universal. This means that experimental optimisation for optimum SERS response is vital. Most researchers optimise one factor at a time, where a single parameter is altered first before going onto optimise the next. This is a very inefficient way of searching the experimental landscape. In this review, we explore the use of more powerful multivariate approaches to SERS experimental optimisation based on design of experiments and evolutionary computational methods. We particularly focus on colloidal‐based SERS rather than thin film preparations as a result of their popularity. © 2015 The Authors. Journal of Raman Spectroscopy published by John Wiley & Sons, Ltd. PMID:27587905

Achieving optimal SERS through enhanced experimental design.

PubMed

Fisk, Heidi; Westley, Chloe; Turner, Nicholas J; Goodacre, Royston

2016-01-01

One of the current limitations surrounding surface-enhanced Raman scattering (SERS) is the perceived lack of reproducibility. SERS is indeed challenging, and for analyte detection, it is vital that the analyte interacts with the metal surface. However, as this is analyte dependent, there is not a single set of SERS conditions that are universal. This means that experimental optimisation for optimum SERS response is vital. Most researchers optimise one factor at a time, where a single parameter is altered first before going onto optimise the next. This is a very inefficient way of searching the experimental landscape. In this review, we explore the use of more powerful multivariate approaches to SERS experimental optimisation based on design of experiments and evolutionary computational methods. We particularly focus on colloidal-based SERS rather than thin film preparations as a result of their popularity. © 2015 The Authors. Journal of Raman Spectroscopy published by John Wiley & Sons, Ltd.

Lack of correlation between reaction speed and analytical sensitivity in isothermal amplification reveals the value of digital methods for optimization: validation using digital real-time RT-LAMP

PubMed Central

Khorosheva, Eugenia M.; Karymov, Mikhail A.; Selck, David A.; Ismagilov, Rustem F.

2016-01-01

In this paper, we asked if it is possible to identify the best primers and reaction conditions based on improvements in reaction speed when optimizing isothermal reactions. We used digital single-molecule, real-time analyses of both speed and efficiency of isothermal amplification reactions, which revealed that improvements in the speed of isothermal amplification reactions did not always correlate with improvements in digital efficiency (the fraction of molecules that amplify) or with analytical sensitivity. However, we observed that the speeds of amplification for single-molecule (in a digital device) and multi-molecule (e.g. in a PCR well plate) formats always correlated for the same conditions. Also, digital efficiency correlated with the analytical sensitivity of the same reaction performed in a multi-molecule format. Our finding was supported experimentally with examples of primer design, the use or exclusion of loop primers in different combinations, and the use of different enzyme mixtures in one-step reverse-transcription loop-mediated amplification (RT-LAMP). Our results show that measuring the digital efficiency of amplification of single-template molecules allows quick, reliable comparisons of the analytical sensitivity of reactions under any two tested conditions, independent of the speeds of the isothermal amplification reactions. PMID:26358811

Flexible nano- and microliter injections on a single liquid chromatography-mass spectrometry system: Minimizing sample preparation and maximizing linear dynamic range.

PubMed

Lubin, Arnaud; Sheng, Sheng; Cabooter, Deirdre; Augustijns, Patrick; Cuyckens, Filip

2017-11-17

Lack of knowledge on the expected concentration range or insufficient linear dynamic range of the analytical method applied are common challenges for the analytical scientist. Samples that are above the upper limit of quantification are typically diluted and reanalyzed. The analysis of undiluted highly concentrated samples can cause contamination of the system, while the dilution step is time consuming and as the case for any sample preparation step, also potentially leads to precipitation, adsorption or degradation of the analytes. Copyright © 2017 Elsevier B.V. All rights reserved.

Matrix vapor deposition/recrystallization and dedicated spray preparation for high-resolution scanning microprobe matrix-assisted laser desorption/ionization imaging mass spectrometry (SMALDI-MS) of tissue and single cells.

PubMed

Bouschen, Werner; Schulz, Oliver; Eikel, Daniel; Spengler, Bernhard

2010-02-01

Matrix preparation techniques such as air spraying or vapor deposition were investigated with respect to lateral migration, integration of analyte into matrix crystals and achievable lateral resolution for the purpose of high-resolution biological imaging. The accessible mass range was found to be beyond 5000 u with sufficient analytical sensitivity. Gas-assisted spraying methods (using oxygen-free gases) provide a good compromise between crystal integration of analyte and analyte migration within the sample. Controlling preparational parameters with this method, however, is difficult. Separation of the preparation procedure into two steps, instead, leads to an improved control of migration and incorporation. The first step is a dry vapor deposition of matrix onto the investigated sample. In a second step, incorporation of analyte into the matrix crystal is enhanced by a controlled recrystallization of matrix in a saturated water atmosphere. With this latter method an effective analytical resolution of 2 microm in the x and y direction was achieved for scanning microprobe matrix-assisted laser desorption/ionization imaging mass spectrometry (SMALDI-MS). Cultured A-498 cells of human renal carcinoma were successfully investigated by high-resolution MALDI imaging using the new preparation techniques. Copyright 2010 John Wiley & Sons, Ltd.

Method development and validation for simultaneous quantification of 15 drugs of abuse and prescription drugs and 7 of their metabolites in whole blood relevant in the context of driving under the influence of drugs--usefulness of multi-analyte calibration.

PubMed

Steuer, Andrea E; Forss, Anna-Maria; Dally, Annika M; Kraemer, Thomas

2014-11-01

In the context of driving under the influence of drugs (DUID), not only common drugs of abuse may have an influence, but also medications with similar mechanisms of action. Simultaneous quantification of a variety of drugs and medications relevant in this context allows faster and more effective analyses. Therefore, multi-analyte approaches have gained more and more popularity in recent years. Usually, calibration curves for such procedures contain a mixture of all analytes, which might lead to mutual interferences. In this study we investigated whether the use of such mixtures leads to reliable results for authentic samples containing only one or two analytes. Five hundred microliters of whole blood were extracted by routine solid-phase extraction (SPE, HCX). Analysis was performed on an ABSciex 3200 QTrap instrument with ESI+ in scheduled MRM mode. The method was fully validated according to international guidelines including selectivity, recovery, matrix effects, accuracy and precision, stabilities, and limit of quantification. The selected SPE provided recoveries >60% for all analytes except 6-monoacetylmorphine (MAM) with coefficients of variation (CV) below 15% or 20% for quality controls (QC) LOW and HIGH, respectively. Ion suppression >30% was found for benzoylecgonine, hydrocodone, hydromorphone, MDA, oxycodone, and oxymorphone at QC LOW, however CVs were always below 10% (n=6 different whole blood samples). Accuracy and precision criteria were fulfilled for all analytes except for MAM. Systematic investigation of accuracy determined for QC MED in a multi-analyte mixture compared to samples containing only single analytes revealed no relevant differences for any analyte, indicating that a multi-analyte calibration is suitable for the presented method. Comparison of approximately 60 samples to a former GC-MS method showed good correlation. The newly validated method was successfully applied to more than 1600 routine samples and 3 proficiency tests. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Class-modelling in food analytical chemistry: Development, sampling, optimisation and validation issues - A tutorial.

PubMed

Oliveri, Paolo

2017-08-22

Qualitative data modelling is a fundamental branch of pattern recognition, with many applications in analytical chemistry, and embraces two main families: discriminant and class-modelling methods. The first strategy is appropriate when at least two classes are meaningfully defined in the problem under study, while the second strategy is the right choice when the focus is on a single class. For this reason, class-modelling methods are also referred to as one-class classifiers. Although, in the food analytical field, most of the issues would be properly addressed by class-modelling strategies, the use of such techniques is rather limited and, in many cases, discriminant methods are forcedly used for one-class problems, introducing a bias in the outcomes. Key aspects related to the development, optimisation and validation of suitable class models for the characterisation of food products are critically analysed and discussed. Copyright © 2017 Elsevier B.V. All rights reserved.

A Generalized Approach to Forensic Dye Identification: Development and Utility of Reference Libraries.

PubMed

Groves, Ethan; Palenik, Skip; Palenik, Christopher S

2018-04-18

While color is arguably the most important optical property of evidential fibers, the actual dyestuffs responsible for its expression in them are, in forensic trace evidence examinations, rarely analyzed and still less often identified. This is due, primarily, to the exceedingly small quantities of dye present in a single fiber as well as to the fact that dye identification is a challenging analytical problem, even when large quantities are available for analysis. Among the practical reasons for this are the wide range of dyestuffs available (and the even larger number of trade names), the low total concentration of dyes in the finished product, the limited amount of sample typically available for analysis in forensic cases, and the complexity of the dye mixtures that may exist within a single fiber. Literature on the topic of dye analysis is often limited to a specific method, subset of dyestuffs, or an approach that is not applicable given the constraints of a forensic analysis. Here, we present a generalized approach to dye identification that ( 1 ) combines several robust analytical methods, ( 2 ) is broadly applicable to a wide range of dye chemistries, application classes, and fiber types, and ( 3 ) can be scaled down to forensic casework-sized samples. The approach is based on the development of a reference collection of 300 commercially relevant textile dyes that have been characterized by a variety of microanalytical methods (HPTLC, Raman microspectroscopy, infrared microspectroscopy, UV-Vis spectroscopy, and visible microspectrophotometry). Although there is no single approach that is applicable to all dyes on every type of fiber, a combination of these analytical methods has been applied using a reproducible approach that permits the use of reference libraries to constrain the identity of and, in many cases, identify the dye (or dyes) present in a textile fiber sample.

Application of laser Raman spectroscopy in concentration measurements of multiple analytes in human body fluids

NASA Astrophysics Data System (ADS)

Qu, Jianan Y.; Suria, David; Wilson, Brian C.

1998-05-01

The primary goal of these studies was to demonstrate that NIR Raman spectroscopy is feasible as a rapid and reagentless analytic method for clinical diagnostics. Raman spectra were collected on human serum and urine samples using a 785 nm excitation laser and a single-stage holographic spectrometer. A partial east squares method was used to predict the analyte concentrations of interest. The actual concentrations were determined by a standard clinical chemistry. The prediction accuracy of total protein, albumin, triglyceride and glucose in human sera ranged from 1.5 percent to 5 percent which is greatly acceptable for clinical diagnostics. The concentration measurements of acetaminophen, ethanol and codeine inhuman urine have demonstrated the potential of NIR Raman technology in screening of therapeutic drugs and substances of abuse.

Transient analysis of an adaptive system for optimization of design parameters

NASA Technical Reports Server (NTRS)

Bayard, D. S.

1992-01-01

Averaging methods are applied to analyzing and optimizing the transient response associated with the direct adaptive control of an oscillatory second-order minimum-phase system. The analytical design methods developed for a second-order plant can be applied with some approximation to a MIMO flexible structure having a single dominant mode.

Using FTIR-ATR Spectroscopy to Teach the Internal Standard Method

ERIC Educational Resources Information Center

Bellamy, Michael K.

2010-01-01

The internal standard method is widely applied in quantitative analyses. However, most analytical chemistry textbooks either omit this topic or only provide examples of a single-point internal standardization. An experiment designed to teach students how to prepare an internal standard calibration curve is described. The experiment is a modified…

Analytic energy gradients for the orbital-optimized third-order Møller-Plesset perturbation theory

NASA Astrophysics Data System (ADS)

Bozkaya, Uǧur

2013-09-01

Analytic energy gradients for the orbital-optimized third-order Møller-Plesset perturbation theory (OMP3) [U. Bozkaya, J. Chem. Phys. 135, 224103 (2011)], 10.1063/1.3665134 are presented. The OMP3 method is applied to problematic chemical systems with challenging electronic structures. The performance of the OMP3 method is compared with those of canonical second-order Møller-Plesset perturbation theory (MP2), third-order Møller-Plesset perturbation theory (MP3), coupled-cluster singles and doubles (CCSD), and coupled-cluster singles and doubles with perturbative triples [CCSD(T)] for investigating equilibrium geometries, vibrational frequencies, and open-shell reaction energies. For bond lengths, the performance of OMP3 is in between those of MP3 and CCSD. For harmonic vibrational frequencies, the OMP3 method significantly eliminates the singularities arising from the abnormal response contributions observed for MP3 in case of symmetry-breaking problems, and provides noticeably improved vibrational frequencies for open-shell molecules. For open-shell reaction energies, OMP3 exhibits a better performance than MP3 and CCSD as in case of barrier heights and radical stabilization energies. As discussed in previous studies, the OMP3 method is several times faster than CCSD in energy computations. Further, in analytic gradient computations for the CCSD method one needs to solve λ-amplitude equations, however for OMP3 one does not since λ _{ab}^{ij(1)} = t_{ij}^{ab(1)} and λ _{ab}^{ij(2)} = t_{ij}^{ab(2)}. Additionally, one needs to solve orbital Z-vector equations for CCSD, but for OMP3 orbital response contributions are zero owing to the stationary property of OMP3. Overall, for analytic gradient computations the OMP3 method is several times less expensive than CCSD (roughly ˜4-6 times). Considering the balance of computational cost and accuracy we conclude that the OMP3 method emerges as a very useful tool for the study of electronically challenging chemical systems.

Analytic energy gradients for the orbital-optimized third-order Møller-Plesset perturbation theory.

PubMed

Bozkaya, Uğur

2013-09-14

Analytic energy gradients for the orbital-optimized third-order Møller-Plesset perturbation theory (OMP3) [U. Bozkaya, J. Chem. Phys. 135, 224103 (2011)] are presented. The OMP3 method is applied to problematic chemical systems with challenging electronic structures. The performance of the OMP3 method is compared with those of canonical second-order Møller-Plesset perturbation theory (MP2), third-order Møller-Plesset perturbation theory (MP3), coupled-cluster singles and doubles (CCSD), and coupled-cluster singles and doubles with perturbative triples [CCSD(T)] for investigating equilibrium geometries, vibrational frequencies, and open-shell reaction energies. For bond lengths, the performance of OMP3 is in between those of MP3 and CCSD. For harmonic vibrational frequencies, the OMP3 method significantly eliminates the singularities arising from the abnormal response contributions observed for MP3 in case of symmetry-breaking problems, and provides noticeably improved vibrational frequencies for open-shell molecules. For open-shell reaction energies, OMP3 exhibits a better performance than MP3 and CCSD as in case of barrier heights and radical stabilization energies. As discussed in previous studies, the OMP3 method is several times faster than CCSD in energy computations. Further, in analytic gradient computations for the CCSD method one needs to solve λ-amplitude equations, however for OMP3 one does not since λ(ab)(ij(1))=t(ij)(ab(1)) and λ(ab)(ij(2))=t(ij)(ab(2)). Additionally, one needs to solve orbital Z-vector equations for CCSD, but for OMP3 orbital response contributions are zero owing to the stationary property of OMP3. Overall, for analytic gradient computations the OMP3 method is several times less expensive than CCSD (roughly ~4-6 times). Considering the balance of computational cost and accuracy we conclude that the OMP3 method emerges as a very useful tool for the study of electronically challenging chemical systems.

A UPLC-MS/MS method for simultaneous quantitation of three monoterpene glycosides and four alkaloids in rat plasma: application to a comparative pharmacokinetic study of Huo Luo Xiao Ling Dan and single herb extract.

PubMed

Ai, Yu; Wu, Yun; Wang, Fenrong; Ma, Wen; Bian, Qiaoxia; Lee, David Y-W; Dai, Ronghua

2015-03-01

The objective of this study was to develop a sensitive and reliable ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for simultaneous quantitation of three monoterpene glycosides (paeoniflorin, alibiflorin and oxypaeoniflorin) and four alkaloids (tetrahydropalmatine, corydaline, dehydrocorydaline and berberine), the main active ingredients of Radix Paeoniae Rubra extract (RPE) and Corydalis yanhusuo extract (CYE) in Huo Luo Xiao Ling Dan (HLXLD), and to compare the pharmacokinetics of these active ingredients in normal and arthritic rats orally administrated with HLXLD or RPE/CYE alone. The analytes and internal standard (IS) (geniposide) were separated on a XBridge C18 column (150 × 4.6 mm, 3.5 µm) using gradient elution with the mobile phase consisting of methanol and 0.01% formic acid in water at a flow rate of 0.6 ml/min. The detection of the analytes was performed on Acquity UPLC-MS/MS system with an electrospray ionization and multiple reaction monitoring mode via polarity switching between negative (for monoterpene glycosides) and positive (for alkaloids) ionization mode. The lower limits of quantification were 2.5, 1, 0.5, 0.2, 0.2, 0.02 and 0.01 ng/ml for paeoniflorin, alibiflorin, oxypaeoniflorin, tetrahydropalmatine, corydaline, dehydrocorydaline and berberine, respectively. Intra-day and inter-day precision and accuracy of analytes were well within acceptance criteria (15%). The mean extraction recoveries of analytes and IS from rat plasma were all more than 83.1%. The validated method has been successfully applied to determination of the analytes. Results showed that there were remarkable differences in pharmacokinetic properties of the analytes between herbal formula and single herb group, normal and arthritic group. Copyright © 2015 John Wiley & Sons, Ltd.

PLE in the analysis of plant compounds. Part II: One-cycle PLE in determining total amount of analyte in plant material.

PubMed

Dawidowicz, Andrzej L; Wianowska, Dorota

2005-04-29

Pressurised liquid extraction (PLE) is recognised as one of the most effective sample preparation methods. Despite the enhanced extraction power of PLE, the full recovery of an analyte from plant material may require multiple extractions of the same sample. The presented investigations show the possibility of estimating the true concentration value of an analyte in plant material employing one-cycle PLE in which plant samples of different weight are used. The performed experiments show a linear dependence between the reciprocal value of the analyte amount (E*), extracted in single-step PLE from a plant matrix, and the ratio of plant material mass to extrahent volume (m(p)/V(s)). Hence, time-consuming multi-step PLE can be replaced by a few single-step PLEs performed at different (m(p)/V(s)) ratios. The concentrations of rutin in Sambucus nigra L. and caffeine in tea and coffee estimated by means of the tested procedure are almost the same as their concentrations estimated by multiple PLE.

Remote detection of single emitters via optical waveguides

NASA Astrophysics Data System (ADS)

Then, Patrick; Razinskas, Gary; Feichtner, Thorsten; Haas, Philippe; Wild, Andreas; Bellini, Nicola; Osellame, Roberto; Cerullo, Giulio; Hecht, Bert

2014-05-01

The integration of lab-on-a-chip technologies with single-molecule detection techniques may enable new applications in analytical chemistry, biotechnology, and medicine. We describe a method based on the reciprocity theorem of electromagnetic theory to determine and optimize the detection efficiency of photons emitted by single quantum emitters through truncated dielectric waveguides of arbitrary shape positioned in their proximity. We demonstrate experimentally that detection of single quantum emitters via such waveguides is possible, confirming the predicted behavior of the detection efficiency. Our findings blaze the trail towards efficient lensless single-emitter detection compatible with large-scale optofluidic integration.

An accelerated photo-magnetic imaging reconstruction algorithm based on an analytical forward solution and a fast Jacobian assembly method

NASA Astrophysics Data System (ADS)

Nouizi, F.; Erkol, H.; Luk, A.; Marks, M.; Unlu, M. B.; Gulsen, G.

2016-10-01

We previously introduced photo-magnetic imaging (PMI), an imaging technique that illuminates the medium under investigation with near-infrared light and measures the induced temperature increase using magnetic resonance thermometry (MRT). Using a multiphysics solver combining photon migration and heat diffusion, PMI models the spatiotemporal distribution of temperature variation and recovers high resolution optical absorption images using these temperature maps. In this paper, we present a new fast non-iterative reconstruction algorithm for PMI. This new algorithm uses analytic methods during the resolution of the forward problem and the assembly of the sensitivity matrix. We validate our new analytic-based algorithm with the first generation finite element method (FEM) based reconstruction algorithm previously developed by our team. The validation is performed using, first synthetic data and afterwards, real MRT measured temperature maps. Our new method accelerates the reconstruction process 30-fold when compared to a single iteration of the FEM-based algorithm.

Cellular dosimetry of (111)In using monte carlo N-particle computer code: comparison with analytic methods and correlation with in vitro cytotoxicity.

PubMed

Cai, Zhongli; Pignol, Jean-Philippe; Chan, Conrad; Reilly, Raymond M

2010-03-01

Our objective was to compare Monte Carlo N-particle (MCNP) self- and cross-doses from (111)In to the nucleus of breast cancer cells with doses calculated by reported analytic methods (Goddu et al. and Farragi et al.). A further objective was to determine whether the MCNP-predicted surviving fraction (SF) of breast cancer cells exposed in vitro to (111)In-labeled diethylenetriaminepentaacetic acid human epidermal growth factor ((111)In-DTPA-hEGF) could accurately predict the experimentally determined values. MCNP was used to simulate the transport of electrons emitted by (111)In from the cell surface, cytoplasm, or nucleus. The doses to the nucleus per decay (S values) were calculated for single cells, closely packed monolayer cells, or cell clusters. The cell and nucleus dimensions of 6 breast cancer cell lines were measured, and cell line-specific S values were calculated. For self-doses, MCNP S values of nucleus to nucleus agreed very well with those of Goddu et al. (ratio of S values using analytic methods vs. MCNP = 0.962-0.995) and Faraggi et al. (ratio = 1.011-1.024). MCNP S values of cytoplasm and cell surface to nucleus compared fairly well with the reported values (ratio = 0.662-1.534 for Goddu et al.; 0.944-1.129 for Faraggi et al.). For cross doses, the S values to the nucleus were independent of (111)In subcellular distribution but increased with cluster size. S values for monolayer cells were significantly different from those of single cells and cell clusters. The MCNP-predicted SF for monolayer MDA-MB-468, MDA-MB-231, and MCF-7 cells agreed with the experimental data (relative error of 3.1%, -1.0%, and 1.7%). The single-cell and cell cluster models were less accurate in predicting the SF. For MDA-MB-468 cells, relative error was 8.1% using the single-cell model and -54% to -67% using the cell cluster model. Individual cell-line dimensions had large effects on S values and were needed to estimate doses and SF accurately. MCNP simulation compared well with the reported analytic methods in the calculation of subcellular S values for single cells and cell clusters. Application of a monolayer model was most accurate in predicting the SF of breast cancer cells exposed in vitro to (111)In-DTPA-hEGF.

Stereoselective method to quantify bupropion and its three major metabolites, hydroxybupropion, erythro-dihydrobupropion, and threo-dihydrobupropion using HPLC-MS/MS.

PubMed

Masters, Andrea R; McCoy, Michael; Jones, David R; Desta, Zeruesenay

2016-03-15

Bupropion metabolites formed via oxidation and reduction exhibit pharmacological activity, but little is known regarding their stereoselective disposition. A novel stereoselective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed to separate and quantify enantiomers of bupropion, 4-hydroxybupropion, and erythro- and threo-dihydrobupropion. Liquid-liquid extraction was implemented to extract all analytes from 50 μL human plasma. Acetaminophen (APAP) was used as an internal standard. The analytes were separated on a Lux 3 μ Cellulose-3 250×4.6 mm column by methanol: acetonitrile: ammonium bicarbonate: ammonium hydroxide gradient elution and monitored using an ABSciex 5500 QTRAP triple-quadrupole mass spectrometer equipped with electrospray ionization probe in positive mode. Extraction efficiency for all analytes was ≥70%. The stability at a single non-extracted concentration for over 48 h at ambient temperature resulted in less than 9.8% variability for all analytes. The limit of quantification (LOQ) for enantiomers of bupropion and 4-hydroxybupropion was 0.3 ng/mL, while the LOQ for enantiomers of erythro- and threo-hydrobupropion was 0.15 ng/mL. The intra-day precision and accuracy estimates for enantiomers of bupropion and its metabolites ranged from 3.4% to 15.4% and from 80.6% to 97.8%, respectively, while the inter-day precision and accuracy ranged from 6.1% to 19.9% and from 88.5% to 99.9%, respectively. The current method was successfully implemented to determine the stereoselective pharmacokinetics of bupropion and its metabolites in 3 healthy volunteers administered a single 100mg oral dose of racemic bupropion. This novel, accurate, and precise HPLC-MS/MS method should enhance further research into bupropion stereoselective metabolism and drug interactions. Copyright © 2016 Elsevier B.V. All rights reserved.

Utilizing global data to estimate analytical performance on the Sigma scale: A global comparative analysis of methods, instruments, and manufacturers through external quality assurance and proficiency testing programs.

PubMed

Westgard, Sten A

2016-06-01

To assess the analytical performance of instruments and methods through external quality assessment and proficiency testing data on the Sigma scale. A representative report from five different EQA/PT programs around the world (2 US, 1 Canadian, 1 UK, and 1 Australasian) was accessed. The instrument group standard deviations were used as surrogate estimates of instrument imprecision. Performance specifications from the US CLIA proficiency testing criteria were used to establish a common quality goal. Then Sigma-metrics were calculated to grade the analytical performance. Different methods have different Sigma-metrics for each analyte reviewed. Summary Sigma-metrics estimate the percentage of the chemistry analytes that are expected to perform above Five Sigma, which is where optimized QC design can be implemented. The range of performance varies from 37% to 88%, exhibiting significant differentiation between instruments and manufacturers. Median Sigmas for the different manufacturers in three analytes (albumin, glucose, sodium) showed significant differentiation. Chemistry tests are not commodities. Quality varies significantly from manufacturer to manufacturer, instrument to instrument, and method to method. The Sigma-assessments from multiple EQA/PT programs provide more insight into the performance of methods and instruments than any single program by itself. It is possible to produce a ranking of performance by manufacturer, instrument and individual method. Laboratories seeking optimal instrumentation would do well to consult this data as part of their decision-making process. To confirm that these assessments are stable and reliable, a longer term study should be conducted that examines more results over a longer time period. Copyright © 2016 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Conversion of multiple analyte cation types to a single analyte anion type via ion/ion charge inversion.

PubMed

Hassell, Kerry M; LeBlanc, Yves; McLuckey, Scott A

2009-11-01

Charge inversion ion/ion reactions can convert several cation types associated with a single analyte molecule to a single anion type for subsequent mass analysis. Specifically, analyte ions present with one of a variety of cationizing agents, such as an excess proton, excess sodium ion, or excess potassium ion, can all be converted to the deprotonated molecule, provided that a stable anion can be generated for the analyte. Multiply deprotonated species that are capable of exchanging a proton for a metal ion serve as the reagent anions for the reaction. This process is demonstrated here for warfarin and for a glutathione conjugate. Examples for several other glutathione conjugates are provided as supplementary material to demonstrate the generality of the reaction. In the case of glutathione conjugates, multiple metal ions can be associated with the singly-charged analyte due to the presence of two carboxylate groups. The charge inversion reaction involves the removal of the excess cationizing agent, as well as any metal ions associated with anionic groups to yield a singly deprotonated analyte molecule. The ability to convert multiple cation types to a single anion type is analytically desirable in cases in which the analyte signal is distributed among several cation types, as is common in the electrospray ionization of solutions with relatively high salt contents. For analyte species that undergo efficient charge inversion, such as glutathione conjugates, there is the additional potential advantage for significantly improved signal-to-noise ratios when species that give rise to 'chemical noise' in the positive ion spectrum do not undergo efficient charge inversion.

Optimization and single-laboratory validation of a method for the determination of flavonolignans in milk thistle seeds by high-performance liquid chromatography with ultraviolet detection.

PubMed

Mudge, Elizabeth; Paley, Lori; Schieber, Andreas; Brown, Paula N

2015-10-01

Seeds of milk thistle, Silybum marianum (L.) Gaertn., are used for treatment and prevention of liver disorders and were identified as a high priority ingredient requiring a validated analytical method. An AOAC International expert panel reviewed existing methods and made recommendations concerning method optimization prior to validation. A series of extraction and separation studies were undertaken on the selected method for determining flavonolignans from milk thistle seeds and finished products to address the review panel recommendations. Once optimized, a single-laboratory validation study was conducted. The method was assessed for repeatability, accuracy, selectivity, LOD, LOQ, analyte stability, and linearity. Flavonolignan content ranged from 1.40 to 52.86% in raw materials and dry finished products and ranged from 36.16 to 1570.7 μg/mL in liquid tinctures. Repeatability for the individual flavonolignans in raw materials and finished products ranged from 1.03 to 9.88% RSDr, with HorRat values between 0.21 and 1.55. Calibration curves for all flavonolignan concentrations had correlation coefficients of >99.8%. The LODs for the flavonolignans ranged from 0.20 to 0.48 μg/mL at 288 nm. Based on the results of this single-laboratory validation, this method is suitable for the quantitation of the six major flavonolignans in milk thistle raw materials and finished products, as well as multicomponent products containing dandelion, schizandra berry, and artichoke extracts. It is recommended that this method be adopted as First Action Official Method status by AOAC International.

Developing automated analytical methods for scientific environments using LabVIEW.

PubMed

Wagner, Christoph; Armenta, Sergio; Lendl, Bernhard

2010-01-15

The development of new analytical techniques often requires the building of specially designed devices, each requiring its own dedicated control software. Especially in the research and development phase, LabVIEW has proven to be one highly useful tool for developing this software. Yet, it is still common practice to develop individual solutions for different instruments. In contrast to this, we present here a single LabVIEW-based program that can be directly applied to various analytical tasks without having to change the program code. Driven by a set of simple script commands, it can control a whole range of instruments, from valves and pumps to full-scale spectrometers. Fluid sample (pre-)treatment and separation procedures can thus be flexibly coupled to a wide range of analytical detection methods. Here, the capabilities of the program have been demonstrated by using it for the control of both a sequential injection analysis - capillary electrophoresis (SIA-CE) system with UV detection, and an analytical setup for studying the inhibition of enzymatic reactions using a SIA system with FTIR detection.

Development and single-laboratory validation of an HPLC method for the determination of cyclamate sweetener in foodstuffs.

PubMed

Scotter, M J; Castle, L; Roberts, D P T; Macarthur, R; Brereton, P A; Hasnip, S K; Katz, N

2009-05-01

A method for the determination of cyclamate has been developed and single-laboratory validated for a range of foodstuffs including carbonated and fruit-juice drinks, fruit preserves, spreads, and dairy desserts. The method uses the peroxide oxidation of cyclamate to cyclohexylamine followed by derivatization with trinitrobenzenesulfonic acid and analysis by a modified reversed-phase high-performance liquid chromatography-ultraviolet light (HPLC-UV). Cycloheptylamine is used as an internal standard. The limits of detection were in the range 1-20 mg kg(-1) and the analysis was linear up to 1300 mg kg(-1) cyclamic acid in foods and up to 67 mg l(-1) in beverages. Analytical recovery was between 82% and 123%, and results were recovery corrected. Precision was within experimentally predicted levels for all of the matrices tested and Horrat values for the combined standard uncertainty associated with the measurement of cyclamate between 0.4 (water-based drinks) and 1.7 (spreads). The method was used successfully to test three soft drink samples for homogeneity before analytical performance assessment. The method is recommended for use in monitoring compliance and for formal testing by collaborative trial.

Monte Carlo simulation of the radiant field produced by a multiple-lamp quartz heating system

NASA Technical Reports Server (NTRS)

Turner, Travis L.

1991-01-01

A method is developed for predicting the radiant heat flux distribution produced by a reflected bank of tungsten-filament tubular-quartz radiant heaters. The method is correlated with experimental results from two cases, one consisting of a single lamp and a flat reflector and the other consisting of a single lamp and a parabolic reflector. The simulation methodology, computer implementation, and experimental procedures are discussed. Analytical refinements necessary for comparison with experiment are discussed and applied to a multilamp, common reflector heating system.

Quantitative evaluation of cross correlation between two finite-length time series with applications to single-molecule FRET.

PubMed

Hanson, Jeffery A; Yang, Haw

2008-11-06

The statistical properties of the cross correlation between two time series has been studied. An analytical expression for the cross correlation function's variance has been derived. On the basis of these results, a statistically robust method has been proposed to detect the existence and determine the direction of cross correlation between two time series. The proposed method has been characterized by computer simulations. Applications to single-molecule fluorescence spectroscopy are discussed. The results may also find immediate applications in fluorescence correlation spectroscopy (FCS) and its variants.

Reducing background contributions in fluorescence fluctuation time-traces for single-molecule measurements in solution.

PubMed

Földes-Papp, Zeno; Liao, Shih-Chu Jeff; You, Tiefeng; Barbieri, Beniamino

2009-08-01

We first report on the development of new microscope means that reduce background contributions in fluorescence fluctuation methods: i) excitation shutter, ii) electronic switches, and iii) early and late time-gating. The elements allow for measuring molecules at low analyte concentrations. We first found conditions of early and late time-gating with time-correlated single-photon counting that made the fluorescence signal as bright as possible compared with the fluctuations in the background count rate in a diffraction-limited optical set-up. We measured about a 140-fold increase in the amplitude of autocorrelated fluorescence fluctuations at the lowest analyte concentration of about 15 pM, which gave a signal-to-background advantage of more than two-orders of magnitude. The results of this original article pave the way for single-molecule detection in solution and in live cells without immobilization or hydrodynamic/electrokinetic focusing at longer observation times than are currently available.

Nondestructive assessment of timber bridges using a vibration-based method

Treesearch

Xiping Wang; James P. Wacker; Robert J. Ross; Brian K. Brashaw

2005-01-01

This paper describes an effort to develop a global dynamic testing technique for evaluating the overall stiffness of timber bridge superstructures. A forced vibration method was used to measure the natural frequency of single-span timber bridges in the laboratory and field. An analytical model based on simple beam theory was proposed to represent the relationship...

An Analytical Assessment of NASA's N+1 Subsonic Fixed Wing Project Noise Goal

NASA Technical Reports Server (NTRS)

Berton, Jeffrey J.; Envia, Edmane; Burley, Casey L.

2009-01-01

The Subsonic Fixed Wing Project of NASA's Fundamental Aeronautics Program has adopted a noise reduction goal for new, subsonic, single-aisle, civil aircraft expected to replace current 737 and A320 airplanes. These so-called 'N+1' aircraft - designated in NASA vernacular as such since they will follow the current, in-service, 'N' airplanes - are hoped to achieve certification noise goal levels of 32 cumulative EPNdB under current Stage 4 noise regulations. A notional, N+1, single-aisle, twinjet transport with ultrahigh bypass ratio turbofan engines is analyzed in this study using NASA software and methods. Several advanced noise-reduction technologies are analytically applied to the propulsion system and airframe. Certification noise levels are predicted and compared with the NASA goal.

Environmental and human monitoring of Americium-241 utilizing extraction chromatography and {alpha}-Spectrometry

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

Goldstein, S.J.; Hensley, C.A.; Armenta, C.E.

1997-03-01

Recent developments in extraction chromatography have simplified the separation of americium from complex matrices in preparation for {alpha}-spectroscopy relative to traditional methods. Here we present results of procedures developed/adapted for water, air, and bioassay samples with less than 1 g of inorganic residue. Prior analytical methods required the use of a complex, multistage procedure for separation of americium from these matrices. The newer, simplified procedure requires only a single 2 mL extraction chromatographic separation for isolation of Am and lanthanides from other components of the sample. This method has been implemented on an extensive variety of `real` environmental and bioassaymore » samples from the Los Alamos area, and consistently reliable and accurate results with appropriate detection limits have been obtained. The new method increases analytical throughput by a factor of {approx}2 and decreases environmental hazards from acid and mixed-waste generation relative to the prior technique. Analytical accuracy, reproducibility, and reliability are also significantly improved over the more complex and laborious method used previously. 24 refs., 2 figs., 2 tabs.« less

Lack of correlation between reaction speed and analytical sensitivity in isothermal amplification reveals the value of digital methods for optimization: validation using digital real-time RT-LAMP.

PubMed

Khorosheva, Eugenia M; Karymov, Mikhail A; Selck, David A; Ismagilov, Rustem F

2016-01-29

In this paper, we asked if it is possible to identify the best primers and reaction conditions based on improvements in reaction speed when optimizing isothermal reactions. We used digital single-molecule, real-time analyses of both speed and efficiency of isothermal amplification reactions, which revealed that improvements in the speed of isothermal amplification reactions did not always correlate with improvements in digital efficiency (the fraction of molecules that amplify) or with analytical sensitivity. However, we observed that the speeds of amplification for single-molecule (in a digital device) and multi-molecule (e.g. in a PCR well plate) formats always correlated for the same conditions. Also, digital efficiency correlated with the analytical sensitivity of the same reaction performed in a multi-molecule format. Our finding was supported experimentally with examples of primer design, the use or exclusion of loop primers in different combinations, and the use of different enzyme mixtures in one-step reverse-transcription loop-mediated amplification (RT-LAMP). Our results show that measuring the digital efficiency of amplification of single-template molecules allows quick, reliable comparisons of the analytical sensitivity of reactions under any two tested conditions, independent of the speeds of the isothermal amplification reactions. © The Author(s) 2015. Published by Oxford University Press on behalf of Nucleic Acids Research.

Simple functionalization method for single conical pores with a polydopamine layer

NASA Astrophysics Data System (ADS)

Horiguchi, Yukichi; Goda, Tatsuro; Miyahara, Yuji

2018-04-01

Resistive pulse sensing (RPS) is an interesting analytical system in which micro- to nanosized pores are used to evaluate particles or small analytes. Recently, molecular immobilization techniques to improve the performance of RPS have been reported. The problem in functionalization for RPS is that molecular immobilization by chemical reaction is restricted by the pore material type. Herein, a simple functionalization is performed using mussel-inspired polydopamine as an intermediate layer to connect the pore material with functional molecules.

Analytical Energy Gradients for Excited-State Coupled-Cluster Methods

NASA Astrophysics Data System (ADS)

Wladyslawski, Mark; Nooijen, Marcel

The equation-of-motion coupled-cluster (EOM-CC) and similarity transformed equation-of-motion coupled-cluster (STEOM-CC) methods have been firmly established as accurate and routinely applicable extensions of single-reference coupled-cluster theory to describe electronically excited states. An overview of these methods is provided, with emphasis on the many-body similarity transform concept that is the key to a rationalization of their accuracy. The main topic of the paper is the derivation of analytical energy gradients for such non-variational electronic structure approaches, with an ultimate focus on obtaining their detailed algebraic working equations. A general theoretical framework using Lagrange's method of undetermined multipliers is presented, and the method is applied to formulate the EOM-CC and STEOM-CC gradients in abstract operator terms, following the previous work in [P.G. Szalay, Int. J. Quantum Chem. 55 (1995) 151] and [S.R. Gwaltney, R.J. Bartlett, M. Nooijen, J. Chem. Phys. 111 (1999) 58]. Moreover, the systematics of the Lagrange multiplier approach is suitable for automation by computer, enabling the derivation of the detailed derivative equations through a standardized and direct procedure. To this end, we have developed the SMART (Symbolic Manipulation and Regrouping of Tensors) package of automated symbolic algebra routines, written in the Mathematica programming language. The SMART toolkit provides the means to expand, differentiate, and simplify equations by manipulation of the detailed algebraic tensor expressions directly. The Lagrangian multiplier formulation establishes a uniform strategy to perform the automated derivation in a standardized manner: A Lagrange multiplier functional is constructed from the explicit algebraic equations that define the energy in the electronic method; the energy functional is then made fully variational with respect to all of its parameters, and the symbolic differentiations directly yield the explicit equations for the wavefunction amplitudes, the Lagrange multipliers, and the analytical gradient via the perturbation-independent generalized Hellmann-Feynman effective density matrix. This systematic automated derivation procedure is applied to obtain the detailed gradient equations for the excitation energy (EE-), double ionization potential (DIP-), and double electron affinity (DEA-) similarity transformed equation-of-motion coupled-cluster singles-and-doubles (STEOM-CCSD) methods. In addition, the derivatives of the closed-shell-reference excitation energy (EE-), ionization potential (IP-), and electron affinity (EA-) equation-of-motion coupled-cluster singles-and-doubles (EOM-CCSD) methods are derived. Furthermore, the perturbative EOM-PT and STEOM-PT gradients are obtained. The algebraic derivative expressions for these dozen methods are all derived here uniformly through the automated Lagrange multiplier process and are expressed compactly in a chain-rule/intermediate-density formulation, which facilitates a unified modular implementation of analytic energy gradients for CCSD/PT-based electronic methods. The working equations for these analytical gradients are presented in full detail, and their factorization and implementation into an efficient computer code are discussed.

A rapid and sensitive LC-MS/MS assay for the determination of saxagliptin and its active metabolite 5-hydroxy saxagliptin in human plasma and its application to a pharmacokinetic study.

PubMed

Batta, N; Pilli, N R; Derangula, V R; Vurimindi, H B; Damaramadugu, R; Yejella, R P

2015-03-01

The authors proposed a simple, rapid and sensitive liquid chromatography-tandem mass spectrometric (LC-MS/MS) assay method for the simultaneous determination of saxagliptin and its active metabolite 5-hydroxy saxagliptin in human plasma. The developed method was fully validated as per the US FDA guidelines. The method utilized stable labeled isotopes saxagliptin-15 N d2 (IS1) and 5-hydroxy saxagliptin-15 N-d2 (IS2) as internal standards for the quantification of saxagliptin and 5-hydroxy saxagliptin, respectively. Analytes and the internal standards were extracted from human plasma by a single step solid-phase extraction technique without drying, evaporation and reconstitution steps. The optimized mobile phase was composed of 0.1% acetic acid in 5 mM ammonium acetate and acetonitrile (30:70, v/v) and delivered at a flow rate of 0.85 mL/min. The method exhibits the linear calibration range of 0.05-100 ng/mL for both the analytes. The precision and accuracy results for both the analytes were well within the acceptance limits. The different stability experiments conducted in aqueous samples and in matrix samples are meeting the acceptance criteria. The chromatographic run time was set at 1.8 min; hence more than 400 samples can be analyzed in a single day. © Georg Thieme Verlag KG Stuttgart · New York.

Dimensional transitions in thermodynamic properties of ideal Maxwell-Boltzmann gases

NASA Astrophysics Data System (ADS)

Aydin, Alhun; Sisman, Altug

2015-04-01

An ideal Maxwell-Boltzmann gas confined in various rectangular nanodomains is considered under quantum size effects. Thermodynamic quantities are calculated from their relations with the partition function, which consists of triple infinite summations over momentum states in each direction. To obtain analytical expressions, summations are converted to integrals for macrosystems by a continuum approximation, which fails at the nanoscale. To avoid both the numerical calculation of summations and the failure of their integral approximations at the nanoscale, a method which gives an analytical expression for a single particle partition function (SPPF) is proposed. It is shown that a dimensional transition in momentum space occurs at a certain magnitude of confinement. Therefore, to represent the SPPF by lower-dimensional analytical expressions becomes possible, rather than numerical calculation of summations. Considering rectangular domains with different aspect ratios, a comparison of the results of derived expressions with those of summation forms of the SPPF is made. It is shown that analytical expressions for the SPPF give very precise results with maximum relative errors of around 1%, 2% and 3% at exactly the transition point for single, double and triple transitions, respectively. Based on dimensional transitions, expressions for free energy, entropy, internal energy, chemical potential, heat capacity and pressure are given analytically valid for any scale.

Recursively constructing analytic expressions for equilibrium distributions of stochastic biochemical reaction networks.

PubMed

Meng, X Flora; Baetica, Ania-Ariadna; Singhal, Vipul; Murray, Richard M

2017-05-01

Noise is often indispensable to key cellular activities, such as gene expression, necessitating the use of stochastic models to capture its dynamics. The chemical master equation (CME) is a commonly used stochastic model of Kolmogorov forward equations that describe how the probability distribution of a chemically reacting system varies with time. Finding analytic solutions to the CME can have benefits, such as expediting simulations of multiscale biochemical reaction networks and aiding the design of distributional responses. However, analytic solutions are rarely known. A recent method of computing analytic stationary solutions relies on gluing simple state spaces together recursively at one or two states. We explore the capabilities of this method and introduce algorithms to derive analytic stationary solutions to the CME. We first formally characterize state spaces that can be constructed by performing single-state gluing of paths, cycles or both sequentially. We then study stochastic biochemical reaction networks that consist of reversible, elementary reactions with two-dimensional state spaces. We also discuss extending the method to infinite state spaces and designing the stationary behaviour of stochastic biochemical reaction networks. Finally, we illustrate the aforementioned ideas using examples that include two interconnected transcriptional components and biochemical reactions with two-dimensional state spaces. © 2017 The Author(s).

Recursively constructing analytic expressions for equilibrium distributions of stochastic biochemical reaction networks

PubMed Central

Baetica, Ania-Ariadna; Singhal, Vipul; Murray, Richard M.

2017-01-01

Noise is often indispensable to key cellular activities, such as gene expression, necessitating the use of stochastic models to capture its dynamics. The chemical master equation (CME) is a commonly used stochastic model of Kolmogorov forward equations that describe how the probability distribution of a chemically reacting system varies with time. Finding analytic solutions to the CME can have benefits, such as expediting simulations of multiscale biochemical reaction networks and aiding the design of distributional responses. However, analytic solutions are rarely known. A recent method of computing analytic stationary solutions relies on gluing simple state spaces together recursively at one or two states. We explore the capabilities of this method and introduce algorithms to derive analytic stationary solutions to the CME. We first formally characterize state spaces that can be constructed by performing single-state gluing of paths, cycles or both sequentially. We then study stochastic biochemical reaction networks that consist of reversible, elementary reactions with two-dimensional state spaces. We also discuss extending the method to infinite state spaces and designing the stationary behaviour of stochastic biochemical reaction networks. Finally, we illustrate the aforementioned ideas using examples that include two interconnected transcriptional components and biochemical reactions with two-dimensional state spaces. PMID:28566513

Force and Conductance Spectroscopy of Single Molecule Junctions

NASA Astrophysics Data System (ADS)

Frei, Michael

Investigation of mechanical properties of single molecule junctions is crucial to develop an understanding and enable control of single molecular junctions. This work presents an experimental and analytical approach that enables the statistical evaluation of force and simultaneous conductance data of metallic atomic point contacts and molecular junctions. A conductive atomic force microscope based break junction technique is developed to form single molecular junctions and collect conductance and force data simultaneously. Improvements of the optical components have been achieved through the use of a super-luminescent diode, enabling tremendous increases in force resolution. An experimental procedure to collect data for various molecular junctions has been developed and includes deposition, calibration, and analysis methods. For the statistical analysis of force, novel approaches based on two dimensional histograms and a direct force identification method are presented. The two dimensional method allows for an unbiased evaluation of force events that are identified using corresponding conductance signatures. This is not always possible however, and in these situations, the force based identification of junction rearrangement events is an attractive alternative method. This combined experimental and analytical approach is then applied to three studies: First, the impact of molecular backbones to the mechanical behavior of single molecule junctions is investigated and it is found that junctions formed with identical linkers but different backbone structure result in junctions with varying breaking forces. All molecules used show a clear molecular signature and force data can be evaluated using the 2D method. Second, the effects of the linker group used to attach molecules to gold electrodes are investigated. A study of four alkane molecules with different linkers finds a drastic difference in the evolution of donor-acceptor and covalently bonded molecules respectively. In fact, the covalent bond is found to significantly distort the metal electrode rearrangement such that junction rearrangement events can no longer be identified with a clean and well defined conductance signature. For this case, the force based identification process is used. Third, results for break junction measurements with different metals are presented. It is found that silver and palladium junctions rupture with forces different from those of gold contacts. In the case of silver experiments in ambient conditions, we can also identify oxygen impurities in the silver contact formation process, leading to force and conductance measurements of silver-oxygen structures. For the future, this work provides an experimental and analytical foundation that will enable insights into single molecule systems not previously accessible.

Analysis of Ethanolamines: Validation of Semi-Volatile Analysis by HPLC-MS/MS by EPA Method MS888

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

Owens, J; Vu, A; Koester, C

The Environmental Protection Agency's (EPA) Region 5 Chicago Regional Laboratory (CRL) developed a method titled 'Analysis of Diethanolamine, Triethanolamine, n-Methyldiethanolamine, and n-Ethyldiethanolamine in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS): EPA Method MS888'. This draft standard operating procedure (SOP) was distributed to multiple EPA laboratories and to Lawrence Livermore National Laboratory, which was tasked to serve as a reference laboratory for EPA's Environmental Reference Laboratory Network (ERLN) and to develop and validate analytical procedures. The primary objective of this study was to validate and verify the analytical procedures described in 'EPA Method MS888' for analysis of themore » listed ethanolamines in aqueous samples. The gathered data from this validation study will be used to: (1) demonstrate analytical method performance; (2) generate quality control acceptance criteria; and (3) revise the SOP to provide a validated method that would be available for use during a homeland security event. The data contained in this report will be compiled, by EPA CRL, with data generated by other EPA Regional laboratories so that performance metrics of 'EPA Method MS888' can be determined.« less

On the critical forcing amplitude of forced nonlinear oscillators

NASA Astrophysics Data System (ADS)

Febbo, Mariano; Ji, Jinchen C.

2013-12-01

The steady-state response of forced single degree-of-freedom weakly nonlinear oscillators under primary resonance conditions can exhibit saddle-node bifurcations, jump and hysteresis phenomena, if the amplitude of the excitation exceeds a certain value. This critical value of excitation amplitude or critical forcing amplitude plays an important role in determining the occurrence of saddle-node bifurcations in the frequency-response curve. This work develops an alternative method to determine the critical forcing amplitude for single degree-of-freedom nonlinear oscillators. Based on Lagrange multipliers approach, the proposed method considers the calculation of the critical forcing amplitude as an optimization problem with constraints that are imposed by the existence of locations of vertical tangency. In comparison with the Gröbner basis method, the proposed approach is more straightforward and thus easy to apply for finding the critical forcing amplitude both analytically and numerically. Three examples are given to confirm the validity of the theoretical predictions. The first two present the analytical form for the critical forcing amplitude and the third one is an example of a numerically computed solution.

MODULAR ANALYTICS: A New Approach to Automation in the Clinical Laboratory.

PubMed

Horowitz, Gary L; Zaman, Zahur; Blanckaert, Norbert J C; Chan, Daniel W; Dubois, Jeffrey A; Golaz, Olivier; Mensi, Noury; Keller, Franz; Stolz, Herbert; Klingler, Karl; Marocchi, Alessandro; Prencipe, Lorenzo; McLawhon, Ronald W; Nilsen, Olaug L; Oellerich, Michael; Luthe, Hilmar; Orsonneau, Jean-Luc; Richeux, Gérard; Recio, Fernando; Roldan, Esther; Rymo, Lars; Wicktorsson, Anne-Charlotte; Welch, Shirley L; Wieland, Heinrich; Grawitz, Andrea Busse; Mitsumaki, Hiroshi; McGovern, Margaret; Ng, Katherine; Stockmann, Wolfgang

2005-01-01

MODULAR ANALYTICS (Roche Diagnostics) (MODULAR ANALYTICS, Elecsys and Cobas Integra are trademarks of a member of the Roche Group) represents a new approach to automation for the clinical chemistry laboratory. It consists of a control unit, a core unit with a bidirectional multitrack rack transportation system, and three distinct kinds of analytical modules: an ISE module, a P800 module (44 photometric tests, throughput of up to 800 tests/h), and a D2400 module (16 photometric tests, throughput up to 2400 tests/h). MODULAR ANALYTICS allows customised configurations for various laboratory workloads. The performance and practicability of MODULAR ANALYTICS were evaluated in an international multicentre study at 16 sites. Studies included precision, accuracy, analytical range, carry-over, and workflow assessment. More than 700 000 results were obtained during the course of the study. Median between-day CVs were typically less than 3% for clinical chemistries and less than 6% for homogeneous immunoassays. Median recoveries for nearly all standardised reference materials were within 5% of assigned values. Method comparisons versus current existing routine instrumentation were clinically acceptable in all cases. During the workflow studies, the work from three to four single workstations was transferred to MODULAR ANALYTICS, which offered over 100 possible methods, with reduction in sample splitting, handling errors, and turnaround time. Typical sample processing time on MODULAR ANALYTICS was less than 30 minutes, an improvement from the current laboratory systems. By combining multiple analytic units in flexible ways, MODULAR ANALYTICS met diverse laboratory needs and offered improvement in workflow over current laboratory situations. It increased overall efficiency while maintaining (or improving) quality.

MODULAR ANALYTICS: A New Approach to Automation in the Clinical Laboratory

PubMed Central

Zaman, Zahur; Blanckaert, Norbert J. C.; Chan, Daniel W.; Dubois, Jeffrey A.; Golaz, Olivier; Mensi, Noury; Keller, Franz; Stolz, Herbert; Klingler, Karl; Marocchi, Alessandro; Prencipe, Lorenzo; McLawhon, Ronald W.; Nilsen, Olaug L.; Oellerich, Michael; Luthe, Hilmar; Orsonneau, Jean-Luc; Richeux, Gérard; Recio, Fernando; Roldan, Esther; Rymo, Lars; Wicktorsson, Anne-Charlotte; Welch, Shirley L.; Wieland, Heinrich; Grawitz, Andrea Busse; Mitsumaki, Hiroshi; McGovern, Margaret; Ng, Katherine; Stockmann, Wolfgang

2005-01-01

MODULAR ANALYTICS (Roche Diagnostics) (MODULAR ANALYTICS, Elecsys and Cobas Integra are trademarks of a member of the Roche Group) represents a new approach to automation for the clinical chemistry laboratory. It consists of a control unit, a core unit with a bidirectional multitrack rack transportation system, and three distinct kinds of analytical modules: an ISE module, a P800 module (44 photometric tests, throughput of up to 800 tests/h), and a D2400 module (16 photometric tests, throughput up to 2400 tests/h). MODULAR ANALYTICS allows customised configurations for various laboratory workloads. The performance and practicability of MODULAR ANALYTICS were evaluated in an international multicentre study at 16 sites. Studies included precision, accuracy, analytical range, carry-over, and workflow assessment. More than 700 000 results were obtained during the course of the study. Median between-day CVs were typically less than 3% for clinical chemistries and less than 6% for homogeneous immunoassays. Median recoveries for nearly all standardised reference materials were within 5% of assigned values. Method comparisons versus current existing routine instrumentation were clinically acceptable in all cases. During the workflow studies, the work from three to four single workstations was transferred to MODULAR ANALYTICS, which offered over 100 possible methods, with reduction in sample splitting, handling errors, and turnaround time. Typical sample processing time on MODULAR ANALYTICS was less than 30 minutes, an improvement from the current laboratory systems. By combining multiple analytic units in flexible ways, MODULAR ANALYTICS met diverse laboratory needs and offered improvement in workflow over current laboratory situations. It increased overall efficiency while maintaining (or improving) quality. PMID:18924721

Nonadiabatic dynamics of electron transfer in solution: Explicit and implicit solvent treatments that include multiple relaxation time scales

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

Schwerdtfeger, Christine A.; Soudackov, Alexander V.; Hammes-Schiffer, Sharon, E-mail: shs3@illinois.edu

2014-01-21

The development of efficient theoretical methods for describing electron transfer (ET) reactions in condensed phases is important for a variety of chemical and biological applications. Previously, dynamical dielectric continuum theory was used to derive Langevin equations for a single collective solvent coordinate describing ET in a polar solvent. In this theory, the parameters are directly related to the physical properties of the system and can be determined from experimental data or explicit molecular dynamics simulations. Herein, we combine these Langevin equations with surface hopping nonadiabatic dynamics methods to calculate the rate constants for thermal ET reactions in polar solvents formore » a wide range of electronic couplings and reaction free energies. Comparison of explicit and implicit solvent calculations illustrates that the mapping from explicit to implicit solvent models is valid even for solvents exhibiting complex relaxation behavior with multiple relaxation time scales and a short-time inertial response. The rate constants calculated for implicit solvent models with a single solvent relaxation time scale corresponding to water, acetonitrile, and methanol agree well with analytical theories in the Golden rule and solvent-controlled regimes, as well as in the intermediate regime. The implicit solvent models with two relaxation time scales are in qualitative agreement with the analytical theories but quantitatively overestimate the rate constants compared to these theories. Analysis of these simulations elucidates the importance of multiple relaxation time scales and the inertial component of the solvent response, as well as potential shortcomings of the analytical theories based on single time scale solvent relaxation models. This implicit solvent approach will enable the simulation of a wide range of ET reactions via the stochastic dynamics of a single collective solvent coordinate with parameters that are relevant to experimentally accessible systems.« less

Aerosol hygroscopic growth parameterization based on a solute specific coefficient

NASA Astrophysics Data System (ADS)

Metzger, S.; Steil, B.; Xu, L.; Penner, J. E.; Lelieveld, J.

2011-09-01

Water is a main component of atmospheric aerosols and its amount depends on the particle chemical composition. We introduce a new parameterization for the aerosol hygroscopic growth factor (HGF), based on an empirical relation between water activity (aw) and solute molality (μs) through a single solute specific coefficient νi. Three main advantages are: (1) wide applicability, (2) simplicity and (3) analytical nature. (1) Our approach considers the Kelvin effect and covers ideal solutions at large relative humidity (RH), including CCN activation, as well as concentrated solutions with high ionic strength at low RH such as the relative humidity of deliquescence (RHD). (2) A single νi coefficient suffices to parameterize the HGF for a wide range of particle sizes, from nanometer nucleation mode to micrometer coarse mode particles. (3) In contrast to previous methods, our analytical aw parameterization depends not only on a linear correction factor for the solute molality, instead νi also appears in the exponent in form x · ax. According to our findings, νi can be assumed constant for the entire aw range (0-1). Thus, the νi based method is computationally efficient. In this work we focus on single solute solutions, where νi is pre-determined with the bisection method from our analytical equations using RHD measurements and the saturation molality μssat. The computed aerosol HGF and supersaturation (Köhler-theory) compare well with the results of the thermodynamic reference model E-AIM for the key compounds NaCl and (NH4)2SO4 relevant for CCN modeling and calibration studies. The equations introduced here provide the basis of our revised gas-liquid-solid partitioning model, i.e. version 4 of the EQuilibrium Simplified Aerosol Model (EQSAM4), described in a companion paper.

Analytical methods for determination of mycotoxins: a review.

PubMed

Turner, Nicholas W; Subrahmanyam, Sreenath; Piletsky, Sergey A

2009-01-26

Mycotoxins are small (MW approximately 700), toxic chemical products formed as secondary metabolites by a few fungal species that readily colonise crops and contaminate them with toxins in the field or after harvest. Ochratoxins and Aflatoxins are mycotoxins of major significance and hence there has been significant research on broad range of analytical and detection techniques that could be useful and practical. Due to the variety of structures of these toxins, it is impossible to use one standard technique for analysis and/or detection. Practical requirements for high-sensitivity analysis and the need for a specialist laboratory setting create challenges for routine analysis. Several existing analytical techniques, which offer flexible and broad-based methods of analysis and in some cases detection, have been discussed in this manuscript. There are a number of methods used, of which many are lab-based, but to our knowledge there seems to be no single technique that stands out above the rest, although analytical liquid chromatography, commonly linked with mass spectroscopy is likely to be popular. This review manuscript discusses (a) sample pre-treatment methods such as liquid-liquid extraction (LLE), supercritical fluid extraction (SFE), solid phase extraction (SPE), (b) separation methods such as (TLC), high performance liquid chromatography (HPLC), gas chromatography (GC), and capillary electrophoresis (CE) and (c) others such as ELISA. Further currents trends, advantages and disadvantages and future prospects of these methods have been discussed.

Ultra-performance liquid chromatography/tandem mass spectrometric quantification of structurally diverse drug mixtures using an ESI-APCI multimode ionization source.

PubMed

Yu, Kate; Di, Li; Kerns, Edward; Li, Susan Q; Alden, Peter; Plumb, Robert S

2007-01-01

We report in this paper an ultra-performance liquid chromatography/tandem mass spectrometric (UPLC(R)/MS/MS) method utilizing an ESI-APCI multimode ionization source to quantify structurally diverse analytes. Eight commercial drugs were used as test compounds. Each LC injection was completed in 1 min using a UPLC system coupled with MS/MS multiple reaction monitoring (MRM) detection. Results from three separate sets of experiments are reported. In the first set of experiments, the eight test compounds were analyzed as a single mixture. The mass spectrometer was switching rapidly among four ionization modes (ESI+, ESI-, APCI-, and APCI+) during an LC run. Approximately 8-10 data points were collected across each LC peak. This was insufficient for a quantitative analysis. In the second set of experiments, four compounds were analyzed as a single mixture. The mass spectrometer was switching rapidly among four ionization modes during an LC run. Approximately 15 data points were obtained for each LC peak. Quantification results were obtained with a limit of detection (LOD) as low as 0.01 ng/mL. For the third set of experiments, the eight test compounds were analyzed as a batch. During each LC injection, a single compound was analyzed. The mass spectrometer was detecting at a particular ionization mode during each LC injection. More than 20 data points were obtained for each LC peak. Quantification results were also obtained. This single-compound analytical method was applied to a microsomal stability test. Compared with a typical HPLC method currently used for the microsomal stability test, the injection-to-injection cycle time was reduced to 1.5 min (UPLC method) from 3.5 min (HPLC method). The microsome stability results were comparable with those obtained by traditional HPLC/MS/MS.

Combined use of optical and electron microscopic techniques for the measurement of hygroscopic property, chemical composition, and morphology of individual aerosol particles.

PubMed

Ahn, Kang-Ho; Kim, Sun-Man; Jung, Hae-Jin; Lee, Mi-Jung; Eom, Hyo-Jin; Maskey, Shila; Ro, Chul-Un

2010-10-01

In this work, an analytical method for the characterization of the hygroscopic property, chemical composition, and morphology of individual aerosol particles is introduced. The method, which is based on the combined use of optical and electron microscopic techniques, is simple and easy to apply. An optical microscopic technique was used to perform the visual observation of the phase transformation and hygroscopic growth of aerosol particles on a single particle level. A quantitative energy-dispersive electron probe X-ray microanalysis, named low-Z particle EPMA, was used to perform a quantitative chemical speciation of the same individual particles after the measurement of the hygroscopic property. To validate the analytical methodology, the hygroscopic properties of artificially generated NaCl, KCl, (NH(4))(2)SO(4), and Na(2)SO(4) aerosol particles of micrometer size were investigated. The practical applicability of the analytical method for studying the hygroscopic property, chemical composition, and morphology of ambient aerosol particles is demonstrated.

Simultaneous analysis of nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry.

PubMed

Huang, Yang; Zhang, Tingting; Zhao, Yumei; Zhou, Haibo; Tang, Guangyun; Fillet, Marianne; Crommen, Jacques; Jiang, Zhengjin

2017-09-10

Nucleobases, nucleosides and ginsenosides, which have a significant impact on the physiological activity of organisms, are reported to be the active components of ginseng, while they are less present in ginseng extracts. Few analytical methods have been developed so far to simultaneously analyze these three classes of compounds with different polarities present in ginseng extracts. In the present study, a simple and efficient analytical method was successfully developed for the simultaneous separation of 17 nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry (SFC-MS). The effect of various experimental factors on the separation performance, such as the column type, temperature and backpressure, the type of modifier and additive, and the concentration of make-up solvent were systematically investigated. Under the selected conditions, the developed method was successfully applied to the quality evaluation of 14 batches of ginseng extracts from different origins. The results obtained for the different batches indicate that this method could be employed for the quality assessment of ginseng extracts. Copyright © 2017 Elsevier B.V. All rights reserved.

[Determination of the content of sulfur of coal by the infrared absorption method with high acccuracy].

PubMed

Wang, Hai-Feng; Lu, Hai; Li, Jia; Sun, Guo-Hua; Wang, Jun; Dai, Xin-Hua

2014-02-01

The present paper reported the differential scanning calorimetry-thermogravimetry curves and the infrared (IR) absorption spectrometry under the temperature program analyzed by the combined simultaneous thermal analysis-IR spectrometer. The gas products of coal were identified by the IR spectrometry. This paper emphasized on the combustion at high temperature-IR absorption method, a convenient and accurate method, which measures the content of sulfur in coal indirectly through the determination of the content of sulfur dioxide in the mixed gas products by IR absorption. It was demonstrated, when the instrument was calibrated by varied pure compounds containing sulfur and certified reference materials (CRMs) for coal, that there was a large deviation in the measured sulfur contents. It indicates that the difference in chemical speciations of sulfur between CRMs and the analyte results in a systematic error. The time-IR absorption curve was utilized to analyze the composition of sulfur at low temperatures and high temperatures and then the sulfur content of coal sample was determined by using a CRM for coal with a close composition of sulfur. Therefore, the systematic error due to the difference in chemical speciations of sulfur between the CRM and analyte was eliminated. On the other hand, in this combustion at high temperature-IR absorption method, the mass of CRM and analyte were adjusted to assure the sulfur mass equal and then the CRM and the analyte were measured alternately. This single-point calibration method reduced the effect of the drift of the IR detector and improved the repeatability of results, compared with the conventional multi-point calibration method using the calibration curves of signal intensity vs sulfur mass. The sulfur content results and their standard deviations of an anthracite coal and a bituminous coal with a low sulfur content determined by this modified method were 0.345% (0.004%) and 0.372% (0.008%), respectively. The uncertainty (U, k =2) of sulfur contents of two coal samples was evaluated to be 0.019% and 0.021%, respectively. Two main modifications, namely the calibration using the coal CRM with a similar composition of low-temperature sulfur and high temperature sulfur, and the single-point calibration alternating CRM and analyte, endow the combustion at high temperature-IR absorption method with an accuracy obviously better than that of the ASTM method. Therefore, this modified method has a well potential in the analysis of sulfur content.

Simultaneous detection and quantification of amphetamines, diazepam and its metabolites, cocaine and its metabolites, and opiates in hair by LC-ESI-MS-MS using a single extraction method.

PubMed

Miller, Eleanor I; Wylie, Fiona M; Oliver, John S

2008-09-01

A liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous identification and quantification of amphetamines, diazepam and its metabolites, cocaine and its metabolites, and opiates from hair using a single extraction method. As part of the method development, Gemini C18, Synergi Hydro RP, and Zorbax Stablebond-Phenyl LC columns were tested with three different mobile phases. Analyte recovery and limit of detection were evaluated for two different solid-phase extraction methods that used Bond Elut Certify and Clean Screen cartridges. Phosphate buffer (pH 5.0) was chosen as the optimum hair incubation medium because of the high stability of cocaine and 6-monoacetylmorphine using this method and faster sample preparation. The optimized method was fully validated. Linearity was established over the concentration range 0.2-10 ng/mg hair, and the correlation coefficients were all greater than 0.99. Total extraction recoveries were greater than 76%, detection limits were between 0.02 and 0.09 ng/mg, and the intra- and interday imprecisions were generally less than 20% in spiked hair. The intra- and interbatch imprecision of the method for a pooled authentic hair sample ranged from 1.4 to 23.4% relative standard deviation (RSD) and 8.3 to 25.4% RSD, respectively, for representative analytes from the different drug groups. The percent matrix effect ranged from 63.5 to 135.6%, with most analytes demonstrating ion suppression. Sixteen postmortem samples collected from suspected drug-related deaths were analyzed for the 17 drugs of abuse and metabolites included in the method. The method was sufficiently sensitive and specific for the analysis of drugs and metabolites in postmortem hair samples. There is scope for the inclusion of other target drugs and metabolites in the method.

Analytical Expressions for the Mixed-Order Kinetics Parameters of TL Glow Peaks Based on the two Heating Rates Method.

PubMed

Maghrabi, Mufeed; Al-Abdullah, Tariq; Khattari, Ziad

2018-03-24

The two heating rates method (originally developed for first-order glow peaks) was used for the first time to evaluate the activation energy (E) from glow peaks obeying mixed-order (MO) kinetics. The derived expression for E has an insignificant additional term (on the scale of a few meV) when compared with the first-order case. Hence, the original expression for E using the two heating rates method can be used with excellent accuracy in the case of MO glow peaks. In addition, we derived a simple analytical expression for the MO parameter. The present procedure has the advantage that the MO parameter can now be evaluated using analytical expression instead of using the graphical representation between the geometrical factor and the MO parameter as given by the existing peak shape methods. The applicability of the derived expressions for real samples was demonstrated for the glow curve of Li 2 B 4 O 7 :Mn single crystal. The obtained parameters compare very well with those obtained by glow curve fitting and with the available published data.

Analytical solutions for efficient interpretation of single-well push-pull tracer tests

EPA Science Inventory

Single-well push-pull tracer tests have been used to characterize the extent, fate, and transport of subsurface contamination. Analytical solutions provide one alternative for interpreting test results. In this work, an exact analytical solution to two-dimensional equations descr...

Analytical Modeling for the Bending Resonant Frequency of Multilayered Microresonators with Variable Cross-Section

PubMed Central

Herrera-May, Agustín L.; Aguilera-Cortés, Luz A.; Plascencia-Mora, Hector; Rodríguez-Morales, Ángel L.; Lu, Jian

2011-01-01

Multilayered microresonators commonly use sensitive coating or piezoelectric layers for detection of mass and gas. Most of these microresonators have a variable cross-section that complicates the prediction of their fundamental resonant frequency (generally of the bending mode) through conventional analytical models. In this paper, we present an analytical model to estimate the first resonant frequency and deflection curve of single-clamped multilayered microresonators with variable cross-section. The analytical model is obtained using the Rayleigh and Macaulay methods, as well as the Euler-Bernoulli beam theory. Our model is applied to two multilayered microresonators with piezoelectric excitation reported in the literature. Both microresonators are composed by layers of seven different materials. The results of our analytical model agree very well with those obtained from finite element models (FEMs) and experimental data. Our analytical model can be used to determine the suitable dimensions of the microresonator’s layers in order to obtain a microresonator that operates at a resonant frequency necessary for a particular application. PMID:22164071

Image analysis driven single-cell analytics for systems microbiology.

PubMed

Balomenos, Athanasios D; Tsakanikas, Panagiotis; Aspridou, Zafiro; Tampakaki, Anastasia P; Koutsoumanis, Konstantinos P; Manolakos, Elias S

2017-04-04

Time-lapse microscopy is an essential tool for capturing and correlating bacterial morphology and gene expression dynamics at single-cell resolution. However state-of-the-art computational methods are limited in terms of the complexity of cell movies that they can analyze and lack of automation. The proposed Bacterial image analysis driven Single Cell Analytics (BaSCA) computational pipeline addresses these limitations thus enabling high throughput systems microbiology. BaSCA can segment and track multiple bacterial colonies and single-cells, as they grow and divide over time (cell segmentation and lineage tree construction) to give rise to dense communities with thousands of interacting cells in the field of view. It combines advanced image processing and machine learning methods to deliver very accurate bacterial cell segmentation and tracking (F-measure over 95%) even when processing images of imperfect quality with several overcrowded colonies in the field of view. In addition, BaSCA extracts on the fly a plethora of single-cell properties, which get organized into a database summarizing the analysis of the cell movie. We present alternative ways to analyze and visually explore the spatiotemporal evolution of single-cell properties in order to understand trends and epigenetic effects across cell generations. The robustness of BaSCA is demonstrated across different imaging modalities and microscopy types. BaSCA can be used to analyze accurately and efficiently cell movies both at a high resolution (single-cell level) and at a large scale (communities with many dense colonies) as needed to shed light on e.g. how bacterial community effects and epigenetic information transfer play a role on important phenomena for human health, such as biofilm formation, persisters' emergence etc. Moreover, it enables studying the role of single-cell stochasticity without losing sight of community effects that may drive it.

Model independent approach to the single photoelectron calibration of photomultiplier tubes

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

Saldanha, R.; Grandi, L.; Guardincerri, Y.

2017-08-01

The accurate calibration of photomultiplier tubes is critical in a wide variety of applications in which it is necessary to know the absolute number of detected photons or precisely determine the resolution of the signal. Conventional calibration methods rely on fitting the photomultiplier response to a low intensity light source with analytical approximations to the single photoelectron distribution, often leading to biased estimates due to the inability to accurately model the full distribution, especially at low charge values. In this paper we present a simple statistical method to extract the relevant single photoelectron calibration parameters without making any assumptions aboutmore » the underlying single photoelectron distribution. We illustrate the use of this method through the calibration of a Hamamatsu R11410 photomultiplier tube and study the accuracy and precision of the method using Monte Carlo simulations. The method is found to have significantly reduced bias compared to conventional methods and works under a wide range of light intensities, making it suitable for simultaneously calibrating large arrays of photomultiplier tubes.« less

Single Particle Analysis by Combined Chemical Imaging to Study Episodic Air Pollution Events in Vienna

NASA Astrophysics Data System (ADS)

Ofner, Johannes; Eitenberger, Elisabeth; Friedbacher, Gernot; Brenner, Florian; Hutter, Herbert; Schauer, Gerhard; Kistler, Magdalena; Greilinger, Marion; Lohninger, Hans; Lendl, Bernhard; Kasper-Giebl, Anne

2017-04-01

The aerosol composition of a city like Vienna is characterized by a complex interaction of local emissions and atmospheric input on a regional and continental scale. The identification of major aerosol constituents for basic source appointment and air quality issues needs a high analytical effort. Exceptional episodic air pollution events strongly change the typical aerosol composition of a city like Vienna on a time-scale of few hours to several days. Analyzing the chemistry of particulate matter from these events is often hampered by the sampling time and related sample amount necessary to apply the full range of bulk analytical methods needed for chemical characterization. Additionally, morphological and single particle features are hardly accessible. Chemical Imaging evolved to a powerful tool for image-based chemical analysis of complex samples. As a complementary technique to bulk analytical methods, chemical imaging can address a new access to study air pollution events by obtaining major aerosol constituents with single particle features at high temporal resolutions and small sample volumes. The analysis of the chemical imaging datasets is assisted by multivariate statistics with the benefit of image-based chemical structure determination for direct aerosol source appointment. A novel approach in chemical imaging is combined chemical imaging or so-called multisensor hyperspectral imaging, involving elemental imaging (electron microscopy-based energy dispersive X-ray imaging), vibrational imaging (Raman micro-spectroscopy) and mass spectrometric imaging (Time-of-Flight Secondary Ion Mass Spectrometry) with subsequent combined multivariate analytics. Combined chemical imaging of precipitated aerosol particles will be demonstrated by the following examples of air pollution events in Vienna: Exceptional episodic events like the transformation of Saharan dust by the impact of the city of Vienna will be discussed and compared to samples obtained at a high alpine background site (Sonnblick Observatory, Saharan Dust Event from April 2016). Further, chemical imaging of biological aerosol constituents of an autumnal pollen breakout in Vienna, with background samples from nearby locations from November 2016 will demonstrate the advantages of the chemical imaging approach. Additionally, the chemical fingerprint of an exceptional air pollution event from a local emission source, caused by the pull down process of a building in Vienna will unravel the needs for multisensor imaging, especially the combinational access. Obtained chemical images will be correlated to bulk analytical results. Benefits of the overall methodical access by combining bulk analytics and combined chemical imaging of exceptional episodic air pollution events will be discussed.

New aspects in single-body meteor physics

NASA Astrophysics Data System (ADS)

Pecina, P.; Ceplecha, Z.

1983-03-01

An exact analytical solution of the atmospheric meteoroid single-body problem is presented expressing the distance along the trajectory as a function of time, which yields a least-square fit of the observed trajectory, and analytical expressions for the velocity at the point of maximum deceleration are derived. These results are used to determine the ablation coefficient from observations. These methods are applied to 17 Prairie Network fireballs observed below the maximum deceleration point and to the Innisfree fireball, and the results are found to be superior to the ones obtained with the usual interpolation formula. A model of luminous efficiencies for small velocities and for masses up to several hundred grams based on data on Innisfree and on artificial rocketry meteors is proposed and applied to separate the shape-density coefficient from the meteoroid mass.

Dynamic analysis of fixed-free single-walled carbon nanotube-based bio-sensors because of various viruses.

PubMed

Gupta, A; Joshi, A Y; Sharma, S C; Harsha, S P

2012-09-01

In the present study, the vibrations of the fixed-free single-walled carbon nanotube (SWCNT) with attached bacterium/virus on the tip have been investigated. To explore the suitability of the SWCNT as a bacterium/virus detector device, first the various types of virus have been taken for the study and then the resonant frequencies of fixed-free SWCNT with attachment of those viruses have been simulated. These resonant frequencies are compared with the published analytical data, and it is shown that the finite element method (FEM) simulation results are in good agreement with the analytical data. The results showed the sensitivity and suitability of the SWCNT having different length and different masses (attached at the tip SWCNT) to identify the bacterium or virus.

Viscoelastic stability in a single-screw channel flow

NASA Astrophysics Data System (ADS)

Agbessi, Y.; Bu, L. X.; Béreaux, Y.; Charmeau, J.-Y.

2018-05-01

In this work, we perform a linear stability analysis on pressure and drag flows of an Upper Convected Maxwell viscoelastic fluid. We use the well-recognised method of expanding the disturbances in Chebyschev polynomials and solve the resulting generalized eigenvalues problem with a collocation spectra method. Both the level of elasticity and the back-pressure vary. In a second stage, recent analytic solutions of viscoelastic fluid flows in slowly varying sections [1] are used to extend this stability analysis to flows in a compression or in a diverging section of a single screw channel, for example a wave mixing screw.

An orientation soil survey at the Pebble Cu-Au-Mo porphyry deposit, Alaska

USGS Publications Warehouse

Smith, Steven M.; Eppinger, Robert G.; Fey, David L.; Kelley, Karen D.; Giles, S.A.

2009-01-01

Soil samples were collected in 2007 and 2008 along three traverses across the giant Pebble Cu-Au-Mo porphyry deposit. Within each soil pit, four subsamples were collected following recommended protocols for each of ten commonly-used and proprietary leach/digestion techniques. The significance of geochemical patterns generated by these techniques was classified by visual inspection of plots showing individual element concentration by each analytical method along the 2007 traverse. A simple matrix by element versus method, populated with a value based on the significance classification, provides a method for ranking the utility of methods and elements at this deposit. The interpretation of a complex multi-element dataset derived from multiple analytical techniques is challenging. An example of vanadium results from a single leach technique is used to illustrate the several possible interpretations of the data.

A general statistical test for correlations in a finite-length time series.

PubMed

Hanson, Jeffery A; Yang, Haw

2008-06-07

The statistical properties of the autocorrelation function from a time series composed of independently and identically distributed stochastic variables has been studied. Analytical expressions for the autocorrelation function's variance have been derived. It has been found that two common ways of calculating the autocorrelation, moving-average and Fourier transform, exhibit different uncertainty characteristics. For periodic time series, the Fourier transform method is preferred because it gives smaller uncertainties that are uniform through all time lags. Based on these analytical results, a statistically robust method has been proposed to test the existence of correlations in a time series. The statistical test is verified by computer simulations and an application to single-molecule fluorescence spectroscopy is discussed.

Analytical approaches for the characterization and quantification of nanoparticles in food and beverages.

PubMed

Mattarozzi, Monica; Suman, Michele; Cascio, Claudia; Calestani, Davide; Weigel, Stefan; Undas, Anna; Peters, Ruud

2017-01-01

Estimating consumer exposure to nanomaterials (NMs) in food products and predicting their toxicological properties are necessary steps in the assessment of the risks of this technology. To this end, analytical methods have to be available to detect, characterize and quantify NMs in food and materials related to food, e.g. food packaging and biological samples following metabolization of food. The challenge for the analytical sciences is that the characterization of NMs requires chemical as well as physical information. This article offers a comprehensive analysis of methods available for the detection and characterization of NMs in food and related products. Special attention was paid to the crucial role of sample preparation methods since these have been partially neglected in the scientific literature so far. The currently available instrumental methods are grouped as fractionation, counting and ensemble methods, and their advantages and limitations are discussed. We conclude that much progress has been made over the last 5 years but that many challenges still exist. Future perspectives and priority research needs are pointed out. Graphical Abstract Two possible analytical strategies for the sizing and quantification of Nanoparticles: Asymmetric Flow Field-Flow Fractionation with multiple detectors (allows the determination of true size and mass-based particle size distribution); Single Particle Inductively Coupled Plasma Mass Spectrometry (allows the determination of a spherical equivalent diameter of the particle and a number-based particle size distribution).

Local CC2 response method based on the Laplace transform: analytic energy gradients for ground and excited states.

PubMed

Ledermüller, Katrin; Schütz, Martin

2014-04-28

A multistate local CC2 response method for the calculation of analytic energy gradients with respect to nuclear displacements is presented for ground and electronically excited states. The gradient enables the search for equilibrium geometries of extended molecular systems. Laplace transform is used to partition the eigenvalue problem in order to obtain an effective singles eigenvalue problem and adaptive, state-specific local approximations. This leads to an approximation in the energy Lagrangian, which however is shown (by comparison with the corresponding gradient method without Laplace transform) to be of no concern for geometry optimizations. The accuracy of the local approximation is tested and the efficiency of the new code is demonstrated by application calculations devoted to a photocatalytic decarboxylation process of present interest.

Computing sensitivity and selectivity in parallel factor analysis and related multiway techniques: the need for further developments in net analyte signal theory.

PubMed

Olivieri, Alejandro C

2005-08-01

Sensitivity and selectivity are important figures of merit in multiway analysis, regularly employed for comparison of the analytical performance of methods and for experimental design and planning. They are especially interesting in the second-order advantage scenario, where the latter property allows for the analysis of samples with a complex background, permitting analyte determination even in the presence of unsuspected interferences. Since no general theory exists for estimating the multiway sensitivity, Monte Carlo numerical calculations have been developed for estimating variance inflation factors, as a convenient way of assessing both sensitivity and selectivity parameters for the popular parallel factor (PARAFAC) analysis and also for related multiway techniques. When the second-order advantage is achieved, the existing expressions derived from net analyte signal theory are only able to adequately cover cases where a single analyte is calibrated using second-order instrumental data. However, they fail for certain multianalyte cases, or when third-order data are employed, calling for an extension of net analyte theory. The results have strong implications in the planning of multiway analytical experiments.

Expansion of the scope of AOAC first action method 2012.25 - single-laboratory validation of triphenylmethane dye and leuco metabolite analysis in shrimp, tilapia, catfish, and salmon by LC-MS/MS

USDA-ARS?s Scientific Manuscript database

Prior to conducting a collaborative study of AOAC First Action 2012.25 LC-MS/MS analytical method for the determination of residues of three triphenylmethane dyes (malachite green, crystal violet, and brilliant green) and their metabolites (leucomalachite green and leucocrystal violet) in seafood, a...

Model of separation performance of bilinear gradients in scanning format counter-flow gradient electrofocusing techniques.

PubMed

Shameli, Seyed Mostafa; Glawdel, Tomasz; Ren, Carolyn L

2015-03-01

Counter-flow gradient electrofocusing allows the simultaneous concentration and separation of analytes by generating a gradient in the total velocity of each analyte that is the sum of its electrophoretic velocity and the bulk counter-flow velocity. In the scanning format, the bulk counter-flow velocity is varying with time so that a number of analytes with large differences in electrophoretic mobility can be sequentially focused and passed by a single detection point. Studies have shown that nonlinear (such as a bilinear) velocity gradients along the separation channel can improve both peak capacity and separation resolution simultaneously, which cannot be realized by using a single linear gradient. Developing an effective separation system based on the scanning counter-flow nonlinear gradient electrofocusing technique usually requires extensive experimental and numerical efforts, which can be reduced significantly with the help of analytical models for design optimization and guiding experimental studies. Therefore, this study focuses on developing an analytical model to evaluate the separation performance of scanning counter-flow bilinear gradient electrofocusing methods. In particular, this model allows a bilinear gradient and a scanning rate to be optimized for the desired separation performance. The results based on this model indicate that any bilinear gradient provides a higher separation resolution (up to 100%) compared to the linear case. This model is validated by numerical studies. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Review of recent advances in analytical techniques for the determination of neurotransmitters

PubMed Central

Perry, Maura; Li, Qiang; Kennedy, Robert T.

2009-01-01

Methods and advances for monitoring neurotransmitters in vivo or for tissue analysis of neurotransmitters over the last five years are reviewed. The review is organized primarily by neurotransmitter type. Transmitter and related compounds may be monitored by either in vivo sampling coupled to analytical methods or implanted sensors. Sampling is primarily performed using microdialysis, but low-flow push-pull perfusion may offer advantages of spatial resolution while minimizing the tissue disruption associated with higher flow rates. Analytical techniques coupled to these sampling methods include liquid chromatography, capillary electrophoresis, enzyme assays, sensors, and mass spectrometry. Methods for the detection of amino acid, monoamine, neuropeptide, acetylcholine, nucleoside, and soluable gas neurotransmitters have been developed and improved upon. Advances in the speed and sensitivity of these methods have enabled improvements in temporal resolution and increased the number of compounds detectable. Similar advances have enabled improved detection at tissue samples, with a substantial emphasis on single cell and other small samples. Sensors provide excellent temporal and spatial resolution for in vivo monitoring. Advances in application to catecholamines, indoleamines, and amino acids have been prominent. Improvements in stability, sensitivity, and selectivity of the sensors have been of paramount interest. PMID:19800472

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

PubMed

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

2016-11-01

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

Analytic approach to photoelectron transport.

NASA Technical Reports Server (NTRS)

Stolarski, R. S.

1972-01-01

The equation governing the transport of photoelectrons in the ionosphere is shown to be equivalent to the equation of radiative transfer. In the single-energy approximation this equation is solved in closed form by the method of discrete ordinates for isotropic scattering and for a single-constituent atmosphere. The results include prediction of the angular distribution of photoelectrons at all altitudes and, in particular, the angular distribution of the escape flux. The implications of these solutions in real atmosphere calculations are discussed.

Analytical Modeling of a Double-Sided Flux Concentrating E-Core Transverse Flux Machine with Pole Windings

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

Muljadi, Eduard; Hasan, Iftekhar; Husain, Tausif

In this paper, a nonlinear analytical model based on the Magnetic Equivalent Circuit (MEC) method is developed for a double-sided E-Core Transverse Flux Machine (TFM). The proposed TFM has a cylindrical rotor, sandwiched between E-core stators on both sides. Ferrite magnets are used in the rotor with flux concentrating design to attain high airgap flux density, better magnet utilization, and higher torque density. The MEC model was developed using a series-parallel combination of flux tubes to estimate the reluctance network for different parts of the machine including air gaps, permanent magnets, and the stator and rotor ferromagnetic materials, in amore » two-dimensional (2-D) frame. An iterative Gauss-Siedel method is integrated with the MEC model to capture the effects of magnetic saturation. A single phase, 1 kW, 400 rpm E-Core TFM is analytically modeled and its results for flux linkage, no-load EMF, and generated torque, are verified with Finite Element Analysis (FEA). The analytical model significantly reduces the computation time while estimating results with less than 10 percent error.« less

Double injection/single detection asymmetric flow injection manifold for spectrophotometric determination of ascorbic acid and uric acid: Selection the optimal conditions by MCDM approach based on different criteria weighting methods.

PubMed

Boroumand, Samira; Chamjangali, Mansour Arab; Bagherian, Ghadamali

2017-03-05

A simple and sensitive double injection/single detector flow injection analysis (FIA) method is proposed for the simultaneous kinetic determination of ascorbic acid (AA) and uric acid (UA). This method is based upon the difference between the rates of the AA and UA reactions with Fe 3+ in the presence of 1, 10-phenanthroline (phen). The absorbance of Fe 2+ /1, 10-phenanthroline (Fe-phen) complex obtained as the product was measured spectrophotometrically at 510nm. To reach a good accuracy in the differential kinetic determination via the mathematical manipulations of the transient signals, different criteria were considered in the selection of the optimum conditions. The multi criteria decision making (MCDM) approach was applied for the selection of the optimum conditions. The importance weights of the evaluation criteria were determined using the analytic hierarchy process, entropy method, and compromised weighting (CW). The experimental conditions (alternatives) were ranked by the technique for order preference by similarity to an ideal solution. Under the selected optimum conditions, the obtained analytical signals were linear in the ranges of 0.50-5.00 and 0.50-4.00mgL -1 for AA and UA, respectively. The 3σ detection limits were 0.07mgL -1 for AA and 0.12mgL -1 for UA. The relative standard deviations for four replicate determinations of AA and UA were 2.03% and 3.30% respectively. The method was also applied for the analysis of analytes in the blood serum, Vitamine C tablets, and tap water with satisfactory results. Copyright © 2016. Published by Elsevier B.V.

Double injection/single detection asymmetric flow injection manifold for spectrophotometric determination of ascorbic acid and uric acid: Selection the optimal conditions by MCDM approach based on different criteria weighting methods

NASA Astrophysics Data System (ADS)

Boroumand, Samira; Chamjangali, Mansour Arab; Bagherian, Ghadamali

2017-03-01

A simple and sensitive double injection/single detector flow injection analysis (FIA) method is proposed for the simultaneous kinetic determination of ascorbic acid (AA) and uric acid (UA). This method is based upon the difference between the rates of the AA and UA reactions with Fe3 + in the presence of 1, 10-phenanthroline (phen). The absorbance of Fe2 +/1, 10-phenanthroline (Fe-phen) complex obtained as the product was measured spectrophotometrically at 510 nm. To reach a good accuracy in the differential kinetic determination via the mathematical manipulations of the transient signals, different criteria were considered in the selection of the optimum conditions. The multi criteria decision making (MCDM) approach was applied for the selection of the optimum conditions. The importance weights of the evaluation criteria were determined using the analytic hierarchy process, entropy method, and compromised weighting (CW). The experimental conditions (alternatives) were ranked by the technique for order preference by similarity to an ideal solution. Under the selected optimum conditions, the obtained analytical signals were linear in the ranges of 0.50-5.00 and 0.50-4.00 mg L- 1 for AA and UA, respectively. The 3σ detection limits were 0.07 mg L- 1 for AA and 0.12 mg L- 1 for UA. The relative standard deviations for four replicate determinations of AA and UA were 2.03% and 3.30% respectively. The method was also applied for the analysis of analytes in the blood serum, Vitamine C tablets, and tap water with satisfactory results.

Nanomanipulation-Coupled Matrix-Assisted Laser Desorption/ Ionization-Direct Organelle Mass Spectrometry: A Technique for the Detailed Analysis of Single Organelles

NASA Astrophysics Data System (ADS)

Phelps, Mandy S.; Sturtevant, Drew; Chapman, Kent D.; Verbeck, Guido F.

2016-02-01

We describe a novel technique combining precise organelle microextraction with deposition and matrix-assisted laser desorption/ionization (MALDI) for a rapid, minimally invasive mass spectrometry (MS) analysis of single organelles from living cells. A dual-positioner nanomanipulator workstation was utilized for both extraction of organelle content and precise co-deposition of analyte and matrix solution for MALDI-direct organelle mass spectrometry (DOMS) analysis. Here, the triacylglycerol (TAG) profiles of single lipid droplets from 3T3-L1 adipocytes were acquired and results validated with nanoelectrospray ionization (NSI) MS. The results demonstrate the utility of the MALDI-DOMS technique as it enabled longer mass analysis time, higher ionization efficiency, MS imaging of the co-deposited spot, and subsequent MS/MS capabilities of localized lipid content in comparison to NSI-DOMS. This method provides selective organellar resolution, which complements current biochemical analyses and prompts for subsequent subcellular studies to be performed where limited samples and analyte volume are of concern.

Computing the optimal path in stochastic dynamical systems

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

Bauver, Martha; Forgoston, Eric, E-mail: eric.forgoston@montclair.edu; Billings, Lora

2016-08-15

In stochastic systems, one is often interested in finding the optimal path that maximizes the probability of escape from a metastable state or of switching between metastable states. Even for simple systems, it may be impossible to find an analytic form of the optimal path, and in high-dimensional systems, this is almost always the case. In this article, we formulate a constructive methodology that is used to compute the optimal path numerically. The method utilizes finite-time Lyapunov exponents, statistical selection criteria, and a Newton-based iterative minimizing scheme. The method is applied to four examples. The first example is a two-dimensionalmore » system that describes a single population with internal noise. This model has an analytical solution for the optimal path. The numerical solution found using our computational method agrees well with the analytical result. The second example is a more complicated four-dimensional system where our numerical method must be used to find the optimal path. The third example, although a seemingly simple two-dimensional system, demonstrates the success of our method in finding the optimal path where other numerical methods are known to fail. In the fourth example, the optimal path lies in six-dimensional space and demonstrates the power of our method in computing paths in higher-dimensional spaces.« less

Analytical technologies for influenza virus-like particle candidate vaccines: challenges and emerging approaches

PubMed Central

2013-01-01

Influenza virus-like particle vaccines are one of the most promising ways to respond to the threat of future influenza pandemics. VLPs are composed of viral antigens but lack nucleic acids making them non-infectious which limit the risk of recombination with wild-type strains. By taking advantage of the advancements in cell culture technologies, the process from strain identification to manufacturing has the potential to be completed rapidly and easily at large scales. After closely reviewing the current research done on influenza VLPs, it is evident that the development of quantification methods has been consistently overlooked. VLP quantification at all stages of the production process has been left to rely on current influenza quantification methods (i.e. Hemagglutination assay (HA), Single Radial Immunodiffusion assay (SRID), NA enzymatic activity assays, Western blot, Electron Microscopy). These are analytical methods developed decades ago for influenza virions and final bulk influenza vaccines. Although these methods are time-consuming and cumbersome they have been sufficient for the characterization of final purified material. Nevertheless, these analytical methods are impractical for in-line process monitoring because VLP concentration in crude samples generally falls out of the range of detection for these methods. This consequently impedes the development of robust influenza-VLP production and purification processes. Thus, development of functional process analytical techniques, applicable at every stage during production, that are compatible with different production platforms is in great need to assess, optimize and exploit the full potential of novel manufacturing platforms. PMID:23642219

Novel HPLC-UV Method for Simultaneous Determination of Fat-soluble Vitamins and Coenzyme Q10 in Medicines and Supplements.

PubMed

Temova-Rakuša, Žane; Srečnik, Eva; Roškar, Robert

2017-09-01

A precise, accurate and rapid HPLC-UV method for simultaneous determination of fat-soluble vitamins (vitamin D3, E-acetate, K1, β-carotene, A-palmitate) and coenzyme Q10 was developed and validated according to ICH guidelines. Optimal chromatographic separation of the analytes in minimal analysis time (8 min) was achieved on a Luna C18 150 × 4.6 mm column using a mixture of acetonitrile, tetrahydrofuran and water (50:45:5, v/v/v). The described reversed phase HPLC method is the first published for quantification of these five fat-soluble vitamins and coenzyme Q10 within a single chromatographic run. The method was further applied for quantification of the analytes in selected liquid and solid dosage forms, registered as nutritional supplements and prescription medicines, which confirmed its suitability for routine analysis.

Development of an Analytical Method for the Determination of Amoxicillin in Commercial Drugs and Wastewater Samples, and Assessing its Stability in Simulated Gastric Digestion.

PubMed

Unutkan, Tugçe; Bakirdere, Sezgin; Keyf, Seyfullah

2018-01-01

A highly sensitive analytical HPLC-UV method was developed for the determination of amoxicillin in drugs and wastewater samples at a single wavelength (230 nm). In order to substantially predict the in vivo behavior of amoxicillin, drug samples were subjected to simulated gastric conditions. The calibration plot of the method was linear from 0.050 to 500 mg L-1 with a correlation coefficient of 0.9999. The limit of detection and limit of quantitation were found to be 16 and 54 μg L-1, respectively. The percentage recovery of amoxicillin in wastewater was found to be 97.0 ± 1.6%. The method was successfully applied for the qualitative and quantitative determination of amoxicillin in drug samples including tablets and suspensions. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Use of multiple colorimetric indicators for paper-based microfluidic devices.

PubMed

Dungchai, Wijitar; Chailapakul, Orawon; Henry, Charles S

2010-08-03

We report here the use of multiple indicators for a single analyte for paper-based microfluidic devices (microPAD) in an effort to improve the ability to visually discriminate between analyte concentrations. In existing microPADs, a single dye system is used for the measurement of a single analyte. In our approach, devices are designed to simultaneously quantify analytes using multiple indicators for each analyte improving the accuracy of the assay. The use of multiple indicators for a single analyte allows for different indicator colors to be generated at different analyte concentration ranges as well as increasing the ability to better visually discriminate colors. The principle of our devices is based on the oxidation of indicators by hydrogen peroxide produced by oxidase enzymes specific for each analyte. Each indicator reacts at different peroxide concentrations and therefore analyte concentrations, giving an extended range of operation. To demonstrate the utility of our approach, the mixture of 4-aminoantipyrine and 3,5-dichloro-2-hydroxy-benzenesulfonic acid, o-dianisidine dihydrochloride, potassium iodide, acid black, and acid yellow were chosen as the indicators for simultaneous semi-quantitative measurement of glucose, lactate, and uric acid on a microPAD. Our approach was successfully applied to quantify glucose (0.5-20 mM), lactate (1-25 mM), and uric acid (0.1-7 mM) in clinically relevant ranges. The determination of glucose, lactate, and uric acid in control serum and urine samples was also performed to demonstrate the applicability of this device for biological sample analysis. Finally results for the multi-indicator and single indicator system were compared using untrained readers to demonstrate the improvements in accuracy achieved with the new system. 2010 Elsevier B.V. All rights reserved.

Generalized model of electromigration with 1:1 (analyte:selector) complexation stoichiometry: part II. Application to dual systems and experimental verification.

PubMed

Müllerová, Ludmila; Dubský, Pavel; Gaš, Bohuslav

2015-03-06

Interactions among analyte forms that undergo simultaneous dissociation/protonation and complexation with multiple selectors take the shape of a highly interconnected multi-equilibrium scheme. This makes it difficult to express the effective mobility of the analyte in these systems, which are often encountered in electrophoretical separations, unless a generalized model is introduced. In the first part of this series, we presented the theory of electromigration of a multivalent weakly acidic/basic/amphoteric analyte undergoing complexation with a mixture of an arbitrary number of selectors. In this work we demonstrate the validity of this concept experimentally. The theory leads to three useful perspectives, each of which is closely related to the one originally formulated for simpler systems. If pH, IS and the selector mixture composition are all kept constant, the system is treated as if only a single analyte form interacted with a single selector. If the pH changes at constant IS and mixture composition, the already well-established models of a weakly acidic/basic analyte interacting with a single selector can be employed. Varying the mixture composition at constant IS and pH leads to a situation where virtually a single analyte form interacts with a mixture of selectors. We show how to switch between the three perspectives in practice and confirm that they can be employed interchangeably according to the specific needs by measurements performed in single- and dual-selector systems at a pH where the analyte is fully dissociated, partly dissociated or fully protonated. Weak monoprotic analyte (R-flurbiprofen) and two selectors (native β-cyclodextrin and monovalent positively charged 6-monodeoxy-6-monoamino-β-cyclodextrin) serve as a model system. Copyright © 2015 Elsevier B.V. All rights reserved.

Optical bandgap of semiconductor nanostructures: Methods for experimental data analysis

NASA Astrophysics Data System (ADS)

Raciti, R.; Bahariqushchi, R.; Summonte, C.; Aydinli, A.; Terrasi, A.; Mirabella, S.

2017-06-01

Determination of the optical bandgap (Eg) in semiconductor nanostructures is a key issue in understanding the extent of quantum confinement effects (QCE) on electronic properties and it usually involves some analytical approximation in experimental data reduction and modeling of the light absorption processes. Here, we compare some of the analytical procedures frequently used to evaluate the optical bandgap from reflectance (R) and transmittance (T) spectra. Ge quantum wells and quantum dots embedded in SiO2 were produced by plasma enhanced chemical vapor deposition, and light absorption was characterized by UV-Vis/NIR spectrophotometry. R&T elaboration to extract the absorption spectra was conducted by two approximated methods (single or double pass approximation, single pass analysis, and double pass analysis, respectively) followed by Eg evaluation through linear fit of Tauc or Cody plots. Direct fitting of R&T spectra through a Tauc-Lorentz oscillator model is used as comparison. Methods and data are discussed also in terms of the light absorption process in the presence of QCE. The reported data show that, despite the approximation, the DPA approach joined with Tauc plot gives reliable results, with clear advantages in terms of computational efforts and understanding of QCE.

Optical Parametric Amplification of Single Photon: Statistical Properties and Quantum Interference

NASA Astrophysics Data System (ADS)

Xu, Xue-Xiang; Yuan, Hong-Chun

2014-05-01

By using phase space method, we theoretically investigate the quantum statistical properties and quantum interference of optical parametric amplification of single photon. The statistical properties, such as the Wigner function (WF), average photon number, photon number distribution and parity, are derived analytically for the fields of the two output ports. The results indicate that the fields in the output ports are multiphoton states rather than single photon state due to the amplification of the optical parametric amplifiers (OPA). In addition, the phase sensitivity is also examined by using the detection scheme of parity measurement.

Physical-geometric optics method for large size faceted particles.

PubMed

Sun, Bingqiang; Yang, Ping; Kattawar, George W; Zhang, Xiaodong

2017-10-02

A new physical-geometric optics method is developed to compute the single-scattering properties of faceted particles. It incorporates a general absorption vector to accurately account for inhomogeneous wave effects, and subsequently yields the relevant analytical formulas effective and computationally efficient for absorptive scattering particles. A bundle of rays incident on a certain facet can be traced as a single beam. For a beam incident on multiple facets, a systematic beam-splitting technique based on computer graphics is used to split the original beam into several sub-beams so that each sub-beam is incident only on an individual facet. The new beam-splitting technique significantly reduces the computational burden. The present physical-geometric optics method can be generalized to arbitrary faceted particles with either convex or concave shapes and with a homogeneous or an inhomogeneous (e.g., a particle with a core) composition. The single-scattering properties of irregular convex homogeneous and inhomogeneous hexahedra are simulated and compared to their counterparts from two other methods including a numerically rigorous method.

Monte Carlo calculation of dynamical properties of the two-dimensional Hubbard model

NASA Technical Reports Server (NTRS)

White, S. R.; Scalapino, D. J.; Sugar, R. L.; Bickers, N. E.

1989-01-01

A new method is introduced for analytically continuing imaginary-time data from quantum Monte Carlo calculations to the real-frequency axis. The method is based on a least-squares-fitting procedure with constraints of positivity and smoothness on the real-frequency quantities. Results are shown for the single-particle spectral-weight function and density of states for the half-filled, two-dimensional Hubbard model.

Optimization of detection conditions and single-laboratory validation of a multiresidue method for the determination of 135 pesticides and 25 organic pollutants in grapes and wine by gas chromatography time-of-flight mass spectrometry.

PubMed

Dasgupta, Soma; Banerjee, Kaushik; Dhumal, Kondiba N; Adsule, Pandurang G

2011-01-01

This paper describes single-laboratory validation of a multiresidue method for the determination of 135 pesticides, 12 dioxin-like polychlorinated biphenyls, 12 polyaromatic hydrocarbons, and bisphenol A in grapes and wine by GC/time-of-flight MS in a total run time of 48 min. The method is based on extraction with ethyl acetate in a sample-to-solvent ratio of 1:1, followed by selective dispersive SPE cleanup for grapes and wine. The GC/MS conditions were optimized for the chromatographic separation and to achieve highest S/N for all 160 target analytes, including the temperature-sensitive compounds, like captan and captafol, that are prone to degradation during analysis. An average recovery of 80-120% with RSD < 10% could be attained for all analytes except 17, for which the average recoveries were 70-80%. LOQ ranged within 10-50 ng/g, with < 25% expanded uncertainties, for 155 compounds in grapes and 151 in wine. In the incurred grape and wine samples, the residues of buprofezin, chlorpyriphos, metalaxyl, and myclobutanil were detected, with an RSD of < 5% (n = 6); the results were statistically similar to previously reported validated methods.

How Should Blood Glucose Meter System Analytical Performance Be Assessed?

PubMed

Simmons, David A

2015-08-31

Blood glucose meter system analytical performance is assessed by comparing pairs of meter system and reference instrument blood glucose measurements measured over time and across a broad array of glucose values. Consequently, no single, complete, and ideal parameter can fully describe the difference between meter system and reference results. Instead, a number of assessment tools, both graphical (eg, regression plots, modified Bland-Altman plots, and error grid analysis) and tabular (eg, International Organization for Standardization guidelines, mean absolute difference, and mean absolute relative difference) have been developed to evaluate meter system performance. The strengths and weaknesses of these methods of presenting meter system performance data, including a new method known as Radar Plots, are described here. © 2015 Diabetes Technology Society.

GraphPrints: Towards a Graph Analytic Method for Network Anomaly Detection

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

Harshaw, Chris R; Bridges, Robert A; Iannacone, Michael D

This paper introduces a novel graph-analytic approach for detecting anomalies in network flow data called \\textit{GraphPrints}. Building on foundational network-mining techniques, our method represents time slices of traffic as a graph, then counts graphlets\\textemdash small induced subgraphs that describe local topology. By performing outlier detection on the sequence of graphlet counts, anomalous intervals of traffic are identified, and furthermore, individual IPs experiencing abnormal behavior are singled-out. Initial testing of GraphPrints is performed on real network data with an implanted anomaly. Evaluation shows false positive rates bounded by 2.84\\% at the time-interval level, and 0.05\\% at the IP-level with 100\\% truemore » positive rates at both.« less

ddClone: joint statistical inference of clonal populations from single cell and bulk tumour sequencing data.

PubMed

Salehi, Sohrab; Steif, Adi; Roth, Andrew; Aparicio, Samuel; Bouchard-Côté, Alexandre; Shah, Sohrab P

2017-03-01

Next-generation sequencing (NGS) of bulk tumour tissue can identify constituent cell populations in cancers and measure their abundance. This requires computational deconvolution of allelic counts from somatic mutations, which may be incapable of fully resolving the underlying population structure. Single cell sequencing (SCS) is a more direct method, although its replacement of NGS is impeded by technical noise and sampling limitations. We propose ddClone, which analytically integrates NGS and SCS data, leveraging their complementary attributes through joint statistical inference. We show on real and simulated datasets that ddClone produces more accurate results than can be achieved by either method alone.

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

Griffin, Brian M.; Larson, Vincent E.

Microphysical processes, such as the formation, growth, and evaporation of precipitation, interact with variability and covariances (e.g., fluxes) in moisture and heat content. For instance, evaporation of rain may produce cold pools, which in turn may trigger fresh convection and precipitation. These effects are usually omitted or else crudely parameterized at subgrid scales in weather and climate models.A more formal approach is pursued here, based on predictive, horizontally averaged equations for the variances, covariances, and fluxes of moisture and heat content. These higher-order moment equations contain microphysical source terms. The microphysics terms can be integrated analytically, given a suitably simplemore » warm-rain microphysics scheme and an approximate assumption about the multivariate distribution of cloud-related and precipitation-related variables. Performing the integrations provides exact expressions within an idealized context.A large-eddy simulation (LES) of a shallow precipitating cumulus case is performed here, and it indicates that the microphysical effects on (co)variances and fluxes can be large. In some budgets and altitude ranges, they are dominant terms. The analytic expressions for the integrals are implemented in a single-column, higher-order closure model. Interactive single-column simulations agree qualitatively with the LES. The analytic integrations form a parameterization of microphysical effects in their own right, and they also serve as benchmark solutions that can be compared to non-analytic integration methods.« less

Gold Nanoparticle-Aptamer-Based LSPR Sensing of Ochratoxin A at a Widened Detection Range by Double Calibration Curve Method

NASA Astrophysics Data System (ADS)

Liu, Boshi; Huang, Renliang; Yu, Yanjun; Su, Rongxin; Qi, Wei; He, Zhimin

2018-04-01

Ochratoxin A (OTA) is a type of mycotoxin generated from the metabolism of Aspergillus and Penicillium, and is extremely toxic to humans, livestock, and poultry. However, traditional assays for the detection of OTA are expensive and complicated. Other than OTA aptamer, OTA itself at high concentration can also adsorb on the surface of gold nanoparticles (AuNPs), and further inhibit AuNPs salt aggregation. We herein report a new OTA assay by applying the localized surface plasmon resonance effect of AuNPs and their aggregates. The result obtained from only one single linear calibration curve is not reliable, and so we developed a “double calibration curve” method to address this issue and widen the OTA detection range. A number of other analytes were also examined, and the structural properties of analytes that bind with the AuNPs were further discussed. We found that various considerations must be taken into account in the detection of these analytes when applying AuNP aggregation-based methods due to their different binding strengths.

Attenuation of stress waves in single and multi-layered structures. [mitigation of elastic and plastic stress waves during spacecraft landing

NASA Technical Reports Server (NTRS)

Yang, J. C. S.; Tsui, C. Y.

1972-01-01

Analytical and experimental studies were made of the attenuation of the stress waves during passage through single and multilayer structures. The investigation included studies on elastic and plastic stress wave propagation in the composites and those on shock mitigating material characteristics such as dynamic stress-strain relations and energy absorbing properties. The results of the studies are applied to methods for reducing the stresses imposed on a spacecraft during planetary or ocean landings.

Simplex and duplex event-specific analytical methods for functional biotech maize.

PubMed

Lee, Seong-Hun; Kim, Su-Jeong; Yi, Bu-Young

2009-08-26

Analytical methods are very important in the control of genetically modified organism (GMO) labeling systems or living modified organism (LMO) management for biotech crops. Event-specific primers and probes were developed for qualitative and quantitative analysis for biotech maize event 3272 and LY 038 on the basis of the 3' flanking regions, respectively. The qualitative primers confirmed the specificity by a single PCR product and sensitivity to 0.05% as a limit of detection (LOD). Simplex and duplex quantitative methods were also developed using TaqMan real-time PCR. One synthetic plasmid was constructed from two taxon-specific DNA sequences of maize and two event-specific 3' flanking DNA sequences of event 3272 and LY 038 as reference molecules. In-house validation of the quantitative methods was performed using six levels of mixing samples, from 0.1 to 10.0%. As a result, the biases from the true value and the relative deviations were all within the range of +/-30%. Limits of quantitation (LOQs) of the quantitative methods were all 0.1% for simplex real-time PCRs of event 3272 and LY 038 and 0.5% for duplex real-time PCR of LY 038. This study reports that event-specific analytical methods were applicable for qualitative and quantitative analysis for biotech maize event 3272 and LY 038.

Two Analyte Calibration From The Transient Response Of Potentiometric Sensors Employed With The SIA Technique

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

Cartas, Raul; Mimendia, Aitor; Valle, Manel del

2009-05-23

Calibration models for multi-analyte electronic tongues have been commonly built using a set of sensors, at least one per analyte under study. Complex signals recorded with these systems are formed by the sensors' responses to the analytes of interest plus interferents, from which a multivariate response model is then developed. This work describes a data treatment method for the simultaneous quantification of two species in solution employing the signal from a single sensor. The approach used here takes advantage of the complex information recorded with one electrode's transient after insertion of sample for building the calibration models for both analytes.more » The departure information from the electrode was firstly processed by discrete wavelet for transforming the signals to extract useful information and reduce its length, and then by artificial neural networks for fitting a model. Two different potentiometric sensors were used as study case for simultaneously corroborating the effectiveness of the approach.« less

Inferring subunit stoichiometry from single molecule photobleaching

PubMed Central

2013-01-01

Single molecule photobleaching is a powerful tool for determining the stoichiometry of protein complexes. By attaching fluorophores to proteins of interest, the number of associated subunits in a complex can be deduced by imaging single molecules and counting fluorophore photobleaching steps. Because some bleaching steps might be unobserved, the ensemble of steps will be binomially distributed. In this work, it is shown that inferring the true composition of a complex from such data is nontrivial because binomially distributed observations present an ill-posed inference problem. That is, a unique and optimal estimate of the relevant parameters cannot be extracted from the observations. Because of this, a method has not been firmly established to quantify confidence when using this technique. This paper presents a general inference model for interpreting such data and provides methods for accurately estimating parameter confidence. The formalization and methods presented here provide a rigorous analytical basis for this pervasive experimental tool. PMID:23712552

Biological Nanopores: Confined Spaces for Electrochemical Single-Molecule Analysis.

PubMed

Cao, Chan; Long, Yi-Tao

2018-02-20

Nanopore sensing is developing into a powerful single-molecule approach to investigate the features of biomolecules that are not accessible by studying ensemble systems. When a target molecule is transported through a nanopore, the ions occupying the pore are excluded, resulting in an electrical signal from the intermittent ionic blockade event. By statistical analysis of the amplitudes, duration, frequencies, and shapes of the blockade events, many properties of the target molecule can be obtained in real time at the single-molecule level, including its size, conformation, structure, charge, geometry, and interactions with other molecules. With the development of the use of α-hemolysin to characterize individual polynucleotides, nanopore technology has attracted a wide range of research interest in the fields of biology, physics, chemistry, and nanoscience. As a powerful single-molecule analytical method, nanopore technology has been applied for the detection of various biomolecules, including oligonucleotides, peptides, oligosaccharides, organic molecules, and disease-related proteins. In this Account, we highlight recent developments of biological nanopores in DNA-based sensing and in studying the conformational structures of DNA and RNA. Furthermore, we introduce the application of biological nanopores to investigate the conformations of peptides affected by charge, length, and dipole moment and to study disease-related proteins' structures and aggregation transitions influenced by an inhibitor, a promoter, or an applied voltage. To improve the sensing ability of biological nanopores and further extend their application to a wider range of molecular sensing, we focus on exploring novel biological nanopores, such as aerolysin and Stable Protein 1. Aerolysin exhibits an especially high sensitivity for the detection of single oligonucleotides both in current separation and duration. Finally, to facilitate the use of nanopore measurements and statistical analysis, we develop an integrated current measurement system and an accurate data processing method for nanopore sensing. The unique geometric structure of a biological nanopore offers a distinct advantage as a nanosensor for single-molecule sensing. The construction of the pore entrance is responsible for capturing the target molecule, while the lumen region determines the translocation process of the single molecule. Since the capture of the target molecule is predominantly diffusion-limited, it is expected that the capture ability of the nanopore toward the target analyte could be effectively enhanced by site-directed mutations of key amino acids with desirable groups. Additionally, changing the side chains inside the wall of the biological nanopore could optimize the geometry of the pore and realize an optimal interaction between the single-molecule interface and the analyte. These improvements would allow for high spatial and current resolution of nanopore sensors, which would ensure the possibility of dynamic study of single biomolecules, including their metastable conformations, charge distributions, and interactions. In the future, data analysis with powerful algorithms will make it possible to automatically and statistically extract detailed information while an analyte translocates through the pore. We conclude that these improvements could have tremendous potential applications for nanopore sensing in the near future.

Trace analysis of trimethoprim and sulfonamide, macrolide, quinolone, and tetracycline antibiotics in chlorinated drinking water using liquid chromatography electrospray tandem mass spectrometry

USGS Publications Warehouse

Ye, Z.; Weinberg, H.S.; Meyer, M.T.

2007-01-01

A multirun analytical method has been developed and validated for trace determination of 24 antibiotics including 7 sulfonamides, 3 macrolides, 7 quinolones, 6 tetracyclines, and trimethoprim in chlorine-disinfected drinking water using a single solid-phase extraction method coupled to liquid chromatography with positive electrospray tandem mass spectrometry detection. The analytes were extracted by a hydrophilic-lipophilic balanced resin and eluted with acidified methanol (0.1% formic acid), resulting in analyte recoveries generally above 90%. The limits of quantitation were mostly below 10 ng/L in drinking water. Since the concentrated sample matrix typically caused ion suppression during electrospray ionization, the method of standard addition was used for quantitation. Chlorine residuals in drinking water can react with some antibiotics, but ascorbic acid was found to be an effective chlorine quenching agent without affecting the analysis and stability of the antibiotics in water. A preliminary occurrence study using this method revealed the presence of some antibiotics in drinking waters, including sulfamethoxazole (3.0-3.4 ng/L), macrolides (1.4-4.9 ng/L), and quinolones (1.2-4.0 ng/L). ?? 2007 American Chemical Society.

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.

Simple and Robust N-Glycan Analysis Based on Improved 2-Aminobenzoic Acid Labeling for Recombinant Therapeutic Glycoproteins.

PubMed

Jeong, Yeong Ran; Kim, Sun Young; Park, Young Sam; Lee, Gyun Min

2018-03-21

N-glycans of therapeutic glycoproteins are critical quality attributes that should be monitored throughout all stages of biopharmaceutical development. To reduce both the time for sample preparation and the variations in analytical results, we have developed an N-glycan analysis method that includes improved 2-aminobenzoic acid (2-AA) labeling to easily remove deglycosylated proteins. Using this analytical method, 15 major 2-AA-labeled N-glycans of Enbrel ® were separated into single peaks in hydrophilic interaction chromatography mode and therefore could be quantitated. 2-AA-labeled N-glycans were also highly compatible with in-line quadrupole time-of-flight mass spectrometry (MS) for structural identification. The structures of 15 major and 18 minor N-glycans were identified from their mass values determined by quadrupole time-of-flight MS. Furthermore, the structures of 14 major N-glycans were confirmed by interpreting the MS/MS data of each N-glycan. This analytical method was also successfully applied to neutral N-glycans of Humira ® and highly sialylated N-glycans of NESP ® . Furthermore, the analysis data of Enbrel ® that were accumulated for 2.5 years demonstrated the high-level consistency of this analytical method. Taken together, the results show that a wide repertoire of N-glycans of therapeutic glycoproteins can be analyzed with high efficiency and consistency using the improved 2-AA labeling-based N-glycan analysis method. Copyright © 2018 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Transient vibration analytical modeling and suppressing for vibration absorber system under impulse excitation

NASA Astrophysics Data System (ADS)

Wang, Xi; Yang, Bintang; Yu, Hu; Gao, Yulong

2017-04-01

The impulse excitation of mechanism causes transient vibration. In order to achieve adaptive transient vibration control, a method which can exactly model the response need to be proposed. This paper presents an analytical model to obtain the response of the primary system attached with dynamic vibration absorber (DVA) under impulse excitation. The impulse excitation which can be divided into single-impulse excitation and multi-impulse excitation is simplified as sinusoidal wave to establish the analytical model. To decouple the differential governing equations, a transform matrix is applied to convert the response from the physical coordinate to model coordinate. Therefore, the analytical response in the physical coordinate can be obtained by inverse transformation. The numerical Runge-Kutta method and experimental tests have demonstrated the effectiveness of the analytical model proposed. The wavelet of the response indicates that the transient vibration consists of components with multiple frequencies, and it shows that the modeling results coincide with the experiments. The optimizing simulations based on genetic algorithm and experimental tests demonstrate that the transient vibration of the primary system can be decreased by changing the stiffness of the DVA. The results presented in this paper are the foundations for us to develop the adaptive transient vibration absorber in the future.

Tuning fuzzy PD and PI controllers using reinforcement learning.

PubMed

Boubertakh, Hamid; Tadjine, Mohamed; Glorennec, Pierre-Yves; Labiod, Salim

2010-10-01

In this paper, we propose a new auto-tuning fuzzy PD and PI controllers using reinforcement Q-learning (QL) algorithm for SISO (single-input single-output) and TITO (two-input two-output) systems. We first, investigate the design parameters and settings of a typical class of Fuzzy PD (FPD) and Fuzzy PI (FPI) controllers: zero-order Takagi-Sugeno controllers with equidistant triangular membership functions for inputs, equidistant singleton membership functions for output, Larsen's implication method, and average sum defuzzification method. Secondly, the analytical structures of these typical fuzzy PD and PI controllers are compared to their classical counterpart PD and PI controllers. Finally, the effectiveness of the proposed method is proven through simulation examples. Copyright © 2010 ISA. Published by Elsevier Ltd. All rights reserved.

Beyond single-stream with the Schrödinger method

NASA Astrophysics Data System (ADS)

Uhlemann, Cora; Kopp, Michael

2016-10-01

We investigate large scale structure formation of collisionless dark matter in the phase space description based on the Vlasov-Poisson equation. We present the Schrödinger method, originally proposed by \\cite{WK93} as numerical technique based on the Schrödinger Poisson equation, as an analytical tool which is superior to the common standard pressureless fluid model. Whereas the dust model fails and develops singularities at shell crossing the Schrödinger method encompasses multi-streaming and even virialization.

Headspace single drop microextraction versus dispersive liquid-liquid microextraction using magnetic ionic liquid extraction solvents.

PubMed

An, Jiwoo; Rahn, Kira L; Anderson, Jared L

2017-05-15

A headspace single drop microextraction (HS-SDME) method and a dispersive liquid-liquid microextraction (DLLME) method were developed using two tetrachloromanganate ([MnCl 4 2- ])-based magnetic ionic liquids (MIL) as extraction solvents for the determination of twelve aromatic compounds, including four polyaromatic hydrocarbons, by reversed phase high-performance liquid chromatography (HPLC). The analytical performance of the developed HS-SDME method was compared to the DLLME approach employing the same MILs. In the HS-SDME approach, the magnetic field generated by the magnet was exploited to suspend the MIL solvent from the tip of a rod magnet. The utilization of MILs in HS-SDME resulted in a highly stable microdroplet under elevated temperatures and long extraction times, overcoming a common challenge encountered in traditional SDME approaches of droplet instability. The low UV absorbance of the [MnCl 4 2- ]-based MILs permitted direct analysis of the analyte enriched extraction solvent by HPLC. In HS-SDME, the effects of ionic strength of the sample solution, temperature of the extraction system, extraction time, stir rate, and headspace volume on extraction efficiencies were examined. Coefficients of determination (R 2 ) ranged from 0.994 to 0.999 and limits of detection (LODs) varied from 0.04 to 1.0μgL -1 with relative recoveries from lake water ranging from 70.2% to 109.6%. For the DLLME method, parameters including disperser solvent type and volume, ionic strength of the sample solution, mass of extraction solvent, and extraction time were studied and optimized. Coefficients of determination for the DLLME method varied from 0.997 to 0.999 with LODs ranging from 0.05 to 1.0μgL -1 . Relative recoveries from lake water samples ranged from 68.7% to 104.5%. Overall, the DLLME approach permitted faster extraction times and higher enrichment factors for analytes with low vapor pressure whereas the HS-SDME approach exhibited better extraction efficiencies for analytes with relatively higher vapor pressure. Copyright © 2017 Elsevier B.V. All rights reserved.

The effect of finite geometry on the three-dimensional transfer of solar irradiance in clouds

NASA Technical Reports Server (NTRS)

Davies, R.

1978-01-01

Results are presented for a Monte Carlo model applied to a wide range of cloud widths and heights, and for an analytical model restricted in its application to cuboidally shaped clouds whose length, breadth, and depth may be varied independently; the clouds must be internally homogeneous with respect to their intrinsic radiative properties. Comparative results from the Monte Carlo method and the derived analytical model are presented for a wide range of cloud sizes, with special emphasis on the effects of varying the single scatter albedo, the solar zenith angle, and the scattering phase angle.

Analytic few-photon scattering in waveguide QED

NASA Astrophysics Data System (ADS)

Hurst, David L.; Kok, Pieter

2018-04-01

We develop an approach to light-matter coupling in waveguide QED based upon scattering amplitudes evaluated via Dyson series. For optical states containing more than single photons, terms in this series become increasingly complex, and we provide a diagrammatic recipe for their evaluation, which is capable of yielding analytic results. Our method fully specifies a combined emitter-optical state that permits investigation of light-matter entanglement generation protocols. We use our expressions to study two-photon scattering from a Λ -system and find that the pole structure of the transition amplitude is dramatically altered as the two ground states are tuned from degeneracy.

A mass spectrometry primer for mass spectrometry imaging

PubMed Central

Rubakhin, Stanislav S.; Sweedler, Jonathan V.

2011-01-01

Mass spectrometry imaging (MSI), a rapidly growing subfield of chemical imaging, employs mass spectrometry (MS) technologies to create single- and multi-dimensional localization maps for a variety of atoms and molecules. Complimentary to other imaging approaches, MSI provides high chemical specificity and broad analyte coverage. This powerful analytical toolset is capable of measuring the distribution of many classes of inorganics, metabolites, proteins and pharmaceuticals in chemically and structurally complex biological specimens in vivo, in vitro, and in situ. The MSI approaches highlighted in this Methods in Molecular Biology volume provide flexibility of detection, characterization, and identification of multiple known and unknown analytes. The goal of this chapter is to introduce investigators who may be unfamiliar with MS to the basic principles of the mass spectrometric approaches as used in MSI. In addition to guidelines for choosing the most suitable MSI method for specific investigations, cross-references are provided to the chapters in this volume that describe the appropriate experimental protocols. PMID:20680583

An analytical model for pressure of volume fractured tight oil reservoir with horizontal well

NASA Astrophysics Data System (ADS)

Feng, Qihong; Dou, Kaiwen; Zhang, Xianmin; Xing, Xiangdong; Xia, Tian

2017-05-01

The property of tight oil reservoir is worse than common reservoir that we usually seen before, the porosity and permeability is low, the diffusion is very complex. Therefore, the ordinary depletion method is useless here. The volume fracture breaks through the conventional EOR mechanism, which set the target by amplifying the contact area of fracture and reservoir so as to improving the production of every single well. In order to forecast the production effectively, we use the traditional dual-porosity model, build an analytical model for production of volume fractured tight oil reservoir with horizontal well, and get the analytical solution in Laplace domain. Then we construct the log-log plot of dimensionless pressure and time by stiffest conversion. After that, we discuss the influential factors of pressure. Several factors like cross flow, skin factors and threshold pressure gradient was analyzed in the article. This model provides a useful method for tight oil production forecast and it has certain guiding significance for the production capacity prediction and dynamic analysis.

Nanometrology and its perspectives in environmental research.

PubMed

Kim, Hyun-A; Seo, Jung-Kwan; Kim, Taksoo; Lee, Byung-Tae

2014-01-01

Rapid increase in engineered nanoparticles (ENPs) in many goods has raised significant concern about their environmental safety. Proper methodologies are therefore needed to conduct toxicity and exposure assessment of nanoparticles in the environment. This study reviews several analytical techniques for nanoparticles and summarizes their principles, advantages and disadvantages, reviews the state of the art, and offers the perspectives of nanometrology in relation to ENP studies. Nanometrology is divided into five techniques with regard to the instrumental principle: microscopy, light scattering, spectroscopy, separation, and single particle inductively coupled plasma-mass spectrometry. Each analytical method has its own drawbacks, such as detection limit, ability to quantify or qualify ENPs, and matrix effects. More than two different analytical methods should be used to better characterize ENPs. In characterizing ENPs, the researchers should understand the nanometrology and its demerits, as well as its merits, to properly interpret their experimental results. Challenges lie in the nanometrology and pretreatment of ENPs from various matrices; in the extraction without dissolution or aggregation, and concentration of ENPs to satisfy the instrumental detection limit.

Analytical Optimization of the Net Residual Dispersion in SPM-Limited Dispersion-Managed Systems

NASA Astrophysics Data System (ADS)

Xiao, Xiaosheng; Gao, Shiming; Tian, Yu; Yang, Changxi

2006-05-01

Dispersion management is an effective technique to suppress the nonlinear impairment in fiber transmission systems, which includes tuning the amounts of precompensation, residual dispersion per span (RDPS), and net residual dispersion (NRD) of the systems. For self-phase modulation (SPM)-limited systems, optimizing the NRD is necessary because it can greatly improve the system performance. In this paper, an analytical method is presented to optimize NRD for SPM-limited dispersion-managed systems. The method is based on the correlation between the nonlinear impairment and the output pulse broadening of SPM-limited systems; therefore, dispersion-managed systems can be optimized through minimizing the output single-pulse broadening. A set of expressions is derived to calculate the output pulse broadening of the SPM-limited dispersion-managed system, from which the analytical result of optimal NRD is obtained. Furthermore, with the expressions of pulse broadening, how the nonlinear impairment depends on the amounts of precompensation and RDPS can be revealed conveniently.

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

PubMed

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

2016-01-01

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

Quantitative Profiling of Endogenous Fat-Soluble Vitamins and Carotenoids in Human Plasma Using an Improved UHPSFC-ESI-MS Interface.

PubMed

Petruzziello, Filomena; Grand-Guillaume Perrenoud, Alexandre; Thorimbert, Anita; Fogwill, Michael; Rezzi, Serge

2017-07-18

Analytical solutions enabling the quantification of circulating levels of liposoluble micronutrients such as vitamins and carotenoids are currently limited to either single or a reduced panel of analytes. The requirement to use multiple approaches hampers the investigation of the biological variability on a large number of samples in a time and cost efficient manner. With the goal to develop high-throughput and robust quantitative methods for the profiling of micronutrients in human plasma, we introduce a novel, validated workflow for the determination of 14 fat-soluble vitamins and carotenoids in a single run. Automated supported liquid extraction was optimized and implemented to simultaneously parallelize 48 samples in 1 h, and the analytes were measured using ultrahigh-performance supercritical fluid chromatography coupled to tandem mass spectrometry in less than 8 min. An improved mass spectrometry interface hardware was built up to minimize the post-decompression volume and to allow better control of the chromatographic effluent density on its route toward and into the ion source. In addition, a specific make-up solvent condition was developed to ensure both analytes and matrix constituents solubility after mobile phase decompression. The optimized interface resulted in improved spray plume stability and conserved matrix compounds solubility leading to enhanced hyphenation robustness while ensuring both suitable analytical repeatability and improved the detection sensitivity. The overall developed methodology gives recoveries within 85-115%, as well as within and between-day coefficient of variation of 2 and 14%, respectively.

Determination of a risk management primer at petroleum-contaminated sites: developing new human health risk assessment strategy.

PubMed

Park, In-Sun; Park, Jae-Woo

2011-01-30

Total petroleum hydrocarbon (TPH) is an important environmental contaminant that is toxic to human and environmental receptors. However, human health risk assessment for petroleum, oil, and lubricant (POL)-contaminated sites is especially challenging because TPH is not a single compound, but rather a mixture of numerous substances. To address this concern, this study recommends a new human health risk assessment strategy for POL-contaminated sites. The strategy is based on a newly modified TPH fractionation method and includes an improved analytical protocol. The proposed TPH fractionation method is composed of ten fractions (e.g., aliphatic and aromatic EC8-10, EC10-12, EC12-16, EC16-22 and EC22-40). Physicochemical properties and toxicity values of each fraction were newly defined in this study. The stepwise ultrasonication-based analytical process was established to measure TPH fractions. Analytical results were compared with those from the TPH Criteria Working Group (TPHCWG) Direct Method. Better analytical efficiencies in TPH, aliphatic, and aromatic fractions were achieved when contaminated soil samples were analyzed with the new analytical protocol. Finally, a human health risk assessment was performed based on the developed tiered risk assessment framework. Results showed that a detailed quantitative risk assessment should be conducted to determine scientifically and economically appropriate cleanup target levels, although the phase II process is useful for determining the potency of human health risks posed by POL-contamination. Copyright © 2010 Elsevier B.V. All rights reserved.

Hydrodynamic chromatography coupled to single-particle ICP-MS for the simultaneous characterization of AgNPs and determination of dissolved Ag in plasma and blood of burn patients.

PubMed

Roman, Marco; Rigo, Chiara; Castillo-Michel, Hiram; Munivrana, Ivan; Vindigni, Vincenzo; Mičetić, Ivan; Benetti, Federico; Manodori, Laura; Cairns, Warren R L

2016-07-01

Silver nanoparticles (AgNPs) are increasingly used in medical devices as innovative antibacterial agents, but no data are currently available on their chemical transformations and fate in vivo in the human body, particularly on their potential to reach the circulatory system. To study the processes involving AgNPs in human plasma and blood, we developed an analytical method based on hydrodynamic chromatography (HDC) coupled to inductively coupled plasma mass spectrometry (ICP-MS) in single-particle detection mode. An innovative algorithm was implemented to deconvolute the signals of dissolved Ag and AgNPs and to extrapolate a multiparametric characterization of the particles in the same chromatogram. From a single injection, the method provides the concentration of dissolved Ag and the distribution of AgNPs in terms of hydrodynamic diameter, mass-derived diameter, number and mass concentration. This analytical approach is robust and suitable to study quantitatively the dynamics and kinetics of AgNPs in complex biological fluids, including processes such as agglomeration, dissolution and formation of protein coronas. The method was applied to study the transformations of AgNP standards and an AgNP-coated dressing in human plasma, supported by micro X-ray fluorescence (μXRF) and micro X-ray absorption near-edge spectroscopy (μXANES) speciation analysis and imaging, and to investigate, for the first time, the possible presence of AgNPs in the blood of three burn patients treated with the same dressing. Together with our previous studies, the results strongly support the hypothesis that the systemic mobilization of the metal after topical administration of AgNPs is driven by their dissolution in situ. Graphical Abstract Simplified scheme of the combined analytical approach adopted for studying the chemical dynamics of AgNPs in human plasma/blood.

Nanokit for single-cell electrochemical analyses.

PubMed

Pan, Rongrong; Xu, Mingchen; Jiang, Dechen; Burgess, Jame D; Chen, Hong-Yuan

2016-10-11

The development of more intricate devices for the analysis of small molecules and protein activity in single cells would advance our knowledge of cellular heterogeneity and signaling cascades. Therefore, in this study, a nanokit was produced by filling a nanometer-sized capillary with a ring electrode at the tip with components from traditional kits, which could be egressed outside the capillary by electrochemical pumping. At the tip, femtoliter amounts of the kit components were reacted with the analyte to generate hydrogen peroxide for the electrochemical measurement by the ring electrode. Taking advantage of the nanotip and small volume injection, the nanokit was easily inserted into a single cell to determine the intracellular glucose levels and sphingomyelinase (SMase) activity, which had rarely been achieved. High cellular heterogeneities of these two molecules were observed, showing the significance of the nanokit. Compared with the current methods that use a complicated structural design or surface functionalization for the recognition of the analytes, the nanokit has adapted features of the well-established kits and integrated the kit components and detector in one nanometer-sized capillary, which provides a specific device to characterize the reactivity and concentrations of cellular compounds in single cells.

Untangling Slab Dynamics Using 3-D Numerical and Analytical Models

NASA Astrophysics Data System (ADS)

Holt, A. F.; Royden, L.; Becker, T. W.

2016-12-01

Increasingly sophisticated numerical models have enabled us to make significant strides in identifying the key controls on how subducting slabs deform. For example, 3-D models have demonstrated that subducting plate width, and the related strength of toroidal flow around the plate edge, exerts a strong control on both the curvature and the rate of migration of the trench. However, the results of numerical subduction models can be difficult to interpret, and many first order dynamics issues remain at least partially unresolved. Such issues include the dominant controls on trench migration, the interdependence of asthenospheric pressure and slab dynamics, and how nearby slabs influence each other's dynamics. We augment 3-D, dynamically evolving finite element models with simple, analytical force-balance models to distill the physics associated with subduction into more manageable parts. We demonstrate that for single, isolated subducting slabs much of the complexity of our fully numerical models can be encapsulated by simple analytical expressions. Rates of subduction and slab dip correlate strongly with the asthenospheric pressure difference across the subducting slab. For double subduction, an additional slab gives rise to more complex mantle pressure and flow fields, and significantly extends the range of plate kinematics (e.g., convergence rate, trench migration rate) beyond those present in single slab models. Despite these additional complexities, we show that much of the dynamics of such multi-slab systems can be understood using the physics illuminated by our single slab study, and that a force-balance method can be used to relate intra-plate stress to viscous pressure in the asthenosphere and coupling forces at plate boundaries. This method has promise for rapid modeling of large systems of subduction zones on a global scale.

Nonlinear viscoelastic characterization of structural adhesives

NASA Technical Reports Server (NTRS)

Rochefort, M. A.; Brinson, H. F.

1983-01-01

Measurements of the nonliner viscoelastic behavior of two adhesives, FM-73 and FM-300, are presented and discussed. Analytical methods to quantify the measurements are given and fitted into a framework of an accelerated testing and analysis procedure. The single integral model used is shown to function well and is analogous to a time-temperature stress-superposition procedure (TTSSP). Advantages and disadvantages of the creep power law method used in this study are given.

Analytic method for calculating properties of random walks on networks

NASA Technical Reports Server (NTRS)

Goldhirsch, I.; Gefen, Y.

1986-01-01

A method for calculating the properties of discrete random walks on networks is presented. The method divides complex networks into simpler units whose contribution to the mean first-passage time is calculated. The simplified network is then further iterated. The method is demonstrated by calculating mean first-passage times on a segment, a segment with a single dangling bond, a segment with many dangling bonds, and a looplike structure. The results are analyzed and related to the applicability of the Einstein relation between conductance and diffusion.

A quantitative method for residues of macrolide antibiotics in porcine kidney by liquid chromatography/tandem mass spectrometry.

PubMed

Dickson, Leslie C; O'Byrne, Collin; Chan, Wayne

2012-01-01

An LC/MS/MS-based multiresidue quantitative method was developed for the macrolides erythromycin A, neospiramycin I, oleandomycin, spiramycin I, tilmicosin, and tylosin A in porcine kidney tissues. The Canadian Food Inspection Agency (CFIA) had as part of its analytical scope an LC/UV method for quantification of residues of two macrolide antibiotics, tilmicosin and tylosin A, in the kidney, liver, and muscle of cattle, swine, and poultry. The method could not reliably detect concentrations below 10 microg/kg. To increase the scope of the CFIA's analytical capabilities, a sensitive multiresidue quantitative method for macrolide residues in food animal tissues was required. Porcine kidney samples were extracted with acetonitrile and alkaline buffer and cleaned-up using silica-based C18 SPE cartridges. Sample extracts were analyzed using LC/MS/MS with positive electrospray ionization. Fitness for purpose was verified in a single-laboratory validation study using a second analyst. The working analytical range was 5 to 50 microg/kg. LOD and LOQ were 0.5 to 0.6 microg/kg and 1.5 to 3.0 microg/kg, respectively. Limits of identification were 0.5 to 2.0 microg/kg. Relative intermediate precisions were 8 to 17%. Average absolute recoveries were 68 to 76%.

[Simultaneous quantitative analysis of five alkaloids in Sophora flavescens by multi-components assay by single marker].

PubMed

Chen, Jing; Wang, Shu-Mei; Meng, Jiang; Sun, Fei; Liang, Sheng-Wang

2013-05-01

To establish a new method for quality evaluation and validate its feasibilities by simultaneous quantitative assay of five alkaloids in Sophora flavescens. The new quality evaluation method, quantitative analysis of multi-components by single marker (QAMS), was established and validated with S. flavescens. Five main alkaloids, oxymatrine, sophocarpine, matrine, oxysophocarpine and sophoridine, were selected as analytes to evaluate the quality of rhizome of S. flavescens, and the relative correction factor has good repeatibility. Their contents in 21 batches of samples, collected from different areas, were determined by both external standard method and QAMS. The method was evaluated by comparison of the quantitative results between external standard method and QAMS. No significant differences were found in the quantitative results of five alkaloids in 21 batches of S. flavescens determined by external standard method and QAMS. It is feasible and suitable to evaluate the quality of rhizome of S. flavescens by QAMS.

Probability of identification: a statistical model for the validation of qualitative botanical identification methods.

PubMed

LaBudde, Robert A; Harnly, James M

2012-01-01

A qualitative botanical identification method (BIM) is an analytical procedure that returns a binary result (1 = Identified, 0 = Not Identified). A BIM may be used by a buyer, manufacturer, or regulator to determine whether a botanical material being tested is the same as the target (desired) material, or whether it contains excessive nontarget (undesirable) material. The report describes the development and validation of studies for a BIM based on the proportion of replicates identified, or probability of identification (POI), as the basic observed statistic. The statistical procedures proposed for data analysis follow closely those of the probability of detection, and harmonize the statistical concepts and parameters between quantitative and qualitative method validation. Use of POI statistics also harmonizes statistical concepts for botanical, microbiological, toxin, and other analyte identification methods that produce binary results. The POI statistical model provides a tool for graphical representation of response curves for qualitative methods, reporting of descriptive statistics, and application of performance requirements. Single collaborator and multicollaborative study examples are given.

Development of an analytical method for the simultaneous analysis of MCPD esters and glycidyl esters in oil-based foodstuffs.

PubMed

Ermacora, Alessia; Hrnčiřík, Karel

2014-01-01

Substantial progress has been recently made in the development and optimisation of analytical methods for the quantification of 2-MCPD, 3-MCPD and glycidyl esters in oils and fats, and there are a few methods currently available that allow a reliable quantification of these contaminants in bulk oils and fats. On the other hand, no standard method for the analysis of foodstuffs has yet been established. The aim of this study was the development and validation of a new method for the simultaneous quantification of 2-MCPD, 3-MCPD and glycidyl esters in oil-based food products. The developed protocol includes a first step of liquid-liquid extraction and purification of the lipophilic substances of the sample, followed by the application of a previously developed procedure based on acid transesterification, for the indirect quantification of these contaminants in oils and fats. The method validation was carried out on food products (fat-based spreads, creams, margarine, mayonnaise) manufactured in-house, in order to control the manufacturing process and account for any food matrix-analyte interactions (the sample spiking was carried out on the single components used for the formulations rather than the final products). The method showed good accuracy (the recoveries ranged from 97% to 106% for bound 3-MCPD and 2-MCPD and from 88% to 115% for bound glycidol) and sensitivity (the LOD was 0.04 and 0.05 mg kg(-1) for bound MCPD and glycidol, respectively). Repeatability and reproducibility were satisfactory (RSD below 2% and 5%, respectively) for all analytes. The levels of salts and surface-active compounds in the formulation were found to have no impact on the accuracy and the other parameters of the method.

Subsurface Stress Fields in FCC Single Crystal Anisotropic Contacts

NASA Technical Reports Server (NTRS)

Arakere, Nagaraj K.; Knudsen, Erik; Swanson, Gregory R.; Duke, Gregory; Ham-Battista, Gilda

2004-01-01

Single crystal superalloy turbine blades used in high pressure turbomachinery are subject to conditions of high temperature, triaxial steady and alternating stresses, fretting stresses in the blade attachment and damper contact locations, and exposure to high-pressure hydrogen. The blades are also subjected to extreme variations in temperature during start-up and shutdown transients. The most prevalent high cycle fatigue (HCF) failure modes observed in these blades during operation include crystallographic crack initiation/propagation on octahedral planes, and non-crystallographic initiation with crystallographic growth. Numerous cases of crack initiation and crack propagation at the blade leading edge tip, blade attachment regions, and damper contact locations have been documented. Understanding crack initiation/propagation under mixed-mode loading conditions is critical for establishing a systematic procedure for evaluating HCF life of single crystal turbine blades. This paper presents analytical and numerical techniques for evaluating two and three dimensional subsurface stress fields in anisotropic contacts. The subsurface stress results are required for evaluating contact fatigue life at damper contacts and dovetail attachment regions in single crystal nickel-base superalloy turbine blades. An analytical procedure is presented for evaluating the subsurface stresses in the elastic half-space, based on the adaptation of a stress function method outlined by Lekhnitskii. Numerical results are presented for cylindrical and spherical anisotropic contacts, using finite element analysis (FEA). Effects of crystal orientation on stress response and fatigue life are examined. Obtaining accurate subsurface stress results for anisotropic single crystal contact problems require extremely refined three-dimensional (3-D) finite element grids, especially in the edge of contact region. Obtaining resolved shear stresses (RSS) on the principal slip planes also involves considerable post-processing work. For these reasons it is very advantageous to develop analytical solution schemes for subsurface stresses, whenever possible.

XPS Protocol for the Characterization of Pristine and Functionalized Single Wall Carbon Nanotubes

NASA Technical Reports Server (NTRS)

Sosa, E. D.; Allada, R.; Huffman, C. B.; Arepalli, S.

2009-01-01

Recent interest in developing new applications for carbon nanotubes (CNT) has fueled the need to use accurate macroscopic and nanoscopic techniques to characterize and understand their chemistry. X-ray photoelectron spectroscopy (XPS) has proved to be a useful analytical tool for nanoscale surface characterization of materials including carbon nanotubes. Recent nanotechnology research at NASA Johnson Space Center (NASA-JSC) helped to establish a characterization protocol for quality assessment for single wall carbon nanotubes (SWCNTs). Here, a review of some of the major factors of the XPS technique that can influence the quality of analytical data, suggestions for methods to maximize the quality of data obtained by XPS, and the development of a protocol for XPS characterization as a complementary technique for analyzing the purity and surface characteristics of SWCNTs is presented. The XPS protocol is then applied to a number of experiments including impurity analysis and the study of chemical modifications for SWCNTs.

Single-Step Reagentless Laser Scribing Fabrication of Electrochemical Paper-Based Analytical Devices.

PubMed

de Araujo, William R; Frasson, Carolina M R; Ameku, Wilson A; Silva, José R; Angnes, Lúcio; Paixão, Thiago R L C

2017-11-20

A single-step laser scribing process is used to pattern nanostructured electrodes on paper-based devices. The facile and low-cost technique eliminates the need for chemical reagents or controlled conditions. This process involves the use of a CO 2 laser to pyrolyze the surface of the paperboard, producing a conductive porous non-graphitizing carbon material composed of graphene sheets and composites with aluminosilicate nanoparticles. The new electrode material was extensively characterized, and it exhibits high conductivity and an enhanced active/geometric area ratio; it is thus well-suited for electrochemical purposes. As a proof-of-concept, the devices were successfully employed for different analytical applications in the clinical, pharmaceutical, food, and forensic fields. The scalable and green fabrication method associated with the features of the new material is highly promising for the development of portable electrochemical devices. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Piezoelectric energy harvesting based on shear mode 0.71Pb(Mg(1/3)Nb(2/3))O3-0.29PbTiO3 single crystals.

PubMed

Ren, Bo; Or, Siu Wing; Wang, Feifei; Zhao, Xiangyong; Luo, Haosu; Li, Xiaobing; Zhang, Qinhui; Di, Wenning; Zhang, Yaoyao

2010-06-01

In this paper we theoretically and experimentally present a nonresonant vibration energy harvesting device based on the shear mode of 0.71Pb(Mg(1/3)Nb(2/3))O3-0.29PbTiO3 single crystals. The electrical properties of the energy harvesting device were evaluated using an analytical method. Good consistency was obtained between the analytical and experimental results. Under a mass load of 200 g, a peak voltage of 11.3 V and maximum power of 0.70 mW were obtained at 500 Hz when connecting a matching load resistance of 91 komega. A high output could always be obtained within a very wide frequency range. The results demonstrate the potential of the device in energy harvesting applied to low-power portable electronics and wireless sensors.

Exact solutions for rate and synchrony in recurrent networks of coincidence detectors.

PubMed

Mikula, Shawn; Niebur, Ernst

2008-11-01

We provide analytical solutions for mean firing rates and cross-correlations of coincidence detector neurons in recurrent networks with excitatory or inhibitory connectivity, with rate-modulated steady-state spiking inputs. We use discrete-time finite-state Markov chains to represent network state transition probabilities, which are subsequently used to derive exact analytical solutions for mean firing rates and cross-correlations. As illustrated in several examples, the method can be used for modeling cortical microcircuits and clarifying single-neuron and population coding mechanisms. We also demonstrate that increasing firing rates do not necessarily translate into increasing cross-correlations, though our results do support the contention that firing rates and cross-correlations are likely to be coupled. Our analytical solutions underscore the complexity of the relationship between firing rates and cross-correlations.

Advancements in nano-enabled therapeutics for neuroHIV management.

PubMed

Kaushik, Ajeet; Jayant, Rahul Dev; Nair, Madhavan

This viewpoint is a global call to promote fundamental and applied research aiming toward designing smart nanocarriers of desired properties, novel noninvasive strategies to open the blood-brain barrier (BBB), delivery/release of single/multiple therapeutic agents across the BBB to eradicate neurohuman immunodeficiency virus (HIV), strategies for on-demand site-specific release of antiretroviral therapy, developing novel nanoformulations capable to recognize and eradicate latently infected HIV reservoirs, and developing novel smart analytical diagnostic tools to detect and monitor HIV infection. Thus, investigation of novel nanoformulations, methodologies for site-specific delivery/release, analytical methods, and diagnostic tools would be of high significance to eradicate and monitor neuroacquired immunodeficiency syndrome. Overall, these developments will certainly help to develop personalized nanomedicines to cure HIV and to develop smart HIV-monitoring analytical systems for disease management.

Selectivity in analytical chemistry: two interpretations for univariate methods.

PubMed

Dorkó, Zsanett; Verbić, Tatjana; Horvai, George

2015-01-01

Selectivity is extremely important in analytical chemistry but its definition is elusive despite continued efforts by professional organizations and individual scientists. This paper shows that the existing selectivity concepts for univariate analytical methods broadly fall in two classes: selectivity concepts based on measurement error and concepts based on response surfaces (the response surface being the 3D plot of the univariate signal as a function of analyte and interferent concentration, respectively). The strengths and weaknesses of the different definitions are analyzed and contradictions between them unveiled. The error based selectivity is very general and very safe but its application to a range of samples (as opposed to a single sample) requires the knowledge of some constraint about the possible sample compositions. The selectivity concepts based on the response surface are easily applied to linear response surfaces but may lead to difficulties and counterintuitive results when applied to nonlinear response surfaces. A particular advantage of this class of selectivity is that with linear response surfaces it can provide a concentration independent measure of selectivity. In contrast, the error based selectivity concept allows only yes/no type decision about selectivity. Copyright © 2014 Elsevier B.V. All rights reserved.

Simultaneous liquid chromatography/mass spectrometry determination of both polar and "multiresidue" pesticides in food using parallel hydrophilic interaction/reversed-phase liquid chromatography and a hybrid sample preparation approach.

PubMed

Robles-Molina, José; Gilbert-López, Bienvenida; García-Reyes, Juan F; Molina-Díaz, Antonio

2017-09-29

Pesticide testing of foodstuffs is usually accomplished with generic wide-scope multi-residue methods based on liquid chromatography tandem mass spectrometry (LC-MS/MS). However, this approach does not cover some special pesticides, the so called "single-residue method" compounds, that are hardly compatible with standard reversed-phase (RP) separations due to their specific properties. In this article, we propose a comprehensive strategy for the integration of single residue method compounds and standard multiresidue pesticides within a single run. It is based on the use of a parallel LC column assembly with two different LC gradients performing orthogonal hydrophilic interaction chromatography (HILIC) and reversed-phase (RPLC) chromatography within one analytical run. Two sample aliquots were simultaneously injected on each column, using different gradients, being the eluents merged post-column prior to mass spectrometry detection. The approach was tested with 41 multiclass pesticides covering a wide range of physicochemical properties across several orders of log K ow (from -4 to +5.5). With this assembly, distinct separation from the void was attained for all the pesticides studied, keeping similar performance in terms of sensitivity, peak area reproducibility (<6 RSD% in most cases) and retention time stability of standard single column approaches (better than±0.1min). The application of the proposed approach using parallel HILIC/RPLC and RPLC/aqueous normal phase (Obelisc) were assessed in leek using LC-MS/MS. For this purpose, a hybrid QuEChERS (Quick, easy, cheap, effective, rugged and safe)/QuPPe (quick method for polar pesticides) method was evaluated based on solvent extraction with MeOH and acetonitrile followed by dispersive solid-phase extraction, delivering appropriate recoveries for most of the pesticides included in the study within the log K ow in the range from -4 to +5.5. The proposed strategy may be extended to other fields such as sport drug testing or environmental analysis, where the same type of variety of analytes featuring poor retention within a single chromatographic separation occurs. Copyright © 2017 Elsevier B.V. All rights reserved.

Surprising performance for vibrational frequencies of the distinguishable clusters with singles and doubles (DCSD) and MP2.5 approximations

NASA Astrophysics Data System (ADS)

Kesharwani, Manoj K.; Sylvetsky, Nitai; Martin, Jan M. L.

2017-11-01

We show that the DCSD (distinguishable clusters with all singles and doubles) correlation method permits the calculation of vibrational spectra at near-CCSD(T) quality but at no more than CCSD cost, and with comparatively inexpensive analytical gradients. For systems dominated by a single reference configuration, even MP2.5 is a viable alternative, at MP3 cost. MP2.5 performance for vibrational frequencies is comparable to double hybrids such as DSD-PBEP86-D3BJ, but without resorting to empirical parameters. DCSD is also quite suitable for computing zero-point vibrational energies in computational thermochemistry.

Determination of linuron and related compounds in soil by microwave-assisted solvent extraction and reversed-phase liquid chromatography with UV detection.

PubMed

Molins, C; Hogendoorn, E A; Dijkman, E; Heusinkveld, H A; Baumann, R A

2000-02-11

The combination of microwave-assisted solvent extraction (MASE) and reversed-phase liquid chromatography (RPLC) with UV detection has been investigated for the efficient determination of phenylurea herbicides in soils involving the single-residue method (SRM) approach (linuron) and the multi-residue method (MRM) approach (monuron, monolinuron, isoproturon, metobromuron, diuron and linuron). Critical parameters of MASE, viz, extraction temperature, water content and extraction solvent were varied in order to optimise recoveries of the analytes while simultaneously minimising co-extraction of soil interferences. The optimised extraction procedure was applied to different types of soil with an organic carbon content of 0.4-16.7%. Besides freshly spiked soil samples, method validation included the analysis of samples with aged residues. A comparative study between the applicability of RPLC-UV without and with the use of column switching for the processing of uncleaned extracts, was carried out. For some of the tested analyte/matrix combinations the one-column approach (LC mode) is feasible. In comparison to LC, coupled-column LC (LC-LC mode) provides high selectivity in single-residue analysis (linuron) and, although less pronounced in multi-residue analysis (all six phenylurea herbicides), the clean-up performance of LC-LC improves both time of analysis and sample throughput. In the MRM approach the developed procedure involving MASE and LC-LC-UV provided acceptable recoveries (range, 80-120%) and RSDs (<12%) at levels of 10 microg/kg (n=9) and 50 microg/kg (n=7), respectively, for most analyte/matrix combinations. Recoveries from aged residue samples spiked at a level of 100 microg/kg (n=7) ranged, depending of the analyte/soil type combination, from 41-113% with RSDs ranging from 1-35%. In the SRM approach the developed LC-LC procedure was applied for the determination of linuron in 28 sandy soil samples collected in a field study. Linuron could be determined in soil with a limit of quantitation of 10 microg/kg.

A novel method for quantification of gemcitabine and its metabolites 2',2'-difluorodeoxyuridine and gemcitabine triphosphate in tumour tissue by LC-MS/MS: comparison with (19)F NMR spectroscopy.

PubMed

Bapiro, Tashinga E; Richards, Frances M; Goldgraben, Mae A; Olive, Kenneth P; Madhu, Basetti; Frese, Kristopher K; Cook, Natalie; Jacobetz, Michael A; Smith, Donna-Michelle; Tuveson, David A; Griffiths, John R; Jodrell, Duncan I

2011-11-01

To develop a sensitive analytical method to quantify gemcitabine (2',2'-difluorodeoxycytidine, dFdC) and its metabolites 2',2'-difluorodeoxyuridine (dFdU) and 2',2'-difluorodeoxycytidine-5'-triphosphate (dFdCTP) simultaneously from tumour tissue. Pancreatic ductal adenocarcinoma tumour tissue from genetically engineered mouse models of pancreatic cancer (KP ( FL/FL ) C and KP ( R172H/+) C) was collected after dosing the mice with gemcitabine. (19)F NMR spectroscopy and LC-MS/MS protocols were optimised to detect gemcitabine and its metabolites in homogenates of the tumour tissue. A (19)F NMR protocol was developed, which was capable of distinguishing the three analytes in tumour homogenates. However, it required at least 100 mg of the tissue in question and a long acquisition time per sample, making it impractical for use in large PK/PD studies or clinical trials. The LC-MS/MS protocol was developed using porous graphitic carbon to separate the analytes, enabling simultaneous detection of all three analytes from as little as 10 mg of tissue, with a sensitivity for dFdCTP of 0.2 ng/mg tissue. Multiple pieces of tissue from single tumours were analysed, showing little intra-tumour variation in the concentrations of dFdC or dFdU (both intra- and extra-cellular). Intra-tumoural variation was observed in the concentration of dFdCTP, an intra-cellular metabolite, which may reflect regions of different cellularity within a tumour. We have developed a sensitive LC-MS/MS method capable of quantifying gemcitabine, dFdU and dFdCTP in pancreatic tumour tissue. The requirement for only 10 mg of tissue enables this protocol to be used to analyse multiple areas from a single tumour and to spare tissue for additional pharmacodynamic assays.

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

Alexeev, A. V.; Maltseva, D. V.; Ivanov, V. A., E-mail: ivanov@polly.phys.msu.ru

We study force-extension curves of a single semiflexible chain consisting of several rigid rods connected by flexible spacers. The atomic force microscopy and laser optical or magnetic tweezers apparatus stretching these rod-coil macromolecules are discussed. In addition, the stretching by external isotropic force is analyzed. The main attention is focused on computer simulation and analytical results. We demonstrate that the force-extension curves for rod-coil chains composed of two or three rods of equal length differ not only quantitatively but also qualitatively in different probe methods. These curves have an anomalous shape for a chain of two rods. End-to-end distributions ofmore » rod-coil chains are calculated by Monte Carlo method and compared with analytical equations. The influence of the spacer’s length on the force-extension curves in different probe methods is analyzed. The results can be useful for interpreting experiments on the stretching of rod-coil block-copolymers.« less

Simultaneous analysis of hydrochlorothiazide, triamterene and reserpine in rat plasma by high performance liquid chromatography and tandem solid-phase extraction.

PubMed

Li, Hang; He, Junting; Liu, Qin; Huo, Zhaohui; Liang, Si; Liang, Yong

2011-03-01

A tandem solid-phase extraction method (SPE) of connecting two different cartridges (C(18) and MCX) in series was developed as the extraction procedure in this article, which provided better extraction yields (>86%) for all analytes and more appropriate sample purification from endogenous interference materials compared with a single cartridge. Analyte separation was achieved on a C(18) reversed-phase column at the wavelength of 265 nm by high-performance liquid chromatography (HPLC). The method was validated in terms of extraction yield, precision and accuracy. These assays gave mean accuracy values higher than 89% with RSD values that were always less than 3.8%. The method has been successfully applied to plasma samples from rats after oral administration of target compounds. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Probability theory versus simulation of petroleum potential in play analysis

USGS Publications Warehouse

Crovelli, R.A.

1987-01-01

An analytic probabilistic methodology for resource appraisal of undiscovered oil and gas resources in play analysis is presented. This play-analysis methodology is a geostochastic system for petroleum resource appraisal in explored as well as frontier areas. An objective was to replace an existing Monte Carlo simulation method in order to increase the efficiency of the appraisal process. Underlying the two methods is a single geologic model which considers both the uncertainty of the presence of the assessed hydrocarbon and its amount if present. The results of the model are resource estimates of crude oil, nonassociated gas, dissolved gas, and gas for a geologic play in terms of probability distributions. The analytic method is based upon conditional probability theory and a closed form solution of all means and standard deviations, along with the probabilities of occurrence. ?? 1987 J.C. Baltzer A.G., Scientific Publishing Company.

Consistent approach to describing aircraft HIRF protection

NASA Technical Reports Server (NTRS)

Rimbey, P. R.; Walen, D. B.

1995-01-01

The high intensity radiated fields (HIRF) certification process as currently implemented is comprised of an inconsistent combination of factors that tend to emphasize worst case scenarios in assessing commercial airplane certification requirements. By examining these factors which include the process definition, the external HIRF environment, the aircraft coupling and corresponding internal fields, and methods of measuring equipment susceptibilities, activities leading to an approach to appraising airplane vulnerability to HIRF are proposed. This approach utilizes technically based criteria to evaluate the nature of the threat, including the probability of encountering the external HIRF environment. No single test or analytic method comprehensively addresses the full HIRF threat frequency spectrum. Additional tools such as statistical methods must be adopted to arrive at more realistic requirements to reflect commercial aircraft vulnerability to the HIRF threat. Test and analytic data are provided to support the conclusions of this report. This work was performed under NASA contract NAS1-19360, Task 52.

Use of analyte-modulated modal power distribution in multimode optical fibers for simultaneous single-wavelength evanescent-wave refractometry and spectrometry.

PubMed

Potyrailo, R A; Ruddy, V P; Hieftje, G M

1999-11-01

A new method is described for the simultaneous determination of absorbance and refractive index of a sample medium. The method is based on measurement of the analyte-modulated modal power distribution (MPD) in a multimode waveguide. In turn, the MPD is quantified by the far-field spatial pattern and intensity of light, i.e., the Fraunhofer diffraction pattern (registered on a CCD camera), that emerges from a multimode optical fiber. Operationally, light that is sent down the fiber interacts with the surrounding analyte-containing medium by means of the evanescent wave at the fiber boundary. The light flux in the propagating beam and the internal reflection angles within the fiber are both affected by optical absorption connected with the analyte and by the refractive index of the analyte-containing medium. In turn, these angles are reflected in the angular divergence of the beam as it leaves the fiber. As a result, the Fraunhofer diffraction pattern of that beam yields two parameters that can, together, be used to deduce refractive index and absorbance. This MPD based detection offers important advantages over traditional evanescent-wave detection strategies which rely on recording only the total transmitted optical power or its lost fraction. First, simultaneous determination of sample refractive index and absorbance is possible at a single probe wavelength. Second, the sensitivity of refractometric and absorption measurements can be controlled simply, either by adjusting the distance between the end face of the fiber and the CCD detector or by monitoring selected modal groups at the fiber output. As a demonstration of these capabilities, several weakly absorbing solutions were examined, with refractive indices in the range from 1.3330 to 1.4553 and with absorption coefficients in the range 0-16 cm-1. The new detection strategy is likely to be important in applications in which sample coloration varies and when it is necessary to compensate for variations in the refractive index of a sample.

Analysis of the stress-strain state in single overlap joints using piezo-ceramic actuators

NASA Astrophysics Data System (ADS)

Pǎltânea, Veronica; Pǎltânea, Gheorghe; Popovici, Dorina; Jiga, Gabriel; Papanicolaou, George

2014-05-01

In this paper is presented a 2D approach to finite element modeling and an analytical calculus of a single lap bonded joint. As adherent material were selected a sheet of wood, aluminum and titanium. For adhesive part were selected Bison Super Wood D3 in case of the wood single lap joint and an epoxy resin type DGEBA-TETA for gluing together aluminum and titanium parts. In the article is described a combined method, which consists in the placement of the piezoelectric actuator inside of the adhesive part, in order to determine the tensile stress in the overlap joint. A comparison between the analytical and numerical results has been achieved through a multiphysics modeling - electrical and mechanical coupled problem. The technique used to calculate the mechanical parameters (First Principal Stress, displacements) was the three-point bending test, where different forces were applied in the mid-span of the structure, in order to maintain a constant displacement rate. The length of the overlap joint was modified from 20 to 50 mm.

Ensemble of single quadrupolar nuclei in rotating solids: sidebands in NMR spectrum.

PubMed

Kundla, Enn

2006-07-01

A novel way is proposed to describe the evolution of nuclear magnetic polarization and the induced NMR spectrum. In this method, the effect of a high-intensity external static magnetic field and the effects of proper Hamiltonian left over interaction components, which commute with the first, are taken into account simultaneously and equivalently. The method suits any concrete NMR problem. This brings forth the really existing details in the registered spectra, evoked by Hamiltonian secular terms, which may be otherwise smoothed due to approximate treatment of the effects of the secular terms. Complete analytical expressions are obtained describing the NMR spectra including the rotational sideband sets of single quadrupolar nuclei in rotating solids.

SOIL-AIR PERMEABILITY MEASUREMENT WITH A TRANSIENT PRESSURE BUILDUP METHOD

EPA Science Inventory

An analytical solution for transient pressure change in a single venting well was derived from mass conservation of air, Darcy's law of flow in porous media, and the ideal gas law equation of state. Slopes of plots of Pw2 against ln (t+Δt)/Δt similar to Homer's plot were used to ...

Statistics of stable marriages

NASA Astrophysics Data System (ADS)

Dzierzawa, Michael; Oméro, Marie-José

2000-11-01

In the stable marriage problem N men and N women have to be matched by pairs under the constraint that the resulting matching is stable. We study the statistical properties of stable matchings in the large N limit using both numerical and analytical methods. Generalizations of the model including singles and unequal numbers of men and women are also investigated.

Evaluation of Brazilian Sugarcane Bagasse Characterization: An Interlaboratory Comparison Study

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

Sluiter, Justin B.; Chum, Helena; Gomes, Absai C.

2016-05-01

This paper describes a study of the variability of measured composition for a single bulk sugarcane bagasse conducted across eight laboratories using similar analytical methods, with the purpose of determining the expected variation for compositional analysis performed by different laboratories. The results show good agreement of measured composition within a single laboratory, but greater variability when results are compared among laboratories. These interlaboratory variabilities do not seem to be associated with a specific method or technique or any single piece of instrumentation. The summary censored statistics provide mean values and pooled standard deviations as follows: total extractives 6.7% (0.6%), wholemore » ash 1.5% (0.2%), glucan 42.3% (1.2%), xylan 22.3% (0.5%), total lignin 21.3% (0.4%), and total mass closure 99.4% (2.9%).« less

Nanostructured 2D cellular materials in silicon by sidewall transfer lithography NEMS

NASA Astrophysics Data System (ADS)

Syms, Richard R. A.; Liu, Dixi; Ahmad, Munir M.

2017-07-01

Sidewall transfer lithography (STL) is demonstrated as a method for parallel fabrication of 2D nanostructured cellular solids in single-crystal silicon. The linear mechanical properties of four lattices (perfect and defected diamond; singly and doubly periodic honeycomb) with low effective Young’s moduli and effective Poisson’s ratio ranging from positive to negative are modelled using analytic theory and the matrix stiffness method with an emphasis on boundary effects. The lattices are fabricated with a minimum feature size of 100 nm and an aspect ratio of 40:1 using single- and double-level STL and deep reactive ion etching of bonded silicon-on-insulator. Nanoelectromechanical systems (NEMS) containing cellular materials are used to demonstrate stretching, bending and brittle fracture. Predicted edge effects are observed, theoretical values of Poisson’s ratio are verified and failure patterns are described.

An approach to estimate spatial distribution of analyte within cells using spectrally-resolved fluorescence microscopy.

PubMed

Sharma, Dharmendar Kumar; Irfanullah, Mir; Basu, Santanu Kumar; Madhu, Sheri; De, Suman; Jadhav, Sameer; Ravikanth, Mangalampalli; Chowdhury, Arindam

2017-01-18

While fluorescence microscopy has become an essential tool amongst chemists and biologists for the detection of various analyte within cellular environments, non-uniform spatial distribution of sensors within cells often restricts extraction of reliable information on relative abundance of analytes in different subcellular regions. As an alternative to existing sensing methodologies such as ratiometric or FRET imaging, where relative proportion of analyte with respect to the sensor can be obtained within cells, we propose a methodology using spectrally-resolved fluorescence microscopy, via which both the relative abundance of sensor as well as their relative proportion with respect to the analyte can be simultaneously extracted for local subcellular regions. This method is exemplified using a BODIPY sensor, capable of detecting mercury ions within cellular environments, characterized by spectral blue-shift and concurrent enhancement of emission intensity. Spectral emission envelopes collected from sub-microscopic regions allowed us to compare the shift in transition energies as well as integrated emission intensities within various intracellular regions. Construction of a 2D scatter plot using spectral shifts and emission intensities, which depend on the relative amount of analyte with respect to sensor and the approximate local amounts of the probe, respectively, enabled qualitative extraction of relative abundance of analyte in various local regions within a single cell as well as amongst different cells. Although the comparisons remain semi-quantitative, this approach involving analysis of multiple spectral parameters opens up an alternative way to extract spatial distribution of analyte in heterogeneous systems. The proposed method would be especially relevant for fluorescent probes that undergo relatively nominal shift in transition energies compared to their emission bandwidths, which often restricts their usage for quantitative ratiometric imaging in cellular media due to strong cross-talk between energetically separated detection channels.

An approach to estimate spatial distribution of analyte within cells using spectrally-resolved fluorescence microscopy

NASA Astrophysics Data System (ADS)

Sharma, Dharmendar Kumar; Irfanullah, Mir; Basu, Santanu Kumar; Madhu, Sheri; De, Suman; Jadhav, Sameer; Ravikanth, Mangalampalli; Chowdhury, Arindam

2017-03-01

While fluorescence microscopy has become an essential tool amongst chemists and biologists for the detection of various analyte within cellular environments, non-uniform spatial distribution of sensors within cells often restricts extraction of reliable information on relative abundance of analytes in different subcellular regions. As an alternative to existing sensing methodologies such as ratiometric or FRET imaging, where relative proportion of analyte with respect to the sensor can be obtained within cells, we propose a methodology using spectrally-resolved fluorescence microscopy, via which both the relative abundance of sensor as well as their relative proportion with respect to the analyte can be simultaneously extracted for local subcellular regions. This method is exemplified using a BODIPY sensor, capable of detecting mercury ions within cellular environments, characterized by spectral blue-shift and concurrent enhancement of emission intensity. Spectral emission envelopes collected from sub-microscopic regions allowed us to compare the shift in transition energies as well as integrated emission intensities within various intracellular regions. Construction of a 2D scatter plot using spectral shifts and emission intensities, which depend on the relative amount of analyte with respect to sensor and the approximate local amounts of the probe, respectively, enabled qualitative extraction of relative abundance of analyte in various local regions within a single cell as well as amongst different cells. Although the comparisons remain semi-quantitative, this approach involving analysis of multiple spectral parameters opens up an alternative way to extract spatial distribution of analyte in heterogeneous systems. The proposed method would be especially relevant for fluorescent probes that undergo relatively nominal shift in transition energies compared to their emission bandwidths, which often restricts their usage for quantitative ratiometric imaging in cellular media due to strong cross-talk between energetically separated detection channels. Dedicated to Professor Kankan Bhattacharyya.

Rapid determination of free fatty acid content in waste deodorizer distillates using single bounce-attenuated total reflectance-FTIR spectroscopy.

PubMed

Naz, Saba; Sherazi, Sayed Tufail Hussain; Talpur, Farah N; Mahesar, Sarfaraz A; Kara, Huseyin

2012-01-01

A simple, rapid, economical, and environmentally friendly analytical method was developed for the quantitative assessment of free fatty acids (FFAs) present in deodorizer distillates and crude oils by single bounce-attenuated total reflectance-FTIR spectroscopy. Partial least squares was applied for the calibration model based on the peak region of the carbonyl group (C=O) from 1726 to 1664 cm(-1) associated with the FFAs. The proposed method totally avoided the use of organic solvents or costly standards and could be applied easily in the oil processing industry. The accuracy of the method was checked by comparison to a conventional standard American Oil Chemists' Society (AOCS) titrimetric procedure, which provided good correlation (R = 0.99980), with an SD of +/- 0.05%. Therefore, the proposed method could be used as an alternate to the AOCS titrimetric method for the quantitative determination of FFAs especially in deodorizer distillates.

A facile one-step fluorescence method for the quantitation of low-content single base deamination impurity in synthetic oligonucleotides.

PubMed

Su, Xiaoye; Liang, Ruiting; Stolee, Jessica A

2018-06-05

Oligonucleotides are being researched and developed as potential drug candidates for the treatment of a broad spectrum of diseases. The characterization of antisense oligonucleotide (ASO) impurities caused by base mutations (e.g. deamination) which are closely related to the target ASO is a significant analytical challenge. Herein, we describe a novel one-step method, utilizing a strategy that combines fluorescence-ON detection with competitive hybridization, to achieve single base mutation quantitation in extensively modified synthetic ASOs. Given that this method is highly specific and sensitive (LoQ = 4 nM), we envision that it will find utility for screening other impurities as well as sequencing modified oligonucleotides. Copyright © 2018 Elsevier B.V. All rights reserved.

Two-probe versus van der Pauw method in studying the piezoresistivity of single-wall carbon nanotube thin films

NASA Astrophysics Data System (ADS)

Yao, Yanbo; Duan, Xiaoshuang; Luo, Jiangjiang; Liu, Tao

2017-11-01

The use of the van der Pauw (VDP) method for characterizing and evaluating the piezoresistive behavior of carbon nanomaterial enabled piezoresistive sensors have not been systematically studied. By using single-wall carbon nanotube (SWCNT) thin films as a model system, herein we report a coupled electrical-mechanical experimental study in conjunction with a multiphysics finite element simulation as well as an analytic analysis to compare the two-probe and VDP testing configuration in evaluating the piezoresistive behavior of carbon nanomaterial enabled piezoresistive sensors. The key features regarding the sample aspect ratio dependent piezoresistive sensitivity or gauge factor were identified for the VDP testing configuration. It was found that the VDP test configuration offers consistently higher piezoresistive sensitivity than the two-probe testing method.

The current role of on-line extraction approaches in clinical and forensic toxicology.

PubMed

Mueller, Daniel M

2014-08-01

In today's clinical and forensic toxicological laboratories, automation is of interest because of its ability to optimize processes, to reduce manual workload and handling errors and to minimize exposition to potentially infectious samples. Extraction is usually the most time-consuming step; therefore, automation of this step is reasonable. Currently, from the field of clinical and forensic toxicology, methods using the following on-line extraction techniques have been published: on-line solid-phase extraction, turbulent flow chromatography, solid-phase microextraction, microextraction by packed sorbent, single-drop microextraction and on-line desorption of dried blood spots. Most of these published methods are either single-analyte or multicomponent procedures; methods intended for systematic toxicological analysis are relatively scarce. However, the use of on-line extraction will certainly increase in the near future.

Accurate single-scattering simulation of ice cloud using the invariant-imbedding T-matrix method and the physical-geometric optics method

NASA Astrophysics Data System (ADS)

Sun, B.; Yang, P.; Kattawar, G. W.; Zhang, X.

2017-12-01

The ice cloud single-scattering properties can be accurately simulated using the invariant-imbedding T-matrix method (IITM) and the physical-geometric optics method (PGOM). The IITM has been parallelized using the Message Passing Interface (MPI) method to remove the memory limitation so that the IITM can be used to obtain the single-scattering properties of ice clouds for sizes in the geometric optics regime. Furthermore, the results associated with random orientations can be analytically achieved once the T-matrix is given. The PGOM is also parallelized in conjunction with random orientations. The single-scattering properties of a hexagonal prism with height 400 (in units of lambda/2*pi, where lambda is the incident wavelength) and an aspect ratio of 1 (defined as the height over two times of bottom side length) are given by using the parallelized IITM and compared to the counterparts using the parallelized PGOM. The two results are in close agreement. Furthermore, the integrated single-scattering properties, including the asymmetry factor, the extinction cross-section, and the scattering cross-section, are given in a completed size range. The present results show a smooth transition from the exact IITM solution to the approximate PGOM result. Because the calculation of the IITM method has reached the geometric regime, the IITM and the PGOM can be efficiently employed to accurately compute the single-scattering properties of ice cloud in a wide spectral range.

A structurally based analytic model of growth and biomass dynamics in single species stands of conifers

Treesearch

Robin J. Tausch

2015-01-01

A theoretically based analytic model of plant growth in single species conifer communities based on the species fully occupying a site and fully using the site resources is introduced. Model derivations result in a single equation simultaneously describes changes over both, different site conditions (or resources available), and over time for each variable for each...

Reversed-phase single drop microextraction followed by high-performance liquid chromatography with fluorescence detection for the quantification of synthetic phenolic antioxidants in edible oil samples.

PubMed

Farajmand, Bahman; Esteki, Mahnaz; Koohpour, Elham; Salmani, Vahid

2017-04-01

The reversed-phase mode of single drop microextraction has been used as a preparation method for the extraction of some phenolic antioxidants from edible oil samples. Butylated hydroxyl anisole, tert-butylhydroquinone and butylated hydroxytoluene were employed as target compounds for this study. High-performance liquid chromatography followed by fluorescence detection was applied for final determination of target compounds. The most interesting feature of this study is the application of a disposable insulin syringe with some modification for microextraction procedure that efficiently improved the volume and stability of the solvent microdrop. Different parameters such as the type and volume of solvent, sample stirring rate, extraction temperature, and time were investigated and optimized. Analytical performances of the method were evaluated under optimized conditions. Under the optimal conditions, relative standard deviations were between 4.4 and 10.2%. Linear dynamic ranges were 20-10 000 to 2-1000 μg/g (depending on the analytes). Detection limits were 5-670 ng/g. Finally, the proposed method was successfully used for quantification of the antioxidants in some edible oil samples prepared from market. Relative recoveries were achieved from 88 to 111%. The proposed method had a simplicity of operation, low cost, and successful application for real samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Single-Molecule Electronics: Chemical and Analytical Perspectives.

PubMed

Nichols, Richard J; Higgins, Simon J

2015-01-01

It is now possible to measure the electrical properties of single molecules using a variety of techniques including scanning probe microcopies and mechanically controlled break junctions. Such measurements can be made across a wide range of environments including ambient conditions, organic liquids, ionic liquids, aqueous solutions, electrolytes, and ultra high vacuum. This has given new insights into charge transport across molecule electrical junctions, and these experimental methods have been complemented with increasingly sophisticated theory. This article reviews progress in single-molecule electronics from a chemical perspective and discusses topics such as the molecule-surface coupling in electrical junctions, chemical control, and supramolecular interactions in junctions and gating charge transport. The article concludes with an outlook regarding chemical analysis based on single-molecule conductance.

Analytical characterization of wine and its precursors by capillary electrophoresis.

PubMed

Gomez, Federico J V; Monasterio, Romina P; Vargas, Verónica Carolina Soto; Silva, María F

2012-08-01

The accurate determination of marker chemical species in grape, musts, and wines presents a unique analytical challenge with high impact on diverse areas of knowledge such as health, plant physiology, and economy. Capillary electromigration techniques have emerged as a powerful tool, allowing the separation and identification of highly polar compounds that cannot be easily separated by traditional HPLC methods, providing complementary information and permitting the simultaneous analysis of analytes with different nature in a single run. The main advantage of CE over traditional methods for wine analysis is that in most cases samples require no treatment other than filtration. The purpose of this article is to present a revision on capillary electromigration methods applied to the analysis of wine and its precursors over the last decade. The current state of the art of the topic is evaluated, with special emphasis on the natural compounds that have allowed wine to be considered as a functional food. The most representative revised compounds are phenolic compounds, amino acids, proteins, elemental species, mycotoxins, and organic acids. Finally, a discussion on future trends of the role of capillary electrophoresis in the field of analytical characterization of wines for routine analysis, wine classification, as well as multidisciplinary aspects of the so-called "from soil to glass" chain is presented. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Bioassays as one of the Green Chemistry tools for assessing environmental quality: A review.

PubMed

Wieczerzak, M; Namieśnik, J; Kudłak, B

2016-09-01

For centuries, mankind has contributed to irreversible environmental changes, but due to the modern science of recent decades, scientists are able to assess the scale of this impact. The introduction of laws and standards to ensure environmental cleanliness requires comprehensive environmental monitoring, which should also meet the requirements of Green Chemistry. The broad spectrum of Green Chemistry principle applications should also include all of the techniques and methods of pollutant analysis and environmental monitoring. The classical methods of chemical analyses do not always match the twelve principles of Green Chemistry, and they are often expensive and employ toxic and environmentally unfriendly solvents in large quantities. These solvents can generate hazardous and toxic waste while consuming large volumes of resources. Therefore, there is a need to develop reliable techniques that would not only meet the requirements of Green Analytical Chemistry, but they could also complement and sometimes provide an alternative to conventional classical analytical methods. These alternatives may be found in bioassays. Commercially available certified bioassays often come in the form of ready-to-use toxkits, and they are easy to use and relatively inexpensive in comparison with certain conventional analytical methods. The aim of this study is to provide evidence that bioassays can be a complementary alternative to classical methods of analysis and can fulfil Green Analytical Chemistry criteria. The test organisms discussed in this work include single-celled organisms, such as cell lines, fungi (yeast), and bacteria, and multicellular organisms, such as invertebrate and vertebrate animals and plants. Copyright © 2016 Elsevier Ltd. All rights reserved.

Analytical and Computational Properties of Distributed Approaches to MDO

NASA Technical Reports Server (NTRS)

Alexandrov, Natalia M.; Lewis, Robert Michael

2000-01-01

Historical evolution of engineering disciplines and the complexity of the MDO problem suggest that disciplinary autonomy is a desirable goal in formulating and solving MDO problems. We examine the notion of disciplinary autonomy and discuss the analytical properties of three approaches to formulating and solving MDO problems that achieve varying degrees of autonomy by distributing the problem along disciplinary lines. Two of the approaches-Optimization by Linear Decomposition and Collaborative Optimization-are based on bi-level optimization and reflect what we call a structural perspective. The third approach, Distributed Analysis Optimization, is a single-level approach that arises from what we call an algorithmic perspective. The main conclusion of the paper is that disciplinary autonomy may come at a price: in the bi-level approaches, the system-level constraints introduced to relax the interdisciplinary coupling and enable disciplinary autonomy can cause analytical and computational difficulties for optimization algorithms. The single-level alternative we discuss affords a more limited degree of autonomy than that of the bi-level approaches, but without the computational difficulties of the bi-level methods. Key Words: Autonomy, bi-level optimization, distributed optimization, multidisciplinary optimization, multilevel optimization, nonlinear programming, problem integration, system synthesis

Combined imaging and chemical sensing using a single optical imaging fiber.

PubMed

Bronk, K S; Michael, K L; Pantano, P; Walt, D R

1995-09-01

Despite many innovations and developments in the field of fiber-optic chemical sensors, optical fibers have not been employed to both view a sample and concurrently detect an analyte of interest. While chemical sensors employing a single optical fiber or a noncoherent fiberoptic bundle have been applied to a wide variety of analytical determinations, they cannot be used for imaging. Similarly, coherent imaging fibers have been employed only for their originally intended purpose, image transmission. We herein report a new technique for viewing a sample and measuring surface chemical concentrations that employs a coherent imaging fiber. The method is based on the deposition of a thin, analyte-sensitive polymer layer on the distal surface of a 350-microns-diameter imaging fiber. We present results from a pH sensor array and an acetylcholine biosensor array, each of which contains approximately 6000 optical sensors. The acetylcholine biosensor has a detection limit of 35 microM and a fast (< 1 s) response time. In association with an epifluorescence microscope and a charge-coupled device, these modified imaging fibers can display visual information of a remote sample with 4-microns spatial resolution, allowing for alternating acquisition of both chemical analysis and visual histology.

High-throughput label-free screening of euglena gracilis with optofluidic time-stretch quantitative phase microscopy

NASA Astrophysics Data System (ADS)

Guo, Baoshan; Lei, Cheng; Ito, Takuro; Yaxiaer, Yalikun; Kobayashi, Hirofumi; Jiang, Yiyue; Tanaka, Yo; Ozeki, Yasuyuki; Goda, Keisuke

2017-02-01

The development of reliable, sustainable, and economical sources of alternative fuels is an important, but challenging goal for the world. As an alternative to liquid fossil fuels, microalgal biofuel is expected to play a key role in reducing the detrimental effects of global warming since microalgae absorb atmospheric CO2 via photosynthesis. Unfortunately, conventional analytical methods only provide population-averaged lipid contents and fail to characterize a diverse population of microalgal cells with single-cell resolution in a noninvasive and interference-free manner. Here we demonstrate high-throughput label-free single-cell screening of lipid-producing microalgal cells with optofluidic time-stretch quantitative phase microscopy. In particular, we use Euglena gracilis - an attractive microalgal species that produces wax esters (suitable for biodiesel and aviation fuel after refinement) within lipid droplets. Our optofluidic time-stretch quantitative phase microscope is based on an integration of a hydrodynamic-focusing microfluidic chip, an optical time-stretch phase-contrast microscope, and a digital image processor equipped with machine learning. As a result, it provides both the opacity and phase contents of every single cell at a high throughput of 10,000 cells/s. We characterize heterogeneous populations of E. gracilis cells under two different culture conditions to evaluate their lipid production efficiency. Our method holds promise as an effective analytical tool for microalgaebased biofuel production.

Single frequency GPS measurements in real-time artificial satellite orbit determination

NASA Astrophysics Data System (ADS)

Chiaradia, orbit determination A. P. M.; Kuga, H. K.; Prado, A. F. B. A.

2003-07-01

A simplified and compact algorithm with low computational cost providing an accuracy around tens of meters for artificial satellite orbit determination in real-time and on-board is developed in this work. The state estimation method is the extended Kalman filter. The Cowell's method is used to propagate the state vector, through a simple Runge-Kutta numerical integrator of fourth order with fixed step size. The modeled forces are due to the geopotential up to 50th order and degree of JGM-2 model. To time-update the state error covariance matrix, it is considered a simplified force model. In other words, in computing the state transition matrix, the effect of J 2 (Earth flattening) is analytically considered, which unloads dramatically the processing time. In the measurement model, the single frequency GPS pseudorange is used, considering the effects of the ionospheric delay, clock offsets of the GPS and user satellites, and relativistic effects. To validate this model, real live data are used from Topex/Poseidon satellite and the results are compared with the Topex/Poseidon Precision Orbit Ephemeris (POE) generated by NASA/JPL, for several test cases. It is concluded that this compact algorithm enables accuracies of tens of meters with such simplified force model, analytical approach for computing the transition matrix, and a cheap GPS receiver providing single frequency pseudorange measurements.

An Analytic Approach for Optimal Geometrical Design of GaAs Nanowires for Maximal Light Harvesting in Photovoltaic Cells

PubMed Central

Wu, Dan; Tang, Xiaohong; Wang, Kai; Li, Xianqiang

2017-01-01

Semiconductor nanowires(NWs) with subwavelength scale diameters have demonstrated superior light trapping features, which unravel a new pathway for low cost and high efficiency future generation solar cells. Unlike other published work, a fully analytic design is for the first time proposed for optimal geometrical parameters of vertically-aligned GaAs NW arrays for maximal energy harvesting. Using photocurrent density as the light absorbing evaluation standard, 2 μm length NW arrays whose multiple diameters and periodicity are quantitatively identified achieving the maximal value of 29.88 mA/cm2 under solar illumination. It also turns out that our method has wide suitability for single, double and four different diameters of NW arrays for highest photon energy harvesting. To validate this analytical method, intensive numerical three-dimensional finite-difference time-domain simulations of the NWs’ light harvesting are also carried out. Compared with the simulation results, the predicted maximal photocurrent densities lie within 1.5% tolerance for all cases. Along with the high accuracy, through directly disclosing the exact geometrical dimensions of NW arrays, this method provides an effective and efficient route for high performance photovoltaic design. PMID:28425488

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

PubMed

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

2015-01-01

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

Application of factorial designs to study factors involved in the determination of aldehydes present in beer by on-fiber derivatization in combination with gas chromatography and mass spectrometry.

PubMed

Carrillo, Génesis; Bravo, Adriana; Zufall, Carsten

2011-05-11

With the aim of studying the factors involved in on-fiber derivatization of Strecker aldehydes, furfural, and (E)-2-nonenal with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine in beer, factorial designs were applied. The effect of the temperature, time, and NaCl addition on the analytes' derivatization/extraction efficiency was studied through a factorial 2(3) randomized-block design; all of the factors and their interactions were significant at the 95% confidence level for most of the analytes. The effect of temperature and its interactions separated the analytes in two groups. However, a single sampling condition was selected that optimized response for most aldehydes. The resulting method, combining on-fiber derivatization with gas chromatography-mass spectrometry, was validated. Limits of detections were between 0.015 and 1.60 μg/L, and relative standard deviations were between 1.1 and 12.2%. The efficacy of the internal standardization method was confirmed by recovery percentage (73-117%). The method was applied to the determination of aldehydes in fresh beer and after storage at 28 °C.

RP-HPLC method with electrochemical detection for the determination of metoclopramide in serum and its use in pharmacokinetic studies.

PubMed

Lamparczyk, H; Chmielewska, A; Konieczna, L; Plenis, A; Zarzycki, P K

2001-12-01

A rapid and sensitive reversed-phase high performance liquid chromatographic method has been developed for the determination of metoclopramide in serum. The assay was performed after single extraction with ethyl ether using methyl parahydroxybenzoate as internal standard. Chromatographic separations were performed on C(18) stationary phase with a mobile phase composed of methanol-phosphate buffer pH 3 (30:70 v/v). Analytes were detected electrochemically. The quantification limit for metoclopramide in serum was 2 ng mL(-1). Linearity of the method was confirmed in the range of 5-120 ng mL(-1) (correlation coefficient 0.9998). Within-day relative standard deviations (RSDs) ranged from 0.3 to 5.5% and between-day RSDs from 0.8 to 6.0%. The analytical method was successfully applied for the determination of pharmacokinetic parameters after ingestion of 10 mg dose of metoclopramide. Studies were performed on 18 healthy volunteers of both sexes. Copyright 2001 John Wiley & Sons, Ltd.

Broadband impedance boundary conditions for the simulation of sound propagation in the time domain.

PubMed

Bin, Jonghoon; Yousuff Hussaini, M; Lee, Soogab

2009-02-01

An accurate and practical surface impedance boundary condition in the time domain has been developed for application to broadband-frequency simulation in aeroacoustic problems. To show the capability of this method, two kinds of numerical simulations are performed and compared with the analytical/experimental results: one is acoustic wave reflection by a monopole source over an impedance surface and the other is acoustic wave propagation in a duct with a finite impedance wall. Both single-frequency and broadband-frequency simulations are performed within the framework of linearized Euler equations. A high-order dispersion-relation-preserving finite-difference method and a low-dissipation, low-dispersion Runge-Kutta method are used for spatial discretization and time integration, respectively. The results show excellent agreement with the analytical/experimental results at various frequencies. The method accurately predicts both the amplitude and the phase of acoustic pressure and ensures the well-posedness of the broadband time-domain impedance boundary condition.

Assessment of technological level of stem cell research using principal component analysis.

PubMed

Do Cho, Sung; Hwan Hyun, Byung; Kim, Jae Kyeom

2016-01-01

In general, technological levels have been assessed based on specialist's opinion through the methods such as Delphi. But in such cases, results could be significantly biased per study design and individual expert. In this study, therefore scientific literatures and patents were selected by means of analytic indexes for statistic approach and technical assessment of stem cell fields. The analytic indexes, numbers and impact indexes of scientific literatures and patents, were weighted based on principal component analysis, and then, were summated into the single value. Technological obsolescence was calculated through the cited half-life of patents issued by the United States Patents and Trademark Office and was reflected in technological level assessment. As results, ranks of each nation's in reference to the technology level were rated by the proposed method. Furthermore we were able to evaluate strengthens and weaknesses thereof. Although our empirical research presents faithful results, in the further study, there is a need to compare the existing methods and the suggested method.

Non-volatile analysis in fruits by laser resonant ionization spectrometry: application to resveratrol (3,5,4'-trihydroxystilbene) in grapes

NASA Astrophysics Data System (ADS)

Montero, C.; Orea, J. M.; Soledad Muñoz, M.; Lobo, R. F. M.; González Ureña, A.

A laser desorption (LD) coupled with resonance-enhanced multiphoton ionisation (REMPI) and time-of-flight mass spectrometry (TOFMS) technique for non-volatile trace analysis compounds is presented. Essential features are: (a) an enhanced desorption yield due to the mixing of metal powder with the analyte in the sample preparation, (b) a high resolution, great sensitivity and low detection limit due to laser resonant ionisation and mass spectrometry detection. Application to resveratrol content in grapes demonstrated the capability of the analytical method with a sensitivity of 0.2 pg per single laser shot and a detection limit of 5 ppb.

Analytic energy gradients for the coupled-cluster singles and doubles method with the density-fitting approximation

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

Bozkaya, Uğur, E-mail: ugur.bozkaya@hacettepe.edu.tr; Department of Chemistry, Atatürk University, Erzurum 25240; Sherrill, C. David

2016-05-07

An efficient implementation is presented for analytic gradients of the coupled-cluster singles and doubles (CCSD) method with the density-fitting approximation, denoted DF-CCSD. Frozen core terms are also included. When applied to a set of alkanes, the DF-CCSD analytic gradients are significantly accelerated compared to conventional CCSD for larger molecules. The efficiency of our DF-CCSD algorithm arises from the acceleration of several different terms, which are designated as the “gradient terms”: computation of particle density matrices (PDMs), generalized Fock-matrix (GFM), solution of the Z-vector equation, formation of the relaxed PDMs and GFM, back-transformation of PDMs and GFM to the atomic orbitalmore » (AO) basis, and evaluation of gradients in the AO basis. For the largest member of the alkane set (C{sub 10}H{sub 22}), the computational times for the gradient terms (with the cc-pVTZ basis set) are 2582.6 (CCSD) and 310.7 (DF-CCSD) min, respectively, a speed up of more than 8-folds. For gradient related terms, the DF approach avoids the usage of four-index electron repulsion integrals. Based on our previous study [U. Bozkaya, J. Chem. Phys. 141, 124108 (2014)], our formalism completely avoids construction or storage of the 4-index two-particle density matrix (TPDM), using instead 2- and 3-index TPDMs. The DF approach introduces negligible errors for equilibrium bond lengths and harmonic vibrational frequencies.« less

Development and validation of a single robust HPLC method for the characterization of a pharmaceutical starting material and impurities from three suppliers using three separate synthetic routes.

PubMed

Sheldon, E M; Downar, J B

2000-08-15

Novel approaches to the development of analytical procedures for monitoring incoming starting material in support of chemical/pharmaceutical processes are described. High technology solutions were utilized for timely process development and preparation of high quality clinical supplies. A single robust HPLC method was developed and characterized for the analysis of the key starting material from three suppliers. Each supplier used a different process for the preparation of this material and, therefore, each suppliers' material exhibited a unique impurity profile. The HPLC method utilized standard techniques acceptable for release testing in a QC/manufacturing environment. An automated experimental design protocol was used to characterize the robustness of the HPLC method. The method was evaluated for linearity, limit of quantitation, solution stability, and precision of replicate injections. An LC-MS method that emulated the release HPLC method was developed and the identities of impurities were mapped between the two methods.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by Carbopak-B solid-phase extraction and high-preformance liquid chromatography

USGS Publications Warehouse

Werner, Stephen L.; Burkhardt, Mark R.; DeRusseau, Sabrina N.

1996-01-01

In accordance with the needs of the National Water-Quality Assessment Program (NAWQA), the U.S. Geological Survey has developed and implemented a graphitized carbon-based solid-phase extraction and high-performance liquid chromatographic analytical method. The method is used to determine 41 pesticides and pesticide metabolites that are not readily amenable to gas chromatography or other high-temperature analytical techniques. Pesticides are extracted from filtered environmental water samples using a 0.5-gram graphitized carbon-based solid-phase cartridge, eluted from the cartridge into two analytical fractions, and analyzed using high-performance liquid chromatography with photodiode-array detection. The upper concentration limit is 1.6 micrograms per liter (=B5g/L) for most compounds. Single-operator method detection limits in organic-free water samples ranged from 0.006 to 0.032 =B5g/L= Recoveries in organic-free water samples ranged from 37 to 88 percent. Recoveries in ground- and surface-water samples ranged from 29 to 94 percent. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time of 7 days.

VERTPAK1. Code Verification Analytic Solution

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

Golis, M.J.

1983-04-01

VERTPAK1 is a package of analytical solutions used in verification of numerical codes that simulate fluid flow, rock deformation, and solute transport in fractured and unfractured porous media. VERTPAK1 contains the following: BAREN, an analytical solution developed by Barenblatt, Zhelton and Kochina (1960) for describing transient flow to a well penetrating a (double porosity) confined aquifer; GIBMAC, an analytical solution developed by McNamee and Gibson (1960) for describing consolidation of a semi-infinite soil medium subject to a strip (plane strain) or cylindrical (axisymmetric) loading; GRINRH, an analytical solution developed by Gringarten (1971) for describing transient flow to a partially penetratingmore » well in a confined aquifer containing a single horizontal fracture; GRINRV, an analytical solution developed by Gringarten, Ramey, and Raghavan (1974) for describing transient flow to a fully penetrating well in a confined aquifer containing a single vertical fracture; HART, an analytical solution given by Nowacki (1962) and implemented by HART (1981) for describing the elastic behavior of an infinite solid subject to a line heat source; LESTER, an analytical solution presented by Lester, Jansen, and Burkholder (1975) for describing one-dimensional transport of radionuclide chains through an adsorbing medium; STRELT, an analytical solution presented by Streltsova-Adams (1978) for describing transient flow to a fully penetrating well in a (double porosity) confined aquifer; and TANG, an analytical solution developed by Tang, Frind, and Sudicky (1981) for describing solute transport in a porous medium containing a single fracture.« less

Evaluating statistical and clinical significance of intervention effects in single-case experimental designs: an SPSS method to analyze univariate data.

PubMed

Maric, Marija; de Haan, Else; Hogendoorn, Sanne M; Wolters, Lidewij H; Huizenga, Hilde M

2015-03-01

Single-case experimental designs are useful methods in clinical research practice to investigate individual client progress. Their proliferation might have been hampered by methodological challenges such as the difficulty applying existing statistical procedures. In this article, we describe a data-analytic method to analyze univariate (i.e., one symptom) single-case data using the common package SPSS. This method can help the clinical researcher to investigate whether an intervention works as compared with a baseline period or another intervention type, and to determine whether symptom improvement is clinically significant. First, we describe the statistical method in a conceptual way and show how it can be implemented in SPSS. Simulation studies were performed to determine the number of observation points required per intervention phase. Second, to illustrate this method and its implications, we present a case study of an adolescent with anxiety disorders treated with cognitive-behavioral therapy techniques in an outpatient psychotherapy clinic, whose symptoms were regularly assessed before each session. We provide a description of the data analyses and results of this case study. Finally, we discuss the advantages and shortcomings of the proposed method. Copyright © 2014. Published by Elsevier Ltd.

Exact Solutions for Rate and Synchrony in Recurrent Networks of Coincidence Detectors

PubMed Central

Mikula, Shawn; Niebur, Ernst

2009-01-01

We provide analytical solutions for mean firing rates and cross-correlations of coincidence detector neurons in recurrent networks with excitatory or inhibitory connectivity with rate-modulated steady-state spiking inputs. We use discrete-time finite-state Markov chains to represent network state transition probabilities, which are subsequently used to derive exact analytical solutions for mean firing rates and cross-correlations. As illustrated in several examples, the method can be used for modeling cortical microcircuits and clarifying single-neuron and population coding mechanisms. We also demonstrate that increasing firing rates do not necessarily translate into increasing cross-correlations, though our results do support the contention that firing rates and cross-correlations are likely to be coupled. Our analytical solutions underscore the complexity of the relationship between firing rates and cross-correlations. PMID:18439133

Quantitative Methods Based on Twisted Nematic Liquid Crystals for Mapping Surfaces Patterned with Bio/Chemical Functionality Relevant to Bioanalytical Assays

PubMed Central

Lowe, Aaron M.; Bertics, Paul J.; Abbott, Nicholas L.

2009-01-01

We report methods for the acquisition and analysis of optical images formed by thin films of twisted nematic liquid crystals (LCs) placed into contact with surfaces patterned with bio/chemical functionality relevant to surface-based assays. The methods are simple to implement and are shown to provide easily interpreted maps of chemical transformations on surfaces that are widely exploited in the preparation of analytic devices. The methods involve acquisition of multiple images of the LC as a function of the orientation of a polarizer; data analysis condenses the information present in the stack of images into a spatial map of the twist angle of the LC on the analytic surface. The potential utility of the methods is illustrated by mapping (i) the displacement of a monolayer formed from one alkanethiol on a gold film by a second thiol in solution, (ii) coadsorption of mixtures of amine-terminated and ethyleneglycol-terminated alkanethiols on gold films, which leads to a type of mixed monolayer that is widely exploited for immobilization of proteins on analytic surfaces, and (iii) patterns of antibodies printed onto surfaces. These results show that maps of the twist angle of the LC constructed from families of optical images can be used to reveal surface features that are not apparent in a single image of the LC film. Furthermore, the twist angles of the LC can be used to quantify the energy of interaction of the LC with the surface with a spatial resolution of <10 µm. When combined, the results described in this paper suggest non-destructive methods to monitor and validate chemical transformations on surfaces of the type that are routinely employed in the preparation of surface-based analytic technologies. PMID:18355089

Rapid ultrasensitive single particle surface-enhanced Raman spectroscopy using metallic nanopores.

PubMed

Cecchini, Michael P; Wiener, Aeneas; Turek, Vladimir A; Chon, Hyangh; Lee, Sangyeop; Ivanov, Aleksandar P; McComb, David W; Choo, Jaebum; Albrecht, Tim; Maier, Stefan A; Edel, Joshua B

2013-10-09

Nanopore sensors embedded within thin dielectric membranes have been gaining significant interest due to their single molecule sensitivity and compatibility of detecting a large range of analytes, from DNA and proteins, to small molecules and particles. Building on this concept we utilize a metallic Au solid-state membrane to translocate and rapidly detect single Au nanoparticles (NPs) functionalized with 589 dye molecules using surface-enhanced resonance Raman spectroscopy (SERRS). We show that, due to the plasmonic coupling between the Au metallic nanopore surface and the NP, signal intensities are enhanced when probing analyte molecules bound to the NP surface. Although not single molecule, this nanopore sensing scheme benefits from the ability of SERRS to provide rich vibrational information on the analyte, improving on current nanopore-based electrical and optical detection techniques. We show that the full vibrational spectrum of the analyte can be detected with ultrahigh spectral sensitivity and a rapid temporal resolution of 880 μs.

Improving Sample Distribution Homogeneity in Three-Dimensional Microfluidic Paper-Based Analytical Devices by Rational Device Design.

PubMed

Morbioli, Giorgio Gianini; Mazzu-Nascimento, Thiago; Milan, Luis Aparecido; Stockton, Amanda M; Carrilho, Emanuel

2017-05-02

Paper-based devices are a portable, user-friendly, and affordable technology that is one of the best analytical tools for inexpensive diagnostic devices. Three-dimensional microfluidic paper-based analytical devices (3D-μPADs) are an evolution of single layer devices and they permit effective sample dispersion, individual layer treatment, and multiplex analytical assays. Here, we present the rational design of a wax-printed 3D-μPAD that enables more homogeneous permeation of fluids along the cellulose matrix than other existing designs in the literature. Moreover, we show the importance of the rational design of channels on these devices using glucose oxidase, peroxidase, and 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) reactions. We present an alternative method for layer stacking using a magnetic apparatus, which facilitates fluidic dispersion and improves the reproducibility of tests performed on 3D-μPADs. We also provide the optimized designs for printing, facilitating further studies using 3D-μPADs.

Analytical studies on the instabilities of heterogeneous intelligent traffic flow

NASA Astrophysics Data System (ADS)

Ngoduy, D.

2013-10-01

It has been widely reported in literature that a small perturbation in traffic flow such as a sudden deceleration of a vehicle could lead to the formation of traffic jams without a clear bottleneck. These traffic jams are usually related to instabilities in traffic flow. The applications of intelligent traffic systems are a potential solution to reduce the amplitude or to eliminate the formation of such traffic instabilities. A lot of research has been conducted to theoretically study the effect of intelligent vehicles, for example adaptive cruise control vehicles, using either computer simulation or analytical method. However, most current analytical research has only applied to single class traffic flow. To this end, the main topic of this paper is to perform a linear stability analysis to find the stability threshold of heterogeneous traffic flow using microscopic models, particularly the effect of intelligent vehicles on heterogeneous (or multi-class) traffic flow instabilities. The analytical results will show how intelligent vehicle percentages affect the stability of multi-class traffic flow.

Analytic image reconstruction from partial data for a single-scan cone-beam CT with scatter correction

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

Min, Jonghwan; Pua, Rizza; Cho, Seungryong, E-mail: scho@kaist.ac.kr

Purpose: A beam-blocker composed of multiple strips is a useful gadget for scatter correction and/or for dose reduction in cone-beam CT (CBCT). However, the use of such a beam-blocker would yield cone-beam data that can be challenging for accurate image reconstruction from a single scan in the filtered-backprojection framework. The focus of the work was to develop an analytic image reconstruction method for CBCT that can be directly applied to partially blocked cone-beam data in conjunction with the scatter correction. Methods: The authors developed a rebinned backprojection-filteration (BPF) algorithm for reconstructing images from the partially blocked cone-beam data in amore » circular scan. The authors also proposed a beam-blocking geometry considering data redundancy such that an efficient scatter estimate can be acquired and sufficient data for BPF image reconstruction can be secured at the same time from a single scan without using any blocker motion. Additionally, scatter correction method and noise reduction scheme have been developed. The authors have performed both simulation and experimental studies to validate the rebinned BPF algorithm for image reconstruction from partially blocked cone-beam data. Quantitative evaluations of the reconstructed image quality were performed in the experimental studies. Results: The simulation study revealed that the developed reconstruction algorithm successfully reconstructs the images from the partial cone-beam data. In the experimental study, the proposed method effectively corrected for the scatter in each projection and reconstructed scatter-corrected images from a single scan. Reduction of cupping artifacts and an enhancement of the image contrast have been demonstrated. The image contrast has increased by a factor of about 2, and the image accuracy in terms of root-mean-square-error with respect to the fan-beam CT image has increased by more than 30%. Conclusions: The authors have successfully demonstrated that the proposed scanning method and image reconstruction algorithm can effectively estimate the scatter in cone-beam projections and produce tomographic images of nearly scatter-free quality. The authors believe that the proposed method would provide a fast and efficient CBCT scanning option to various applications particularly including head-and-neck scan.« less

Methods for detection of GMOs in food and feed.

PubMed

Marmiroli, Nelson; Maestri, Elena; Gullì, Mariolina; Malcevschi, Alessio; Peano, Clelia; Bordoni, Roberta; De Bellis, Gianluca

2008-10-01

This paper reviews aspects relevant to detection and quantification of genetically modified (GM) material within the feed/food chain. The GM crop regulatory framework at the international level is evaluated with reference to traceability and labelling. Current analytical methods for the detection, identification, and quantification of transgenic DNA in food and feed are reviewed. These methods include quantitative real-time PCR, multiplex PCR, and multiplex real-time PCR. Particular attention is paid to methods able to identify multiple GM events in a single reaction and to the development of microdevices and microsensors, though they have not been fully validated for application.

Detector response function of an energy-resolved CdTe single photon counting detector.

PubMed

Liu, Xin; Lee, Hyoung Koo

2014-01-01

While spectral CT using single photon counting detector has shown a number of advantages in diagnostic imaging, knowledge of the detector response function of an energy-resolved detector is needed to correct the signal bias and reconstruct the image more accurately. The objective of this paper is to study the photo counting detector response function using laboratory sources, and investigate the signal bias correction method. Our approach is to model the detector response function over the entire diagnostic energy range (20 keV

Brain Connectivity as a DNA Sequencing Problem

NASA Astrophysics Data System (ADS)

Zador, Anthony

The mammalian cortex consists of millions or billions of neurons, each connected to thousands of other neurons. Traditional methods for determining the brain connectivity rely on microscopy to visualize neuronal connections, but such methods are slow, labor-intensive and often lack single neuron resolution. We have recently developed a new method, MAPseq, to recast the determination of brain wiring into a form that can exploit the tremendous recent advances in high-throughput DNA sequencing. DNA sequencing technology has outpaced even Moore's law, so that the cost of sequencing the human genome has dropped from a billion dollars in 2001 to below a thousand dollars today. MAPseq works by introducing random sequences of DNA-``barcodes''-to tag neurons uniquely. With MAPseq, we can determine the connectivity of over 50K single neurons in a single mouse cortex in about a week, an unprecedented throughput, ushering in the era of ``big data'' for brain wiring. We are now developing analytical tools and algorithms to make sense of these novel data sets.

In-flight thrust determination

NASA Technical Reports Server (NTRS)

Abernethy, Robert B.; Adams, Gary R.; Ascough, John C.; Baer-Riedhart, Jennifer L.; Balkcom, George H.; Biesiadny, Thomas

1986-01-01

The major aspects of processes that may be used for the determination of in-flight thrust are reviewed. Basic definitions are presented as well as analytical and ground-test methods for gathering data and calculating the thrust of the propulsion system during the flight development program of the aircraft. Test analysis examples include a single-exhaust turbofan, an intermediate-cowl turbofan, and a mixed-flow afterburning turbofan.

Using Learning Analytics to Identify Medical Student Misconceptions in an Online Virtual Patient Environment

ERIC Educational Resources Information Center

Poitras, Eric G.; Naismith, Laura M.; Doleck, Tenzin; Lajoie, Susanne P.

2016-01-01

This study aimed to identify misconceptions in medical student knowledge by mining user interactions in the MedU online learning environment. Data from 13000 attempts at a single virtual patient case were extracted from the MedU MySQL database. A subgroup discovery method was applied to identify patterns in learner-generated annotations and…

40 CFR 53.33 - Test Procedure for Methods for Lead (Pb).

Code of Federal Regulations, 2014 CFR

2014-07-01

... analytical procedure than specified in 40 CFR Appendix G, may be tested by analyzing pairs of filter strips... Appendix Q, requires the use of two PM 10 reference samplers because a single 46.2-mm filter from a reference sampler may not be divided prior to analysis. It is possible to analyze a 46.2-mm filter first...

40 CFR 53.33 - Test Procedure for Methods for Lead (Pb).

Code of Federal Regulations, 2013 CFR

2013-07-01

... analytical procedure than specified in 40 CFR Appendix G, may be tested by analyzing pairs of filter strips... Appendix Q, requires the use of two PM 10 reference samplers because a single 46.2-mm filter from a reference sampler may not be divided prior to analysis. It is possible to analyze a 46.2-mm filter first...

Illustrating the Steady-State Condition and the Single-Molecule Kinetic Method with the NMDA Receptor

ERIC Educational Resources Information Center

Kosman, Daniel J.

2009-01-01

The steady-state is a fundamental aspect of biochemical pathways in cells; indeed, the concept of steady-state is a definition of life itself. In a simple enzyme kinetic scheme, the steady-state condition is easy to define analytically but experimentally often difficult to capture because of its evanescent quality; the initial, constant velocity…

Irregular analytical errors in diagnostic testing - a novel concept.

PubMed

Vogeser, Michael; Seger, Christoph

2018-02-23

In laboratory medicine, routine periodic analyses for internal and external quality control measurements interpreted by statistical methods are mandatory for batch clearance. Data analysis of these process-oriented measurements allows for insight into random analytical variation and systematic calibration bias over time. However, in such a setting, any individual sample is not under individual quality control. The quality control measurements act only at the batch level. Quantitative or qualitative data derived for many effects and interferences associated with an individual diagnostic sample can compromise any analyte. It is obvious that a process for a quality-control-sample-based approach of quality assurance is not sensitive to such errors. To address the potential causes and nature of such analytical interference in individual samples more systematically, we suggest the introduction of a new term called the irregular (individual) analytical error. Practically, this term can be applied in any analytical assay that is traceable to a reference measurement system. For an individual sample an irregular analytical error is defined as an inaccuracy (which is the deviation from a reference measurement procedure result) of a test result that is so high it cannot be explained by measurement uncertainty of the utilized routine assay operating within the accepted limitations of the associated process quality control measurements. The deviation can be defined as the linear combination of the process measurement uncertainty and the method bias for the reference measurement system. Such errors should be coined irregular analytical errors of the individual sample. The measurement result is compromised either by an irregular effect associated with the individual composition (matrix) of the sample or an individual single sample associated processing error in the analytical process. Currently, the availability of reference measurement procedures is still highly limited, but LC-isotope-dilution mass spectrometry methods are increasingly used for pre-market validation of routine diagnostic assays (these tests also involve substantial sets of clinical validation samples). Based on this definition/terminology, we list recognized causes of irregular analytical error as a risk catalog for clinical chemistry in this article. These issues include reproducible individual analytical errors (e.g. caused by anti-reagent antibodies) and non-reproducible, sporadic errors (e.g. errors due to incorrect pipetting volume due to air bubbles in a sample), which can both lead to inaccurate results and risks for patients.

Recent advances in magnesium assessment: From single selective sensors to multisensory approach.

PubMed

Lvova, Larisa; Gonçalves, Carla Guanais; Di Natale, Corrado; Legin, Andrey; Kirsanov, Dmitry; Paolesse, Roberto

2018-03-01

The development of efficient analytical procedures for the selective detection of magnesium is an important analytical task, since this element is one of the most abundant metals in cells and plays an essential role in a plenty of cellular processes. Magnesium misbalance has been related to several pathologies and diseases both in plants and animals, as far as in humans, but the number of suitable methods for magnesium detection especially in life sample and biological environments is scarce. Chemical sensors, due to their high reliability, simplicity of handling and instrumentation, fast and real-time in situ and on site analysis are promising candidates for magnesium analysis and represent an attractive alternative to the standard instrumental methods. Here the recent achievements in the development of chemical sensors for magnesium ions detection over the last decade are reviewed. The working principles and the main types of sensors applied are described. Focus is placed on the optical sensors and multisensory systems applications for magnesium assessment in different media. Further, a critical outlook on the employment of multisensory approach in comparison to single selective sensors application in biological samples is presented. Copyright © 2017 Elsevier B.V. All rights reserved.

Kinetic Titration Series with Biolayer Interferometry

PubMed Central

Frenzel, Daniel; Willbold, Dieter

2014-01-01

Biolayer interferometry is a method to analyze protein interactions in real-time. In this study, we illustrate the usefulness to quantitatively analyze high affinity protein ligand interactions employing a kinetic titration series for characterizing the interactions between two pairs of interaction patterns, in particular immunoglobulin G and protein G B1 as well as scFv IC16 and amyloid beta (1–42). Kinetic titration series are commonly used in surface plasmon resonance and involve sequential injections of analyte over a desired concentration range on a single ligand coated sensor chip without waiting for complete dissociation between the injections. We show that applying this method to biolayer interferometry is straightforward and i) circumvents problems in data evaluation caused by unavoidable sensor differences, ii) saves resources and iii) increases throughput if screening a multitude of different analyte/ligand combinations. PMID:25229647

Kinetic titration series with biolayer interferometry.

PubMed

Frenzel, Daniel; Willbold, Dieter

2014-01-01

Biolayer interferometry is a method to analyze protein interactions in real-time. In this study, we illustrate the usefulness to quantitatively analyze high affinity protein ligand interactions employing a kinetic titration series for characterizing the interactions between two pairs of interaction patterns, in particular immunoglobulin G and protein G B1 as well as scFv IC16 and amyloid beta (1-42). Kinetic titration series are commonly used in surface plasmon resonance and involve sequential injections of analyte over a desired concentration range on a single ligand coated sensor chip without waiting for complete dissociation between the injections. We show that applying this method to biolayer interferometry is straightforward and i) circumvents problems in data evaluation caused by unavoidable sensor differences, ii) saves resources and iii) increases throughput if screening a multitude of different analyte/ligand combinations.

CREME96 and Related Error Rate Prediction Methods

NASA Technical Reports Server (NTRS)

Adams, James H., Jr.

2012-01-01

Predicting the rate of occurrence of single event effects (SEEs) in space requires knowledge of the radiation environment and the response of electronic devices to that environment. Several analytical models have been developed over the past 36 years to predict SEE rates. The first error rate calculations were performed by Binder, Smith and Holman. Bradford and Pickel and Blandford, in their CRIER (Cosmic-Ray-Induced-Error-Rate) analysis code introduced the basic Rectangular ParallelePiped (RPP) method for error rate calculations. For the radiation environment at the part, both made use of the Cosmic Ray LET (Linear Energy Transfer) spectra calculated by Heinrich for various absorber Depths. A more detailed model for the space radiation environment within spacecraft was developed by Adams and co-workers. This model, together with a reformulation of the RPP method published by Pickel and Blandford, was used to create the CR ME (Cosmic Ray Effects on Micro-Electronics) code. About the same time Shapiro wrote the CRUP (Cosmic Ray Upset Program) based on the RPP method published by Bradford. It was the first code to specifically take into account charge collection from outside the depletion region due to deformation of the electric field caused by the incident cosmic ray. Other early rate prediction methods and codes include the Single Event Figure of Merit, NOVICE, the Space Radiation code and the effective flux method of Binder which is the basis of the SEFA (Scott Effective Flux Approximation) model. By the early 1990s it was becoming clear that CREME and the other early models needed Revision. This revision, CREME96, was completed and released as a WWW-based tool, one of the first of its kind. The revisions in CREME96 included improved environmental models and improved models for calculating single event effects. The need for a revision of CREME also stimulated the development of the CHIME (CRRES/SPACERAD Heavy Ion Model of the Environment) and MACREE (Modeling and Analysis of Cosmic Ray Effects in Electronics). The Single Event Figure of Merit method was also revised to use the solar minimum galactic cosmic ray spectrum and extended to circular orbits down to 200 km at any inclination. More recently a series of commercial codes was developed by TRAD (Test & Radiations) which includes the OMERE code which calculates single event effects. There are other error rate prediction methods which use Monte Carlo techniques. In this chapter the analytic methods for estimating the environment within spacecraft will be discussed.

Geovisual analytics to enhance spatial scan statistic interpretation: an analysis of U.S. cervical cancer mortality

PubMed Central

Chen, Jin; Roth, Robert E; Naito, Adam T; Lengerich, Eugene J; MacEachren, Alan M

2008-01-01

Background Kulldorff's spatial scan statistic and its software implementation – SaTScan – are widely used for detecting and evaluating geographic clusters. However, two issues make using the method and interpreting its results non-trivial: (1) the method lacks cartographic support for understanding the clusters in geographic context and (2) results from the method are sensitive to parameter choices related to cluster scaling (abbreviated as scaling parameters), but the system provides no direct support for making these choices. We employ both established and novel geovisual analytics methods to address these issues and to enhance the interpretation of SaTScan results. We demonstrate our geovisual analytics approach in a case study analysis of cervical cancer mortality in the U.S. Results We address the first issue by providing an interactive visual interface to support the interpretation of SaTScan results. Our research to address the second issue prompted a broader discussion about the sensitivity of SaTScan results to parameter choices. Sensitivity has two components: (1) the method can identify clusters that, while being statistically significant, have heterogeneous contents comprised of both high-risk and low-risk locations and (2) the method can identify clusters that are unstable in location and size as the spatial scan scaling parameter is varied. To investigate cluster result stability, we conducted multiple SaTScan runs with systematically selected parameters. The results, when scanning a large spatial dataset (e.g., U.S. data aggregated by county), demonstrate that no single spatial scan scaling value is known to be optimal to identify clusters that exist at different scales; instead, multiple scans that vary the parameters are necessary. We introduce a novel method of measuring and visualizing reliability that facilitates identification of homogeneous clusters that are stable across analysis scales. Finally, we propose a logical approach to proceed through the analysis of SaTScan results. Conclusion The geovisual analytics approach described in this manuscript facilitates the interpretation of spatial cluster detection methods by providing cartographic representation of SaTScan results and by providing visualization methods and tools that support selection of SaTScan parameters. Our methods distinguish between heterogeneous and homogeneous clusters and assess the stability of clusters across analytic scales. Method We analyzed the cervical cancer mortality data for the United States aggregated by county between 2000 and 2004. We ran SaTScan on the dataset fifty times with different parameter choices. Our geovisual analytics approach couples SaTScan with our visual analytic platform, allowing users to interactively explore and compare SaTScan results produced by different parameter choices. The Standardized Mortality Ratio and reliability scores are visualized for all the counties to identify stable, homogeneous clusters. We evaluated our analysis result by comparing it to that produced by other independent techniques including the Empirical Bayes Smoothing and Kafadar spatial smoother methods. The geovisual analytics approach introduced here is developed and implemented in our Java-based Visual Inquiry Toolkit. PMID:18992163

Determination of mycotoxins in foods: current state of analytical methods and limitations.

PubMed

Köppen, Robert; Koch, Matthias; Siegel, David; Merkel, Stefan; Maul, Ronald; Nehls, Irene

2010-05-01

Mycotoxins are natural contaminants produced by a range of fungal species. Their common occurrence in food and feed poses a threat to the health of humans and animals. This threat is caused either by the direct contamination of agricultural commodities or by a "carry-over" of mycotoxins and their metabolites into animal tissues, milk, and eggs after feeding of contaminated hay or corn. As a consequence of their diverse chemical structures and varying physical properties, mycotoxins exhibit a wide range of biological effects. Individual mycotoxins can be genotoxic, mutagenic, carcinogenic, teratogenic, and oestrogenic. To protect consumer health and to reduce economic losses, surveillance and control of mycotoxins in food and feed has become a major objective for producers, regulatory authorities and researchers worldwide. However, the variety of chemical structures makes it impossible to use one single technique for mycotoxin analysis. Hence, a vast number of analytical methods has been developed and validated. The heterogeneity of food matrices combined with the demand for a fast, simultaneous and accurate determination of multiple mycotoxins creates enormous challenges for routine analysis. The most crucial issues will be discussed in this review. These are (1) the collection of representative samples, (2) the performance of classical and emerging analytical methods based on chromatographic or immunochemical techniques, (3) the validation of official methods for enforcement, and (4) the limitations and future prospects of the current methods.

Development of an analytical solution for thermal single-well injection-withdrawal tests in horizontally fractured reservoirs

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

Jung, Yoojin

In this study, we have developed an analytical solution for thermal single-well injection-withdrawal tests in horizontally fractured reservoirs where fluid flow through the fracture is radial. The dimensionless forms of the governing equations and the initial and boundary conditions in the radial flow system can be written in a form identical to those in the linear flow system developed by Jung and Pruess [Jung, Y., and K. Pruess (2012), A Closed-Form Analytical Solution for Thermal Single-Well Injection-Withdrawal Tests, Water Resour. Res., 48, W03504, doi:10.1029/2011WR010979], and therefore the analytical solutions developed in Jung and Pruess (2012) can be applied to computemore » the time dependence of temperature recovery at the injection/withdrawal well in a horizontally oriented fracture with radial flow.« less

Second order Møller-Plesset and coupled cluster singles and doubles methods with complex basis functions for resonances in electron-molecule scattering

DOE PAGES

White, Alec F.; Epifanovsky, Evgeny; McCurdy, C. William; ...

2017-06-21

The method of complex basis functions is applied to molecular resonances at correlated levels of theory. Møller-Plesset perturbation theory at second order and equation-of-motion electron attachment coupled-cluster singles and doubles (EOM-EA-CCSD) methods based on a non-Hermitian self-consistent-field reference are used to compute accurate Siegert energies for shape resonances in small molecules including N 2 - , CO - , CO 2 - , and CH 2 O - . Analytic continuation of complex θ-trajectories is used to compute Siegert energies, and the θ-trajectories of energy differences are found to yield more consistent results than those of total energies.more » Furthermore, the ability of such methods to accurately compute complex potential energy surfaces is investigated, and the possibility of using EOM-EA-CCSD for Feshbach resonances is explored in the context of e-helium scattering.« less

Second order Møller-Plesset and coupled cluster singles and doubles methods with complex basis functions for resonances in electron-molecule scattering

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

White, Alec F.; Epifanovsky, Evgeny; McCurdy, C. William

The method of complex basis functions is applied to molecular resonances at correlated levels of theory. Møller-Plesset perturbation theory at second order and equation-of-motion electron attachment coupled-cluster singles and doubles (EOM-EA-CCSD) methods based on a non-Hermitian self-consistent-field reference are used to compute accurate Siegert energies for shape resonances in small molecules including N 2 - , CO - , CO 2 - , and CH 2 O - . Analytic continuation of complex θ-trajectories is used to compute Siegert energies, and the θ-trajectories of energy differences are found to yield more consistent results than those of total energies.more » Furthermore, the ability of such methods to accurately compute complex potential energy surfaces is investigated, and the possibility of using EOM-EA-CCSD for Feshbach resonances is explored in the context of e-helium scattering.« less

Microstructured optical fibers for terahertz waveguiding regime by using an analytical field model

NASA Astrophysics Data System (ADS)

Sharma, Dinesh Kumar; Sharma, Anurag; Tripathi, Saurabh Mani

2017-12-01

Microstructured optical fibres (MOFs) are seen as novel optical waveguide for the potential applications in the terahertz (THz) band as they provide a flexible route towards THz waveguiding. Using the analytical field model (Sharma et al., 2014) developed for index-guiding MOFs with hexagonal lattice of circular air-holes in the photonic crystal cladding; we aim to study the propagation characteristics such as effective index, near and the far-field radiation patterns and its evolution from near-to-far-field domain, spot size, effective mode area, and the numerical aperture at the THz regime. Further, we present an analytical field expression for the next higher-order mode of the MOF for studying the modal properties at terahertz frequencies. Also, we investigate the mode cut-off conditions for identifying the single-mode operation range at THz frequencies. Emphasis is put on studying the coupling characteristics of MOF geometries for efficient mode coupling. Comparisons with available experimental and numerical simulation results, e.g., those based on the full-vector finite element method (FEM) and the finite-difference frequency-domain (FDFD) method have been included.

Shape-Dependent Optoelectronic Cell Lysis**

PubMed Central

Kremer, Clemens; Witte, Christian; Neale, Steven L; Reboud, Julien; Barrett, Michael P; Cooper, Jonathan M

2014-01-01

We show an electrical method to break open living cells amongst a population of different cell types, where cell selection is based upon their shape. We implement the technique on an optoelectronic platform, where light, focused onto a semiconductor surface from a video projector creates a reconfigurable pattern of electrodes. One can choose the area of cells to be lysed in real-time, from single cells to large areas, simply by redrawing the projected pattern. We show that the method, based on the “electrical shadow” that the cell casts, allows the detection of rare cell types in blood (including sleeping sickness parasites), and has the potential to enable single cell studies for advanced molecular diagnostics, as well as wider applications in analytical chemistry. PMID:24402800

Analysis of photon count data from single-molecule fluorescence experiments

NASA Astrophysics Data System (ADS)

Burzykowski, T.; Szubiakowski, J.; Rydén, T.

2003-03-01

We consider single-molecule fluorescence experiments with data in the form of counts of photons registered over multiple time-intervals. Based on the observation schemes, linking back to works by Dehmelt [Bull. Am. Phys. Soc. 20 (1975) 60] and Cook and Kimble [Phys. Rev. Lett. 54 (1985) 1023], we propose an analytical approach to the data based on the theory of Markov-modulated Poisson processes (MMPP). In particular, we consider maximum-likelihood estimation. The method is illustrated using a real-life dataset. Additionally, the properties of the proposed method are investigated through simulations and compared to two other approaches developed by Yip et al. [J. Phys. Chem. A 102 (1998) 7564] and Molski [Chem. Phys. Lett. 324 (2000) 301].

Purification of Single-Stranded cDNA Based on RNA Degradation Treatment and Adsorption Chromatography.

PubMed

Trujillo-Esquivel, Elías; Franco, Bernardo; Flores-Martínez, Alberto; Ponce-Noyola, Patricia; Mora-Montes, Héctor M

2016-08-02

Analysis of gene expression is a common research tool to study networks controlling gene expression, the role of genes with unknown function, and environmentally induced responses of organisms. Most of the analytical tools used to analyze gene expression rely on accurate cDNA synthesis and quantification to obtain reproducible and quantifiable results. Thus far, most commercial kits for isolation and purification of cDNA target double-stranded molecules, which do not accurately represent the abundance of transcripts. In the present report, we provide a simple and fast method to purify single-stranded cDNA, exhibiting high purity and yield. This method is based on the treatment with RNase H and RNase A after cDNA synthesis, followed by separation in silica spin-columns and ethanol precipitation. In addition, our method avoids the use of DNase I to eliminate genomic DNA from RNA preparations, which improves cDNA yield. As a case report, our method proved to be useful in the purification of single-stranded cDNA from the pathogenic fungus Sporothrix schenckii.

VERTPAK1

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

Golis, M.J.

1983-04-01

VERTPAK1 is a package of analytical solutions used in verification of numerical codes that simulate fluid flow, rock deformation, and solute transport in fractured and unfractured porous media. VERTPAK1 contains the following: BAREN, an analytical solution developed by Barenblatt, Zhelton and Kochina (1960) for describing transient flow to a well penetrating a (double porosity) confined aquifer; GIBMAC, an analytical solution developed by McNamee and Gibson (1960) for describing consolidation of a semi-infinite soil medium subject to a strip (plane strain) or cylindrical (axisymmetric) loading; GRINRH, an analytical solution developed by Gringarten (1971) for describing transient flow to a partially penetratingmore » well in a confined aquifer containing a single horizontal fracture; GRINRV, an analytical solution developed by Gringarten, Ramey, and Raghavan (1974) for describing transient flow to a fully penetrating well in a confined aquifer containing a single vertical fracture; HART, an analytical solution given by Nowacki (1962) and implemented by HART (1981) for describing the elastic behavior of an infinite solid subject to a line heat source; LESTER, an analytical solution presented by Lester, Jansen, and Burkholder (1975) for describing one-dimensional transport of radionuclide chains through an adsorbing medium; STRELT, an analytical solution presented by Streltsova-Adams (1978) for describing transient flow to a fully penetrating well in a (double porosity) confined aquifer; and TANG, an analytical solution developed by Tang, Frind, and Sudicky (1981) for describing solute transport in a porous medium containing a single fracture.« less

Detecting and Analyzing Genetic Recombination Using RDP4.

PubMed

Martin, Darren P; Murrell, Ben; Khoosal, Arjun; Muhire, Brejnev

2017-01-01

Recombination between nucleotide sequences is a major process influencing the evolution of most species on Earth. The evolutionary value of recombination has been widely debated and so too has its influence on evolutionary analysis methods that assume nucleotide sequences replicate without recombining. When nucleic acids recombine, the evolution of the daughter or recombinant molecule cannot be accurately described by a single phylogeny. This simple fact can seriously undermine the accuracy of any phylogenetics-based analytical approach which assumes that the evolutionary history of a set of recombining sequences can be adequately described by a single phylogenetic tree. There are presently a large number of available methods and associated computer programs for analyzing and characterizing recombination in various classes of nucleotide sequence datasets. Here we examine the use of some of these methods to derive and test recombination hypotheses using multiple sequence alignments.

Geovisual analytics to enhance spatial scan statistic interpretation: an analysis of U.S. cervical cancer mortality.

PubMed

Chen, Jin; Roth, Robert E; Naito, Adam T; Lengerich, Eugene J; Maceachren, Alan M

2008-11-07

Kulldorff's spatial scan statistic and its software implementation - SaTScan - are widely used for detecting and evaluating geographic clusters. However, two issues make using the method and interpreting its results non-trivial: (1) the method lacks cartographic support for understanding the clusters in geographic context and (2) results from the method are sensitive to parameter choices related to cluster scaling (abbreviated as scaling parameters), but the system provides no direct support for making these choices. We employ both established and novel geovisual analytics methods to address these issues and to enhance the interpretation of SaTScan results. We demonstrate our geovisual analytics approach in a case study analysis of cervical cancer mortality in the U.S. We address the first issue by providing an interactive visual interface to support the interpretation of SaTScan results. Our research to address the second issue prompted a broader discussion about the sensitivity of SaTScan results to parameter choices. Sensitivity has two components: (1) the method can identify clusters that, while being statistically significant, have heterogeneous contents comprised of both high-risk and low-risk locations and (2) the method can identify clusters that are unstable in location and size as the spatial scan scaling parameter is varied. To investigate cluster result stability, we conducted multiple SaTScan runs with systematically selected parameters. The results, when scanning a large spatial dataset (e.g., U.S. data aggregated by county), demonstrate that no single spatial scan scaling value is known to be optimal to identify clusters that exist at different scales; instead, multiple scans that vary the parameters are necessary. We introduce a novel method of measuring and visualizing reliability that facilitates identification of homogeneous clusters that are stable across analysis scales. Finally, we propose a logical approach to proceed through the analysis of SaTScan results. The geovisual analytics approach described in this manuscript facilitates the interpretation of spatial cluster detection methods by providing cartographic representation of SaTScan results and by providing visualization methods and tools that support selection of SaTScan parameters. Our methods distinguish between heterogeneous and homogeneous clusters and assess the stability of clusters across analytic scales. We analyzed the cervical cancer mortality data for the United States aggregated by county between 2000 and 2004. We ran SaTScan on the dataset fifty times with different parameter choices. Our geovisual analytics approach couples SaTScan with our visual analytic platform, allowing users to interactively explore and compare SaTScan results produced by different parameter choices. The Standardized Mortality Ratio and reliability scores are visualized for all the counties to identify stable, homogeneous clusters. We evaluated our analysis result by comparing it to that produced by other independent techniques including the Empirical Bayes Smoothing and Kafadar spatial smoother methods. The geovisual analytics approach introduced here is developed and implemented in our Java-based Visual Inquiry Toolkit.

Stability indicating simplified HPLC method for simultaneous analysis of resveratrol and quercetin in nanoparticles and human plasma.

PubMed

Kumar, Sandeep; Lather, Viney; Pandita, Deepti

2016-04-15

Resveratrol and quercetin are well-known polyphenolic compounds present in common foods, which have demonstrated enormous potential in the treatment of a wide variety of diseases. Owing to their exciting synergistic potential and combination delivery applications, we developed a simple and rapid RP-HPLC method based on isosbestic point detection. The separation was carried out on phenomenex Synergi 4μ Hydro-RP 80A column using methanol: acetonitrile (ACN): 0.1% phosphoric acid (60:10:30) as mobile phase. The method was able to quantify nanograms of analytes simultaneously on a single wavelength (269 nm), making it highly sensitive, rapid as well as economical. Additionally, forced degradation studies of resveratrol and quercetin were established and the method's applicability was evaluated on PLGA nanoparticles and human plasma. The analytes peaks were found to be well resolved in the presence of degradation products and excipients. The simplicity of the developed method potentializes its suitability for routine in vitro and in vivo analysis of resveratrol and quercetin. Copyright © 2015 Elsevier Ltd. All rights reserved.

An automated online turboflow cleanup LC/MS/MS method for the determination of 11 plasticizers in beverages and milk.

PubMed

Ates, Ebru; Mittendorf, Klaus; Senyuva, Hamide

2013-01-01

An automated sample preparation technique involving cleanup and analytical separation in a single operation using an online coupled TurboFlow (RP-LC system) is reported. This method eliminates time-consuming sample preparation steps that can be potential sources for cross-contamination in the analysis of plasticizers. Using TurboFlow chromatography, liquid samples were injected directly into the automated system without previous extraction or cleanup. Special cleanup columns enabled specific binding of target compounds; higher MW compounds, i.e., fats and proteins, and other matrix interferences with different chemical properties were removed to waste, prior to LC/MS/MS. Systematic stepwise method development using this new technology in the food safety area is described. Selection of optimum columns and mobile phases for loading onto the cleanup column followed by transfer onto the analytical column and MS detection are critical method parameters. The method was optimized for the assay of 10 phthalates (dimethyl, diethyl, dipropyl, butyl benzyl, diisobutyl, dicyclohexyl, dihexyl, diethylhexyl, diisononyl, and diisododecyl) and one adipate (diethylhexyl) in beverages and milk.

Review on failure prediction techniques of composite single lap joint

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

Ab Ghani, A.F., E-mail: ahmadfuad@utem.edu.my; Rivai, Ahmad, E-mail: ahmadrivai@utem.edu.my

2016-03-29

Adhesive bonding is the most appropriate joining method in construction of composite structures. The use of reliable design and prediction technique will produce better performance of bonded joints. Several papers from recent papers and journals have been reviewed and synthesized to understand the current state of the art in this area. It is done by studying the most relevant analytical solutions for composite adherends with start of reviewing the most fundamental ones involving beam/plate theory. It is then extended to review single lap joint non linearity and failure prediction and finally on the failure prediction on composite single lap joint.more » The review also encompasses the finite element modelling part as tool to predict the elastic response of composite single lap joint and failure prediction numerically.« less

Retention prediction and separation optimization under multilinear gradient elution in liquid chromatography with Microsoft Excel macros.

PubMed

Fasoula, S; Zisi, Ch; Gika, H; Pappa-Louisi, A; Nikitas, P

2015-05-22

A package of Excel VBA macros have been developed for modeling multilinear gradient retention data obtained in single or double gradient elution mode by changing organic modifier(s) content and/or eluent pH. For this purpose, ten chromatographic models were used and four methods were adopted for their application. The methods were based on (a) the analytical expression of the retention time, provided that this expression is available, (b) the retention times estimated using the Nikitas-Pappa approach, (c) the stepwise approximation, and (d) a simple numerical approximation involving the trapezoid rule for integration of the fundamental equation for gradient elution. For all these methods, Excel VBA macros have been written and implemented using two different platforms; the fitting and the optimization platform. The fitting platform calculates not only the adjustable parameters of the chromatographic models, but also the significance of these parameters and furthermore predicts the analyte elution times. The optimization platform determines the gradient conditions that lead to the optimum separation of a mixture of analytes by using the Solver evolutionary mode, provided that proper constraints are set in order to obtain the optimum gradient profile in the minimum gradient time. The performance of the two platforms was tested using experimental and artificial data. It was found that using the proposed spreadsheets, fitting, prediction, and optimization can be performed easily and effectively under all conditions. Overall, the best performance is exhibited by the analytical and Nikitas-Pappa's methods, although the former cannot be used under all circumstances. Copyright © 2015 Elsevier B.V. All rights reserved.

Simultaneous, untargeted metabolic profiling of polar and nonpolar metabolites by LC-Q-TOF mass spectrometry.

PubMed

Kirkwood, Jay S; Maier, Claudia; Stevens, Jan F

2013-05-01

At its most ambitious, untargeted metabolomics aims to characterize and quantify all of the metabolites in a given system. Metabolites are often present at a broad range of concentrations and possess diverse physical properties complicating this task. Performing multiple sample extractions, concentrating sample extracts, and using several separation and detection methods are common strategies to overcome these challenges but require a great amount of resources. This protocol describes the untargeted, metabolic profiling of polar and nonpolar metabolites with a single extraction and using a single analytical platform. © 2013 by John Wiley & Sons, Inc.

Flow tests of a single fuel element coolant channel for a compact fast reactor for space power

NASA Technical Reports Server (NTRS)

Springborn, R. H.

1971-01-01

Water flow tests were conducted on a single-fuel-element cooling channel for a nuclear concept to be used for space power. The tests established a method for measuring coolant flow rate which is applicable to water flow testing of a complete mockup of the reference reactor. The inlet plenum-to-outlet plenum pressure drop, which approximates the overall core pressure drop, was measured and correlated with flow rate. This information can be used for reactor coolant flow and heat transfer calculations. An analytical study of the flow characteristics was also conducted.

Symmetrical Josephson vortex interferometer as an advanced ballistic single-shot detector

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

Soloviev, I. I., E-mail: isol@phys.msu.ru; Lukin Scientific Research Institute of Physical Problems, 124460 Zelenograd, Moscow; Laboratory of Cryogenic Nanoelectronics, Nizhny Novgorod State Technical University n.a. R.E. Alekseev, 603950 Nizhny Novgorod

2014-11-17

We consider a ballistic detector formed in an interferometer manner which operational principle relies on Josephson vortex scattering at a measurement potential. We propose an approach to symmetrize the detector scheme and explore arising advantages in the signal-to-noise ratio and in the back-action on a measured object by means of recently presented numerical and analytical methods for modeling of a soliton scattering dynamics in the presence of thermal fluctuations. The obtained characteristics for experimentally relevant parameters reveal practical applicability of the considered schemes including possibility of coupling with standard digital rapid single flux quantum circuits.

Magnetically controlled multifrequency invisibility cloak with a single shell of ferrite material

NASA Astrophysics Data System (ADS)

Wang, Xiaohua; Liu, Youwen

2015-02-01

A magnetically controlled multifrequency invisibility cloak with a single shell of the isotropic and homogeneous ferrite material has been investigated based on the scattering cancellation method from the Mie scattering theory. The analytical and simulated results have demonstrated that such this shell can drastically reduce the total scattering cross-section of this cloaking system at multiple frequencies. These multiple cloaking frequencies of this shell can be externally controlled since the magnetic permeability of ferrites is well tuned by the applied magnetic field. This may provide a potential way to design a tunable multifrequency invisibility cloak with considerable flexibility.

Functional recognition imaging using artificial neural networks: applications to rapid cellular identification via broadband electromechanical response

NASA Astrophysics Data System (ADS)

Nikiforov, M. P.; Reukov, V. V.; Thompson, G. L.; Vertegel, A. A.; Guo, S.; Kalinin, S. V.; Jesse, S.

2009-10-01

Functional recognition imaging in scanning probe microscopy (SPM) using artificial neural network identification is demonstrated. This approach utilizes statistical analysis of complex SPM responses at a single spatial location to identify the target behavior, which is reminiscent of associative thinking in the human brain, obviating the need for analytical models. We demonstrate, as an example of recognition imaging, rapid identification of cellular organisms using the difference in electromechanical activity over a broad frequency range. Single-pixel identification of model Micrococcus lysodeikticus and Pseudomonas fluorescens bacteria is achieved, demonstrating the viability of the method.

Modal sound transmission loss of a single leaf panel: Effects of inter-modal coupling.

PubMed

Wang, Chong

2015-06-01

Sound transmission through a single leaf panel has mostly been discussed and explained by using the approaching wave concept, from which the well-known mass law can be derived. In this paper, the modal behavior in sound transmission coefficients is explored, and it is shown that the mutual modal radiation impedances in modal sound transmission coefficients may not be ignored even for a panel immersed in a light fluid. By introducing the equivalent modal impedance which incorporates the inter-modal coupling effect, an analytical expression for the modal sound transmission coefficient is derived, and the overall sound transmission coefficient is simply a modal superposition of modal sound transmission coefficients. A good correlation is obtained between analytical calculation and boundary element method. In addition, it is found that inter-modal coupling has noticeable effects in modal sound transmission coefficients in the subsonic region but may be ignored as modes become supersonic. It is also shown that the well-known mass law performance is attributed to all the supersonic modes.

Determination of nanoparticle size distribution together with density or molecular weight by 2D analytical ultracentrifugation

PubMed Central

Carney, Randy P.; Kim, Jin Young; Qian, Huifeng; Jin, Rongchao; Mehenni, Hakim; Stellacci, Francesco; Bakr, Osman M.

2011-01-01

Nanoparticles are finding many research and industrial applications, yet their characterization remains a challenge. Their cores are often polydisperse and coated by a stabilizing shell that varies in size and composition. No single technique can characterize both the size distribution and the nature of the shell. Advances in analytical ultracentrifugation allow for the extraction of the sedimentation (s) and diffusion coefficients (D). Here we report an approach to transform the s and D distributions of nanoparticles in solution into precise molecular weight (M), density (ρP) and particle diameter (dp) distributions. M for mixtures of discrete nanocrystals is found within 4% of the known quantities. The accuracy and the density information we achieve on nanoparticles are unparalleled. A single experimental run is sufficient for full nanoparticle characterization, without the need for standards or other auxiliary measurements. We believe that our method is of general applicability and we discuss its limitations. PMID:21654635

The analysis of non-linear dynamic behavior (including snap-through) of postbuckled plates by simple analytical solution

NASA Technical Reports Server (NTRS)

Ng, C. F.

1988-01-01

Static postbuckling and nonlinear dynamic analysis of plates are usually accomplished by multimode analyses, although the methods are complicated and do not give straightforward understanding of the nonlinear behavior. Assuming single-mode transverse displacement, a simple formula is derived for the transverse load displacement relationship of a plate under in-plane compression. The formula is used to derive a simple analytical expression for the static postbuckling displacement and nonlinear dynamic responses of postbuckled plates under sinusoidal or random excitation. Regions with softening and hardening spring behavior are identified. Also, the highly nonlinear motion of snap-through and its effects on the overall dynamic response can be easily interpreted using the single-mode formula. Theoretical results are compared with experimental results obtained using a buckled aluminum panel, using discrete frequency and broadband point excitation. Some important effects of the snap-through motion on the dynamic response of the postbuckled plates are found.

Local Modelling of Groundwater Flow Using Analytic Element Method Three-dimensional Transient Unconfined Groundwater Flow With Partially Penetrating Wells and Ellipsoidal Inhomogeneites

NASA Astrophysics Data System (ADS)

Jankovic, I.; Barnes, R. J.; Soule, R.

2001-12-01

The analytic element method is used to model local three-dimensional flow in the vicinity of partially penetrating wells. The flow domain is bounded by an impermeable horizontal base, a phreatic surface with recharge and a cylindrical lateral boundary. The analytic element solution for this problem contains (1) a fictitious source technique to satisfy the head and the discharge conditions along the phreatic surface, (2) a fictitious source technique to satisfy specified head conditions along the cylindrical boundary, (3) a method of imaging to satisfy the no-flow condition across the impermeable base, (4) the classical analytic solution for a well and (5) spheroidal harmonics to account for the influence of the inhomogeneities in hydraulic conductivity. Temporal variations of the flow system due to time-dependent recharge and pumping are represented by combining the analytic element method with a finite difference method: analytic element method is used to represent spatial changes in head and discharge, while the finite difference method represents temporal variations. The solution provides a very detailed description of local groundwater flow with an arbitrary number of wells of any orientation and an arbitrary number of ellipsoidal inhomogeneities of any size and conductivity. These inhomogeneities may be used to model local hydrogeologic features (such as gravel packs and clay lenses) that significantly influence the flow in the vicinity of partially penetrating wells. Several options for specifying head values along the lateral domain boundary are available. These options allow for inclusion of the model into steady and transient regional groundwater models. The head values along the lateral domain boundary may be specified directly (as time series). The head values along the lateral boundary may also be assigned by specifying the water-table gradient and a head value at a single point (as time series). A case study is included to demonstrate the application of the model in local modeling of the groundwater flow. Transient three-dimensional capture zones are delineated for a site on Prairie Island, MN. Prairie Island is located on the Mississippi River 40 miles south of the Twin Cities metropolitan area. The case study focuses on a well that has been known to contain viral DNA. The objective of the study was to assess the potential for pathogen migration toward the well.

New insight into the comparative power of quality-control rules that use control observations within a single analytical run.

PubMed

Parvin, C A

1993-03-01

The error detection characteristics of quality-control (QC) rules that use control observations within a single analytical run are investigated. Unlike the evaluation of QC rules that span multiple analytical runs, most of the fundamental results regarding the performance of QC rules applied within a single analytical run can be obtained from statistical theory, without the need for simulation studies. The case of two control observations per run is investigated for ease of graphical display, but the conclusions can be extended to more than two control observations per run. Results are summarized in a graphical format that offers many interesting insights into the relations among the various QC rules. The graphs provide heuristic support to the theoretical conclusions that no QC rule is best under all error conditions, but the multirule that combines the mean rule and a within-run standard deviation rule offers an attractive compromise.

Parameterizing microphysical effects on variances and covariances of moisture and heat content using a multivariate probability density function: a study with CLUBB (tag MVCS)

DOE PAGES

Griffin, Brian M.; Larson, Vincent E.

2016-11-25

Microphysical processes, such as the formation, growth, and evaporation of precipitation, interact with variability and covariances (e.g., fluxes) in moisture and heat content. For instance, evaporation of rain may produce cold pools, which in turn may trigger fresh convection and precipitation. These effects are usually omitted or else crudely parameterized at subgrid scales in weather and climate models.A more formal approach is pursued here, based on predictive, horizontally averaged equations for the variances, covariances, and fluxes of moisture and heat content. These higher-order moment equations contain microphysical source terms. The microphysics terms can be integrated analytically, given a suitably simplemore » warm-rain microphysics scheme and an approximate assumption about the multivariate distribution of cloud-related and precipitation-related variables. Performing the integrations provides exact expressions within an idealized context.A large-eddy simulation (LES) of a shallow precipitating cumulus case is performed here, and it indicates that the microphysical effects on (co)variances and fluxes can be large. In some budgets and altitude ranges, they are dominant terms. The analytic expressions for the integrals are implemented in a single-column, higher-order closure model. Interactive single-column simulations agree qualitatively with the LES. The analytic integrations form a parameterization of microphysical effects in their own right, and they also serve as benchmark solutions that can be compared to non-analytic integration methods.« less

Coping with matrix effects in headspace solid phase microextraction gas chromatography using multivariate calibration strategies.

PubMed

Ferreira, Vicente; Herrero, Paula; Zapata, Julián; Escudero, Ana

2015-08-14

SPME is extremely sensitive to experimental parameters affecting liquid-gas and gas-solid distribution coefficients. Our aims were to measure the weights of these factors and to design a multivariate strategy based on the addition of a pool of internal standards, to minimize matrix effects. Synthetic but real-like wines containing selected analytes and variable amounts of ethanol, non-volatile constituents and major volatile compounds were prepared following a factorial design. The ANOVA study revealed that even using a strong matrix dilution, matrix effects are important and additive with non-significant interaction effects and that it is the presence of major volatile constituents the most dominant factor. A single internal standard provided a robust calibration for 15 out of 47 analytes. Then, two different multivariate calibration strategies based on Partial Least Square Regression were run in order to build calibration functions based on 13 different internal standards able to cope with matrix effects. The first one is based in the calculation of Multivariate Internal Standards (MIS), linear combinations of the normalized signals of the 13 internal standards, which provide the expected area of a given unit of analyte present in each sample. The second strategy is a direct calibration relating concentration to the 13 relative areas measured in each sample for each analyte. Overall, 47 different compounds can be reliably quantified in a single fully automated method with overall uncertainties better than 15%. Copyright © 2015 Elsevier B.V. All rights reserved.

Sensitivity enhancement by multiple-contact cross-polarization under magic-angle spinning.

PubMed

Raya, J; Hirschinger, J

2017-08-01

Multiple-contact cross-polarization (MC-CP) is applied to powder samples of ferrocene and l-alanine under magic-angle spinning (MAS) conditions. The method is described analytically through the density matrix formalism. The combination of a two-step memory function approach and the Anderson-Weiss approximation is found to be particularly useful to derive approximate analytical solutions for single-contact Hartmann-Hahn CP (HHCP) and MC-CP dynamics under MAS. We show that the MC-CP sequence requiring no pulse-shape optimization yields higher polarizations at short contact times than optimized adiabatic passage through the HH condition CP (APHH-CP) when the MAS frequency is comparable to the heteronuclear dipolar coupling, i.e., when APHH-CP through a single sideband matching condition is impossible or difficult to perform. It is also shown that the MC-CP sideband HH conditions are generally much broader than for single-contact HHCP and that efficient polarization transfer at the centerband HH condition can be reintroduced by rotor-asynchronous multiple equilibrations-re-equilibrations with the proton spin bath. Boundary conditions for the successful use of the MC-CP experiment when relying on spin-lattice relaxation for repolarization are also examined. Copyright © 2017 Elsevier Inc. All rights reserved.

Sensitivity enhancement by multiple-contact cross-polarization under magic-angle spinning

NASA Astrophysics Data System (ADS)

Raya, J.; Hirschinger, J.

2017-08-01

Multiple-contact cross-polarization (MC-CP) is applied to powder samples of ferrocene and L-alanine under magic-angle spinning (MAS) conditions. The method is described analytically through the density matrix formalism. The combination of a two-step memory function approach and the Anderson-Weiss approximation is found to be particularly useful to derive approximate analytical solutions for single-contact Hartmann-Hahn CP (HHCP) and MC-CP dynamics under MAS. We show that the MC-CP sequence requiring no pulse-shape optimization yields higher polarizations at short contact times than optimized adiabatic passage through the HH condition CP (APHH-CP) when the MAS frequency is comparable to the heteronuclear dipolar coupling, i.e., when APHH-CP through a single sideband matching condition is impossible or difficult to perform. It is also shown that the MC-CP sideband HH conditions are generally much broader than for single-contact HHCP and that efficient polarization transfer at the centerband HH condition can be reintroduced by rotor-asynchronous multiple equilibrations-re-equilibrations with the proton spin bath. Boundary conditions for the successful use of the MC-CP experiment when relying on spin-lattice relaxation for repolarization are also examined.

Who do we think we are? Analysing the content and form of identity work in the English National Health Service.

PubMed

McDermott, Imelda; Checkland, Kath; Harrison, Stephen; Snow, Stephanie; Coleman, Anna

2013-01-01

The language used by National Health Service (NHS) "commissioning" managers when discussing their roles and responsibilities can be seen as a manifestation of "identity work", defined as a process of identifying. This paper aims to offer a novel approach to analysing "identity work" by triangulation of multiple analytical methods, combining analysis of the content of text with analysis of its form. Fairclough's discourse analytic methodology is used as a framework. Following Fairclough, the authors use analytical methods associated with Halliday's systemic functional linguistics. While analysis of the content of interviews provides some information about NHS Commissioners' perceptions of their roles and responsibilities, analysis of the form of discourse that they use provides a more detailed and nuanced view. Overall, the authors found that commissioning managers have a higher level of certainty about what commissioning is not rather than what commissioning is; GP managers have a high level of certainty of their identity as a GP rather than as a manager; and both GP managers and non-GP managers oscillate between multiple identities depending on the different situations they are in. This paper offers a novel approach to triangulation, based not on the usual comparison of multiple data sources, but rather based on the application of multiple analytical methods to a single source of data. This paper also shows the latent uncertainty about the nature of commissioning enterprise in the English NHS.

Evaluation of calcium alginate beads for Ce, La and Nd preconcentration from groundwater prior to ICP OES analysis.

PubMed

Arantes de Carvalho, Gabriel G; Kondaveeti, Stalin; Petri, Denise F S; Fioroto, Alexandre M; Albuquerque, Luiza G R; Oliveira, Pedro V

2016-12-01

Analytical methods for the determination of rare earth elements (REE) in natural waters by plasma spectrochemical techniques often require sample preparation procedures for analytes preconcentration as well as for removing matrix constituents, that may interfere on the analytical measurements. In the present work, calcium alginate (CA) beads were used for the first time aiming at Ce, La and Nd preconcentration from groundwater samples for further determination by inductively coupled plasma optical emission spectrometry (ICP OES). Test samples were analyzed in batch mode by transferring a 40mL test portion (pH=5±0.2) into a 50mL polyethylene flask containing 125mg CA beads. After 15min contact, the analytes were quantitatively extracted from the loaded CA beads with 2.0mL of 1.0molL -1 HCl solution for further determination by ICP OES, using Ce (II) 456.236, La (II) 379.478 and Nd (II) 430.358nm emission lines. The proposed approach is a reliable alternative for REE single-stage preconcentration from aqueous samples, as it provided accurate results based on the addition and recovery analysis of groundwater. The results obtained by the proposed method were also compared with those from reference method based on inductively coupled plasma mass spectrometry (ICP-MS) and no significant differences were observed after applying the Student's t-test at 95% confidence level. Copyright © 2016 Elsevier B.V. All rights reserved.

Strategies for dealing with missing data in clinical trials: from design to analysis.

PubMed

Dziura, James D; Post, Lori A; Zhao, Qing; Fu, Zhixuan; Peduzzi, Peter

2013-09-01

Randomized clinical trials are the gold standard for evaluating interventions as randomized assignment equalizes known and unknown characteristics between intervention groups. However, when participants miss visits, the ability to conduct an intent-to-treat analysis and draw conclusions about a causal link is compromised. As guidance to those performing clinical trials, this review is a non-technical overview of the consequences of missing data and a prescription for its treatment beyond the typical analytic approaches to the entire research process. Examples of bias from incorrect analysis with missing data and discussion of the advantages/disadvantages of analytic methods are given. As no single analysis is definitive when missing data occurs, strategies for its prevention throughout the course of a trial are presented. We aim to convey an appreciation for how missing data influences results and an understanding of the need for careful consideration of missing data during the design, planning, conduct, and analytic stages.

Nanopore tweezers: voltage-controlled trapping and releasing of analytes.

PubMed

Chinappi, Mauro; Luchian, Tudor; Cecconi, Fabio

2015-09-01

Several devices for single-molecule detection and analysis employ biological and artificial nanopores as core elements. The performance of such devises strongly depends on the amount of time the analytes spend into the pore. This residence time needs to be long enough to allow the recording of a high signal-to-noise ratio analyte-induced blockade. We propose a simple approach, dubbed nanopore tweezing, for enhancing the trapping time of molecules inside the pore via a proper tuning of the applied voltage. This method requires the creation of a strong dipole that can be generated by adding a positive and a negative tail at the two ends of the molecules to be analyzed. Capture rate is shown to increase with the applied voltage while escape rate decreases. In this paper we rationalize the essential ingredients needed to control the residence time and provide a proof of principle based on atomistic simulations.

Coordinates of features on the Galilean satellites

NASA Technical Reports Server (NTRS)

Davies, M. E.; Katayama, F. Y.

1980-01-01

The coordinate systems of each of the Galilean satellites are defined and coordinates of features seen in the Voyager pictures of these satellites are presented. The control nets of the satellites were computed by means of single block analytical triangulations. The normal equations were solved by the conjugate iterative method which is convenient and which converges rapidly as the initial estimates of the parameters are very good.

Development of flexural vibration inspection techniques to rapidly assess the structural health of timber bridge systems

Treesearch

Xiping Wang; James P. Wacker; Robert J. Ross; Brian K. Brashaw; Robert Vatalaro

2005-01-01

This paper describes an effort to develop a global dynamic testing technique for evaluating the overall stiffness of timber bridge superstructures. A forced vibration method was used to measure the natural frequency of single-span timber bridges in the laboratory and field. An analytical model based on simple beam theory was proposed to represent the relationship...

Dark soliton dynamics and interactions in continuous-wave-induced lattices.

PubMed

Tsopelas, Ilias; Kominis, Yannis; Hizanidis, Kyriakos

2007-10-01

The dynamics of dark spatial soliton beams and their interaction under the presence of a continuous wave (CW), which dynamically induces a photonic lattice, are investigated. It is shown that appropriate selection of the characteristic parameters of the CW result in controllable steering of a single soliton as well as controllable interaction between two solitons. Depending on the CW parameters, the soliton angle of propagation can be changed drastically, while two-soliton interaction can be either enhanced or reduced, suggesting a reconfigurable soliton control mechanism. Our analytical approach, based on the variational perturbation method, provides a dynamical system for the dark soliton evolution parameters. Analytical results are shown in good agreement with direct numerical simulations.

Optimal control for Malaria disease through vaccination

NASA Astrophysics Data System (ADS)

Munzir, Said; Nasir, Muhammad; Ramli, Marwan

2018-01-01

Malaria is a disease caused by an amoeba (single-celled animal) type of plasmodium where anopheles mosquito serves as the carrier. This study examines the optimal control problem of malaria disease spread based on Aron and May (1982) SIR type models and seeks the optimal solution by minimizing the prevention of the spreading of malaria by vaccine. The aim is to investigate optimal control strategies on preventing the spread of malaria by vaccination. The problem in this research is solved using analytical approach. The analytical method uses the Pontryagin Minimum Principle with the symbolic help of MATLAB software to obtain optimal control result and to analyse the spread of malaria with vaccination control.

Micro-ring sensor used in the diagnosis of gastric cancer

NASA Astrophysics Data System (ADS)

Shi, Sichao; Cheng, Qing; Lin, Rong; Su, Da; Huang, Ying

2016-01-01

To find a detecting method that can be applied to the clinical screening and diagnosis, the cascaded micro-ring sensor with Vernier effect was used to distinguish gastric cancerous and normal cells. The simulation by FDTD of the cascaded microring sensor with different refractive indexes of the analyte (normal cells and gastric cancer cells) will be presented. In the simulation, with the refractive index's change Δn=0.02 for the two different analyte, the shift of sensor's resonant wavelength is 6.71nm. And the cascaded micro-ring sensor's sensitivity S is 335.5nm/RIU, and it is much larger compared to 19nm/RIU for a single ring sensor.

Derivation of general analytic gradient expressions for density-fitted post-Hartree-Fock methods: An efficient implementation for the density-fitted second-order Møller–Plesset perturbation theory

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

Bozkaya, Uğur, E-mail: ugur.bozkaya@atauni.edu.tr

General analytic gradient expressions (with the frozen-core approximation) are presented for density-fitted post-HF methods. An efficient implementation of frozen-core analytic gradients for the second-order Møller–Plesset perturbation theory (MP2) with the density-fitting (DF) approximation (applying to both reference and correlation energies), which is denoted as DF-MP2, is reported. The DF-MP2 method is applied to a set of alkanes, conjugated dienes, and noncovalent interaction complexes to compare the computational cost of single point analytic gradients with MP2 with the resolution of the identity approach (RI-MP2) [F. Weigend and M. Häser, Theor. Chem. Acc. 97, 331 (1997); R. A. Distasio, R. P. Steele,more » Y. M. Rhee, Y. Shao, and M. Head-Gordon, J. Comput. Chem. 28, 839 (2007)]. In the RI-MP2 method, the DF approach is used only for the correlation energy. Our results demonstrate that the DF-MP2 method substantially accelerate the RI-MP2 method for analytic gradient computations due to the reduced input/output (I/O) time. Because in the DF-MP2 method the DF approach is used for both reference and correlation energies, the storage of 4-index electron repulsion integrals (ERIs) are avoided, 3-index ERI tensors are employed instead. Further, as in case of integrals, our gradient equation is completely avoid construction or storage of the 4-index two-particle density matrix (TPDM), instead we use 2- and 3-index TPDMs. Hence, the I/O bottleneck of a gradient computation is significantly overcome. Therefore, the cost of the generalized-Fock matrix (GFM), TPDM, solution of Z-vector equations, the back transformation of TPDM, and integral derivatives are substantially reduced when the DF approach is used for the entire energy expression. Further application results show that the DF approach introduce negligible errors for closed-shell reaction energies and equilibrium bond lengths.« less

Integration of gas chromatography mass spectrometry methods for differentiating ricin preparation methods.

PubMed

Wunschel, David S; Melville, Angela M; Ehrhardt, Christopher J; Colburn, Heather A; Victry, Kristin D; Antolick, Kathryn C; Wahl, Jon H; Wahl, Karen L

2012-05-07

The investigation of crimes involving chemical or biological agents is infrequent, but presents unique analytical challenges. The protein toxin ricin is encountered more frequently than other agents and is found in the seeds of Ricinus communis, commonly known as the castor plant. Typically, the toxin is extracted from castor seeds utilizing a variety of different recipes that result in varying purity of the toxin. Moreover, these various purification steps can also leave or differentially remove a variety of exogenous and endogenous residual components with the toxin that may indicate the type and number of purification steps involved. We have applied three gas chromatography-mass spectrometry (GC-MS) based analytical methods to measure the variation in seed carbohydrates and castor oil ricinoleic acid, as well as the presence of solvents used for purification. These methods were applied to the same samples prepared using four previously identified toxin preparation methods, starting from four varieties of castor seeds. The individual data sets for seed carbohydrate profiles, ricinoleic acid, or acetone amount each provided information capable of differentiating different types of toxin preparations across seed types. However, the integration of the data sets using multivariate factor analysis provided a clear distinction of all samples based on the preparation method, independent of the seed source. In particular, the abundance of mannose, arabinose, fucose, ricinoleic acid, and acetone were shown to be important differentiating factors. These complementary tools provide a more confident determination of the method of toxin preparation than would be possible using a single analytical method.

Analysis of haloacetic acids, bromate, and dalapon in natural waters by ion chromatography-tandem mass spectrometry.

PubMed

Wu, Shimin; Anumol, Tarun; Gandhi, Jay; Snyder, Shane A

2017-03-03

The addition of oxidants for disinfecting water can lead to the formation of potentially carcinogenic compounds referred to as disinfection byproducts (DBPs). Haloacetic acids (HAAs) are one of the most widely detected DBPs in US water utilities and some of them are regulated by the US Environmental Protection Agency (USEPA). The present study developed a method to analyze all the compounds in the USEPA method 557 (nine HAAs, bromate and dalapon) plus four potentially more toxic iodinated HAAs in water by coupling ion chromatography with tandem mass spectrometry (IC-MS/MS). This aqueous direct injection method has significant advantages over traditional GC methods, which require a derivatization and sample extraction that are laborious, time-consuming, and can negatively impact reproducibility. The method developed in this study requires half the time of the current USEPA method 557 on IC-MS/MS while including more compounds and achieving sub-μg/L level method detection limits (MDLs) for all 15 target analytes. The single laboratory lowest concentration minimum reporting level (LCMRL) has also been determined in reagent water, which ranged from 0.011 to 0.62μg/L for the analytes. The mean recoveries of the analytes during matrix spike recovery tests were 77-125% in finished drinking water and 81-112% in surface water. This method was then applied to untreated, chlorinated, and chloraminated groundwater and surface water samples. Bromate and 9 HAAs were detected at different levels in some of these samples. Copyright © 2017 Elsevier B.V. All rights reserved.

General Methods for Analysis of Sequential “n-step” Kinetic Mechanisms: Application to Single Turnover Kinetics of Helicase-Catalyzed DNA Unwinding

PubMed Central

Lucius, Aaron L.; Maluf, Nasib K.; Fischer, Christopher J.; Lohman, Timothy M.

2003-01-01

Helicase-catalyzed DNA unwinding is often studied using “all or none” assays that detect only the final product of fully unwound DNA. Even using these assays, quantitative analysis of DNA unwinding time courses for DNA duplexes of different lengths, L, using “n-step” sequential mechanisms, can reveal information about the number of intermediates in the unwinding reaction and the “kinetic step size”, m, defined as the average number of basepairs unwound between two successive rate limiting steps in the unwinding cycle. Simultaneous nonlinear least-squares analysis using “n-step” sequential mechanisms has previously been limited by an inability to float the number of “unwinding steps”, n, and m, in the fitting algorithm. Here we discuss the behavior of single turnover DNA unwinding time courses and describe novel methods for nonlinear least-squares analysis that overcome these problems. Analytic expressions for the time courses, fss(t), when obtainable, can be written using gamma and incomplete gamma functions. When analytic expressions are not obtainable, the numerical solution of the inverse Laplace transform can be used to obtain fss(t). Both methods allow n and m to be continuous fitting parameters. These approaches are generally applicable to enzymes that translocate along a lattice or require repetition of a series of steps before product formation. PMID:14507688

General methods for analysis of sequential "n-step" kinetic mechanisms: application to single turnover kinetics of helicase-catalyzed DNA unwinding.

PubMed

Lucius, Aaron L; Maluf, Nasib K; Fischer, Christopher J; Lohman, Timothy M

2003-10-01

Helicase-catalyzed DNA unwinding is often studied using "all or none" assays that detect only the final product of fully unwound DNA. Even using these assays, quantitative analysis of DNA unwinding time courses for DNA duplexes of different lengths, L, using "n-step" sequential mechanisms, can reveal information about the number of intermediates in the unwinding reaction and the "kinetic step size", m, defined as the average number of basepairs unwound between two successive rate limiting steps in the unwinding cycle. Simultaneous nonlinear least-squares analysis using "n-step" sequential mechanisms has previously been limited by an inability to float the number of "unwinding steps", n, and m, in the fitting algorithm. Here we discuss the behavior of single turnover DNA unwinding time courses and describe novel methods for nonlinear least-squares analysis that overcome these problems. Analytic expressions for the time courses, f(ss)(t), when obtainable, can be written using gamma and incomplete gamma functions. When analytic expressions are not obtainable, the numerical solution of the inverse Laplace transform can be used to obtain f(ss)(t). Both methods allow n and m to be continuous fitting parameters. These approaches are generally applicable to enzymes that translocate along a lattice or require repetition of a series of steps before product formation.

Static and dynamic stability of pneumatic vibration isolators and systems of isolators

NASA Astrophysics Data System (ADS)

Ryaboy, Vyacheslav M.

2014-01-01

Pneumatic vibration isolation is the most widespread effective method for creating vibration-free environments that are vital for precise experiments and manufacturing operations in optoelectronics, life sciences, microelectronics, nanotechnology and other areas. The modeling and design principles of a dual-chamber pneumatic vibration isolator, basically established a few decades ago, continue to attract attention of researchers. On the other hand, behavior of systems of such isolators was never explained in the literature in sufficient detail. This paper covers a range of questions essential for understanding the mechanics of pneumatic isolation systems from both design and application perspectives. The theory and a model of a single standalone isolator are presented in concise form necessary for subsequent analysis. Then the dynamics of a system of isolators supporting a payload is considered with main attention directed to two aspects of their behavior: first, the static stability of payloads with high positions of the center of gravity; second, dynamic stability of the feedback system formed by mechanical leveling valves. The direct method of calculating the maximum stable position of the center of gravity is presented and illustrated by three-dimensional stability domains; analytic formulas are given that delineate these domains. A numerical method for feedback stability analysis of self-leveling valve systems is given, and the results are compared with the analytical estimates for a single isolator. The relation between the static and dynamic phenomena is discussed.

A novel quantitation approach for maximizing detectable targets for offensive/volatile odorants with diverse functional groups by thermal desorption-gas chromatography-mass spectrometry

NASA Astrophysics Data System (ADS)

Kim, Yong-Hyun; Kim, Ki-Hyun

2016-07-01

A multitude of analytical systems are needed to analyze diverse odorants with various functionalities. In this study, an experimental method was developed to assess the maximum covering range of odorants using a single experimental setup consisting of a thermal desorber-gas chromatography-mass spectrometry system. To this end, a total of 20 offensive odorants (aldehyde, ketone, ester, alcohol, aromatic, sulfide, amine, and carboxyl) were selected and tested by a single system. The analytical results of standards and environmental samples were evaluated in a number of respects. In the analysis of the standards, all targets were quantified via Carbopack (C + B + X) tube sampling while operating the thermal desorber at -25 °C. The method detection limits of 18 targets (exception of 2 out of the 20 targets: acetaldehyde and methanethiol) were excellent (mean 0.04 ± 0.03 ppb) in terms of their odor threshold values (74.7 ± 140 ~ 624 ± 1,729 ppb). The analysis of organic fertilizer plant samples at a pig farm (slurry treatment facility, compost facility, and ambient air) confirmed the presence of 18 odorants from 0.03 ppb (dimethyldisulfide, ambient sample) to 522 ppb (methyl ethyl ketone, slurry treatment facility). As such, our method allowed simultaneous quantitation of most key odorants with sufficient reliability and sensitivity.

Subtracting infrared renormalons from Wilson coefficients: Uniqueness and power dependences on ΛQCD

NASA Astrophysics Data System (ADS)

Mishima, Go; Sumino, Yukinari; Takaura, Hiromasa

2017-06-01

In the context of operator product expansion (OPE) and using the large-β0 approximation, we propose a method to define Wilson coefficients free from uncertainties due to IR renormalons. We first introduce a general observable X (Q2) with an explicit IR cutoff, and then we extract a genuine UV contribution XUV as a cutoff-independent part. XUV includes power corrections ˜(ΛQCD2/Q2)n which are independent of renormalons. Using the integration-by-regions method, we observe that XUV coincides with the leading Wilson coefficient in OPE and also clarify that the power corrections originate from UV region. We examine scheme dependence of XUV and single out a specific scheme favorable in terms of analytical properties. Our method would be optimal with respect to systematicity, analyticity and stability. We test our formulation with the examples of the Adler function, QCD force between Q Q ¯, and R -ratio in e+e- collision.

Isotope dilution liquid chromatography - mass spectrometry methods for fat- and water-soluble vitamins in nutritional formulations.

PubMed

Phinney, Karen W; Rimmer, Catherine A; Thomas, Jeanice Brown; Sander, Lane C; Sharpless, Katherine E; Wise, Stephen A

2011-01-01

Vitamins are essential to human health, and dietary supplements containing vitamins are widely used by individuals hoping to ensure they have adequate intake of these important nutrients. Measurement of vitamins in nutritional formulations is necessary to monitor regulatory compliance and in studies examining the nutrient intake of specific populations. Liquid chromatographic methods, primarily with UV absorbance detection, are well established for both fat- and water-soluble measurements, but they do have limitations for certain analytes and may suffer from a lack of specificity in complex matrices. Liquid chromatography-mass spectrometry (LC-MS) provides both sensitivity and specificity for the determination of vitamins in these matrices, and simultaneous analysis of multiple vitamins in a single analysis is often possible. In this work, LC-MS methods were developed for both fat- and water-soluble vitamins and applied to the measurement of these analytes in two NIST Standard Reference Materials. When possible, stable isotope labeled internal standards were employed for quantification.

Development Of Antibody-Based Fiber-Optic Sensors

NASA Astrophysics Data System (ADS)

Tromberg, Bruce J.; Sepaniak, Michael J.; Vo-Dinh, Tuan

1988-06-01

The speed and specificity characteristic of immunochemical complex formation has encouraged the development of numerous antibody-based analytical techniques. The scope and versatility of these established methods can be enhanced by combining the principles of conventional immunoassay with laser-based fiber-optic fluorimetry. This merger of spectroscopy and immunochemistry provides the framework for the construction of highly sensitive and selective fiber-optic devices (fluoroimmuno-sensors) capable of in-situ detection of drugs, toxins, and naturally occurring biochemicals. Fluoroimmuno-sensors (FIS) employ an immobilized reagent phase at the sampling terminus of a single quartz optical fiber. Laser excitation of antibody-bound analyte produces a fluorescence signal which is either directly proportional (as in the case of natural fluorophor and "antibody sandwich" assays) or inversely proportional (as in the case of competitive-binding assays) to analyte concentration. Factors which influence analysis time, precision, linearity, and detection limits include the nature (solid or liquid) and amount of the reagent phase, the method of analyte delivery (passive diffusion, convection, etc.), and whether equilibrium or non-equilibrium assays are performed. Data will be presented for optical fibers whose sensing termini utilize: (1) covalently-bound solid antibody reagent phases, and (2) membrane-entrapped liquid antibody reagents. Assays for large-molecular weight proteins (antigens) and small-molecular weight, carcinogenic, polynuclear aromatics (haptens) will be considered. In this manner, the influence of a system's chemical characteristics and measurement requirements on sensor design, and the consequence of various sensor designs on analytical performance will be illustrated.

Simultaneous determination of seven coumarins by UPLC-MS/MS: Application to a comparative pharmacokinetic study in normal and arthritic rats after oral administration of Huo Luo Xiao Ling Dan or single-herb extract.

PubMed

Wu, Yun; Wang, Fenrong; Ai, Yu; Ma, Wen; Bian, Qiaoxia; Lee, David Y-W; Dai, Ronghua

2015-06-01

A simple, sensitive and reliable ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method has been developed and validated for simultaneous quantitation of seven coumarins, the bio-active ingredients of Huo Luo Xiao Ling Dan (HLXLD), in rat plasma. The liquid-liquid extraction method with ether-dichloromethane (2:1, v/v) was used to prepare the plasma samples. Analytes and internal standard (IS) of bifendate were separated on a Shim-pack XR-ODS column (75mm×3.0mm, 2.2μm particles) using gradient elution with the mobile phase consisting of methanol and 0.05% formic acid in water at a flow rate of 0.4mL/min. Detection was performed on a triple quadrupole (TQ) tandem mass spectrometry equipped with an electrospray ionization source in the positive ionization and multiple reaction monitoring (MRM) mode. The lower limits of quantitation (LLOQ) were 0.03-0.25ng/mL for all the analytes. Intra- and inter-day precision and accuracy of the seven analytes were well within acceptance criteria (15%). The matrix effect and the mean extraction recoveries of the analytes and IS from rat plasma were all within satisfaction. The validated method has been successfully applied to compare pharmacokinetic profiles of the seven active ingredients in rat plasma between normal and arthritic rats after oral administration of HLXLD, Angelica pubescens extract and Notopterygium incisum extract, respectively. Results showed that there were remarkable differences in pharmacokinetic properties of the analytes among the different groups. Copyright © 2015. Published by Elsevier B.V.

The Application of a Novel Pressurized Liquid Extraction Method to Quantify Organic Tracers Combined with Historic and Novel Organic Contaminants for the Discover-AQ Houston Field Experiment

NASA Astrophysics Data System (ADS)

Clark, A. E.; Yoon, S.; Sheesley, R. J.; Usenko, S.

2014-12-01

DISCOVER-AQ is a NASA mission seeking to better understand air quality in cities across the United States. In September 2013, flight, satellite and ground-based data was collected in Houston, TX and the surrounding metropolitan area. Over 300 particulate matter filter samples were collected as part of the ground-based sampling efforts, at four sites across Houston. Samples include total suspended particle matter (TSP) and fine particulate matter (less than 2.5 μm in aerodynamic diameter; PM2.5). For this project, an analytical method has been developed for the pressurized liquid extraction (PLE) of a wide variety of organic tracers and contaminants from quartz fiber filters (QFFs). Over 100 compounds were selected including polycyclic aromatic hydrocarbons (PAHs), hopanes, levoglucosan, organochlorine pesticides, polychlorinated biphenyls (PCBs), polybrominated diphenyl ethers (PBDEs), and organophosphate flame retardants (OPFRs). Currently, there is no analytical method validated for the reproducible extraction of all seven compound classes in a single automated technique. Prior to extraction, QFF samples were spiked with known amounts of target analyte standards and isotopically-labeled surrogate standards. The QFF were then extracted with methylene chloride:acetone at high temperatures (100˚C) and pressures (1500 psi) using a Thermo Dionex Accelerated Solvent Extractor system (ASE 350). Extracts were concentrated, spiked with known amounts of isotopically-labeled internal standards, and analyzed by gas chromatography coupled with mass spectrometry utilizing electron ionization and electron capture negative ionization. Target analytes were surrogate recovery-corrected to account for analyte loss during sample preparation. Ambient concentrations of over 100 organic tracers and contaminants will be presented for four sites in Houston during DISCOVER-AQ.

Surface-enhanced Raman spectroscopy for the detection of pathogenic DNA and protein in foods

NASA Astrophysics Data System (ADS)

Chowdhury, Mustafa H.; Atkinson, Brad; Good, Theresa; Cote, Gerard L.

2003-07-01

Traditional Raman spectroscopy while extremely sensitive to structure and conformation, is an ineffective tool for the detection of bioanalytes at the sub milimolar level. Surface Enhanced Raman Spectroscopy (SERS) is a technique developed more recently that has been used with applaudable success to enhance the Raman cross-section of a molecule by factors of 106 to 1014. This technique can be exploited in a nanoscale biosensor for the detection of pathogenic proteins and DNA in foods by using a biorecognition molecule to bring a target analyte in close proximity to the mental surface. This is expected to produce a SERS signal of the target analyte, thus making it possible to easily discriminate between the target analyte and possible confounders. In order for the sensor to be effective, the Raman spectra of the target analyte would have to be distinct from that of the biorecognition molecule, as both would be in close proximity to the metal surface and thus be subjected to the SERS effect. In our preliminary studies we have successfully used citrate reduced silver colloidal particles to obtain unique SERS spectra of α-helical and β-sheet bovine serum albumin (BSA) that served as models of an α helical antiobiody (biorecognition element) and a β-sheet target protein (pathogenic prion). In addition, the unique SERS spectra of double stranded and single stranded DNA were also obtained where the single stranded DNA served as the model for the biorecognition element and the double stranded DNA served as themodel for the DNA probe/target hybrid. This provides a confirmation of the feasibility of the method which opens opportunities for potentially wide spread applications in the detection of food pathogens, biowarefare agents, andother bio-analytes.

In Vitro Electrochemistry of Biological Systems

PubMed Central

Adams, Kelly L.; Puchades, Maja; Ewing, Andrew G.

2009-01-01

This article reviews recent work involving electrochemical methods for in vitro analysis of biomolecules, with an emphasis on detection and manipulation at and of single cells and cultures of cells. The techniques discussed include constant potential amperometry, chronoamperometry, cellular electroporation, scanning electrochemical microscopy, and microfluidic platforms integrated with electrochemical detection. The principles of these methods are briefly described, followed in most cases with a short description of an analytical or biological application and its significance. The use of electrochemical methods to examine specific mechanistic issues in exocytosis is highlighted, as a great deal of recent work has been devoted to this application. PMID:20151038

Calculation of the time resolution of the J-PET tomograph using kernel density estimation

NASA Astrophysics Data System (ADS)

Raczyński, L.; Wiślicki, W.; Krzemień, W.; Kowalski, P.; Alfs, D.; Bednarski, T.; Białas, P.; Curceanu, C.; Czerwiński, E.; Dulski, K.; Gajos, A.; Głowacz, B.; Gorgol, M.; Hiesmayr, B.; Jasińska, B.; Kamińska, D.; Korcyl, G.; Kozik, T.; Krawczyk, N.; Kubicz, E.; Mohammed, M.; Pawlik-Niedźwiecka, M.; Niedźwiecki, S.; Pałka, M.; Rudy, Z.; Rundel, O.; Sharma, N. G.; Silarski, M.; Smyrski, J.; Strzelecki, A.; Wieczorek, A.; Zgardzińska, B.; Zieliński, M.; Moskal, P.

2017-06-01

In this paper we estimate the time resolution of the J-PET scanner built from plastic scintillators. We incorporate the method of signal processing using the Tikhonov regularization framework and the kernel density estimation method. We obtain simple, closed-form analytical formulae for time resolution. The proposed method is validated using signals registered by means of the single detection unit of the J-PET tomograph built from a 30 cm long plastic scintillator strip. It is shown that the experimental and theoretical results obtained for the J-PET scanner equipped with vacuum tube photomultipliers are consistent.

Spacelab Charcoal Analyses

NASA Technical Reports Server (NTRS)

Slivon, L. E.; Hernon-Kenny, L. A.; Katona, V. R.; Dejarme, L. E.

1995-01-01

This report describes analytical methods and results obtained from chemical analysis of 31 charcoal samples in five sets. Each set was obtained from a single scrubber used to filter ambient air on board a Spacelab mission. Analysis of the charcoal samples was conducted by thermal desorption followed by gas chromatography/mass spectrometry (GC/MS). All samples were analyzed using identical methods. The method used for these analyses was able to detect compounds independent of their polarity or volatility. In addition to the charcoal samples, analyses of three Environmental Control and Life Support System (ECLSS) water samples were conducted specifically for trimethylamine.

Novel approaches to analysis by flow injection gradient titration.

PubMed

Wójtowicz, Marzena; Kozak, Joanna; Kościelniak, Paweł

2007-09-26

Two novel procedures for flow injection gradient titration with the use of a single stock standard solution are proposed. In the multi-point single-line (MP-SL) method the calibration graph is constructed on the basis of a set of standard solutions, which are generated in a standard reservoir and subsequently injected into the titrant. According to the single-point multi-line (SP-ML) procedure the standard solution and a sample are injected into the titrant stream from four loops of different capacities, hence four calibration graphs are able to be constructed and the analytical result is calculated on the basis of a generalized slope of these graphs. Both approaches have been tested on the example of spectrophotometric acid-base titration of hydrochloric and acetic acids with using bromothymol blue and phenolphthalein as indicators, respectively, and sodium hydroxide as a titrant. Under optimized experimental conditions the analytical results of precision less than 1.8 and 2.5% (RSD) and of accuracy less than 3.0 and 5.4% (relative error (RE)) were obtained for MP-SL and SP-ML procedures, respectively, in ranges of 0.0031-0.0631 mol L(-1) for samples of hydrochloric acid and of 0.1680-1.7600 mol L(-1) for samples of acetic acid. The feasibility of both methods was illustrated by applying them to the total acidity determination in vinegar samples with precision lower than 0.5 and 2.9% (RSD) for MP-SL and SP-ML procedures, respectively.

ICP-MS: Analytical Method for Identification and Detection of Elemental Impurities.

PubMed

Mittal, Mohini; Kumar, Kapil; Anghore, Durgadas; Rawal, Ravindra K

2017-01-01

Aim of this article is to review and discuss the currently used quantitative analytical method ICP-MS, which is used for quality control of pharmaceutical products. ICP-MS technique has several applications such as determination of single elements, multi element analysis in synthetic drugs, heavy metals in environmental water, trace element content of selected fertilizers and dairy manures. ICP-MS is also used for determination of toxic and essential elements in different varieties of food samples and metal pollutant present in the environment. The pharmaceuticals may generate impurities at various stages of development, transportation and storage which make them risky to be administered. Thus, it is essential that these impurities must be detected and quantified. ICP-MS plays an important function in the recognition and revealing of elemental impurities. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Greenhouse Gas Analysis by GC/MS

NASA Astrophysics Data System (ADS)

Bock, E. M.; Easton, Z. M.; Macek, P.

2015-12-01

Current methods to analyze greenhouse gases rely on designated complex, multiple-column, multiple-detector gas chromatographs. A novel method was developed in partnership with Shimadzu for simultaneous quantification of carbon dioxide (CO2), methane (CH4), and nitrous oxide (N2O) in environmental gas samples. Gas bulbs were used to make custom standard mixtures by injecting small volumes of pure analyte into the nitrogen-filled bulb. Resulting calibration curves were validated using a certified gas standard. The use of GC/MS systems to perform this analysis has the potential to move the analysis of greenhouse gasses from expensive, custom GC systems to standard single-quadrupole GC/MS systems that are available in most laboratories, which wide variety of applications beyond greenhouse gas analysis. Additionally, use of mass spectrometry can provide confirmation of identity of target analytes, and will assist in the identification of unknown peaks should they be present in the chromatogram.

Stabilization of glucose-oxidase in the graphene paste for screen-printed glucose biosensor

NASA Astrophysics Data System (ADS)

Pepłowski, Andrzej; Janczak, Daniel; Jakubowska, Małgorzata

2015-09-01

Various methods and materials for enzyme stabilization within screen-printed graphene sensor were analyzed. Main goal was to develop technology allowing immediate printing of the biosensors in single printing process. Factors being considered were: toxicity of the materials used, ability of the material to be screen-printed (squeezed through the printing mesh) and temperatures required in the fabrication process. Performance of the examined sensors was measured using chemical amperometry method, then appropriate analysis of the measurements was conducted. The analysis results were then compared with the medical requirements. Parameters calculated were: correlation coefficient between concentration of the analyte and the measured electrical current (0.986) and variation coefficient for the particular concentrations of the analyte used as the calibration points. Variation of the measured values was significant only in ranges close to 0, decreasing for the concentrations of clinical importance. These outcomes justify further development of the graphene-based biosensors fabricated through printing techniques.

Analytical study of bound states in graphene nanoribbons and carbon nanotubes: The variable phase method and the relativistic Levinson theorem

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

Miserev, D. S., E-mail: d.miserev@student.unsw.edu.au, E-mail: erazorheader@gmail.com

2016-06-15

The problem of localized states in 1D systems with a relativistic spectrum, namely, graphene stripes and carbon nanotubes, is studied analytically. The bound state as a superposition of two chiral states is completely described by their relative phase, which is the foundation of the variable phase method (VPM) developed herein. Based on our VPM, we formulate and prove the relativistic Levinson theorem. The problem of bound states can be reduced to the analysis of closed trajectories of some vector field. Remarkably, the Levinson theorem appears as the Poincaré index theorem for these closed trajectories. The VPM equation is also reducedmore » to the nonrelativistic and semiclassical limits. The limit of a small momentum p{sub y} of transverse quantization is applicable to an arbitrary integrable potential. In this case, a single confined mode is predicted.« less

Technology advancement for integrative stem cell analyses.

PubMed

Jeong, Yoon; Choi, Jonghoon; Lee, Kwan Hyi

2014-12-01

Scientists have endeavored to use stem cells for a variety of applications ranging from basic science research to translational medicine. Population-based characterization of such stem cells, while providing an important foundation to further development, often disregard the heterogeneity inherent among individual constituents within a given population. The population-based analysis and characterization of stem cells and the problems associated with such a blanket approach only underscore the need for the development of new analytical technology. In this article, we review current stem cell analytical technologies, along with the advantages and disadvantages of each, followed by applications of these technologies in the field of stem cells. Furthermore, while recent advances in micro/nano technology have led to a growth in the stem cell analytical field, underlying architectural concepts allow only for a vertical analytical approach, in which different desirable parameters are obtained from multiple individual experiments and there are many technical challenges that limit vertically integrated analytical tools. Therefore, we propose--by introducing a concept of vertical and horizontal approach--that there is the need of adequate methods to the integration of information, such that multiple descriptive parameters from a stem cell can be obtained from a single experiment.

Technology Advancement for Integrative Stem Cell Analyses

PubMed Central

Jeong, Yoon

2014-01-01

Scientists have endeavored to use stem cells for a variety of applications ranging from basic science research to translational medicine. Population-based characterization of such stem cells, while providing an important foundation to further development, often disregard the heterogeneity inherent among individual constituents within a given population. The population-based analysis and characterization of stem cells and the problems associated with such a blanket approach only underscore the need for the development of new analytical technology. In this article, we review current stem cell analytical technologies, along with the advantages and disadvantages of each, followed by applications of these technologies in the field of stem cells. Furthermore, while recent advances in micro/nano technology have led to a growth in the stem cell analytical field, underlying architectural concepts allow only for a vertical analytical approach, in which different desirable parameters are obtained from multiple individual experiments and there are many technical challenges that limit vertically integrated analytical tools. Therefore, we propose—by introducing a concept of vertical and horizontal approach—that there is the need of adequate methods to the integration of information, such that multiple descriptive parameters from a stem cell can be obtained from a single experiment. PMID:24874188

A silver nanoislands on silica spheres platform: enriching trace amounts of analytes for ultrasensitive and reproducible SERS detection.

PubMed

Wang, Zhongshun; Feng, Lei; Xiao, Dongyang; Li, Ning; Li, Yao; Cao, Danfeng; Shi, Zuosen; Cui, Zhanchen; Lu, Nan

2017-11-09

The performance of surface-enhanced Raman scattering (SERS) for detecting trace amounts of analytes depends highly on the enrichment of the diluted analytes into a small region that can be detected. A super-hydrophobic delivery (SHD) process is an excellent process to enrich even femtomolar analytes for SERS detection. However, it is still challenging to easily fabricate a low detection limit, high sensitivity and reproducible SHD-SERS substrate. In this article, we present a cost-effective and fewer-step method to fabricate a SHD-SERS substrate, named the "silver nanoislands on silica spheres" (SNOSS) platform. It is easily prepared via the thermal evaporation of silver onto a layer of super-hydrophobic paint, which contains single-scale surface-fluorinated silica spheres. The SNOSS platform performs reproducible detection, which brings the relative standard deviation down to 8.85% and 5.63% for detecting 10 -8 M R6G in one spot and spot-to-spot set-ups, respectively. The coefficient of determination (R 2 ) is 0.9773 for R6G. The SNOSS platform can be applied to the quantitative detection of analytes whose concentrations range from sub-micromolar to femtomolar levels.

Peak clustering in two-dimensional gas chromatography with mass spectrometric detection based on theoretical calculation of two-dimensional peak shapes: the 2DAid approach.

PubMed

van Stee, Leo L P; Brinkman, Udo A Th

2011-10-28

A method is presented to facilitate the non-target analysis of data obtained in temperature-programmed comprehensive two-dimensional (2D) gas chromatography coupled to time-of-flight mass spectrometry (GC×GC-ToF-MS). One main difficulty of GC×GC data analysis is that each peak is usually modulated several times and therefore appears as a series of peaks (or peaklets) in the one-dimensionally recorded data. The proposed method, 2DAid, uses basic chromatographic laws to calculate the theoretical shape of a 2D peak (a cluster of peaklets originating from the same analyte) in order to define the area in which the peaklets of each individual compound can be expected to show up. Based on analyte-identity information obtained by means of mass spectral library searching, the individual peaklets are then combined into a single 2D peak. The method is applied, amongst others, to a complex mixture containing 362 analytes. It is demonstrated that the 2D peak shapes can be accurately predicted and that clustering and further processing can reduce the final peak list to a manageable size. Copyright © 2011 Elsevier B.V. All rights reserved.

Automated sample preparation using membrane microtiter extraction for bioanalytical mass spectrometry.

PubMed

Janiszewski, J; Schneider, P; Hoffmaster, K; Swyden, M; Wells, D; Fouda, H

1997-01-01

The development and application of membrane solid phase extraction (SPE) in 96-well microtiter plate format is described for the automated analysis of drugs in biological fluids. The small bed volume of the membrane allows elution of the analyte in a very small solvent volume, permitting direct HPLC injection and negating the need for the time consuming solvent evaporation step. A programmable liquid handling station (Quadra 96) was modified to automate all SPE steps. To avoid drying of the SPE bed and to enhance the analytical precision a novel protocol for performing the condition, load and wash steps in rapid succession was utilized. A block of 96 samples can now be extracted in 10 min., about 30 times faster than manual solvent extraction or single cartridge SPE methods. This processing speed complements the high-throughput speed of contemporary high performance liquid chromatography mass spectrometry (HPLC/MS) analysis. The quantitative analysis of a test analyte (Ziprasidone) in plasma demonstrates the utility and throughput of membrane SPE in combination with HPLC/MS. The results obtained with the current automated procedure compare favorably with those obtained using solvent and traditional solid phase extraction methods. The method has been used for the analysis of numerous drug prototypes in biological fluids to support drug discovery efforts.

Analysis of a variety of inorganic and organic additives in food products by ion-pairing liquid chromatography coupled to high-resolution mass spectrometry.

PubMed

Kaufmann, Anton; Widmer, Mirjam; Maden, Kathryn; Butcher, Patrick; Walker, Stephan

2018-03-05

A reversed-phase ion-pairing chromatographic method was developed for the detection and quantification of inorganic and organic anionic food additives. A single-stage high-resolution mass spectrometer (orbitrap ion trap, Orbitrap) was used to detect the accurate masses of the unfragmented analyte ions. The developed ion-pairing chromatography method was based on a dibutylamine/hexafluoro-2-propanol buffer. Dibutylamine can be charged to serve as a chromatographic ion-pairing agent. This ensures sufficient retention of inorganic and organic anions. Yet, unlike quaternary amines, it can be de-charged in the electrospray to prevent the formation of neutral analyte ion-pairing agent adducts. This process is significantly facilitated by the added hexafluoro-2-propanol. This approach permits the sensitive detection and quantification of additives like nitrate and mono-, di-, and triphosphate as well as citric acid, a number of artificial sweeteners like cyclamate and aspartame, flavor enhancers like glutamate, and preservatives like sorbic acid. This is a major advantage, since the currently used analytical methods as utilized in food safety laboratories are only capable in monitoring a few compounds or a particular category of food additives. Graphical abstract Deptotonation of ion pair agent in the electrospray interface.

Development of multiclass methods for drug residues in eggs: hydrophilic solid-phase extraction cleanup and liquid chromatography/tandem mass spectrometry analysis of tetracycline, fluoroquinolone, sulfonamide, and beta-lactam residues.

PubMed

Heller, David N; Nochetto, Cristina B; Rummel, Nathan G; Thomas, Michael H

2006-07-26

A method was developed for detection of a variety of polar drug residues in eggs via liquid chromatography/tandem mass spectrometry (LC/MS/MS) with electrospray ionization (ESI). A total of twenty-nine target analytes from four drug classes-sulfonamides, tetracyclines, fluoroquinolones, and beta-lactams-were extracted from eggs using a hydrophilic-lipophilic balance polymer solid-phase extraction (SPE) cartridge. The extraction technique was developed for use at a target concentration of 100 ng/mL (ppb), and it was applied to eggs containing incurred residues from dosed laying hens. The ESI source was tuned using a single, generic set of tuning parameters, and analytes were separated with a phenyl-bonded silica cartridge column using an LC gradient. In a related study, residues of beta-lactam drugs were not found by LC/MS/MS in eggs from hens dosed orally with beta-lactam drugs. LC/MS/MS performance was evaluated on two generations of ion trap mass spectrometers, and key operational parameters were identified for each instrument. The ion trap acquisition methods could be set up for screening (a single product ion) or confirmation (multiple product ions). The lower limit of detection for screening purposes was 10-50 ppb (sulfonamides), 10-20 ppb (fluoroquinolones), and 10-50 ppb (tetracyclines), depending on the drug, instrument, and acquisition method. Development of this method demonstrates the feasibility of generic SPE, LC, and MS conditions for multiclass LC/MS residue screening.

Calibrating genomic and allelic coverage bias in single-cell sequencing.

PubMed

Zhang, Cheng-Zhong; Adalsteinsson, Viktor A; Francis, Joshua; Cornils, Hauke; Jung, Joonil; Maire, Cecile; Ligon, Keith L; Meyerson, Matthew; Love, J Christopher

2015-04-16

Artifacts introduced in whole-genome amplification (WGA) make it difficult to derive accurate genomic information from single-cell genomes and require different analytical strategies from bulk genome analysis. Here, we describe statistical methods to quantitatively assess the amplification bias resulting from whole-genome amplification of single-cell genomic DNA. Analysis of single-cell DNA libraries generated by different technologies revealed universal features of the genome coverage bias predominantly generated at the amplicon level (1-10 kb). The magnitude of coverage bias can be accurately calibrated from low-pass sequencing (∼0.1 × ) to predict the depth-of-coverage yield of single-cell DNA libraries sequenced at arbitrary depths. We further provide a benchmark comparison of single-cell libraries generated by multi-strand displacement amplification (MDA) and multiple annealing and looping-based amplification cycles (MALBAC). Finally, we develop statistical models to calibrate allelic bias in single-cell whole-genome amplification and demonstrate a census-based strategy for efficient and accurate variant detection from low-input biopsy samples.

Calibrating genomic and allelic coverage bias in single-cell sequencing

PubMed Central

Francis, Joshua; Cornils, Hauke; Jung, Joonil; Maire, Cecile; Ligon, Keith L.; Meyerson, Matthew; Love, J. Christopher

2016-01-01

Artifacts introduced in whole-genome amplification (WGA) make it difficult to derive accurate genomic information from single-cell genomes and require different analytical strategies from bulk genome analysis. Here, we describe statistical methods to quantitatively assess the amplification bias resulting from whole-genome amplification of single-cell genomic DNA. Analysis of single-cell DNA libraries generated by different technologies revealed universal features of the genome coverage bias predominantly generated at the amplicon level (1–10 kb). The magnitude of coverage bias can be accurately calibrated from low-pass sequencing (~0.1 ×) to predict the depth-of-coverage yield of single-cell DNA libraries sequenced at arbitrary depths. We further provide a benchmark comparison of single-cell libraries generated by multi-strand displacement amplification (MDA) and multiple annealing and looping-based amplification cycles (MALBAC). Finally, we develop statistical models to calibrate allelic bias in single-cell whole-genome amplification and demonstrate a census-based strategy for efficient and accurate variant detection from low-input biopsy samples. PMID:25879913

Technical Evaluation Report of the Aerospace Medical Panel Working Group WG-08 on Evaluation of Methods to Assess Workload.

DTIC Science & Technology

1980-11-01

Occlusion 3.1 Single Measures 3. Primary Task 3.2 Multiple Measures 3.3 Math Modeling 4.1.1 PFF 4.1.2 CSR 4.1.3 M,0 4.1.4 MW 4.1.5 UG3 4.1.6 ZCP 4.1 Single... modeling methodology; and (4) validation of the analytic/predictive methodology In a system design, development, and test effort." Chapter 9: "A central...2.3 Occlusion P S P S S P -P 3.1 Single Measure-Primary S S S S S S S 3.2 Multiple Measure-Primary S S IS S S S S K 3.3 Math Modeling ~ 4.1.7 Eye and

High-throughput, label-free, single-cell, microalgal lipid screening by machine-learning-equipped optofluidic time-stretch quantitative phase microscopy.

PubMed

Guo, Baoshan; Lei, Cheng; Kobayashi, Hirofumi; Ito, Takuro; Yalikun, Yaxiaer; Jiang, Yiyue; Tanaka, Yo; Ozeki, Yasuyuki; Goda, Keisuke

2017-05-01

The development of reliable, sustainable, and economical sources of alternative fuels to petroleum is required to tackle the global energy crisis. One such alternative is microalgal biofuel, which is expected to play a key role in reducing the detrimental effects of global warming as microalgae absorb atmospheric CO 2 via photosynthesis. Unfortunately, conventional analytical methods only provide population-averaged lipid amounts and fail to characterize a diverse population of microalgal cells with single-cell resolution in a non-invasive and interference-free manner. Here high-throughput label-free single-cell screening of lipid-producing microalgal cells with optofluidic time-stretch quantitative phase microscopy was demonstrated. In particular, Euglena gracilis, an attractive microalgal species that produces wax esters (suitable for biodiesel and aviation fuel after refinement), within lipid droplets was investigated. The optofluidic time-stretch quantitative phase microscope is based on an integration of a hydrodynamic-focusing microfluidic chip, an optical time-stretch quantitative phase microscope, and a digital image processor equipped with machine learning. As a result, it provides both the opacity and phase maps of every single cell at a high throughput of 10,000 cells/s, enabling accurate cell classification without the need for fluorescent staining. Specifically, the dataset was used to characterize heterogeneous populations of E. gracilis cells under two different culture conditions (nitrogen-sufficient and nitrogen-deficient) and achieve the cell classification with an error rate of only 2.15%. The method holds promise as an effective analytical tool for microalgae-based biofuel production. © 2017 International Society for Advancement of Cytometry. © 2017 International Society for Advancement of Cytometry.

Analysis of social optimum for staggered shifts in a single-entry traffic corridor with no late arrivals

NASA Astrophysics Data System (ADS)

Li, Chuan-Yao; Huang, Hai-Jun; Tang, Tie-Qiao

2017-03-01

This paper investigates the traffic flow dynamics under the social optimum (SO) principle in a single-entry traffic corridor with staggered shifts from the analytical and numerical perspectives. The LWR (Lighthill-Whitham and Richards) model and the Greenshield's velocity-density function are utilized to describe the dynamic properties of traffic flow. The closed-form SO solution is analytically derived and some numerical examples are used to further testify the analytical solution. The optimum proportion of the numbers of commuters with different desired arrival times is further discussed, where the analytical and numerical results both indicate that the cumulative outflow curve under the SO principle is piecewise smooth.

Impact desolvation of electrosprayed microdroplets--a new ionization method for mass spectrometry of large biomolecules.

PubMed

Aksyonov, S A; Williams, P

2001-01-01

Impact desolvation of electrosprayed microdroplets (IDEM) is a new method for producing gas-phase ions of large biomolecules. Analytes are dissolved in an electrolyte solution which is electrosprayed in vacuum, producing highly charged micron and sub-micron sized droplets (microdroplets). These microdroplets are accelerated through potential differences approximately 5 - 10 kV to velocities of several km/s and allowed to impact a target surface. The energetic impacts vaporize the droplets and release desolvated gas-phase ions of the analyte molecules. Oligonucleotides (2- to 12-mer) and peptides (bradykinin, neurotensin) yield singly and doubly charged molecular ions with no detectable fragmentation. Because the extent of multiple charging is significantly less than in atmospheric pressure electrospray ionization, and the method produces ions largely free of adducts from solutions of high ionic strength, IDEM has some promise as a method for coupling to liquid chromatographic techniques and for mixture analysis. Ions are produced in vacuum at a flat equipotential surface, potentially allowing efficient ion extraction. Copyright 2001 John Wiley & Sons, Ltd.

Improved vertical streambed flux estimation using multiple diurnal temperature methods in series

USGS Publications Warehouse

Irvine, Dylan J.; Briggs, Martin A.; Cartwright, Ian; Scruggs, Courtney; Lautz, Laura K.

2017-01-01

Analytical solutions that use diurnal temperature signals to estimate vertical fluxes between groundwater and surface water based on either amplitude ratios (Ar) or phase shifts (Δϕ) produce results that rarely agree. Analytical solutions that simultaneously utilize Ar and Δϕ within a single solution have more recently been derived, decreasing uncertainty in flux estimates in some applications. Benefits of combined (ArΔϕ) methods also include that thermal diffusivity and sensor spacing can be calculated. However, poor identification of either Ar or Δϕ from raw temperature signals can lead to erratic parameter estimates from ArΔϕ methods. An add-on program for VFLUX 2 is presented to address this issue. Using thermal diffusivity selected from an ArΔϕ method during a reliable time period, fluxes are recalculated using an Ar method. This approach maximizes the benefits of the Ar and ArΔϕ methods. Additionally, sensor spacing calculations can be used to identify periods with unreliable flux estimates, or to assess streambed scour. Using synthetic and field examples, the use of these solutions in series was particularly useful for gaining conditions where fluxes exceeded 1 m/d.

Value assignment and uncertainty evaluation for single-element reference solutions

NASA Astrophysics Data System (ADS)

Possolo, Antonio; Bodnar, Olha; Butler, Therese A.; Molloy, John L.; Winchester, Michael R.

2018-06-01

A Bayesian statistical procedure is proposed for value assignment and uncertainty evaluation for the mass fraction of the elemental analytes in single-element solutions distributed as NIST standard reference materials. The principal novelty that we describe is the use of information about relative differences observed historically between the measured values obtained via gravimetry and via high-performance inductively coupled plasma optical emission spectrometry, to quantify the uncertainty component attributable to between-method differences. This information is encapsulated in a prior probability distribution for the between-method uncertainty component, and it is then used, together with the information provided by current measurement data, to produce a probability distribution for the value of the measurand from which an estimate and evaluation of uncertainty are extracted using established statistical procedures.

Analytic approximation for random muffin-tin alloys

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

Mills, R.; Gray, L.J.; Kaplan, T.

1983-03-15

The methods introduced in a previous paper under the name of ''traveling-cluster approximation'' (TCA) are applied, in a multiple-scattering approach, to the case of a random muffin-tin substitutional alloy. This permits the iterative part of a self-consistent calculation to be carried out entirely in terms of on-the-energy-shell scattering amplitudes. Off-shell components of the mean resolvent, needed for the calculation of spectral functions, are obtained by standard methods involving single-site scattering wave functions. The single-site TCA is just the usual coherent-potential approximation, expressed in a form particularly suited for iteration. A fixed-point theorem is proved for the general t-matrix TCA, ensuringmore » convergence upon iteration to a unique self-consistent solution with the physically essential Herglotz properties.« less

A rapid method for optimization of the rocket propulsion system for single-stage-to-orbit vehicles

NASA Technical Reports Server (NTRS)

Eldred, C. H.; Gordon, S. V.

1976-01-01

A rapid analytical method for the optimization of rocket propulsion systems is presented for a vertical take-off, horizontal landing, single-stage-to-orbit launch vehicle. This method utilizes trade-offs between propulsion characteristics affecting flight performance and engine system mass. The performance results from a point-mass trajectory optimization program are combined with a linearized sizing program to establish vehicle sizing trends caused by propulsion system variations. The linearized sizing technique was developed for the class of vehicle systems studied herein. The specific examples treated are the optimization of nozzle expansion ratio and lift-off thrust-to-weight ratio to achieve either minimum gross mass or minimum dry mass. Assumed propulsion system characteristics are high chamber pressure, liquid oxygen and liquid hydrogen propellants, conventional bell nozzles, and the same fixed nozzle expansion ratio for all engines on a vehicle.

Simultaneous Determination of 10 Ultratrace Elements in Infant Formula, Adult Nutritionals, and Milk Products by ICP/MS After Pressure Digestion: Single-Laboratory Validation.

PubMed

Dubascoux, Stephane; Nicolas, Marine; Rime, Celine Fragniere; Payot, Janique Richoz; Poitevin, Eric

2015-01-01

A single-laboratory validation (SLV) is presented for the simultaneous determination of 10 ultratrace elements (UTEs) including aluminum (Al), arsenic (As), cadmium (Cd), cobalt (Co), chromium (Cr), mercury (Hg), molybdenum (Mo), lead (Pb), selenium (Se), and tin (Sn) in infant formulas, adult nutritionals, and milk based products by inductively coupled plasma (ICP)/MS after acidic pressure digestion. This robust and routine multielemental method is based on several official methods with modifications of sample preparation using either microwave digestion or high pressure ashing and of analytical conditions using ICP/MS with collision cell technology. This SLV fulfills AOAC method performance criteria in terms of linearity, specificity, sensitivity, precision, and accuracy and fully answers most international regulation limits for trace contaminants and/or recommended nutrient levels established for 10 UTEs in targeted matrixes.

Simultaneous determination of 13 fluoroquinolone and 22 sulfonamide residues in milk by a dual-colorimetric enzyme-linked immunosorbent assay

USDA-ARS?s Scientific Manuscript database

Enzyme-linked immunosorbent assays (ELISAs) usually focus on the detection of a single analyte or a single group of analytes, e.g., fluoroquinolones or sulfonamides. However, it is often necessary to simultaneously monitor the two classes of antimicrobial residues in different food matrices. In th...

Development of an analytical method to assess the occupational health risk of therapeutic monoclonal antibodies using LC-HRMS.

PubMed

Reinders, Lars M H; Klassen, Martin D; Jaeger, Martin; Teutenberg, Thorsten; Tuerk, Jochen

2018-04-01

Monoclonal antibodies are a group of commonly used therapeutics, whose occupational health risk is still discussed controversially. The long-term low-dose exposure side effects are insufficiently evaluated; hence, discussions are often based on a theoretical level or extrapolating side effects from therapeutic dosages. While some research groups recommend applying the precautionary principle for monoclonal antibodies, others consider the exposure risk too low for measures taken towards occupational health and safety. However, both groups agree that airborne monoclonal antibodies have the biggest risk potential. Therefore, we developed a peptide-based analytical method for occupational exposure monitoring of airborne monoclonal antibodies. The method will allow collecting data about the occupational exposure to monoclonal antibodies. Thus, the mean daily intake for personnel in pharmacies and the pharmaceutical industry can be determined for the first time and will help to substantiate the risk assessment by relevant data. The introduced monitoring method includes air sampling, sample preparation and detection by liquid chromatography coupled with high-resolution mass spectrometry of individual monoclonal antibodies as well as sum parameter. For method development and validation, a chimeric (rituximab), humanised (trastuzumab) and a fully humanised (daratumumab) monoclonal antibody are used. A limit of detection between 1 μg per sample for daratumumab and 25 μg per sample for the collective peptide is achieved. Graphical abstract Demonstration of the analytical workflow, from the release of monoclonal antibodies to the detection as single substances as well as sum parameter.

Study of different HILIC, mixed-mode, and other aqueous normal-phase approaches for the liquid chromatography/mass spectrometry-based determination of challenging polar pesticides.

PubMed

Vass, Andrea; Robles-Molina, José; Pérez-Ortega, Patricia; Gilbert-López, Bienvenida; Dernovics, Mihaly; Molina-Díaz, Antonio; García-Reyes, Juan F

2016-07-01

The aim of the study was to evaluate the performance of different chromatographic approaches for the liquid chromatography/mass spectrometry (LC-MS(/MS)) determination of 24 highly polar pesticides. The studied compounds, which are in most cases unsuitable for conventional LC-MS(/MS) multiresidue methods were tested with nine different chromatographic conditions, including two different hydrophilic interaction liquid chromatography (HILIC) columns, two zwitterionic-type mixed-mode columns, three normal-phase columns operated in HILIC-mode (bare silica and two silica-based chemically bonded columns (cyano and amino)), and two standard reversed-phase C18 columns. Different sets of chromatographic parameters in positive (for 17 analytes) and negative ionization modes (for nine analytes) were examined. In order to compare the different approaches, a semi-quantitative classification was proposed, calculated as the percentage of an empirical performance value, which consisted of three main features: (i) capacity factor (k) to characterize analyte separation from the void, (ii) relative response factor, and (iii) peak shape based on analytes' peak width. While no single method was able to provide appropriate detection of all the 24 studied species in a single run, the best suited approach for the compounds ionized in positive mode was based on a UHPLC HILIC column with 1.8 μm particle size, providing appropriate results for 22 out of the 24 species tested. In contrast, the detection of glyphosate and aminomethylphosphonic acid could only be achieved with a zwitterionic-type mixed-mode column, which proved to be suitable only for the pesticides detected in negative ion mode. Finally, the selected approach (UHPLC HILIC) was found to be useful for the determination of multiple pesticides in oranges using HILIC-ESI-MS/MS, with limits of quantitation in the low microgram per kilogram in most cases. Graphical Abstract HILIC improves separation of multiclass polar pesticides.

Targeted screening of pesticides, veterinary drugs and mycotoxins in bakery ingredients and food commodities by liquid chromatography-high-resolution single-stage Orbitrap mass spectrometry.

PubMed

De Dominicis, Emiliano; Commissati, Italo; Suman, Michele

2012-09-01

In the food industry, it is frequently necessary to check the quality of an ingredient to decide whether to use it in production and/or to have an idea of the final possible contamination of the finished product. The current need to quickly separate and identify relevant contaminants within different classes, often with legal residue limits on the order of 1-100 µg kg(-1), has led to the need for more effective analytical methods. With thousands of organic compounds present in complex food matrices, the development of new analytical solutions leaned towards simplified extraction/clean-up procedures and chromatography coupled with mass spectrometry. Efforts must also be made regarding the instrumental phase to overcome sensitivity/selectivity limits and interferences. For this purpose, high-resolution full scan analysis in mass spectrometry is an interesting alternative to the traditional tandem mass approach. A fast method for extracting and purifying bakery matrices was therefore developed and combined with the exploitation of ultra-high-pressure liquid chromatography (UHPLC) coupled to a Orbitrap Exactive™ high-resolution mass spectrometer (HRMS). Extracts of blank, naturally contaminated and fortified minicakes, prepared through a combined use of industrial and pilot plant production lines, were analyzed at different concentration levels (1-100 µg kg(-1)) of various contaminants: a limit of detection at 10 µg kg(-1) was possible for most of the analytes within all the categories analyzed, including pesticides, aflatoxins, trichothecene toxins and veterinary drugs. The application of accurate mass targeted screening described in this article demonstrates that current single-stage HRMS analytical instrumentation is well equipped to meet the challenges posed by chemical contaminants in the screening of both bakery raw materials and finished products. Copyright © 2012 John Wiley & Sons, Ltd.

On the half-life of luminescence signals in dosimetric applications: A unified presentation

NASA Astrophysics Data System (ADS)

Pagonis, V.; Kitis, G.; Polymeris, G. S.

2018-06-01

Luminescence signals from natural and man-made materials are widely used in dosimetric and dating applications. In general, there are two types of half-lives of luminescence signals which are of importance to experimental and modeling work in this research area. The first type of half-life is the time required for the population of the trapped charge in a single trap to decay to half its initial value. The second type of half-life is the time required for the luminescence intensity to drop to half of its initial value. While there a handful of analytical expressions available in the literature for the first type of half-life, there are no corresponding analytical expressions for the second type. In this work new analytical expressions are derived for the half-life of luminescence signals during continuous wave optical stimulation luminescence (CW-OSL) or isothermal luminescence (ITL) experiments. The analytical expressions are derived for several commonly used luminescence models which are based on delocalized transitions involving the conduction band: first and second order kinetics, empirical general order kinetics (GOK), mixed order kinetics (MOK) and the one-trap one-recombination center (OTOR) model. In addition, half-life expressions are derived for a different type of luminescence model, which is based on localized transitions in a random distribution of charges. The new half-life expressions contain two parts. The first part is inversely proportional to the thermal or optical excitation rate, and depends on the experimental conditions and on the cross section of the relevant luminescence process. The second part is characteristic of the optical and/or thermal properties of the material, as expressed by the parameters in the model. A new simple and quick method for analyzing luminescence signals is developed, and examples are given of applying the new method to a variety of dosimetric materials. The new test allows quick determination of whether a set of experimentally measured luminescence signals originate in a single trap, or in multiple traps.

Google Analytics: Single Page Traffic Reports

EPA Pesticide Factsheets

These are pages that live outside of Google Analytics (GA) but allow you to view GA data for any individual page on either the public EPA web or EPA intranet. You do need to log in to Google Analytics to view them.

Evolutionary games with coordination and self-dependent interactions

NASA Astrophysics Data System (ADS)

Király, Balázs; Szabó, György

2017-01-01

Multistrategy evolutionary games are studied on a square lattice when the pair interactions are composed of coordinations between strategy pairs and an additional term with self-dependent payoff. We describe a method for determining the strength of each elementary coordination component in n -strategy potential games. Using analytical and numerical methods, the presence and absence of Ising-type order-disorder phase transitions are studied when a single pair coordination is extended by some types of self-dependent elementary games. We also introduce noise-dependent three-strategy equivalents of the n -strategy elementary coordination games.

Thermal desorption of metals from tungsten single crystal surfaces

NASA Technical Reports Server (NTRS)

Bauer, E.; Bonczek, F.; Poppa, H.; Todd, G.

1975-01-01

After a short review of experimental methods used to determine desorption energies and frequencies the assumptions underlying the theoretical analysis of experimental data are discussed. Recent experimental results on the flash desorption of Cu, Ag, and Au from clean, well characterized W (110) and (100) surfaces are presented and analyzed in detail with respect to the coverage dependence. The results obtained clearly reveal the limitations of previous analytical methods and of the experimental technique per se (such as structure and phase changes below and in the temperature region in which desorption occurs).

[Point of Care 2.0: Coagulation Monitoring Using Rotem® Sigma and Teg® 6S].

PubMed

Weber, Christian Friedrich; Zacharowski, Kai

2018-06-01

New-generation methods for point of care based coagulation monitoring enable fully automated viscoelastic analyses for the assessment of particular parts of hemostasis. Contrary to the measuring techniques of former models, the viscoelastic ROTEM ® sigma and TEG ® 6s analyses are performed in single-use test cartridges without time- and personnel-intensive pre-analytical procedures. This review highlights methodical strengths and limitations of the devices and meets concerns associated with their integration in routine clinical practice. Georg Thieme Verlag KG Stuttgart · New York.

Understanding the compatibility of multiple uses on forest land: a survey of multiresource research with application to the Pacific Northwest.

Treesearch

James A. Stevens; Claire A. Montgomery

2002-01-01

In this report, multiresource research is described as it has coevolved with forest policy objectives—from managing for single or dominant uses, to managing for compatible multiple forest uses, to sustaining ecosystem health on the forest. The evolution of analytical methods for multiresource research is traced from impact analysis to multiresource modeling, and...

Time-resolved, single-cell analysis of induced and programmed cell death via non-invasive propidium iodide and counterstain perfusion.

PubMed

Krämer, Christina E M; Wiechert, Wolfgang; Kohlheyer, Dietrich

2016-09-01

Conventional propidium iodide (PI) staining requires the execution of multiple steps prior to analysis, potentially affecting assay results as well as cell vitality. In this study, this multistep analysis method has been transformed into a single-step, non-toxic, real-time method via live-cell imaging during perfusion with 0.1 μM PI inside a microfluidic cultivation device. Dynamic PI staining was an effective live/dead analytical tool and demonstrated consistent results for single-cell death initiated by direct or indirect triggers. Application of this method for the first time revealed the apparent antibiotic tolerance of wild-type Corynebacterium glutamicum cells, as indicated by the conversion of violet fluorogenic calcein acetoxymethyl ester (CvAM). Additional implementation of this method provided insight into the induced cell lysis of Escherichia coli cells expressing a lytic toxin-antitoxin module, providing evidence for non-lytic cell death and cell resistance to toxin production. Finally, our dynamic PI staining method distinguished necrotic-like and apoptotic-like cell death phenotypes in Saccharomyces cerevisiae among predisposed descendants of nutrient-deprived ancestor cells using PO-PRO-1 or green fluorogenic calcein acetoxymethyl ester (CgAM) as counterstains. The combination of single-cell cultivation, fluorescent time-lapse imaging, and PI perfusion facilitates spatiotemporally resolved observations that deliver new insights into the dynamics of cellular behaviour.

Pollutant source identification model for water pollution incidents in small straight rivers based on genetic algorithm

NASA Astrophysics Data System (ADS)

Zhang, Shou-ping; Xin, Xiao-kang

2017-07-01

Identification of pollutant sources for river pollution incidents is an important and difficult task in the emergency rescue, and an intelligent optimization method can effectively compensate for the weakness of traditional methods. An intelligent model for pollutant source identification has been established using the basic genetic algorithm (BGA) as an optimization search tool and applying an analytic solution formula of one-dimensional unsteady water quality equation to construct the objective function. Experimental tests show that the identification model is effective and efficient: the model can accurately figure out the pollutant amounts or positions no matter single pollution source or multiple sources. Especially when the population size of BGA is set as 10, the computing results are sound agree with analytic results for a single source amount and position identification, the relative errors are no more than 5 %. For cases of multi-point sources and multi-variable, there are some errors in computing results for the reasons that there exist many possible combinations of the pollution sources. But, with the help of previous experience to narrow the search scope, the relative errors of the identification results are less than 5 %, which proves the established source identification model can be used to direct emergency responses.

Expanded envelope concepts for aircraft control-element failure detection and identification

NASA Technical Reports Server (NTRS)

Weiss, Jerold L.; Hsu, John Y.

1988-01-01

The purpose of this effort was to develop and demonstrate concepts for expanding the envelope of failure detection and isolation (FDI) algorithms for aircraft-path failures. An algorithm which uses analytic-redundancy in the form of aerodynamic force and moment balance equations was used. Because aircraft-path FDI uses analytical models, there is a tradeoff between accuracy and the ability to detect and isolate failures. For single flight condition operation, design and analysis methods are developed to deal with this robustness problem. When the departure from the single flight condition is significant, algorithm adaptation is necessary. Adaptation requirements for the residual generation portion of the FDI algorithm are interpreted as the need for accurate, large-motion aero-models, over a broad range of velocity and altitude conditions. For the decision-making part of the algorithm, adaptation may require modifications to filtering operations, thresholds, and projection vectors that define the various hypothesis tests performed in the decision mechanism. Methods of obtaining and evaluating adequate residual generation and decision-making designs have been developed. The application of the residual generation ideas to a high-performance fighter is demonstrated by developing adaptive residuals for the AFTI-F-16 and simulating their behavior under a variety of maneuvers using the results of a NASA F-16 simulation.

Channel Temperature Determination for AlGaN/GaN HEMTs on SiC and Sapphire

NASA Technical Reports Server (NTRS)

Freeman, Jon C.; Mueller, Wolfgang

2008-01-01

Numerical simulation results (with emphasis on channel temperature) for a single gate AlGaN/GaN High Electron Mobility Transistor (HEMT) with either a sapphire or SiC substrate are presented. The static I-V characteristics, with concomitant channel temperatures (T(sub ch)) are calculated using the software package ATLAS, from Silvaco, Inc. An in-depth study of analytical (and previous numerical) methods for the determination of T(sub ch) in both single and multiple gate devices is also included. We develop a method for calculating T(sub ch) for the single gate device with the temperature dependence of the thermal conductivity of all material layers included. We also present a new method for determining the temperature on each gate in a multi-gate array. These models are compared with experimental results, and show good agreement. We demonstrate that one may obtain the channel temperature within an accuracy of +/-10 C in some cases. Comparisons between different approaches are given to show the limits, sensitivities, and needed approximations, for reasonable agreement with measurements.

Ultrasonic nebulization extraction-heating gas flow transfer-headspace single drop microextraction of essential oil from pericarp of Zanthoxylum bungeanum Maxim.

PubMed

Wei, Shigang; Zhang, Huihui; Wang, Yeqiang; Wang, Lu; Li, Xueyuan; Wang, Yinghua; Zhang, Hanqi; Xu, Xu; Shi, Yuhua

2011-07-22

The ultrasonic nebulization extraction-heating gas flow transfer coupled with headspace single drop microextraction (UNE-HGFT-HS-SDME) was developed for the extraction of essential oil from Zanthoxylum bungeanum Maxim. The gas chromatography-mass spectrometry was applied to the determination of the constituents in the essential oil. The contents of the constituents from essential oil obtained by the proposed method were found to be more similar to those obtained by hydro-distillation (HD) than those obtained by ultrasonic nebulization extraction coupled with headspace single drop microextraction (UNE-HS-SDME). The heating gas flow was firstly used in the analysis of the essential oil to transfer the analytes from the headspace to the solvent microdrop. The relative standard deviations for determining the five major constituents were in the range from 1.5 to 6.7%. The proposed method is a fast, sensitive, low cost and small sample consumption method for the determination of the volatile and semivolatile constituents in the plant materials. Copyright © 2011 Elsevier B.V. All rights reserved.

Development and validation of a sensitive UHPLC-MS/MS method for the simultaneous analysis of tramadol, dextromethorphan chlorpheniramine and their major metabolites in human plasma in forensic context: application to pharmacokinetics.

PubMed

Heneedak, Hala M; Salama, Ismail; Mostafa, Samia; El-Kady, Ehab; El-Sadek, Mohamed

2015-07-01

The prerequisites for forensic confirmatory analysis by LC/MS/MS with respect to European Union guidelines are chromatographic separation, a minimum number of two MS/MS transitions to obtain the required identification points and predefined thresholds for the variability of the relative intensities of the MS/MS transitions (MRM transitions) in samples and reference standards. In the present study, a fast, sensitive and robust method to quantify tramadol, chlorpheniramine, dextromethorphan and their major metabolites, O-desmethyltramadol, dsmethyl-chlorpheniramine and dextrophan, respectively, in human plasma using ibuprofen as internal standard (IS) is described. The analytes and the IS were extracted from plasma by a liquid-liquid extraction method using ethyl acetate-diethyl-ether (1:1). Extracted samples were analyzed by ultra-high-performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry (UHPLC-ESI-MS/MS). Chromatographic separation was performed by pumping the mobile phase containing acetonitrile, water and formic acid (89.2:11.7:0.1) for 2.0 min at a flow rate of 0.25 μL/min into a Hypersil-Gold C18 column, 20 × 2.0 mm (1.9 µm) from Thermoscientific, New York, USA. The calibration curve was linear for the six analytes. The intraday precision (RSD) and accuracy (RE) of the method were 3-9.8 and -1.7-4.5%, respectively. The analytical procedure herein described was used to assess the pharmacokinetics of the analytes in 24 healthy volunteers after a single oral dose containing 50 mg of tramadol hydrochloride, 3 mg chlorpheniramine maleate and 15 mg of dextromethorphan hydrobromide. Copyright © 2014 John Wiley & Sons, Ltd.

Highly sensitive detection of cancer cells with an electrochemical cytosensor based on boronic acid functional polythiophene.

PubMed

Dervisevic, Muamer; Senel, Mehmet; Sagir, Tugba; Isik, Sevim

2017-04-15

The detection of cancer cells through important molecular recognition target such as sialic acid is significant for the clinical diagnosis and treatment. There are many electrochemical cytosensors developed for cancer cells detection but most of them have complicated fabrication processes which results in poor reproducibility and reliability. In this study, a simple, low-cost, and highly sensitive electrochemical cytosensor was designed based on boronic acid-functionalized polythiophene. In cytosensors fabrication simple single-step procedure was used which includes coating pencil graphite electrode (PGE) by means of electro-polymerization of 3-Thienyl boronic acid and Thiophen. Electrochemical impedance spectroscopy and cyclic voltammetry were used as an analytical methods to optimize and measure analytical performances of PGE/P(TBA 0.5 Th 0.5 ) based electrode. Cytosensor showed extremely good analytical performances in detection of cancer cells with linear rage of 1×10 1 to 1×10 6 cellsmL -1 exhibiting low detection limit of 10 cellsmL -1 and incubation time of 10min. Next to excellent analytical performances, it showed high selectivity towards AGS cancer cells when compared to HEK 293 normal cells and bone marrow mesenchymal stem cells (BM-hMSCs). This method is promising for future applications in early stage cancer diagnosis. Copyright © 2016 Elsevier B.V. All rights reserved.

Comprehensive solid-phase extraction of multitudinous bioactive peptides from equine plasma and urine for doping detection.

PubMed

Guan, Fuyu; Robinson, Mary A

2017-09-08

The ability to analyze biological samples for multitudinous exogenous peptides with a single analytical method is desired for doping control in horse racing. The key to achieving this goal is the capability of extracting all target peptides from the sample matrix. In the present study, theory of mixed-mode solid-phase extraction (SPE) of peptides from plasma is described, and a generic mixed-mode SPE procedure has been developed for recovering multitudinous exogenous peptides with remarkable sequence diversity, from equine plasma and urine in a single procedure. Both the theory and the developed SPE procedure have led to the development of a novel analytical method for comprehensive detection of multitudinous bioactive peptides in equine plasma and urine using liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS). Thirty nine bioactive peptides were extracted with strong anion-exchange mixed-mode SPE sorbent, separated on a reversed-phase C 18 column and detected by HRMS and data-dependent tandem mass spectrometry. The limit of detection (LOD) was 10-50 pg mL -1 in plasma for most of the peptides and 100 pg mL -1 for the remaining. For urine, LOD was 20-400 pg mL -1 for most of the peptides and 1-4 ng mL -1 for the others. In vitro degradation of the peptides in equine plasma and urine was examined at ambient temperature; the peptides except those with a D-amino acid at position 2 were unstable not only in plasma but also in urine. The developed method was successful in analysis of plasma and urine samples from horses administered dermorphin. Additionally, dermorphin metabolites were identified in the absence of reference standards. The developed SPE procedure and LC-HRMS method can theoretically detect virtually all peptides present at a sufficient concentration in a sample. New peptides can be readily included in the method to be detected without method re-development. The developed method also generates such data that can be retrospectively analyzed for peptides unknown at the time of sample analysis. It is the first generic analytical method for comprehensive detection of multitudinous exogenous peptides in biological samples, to the authors' knowledge. Copyright © 2017 Elsevier B.V. All rights reserved.

Orbital-optimized MP2.5 and its analytic gradients: Approaching CCSD(T) quality for noncovalent interactions

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

Bozkaya, Uğur, E-mail: ugur.bozkaya@atauni.edu.tr; Center for Computational Molecular Science and Technology, School of Chemistry and Biochemistry, and School of Computational Science and Engineering, Georgia Institute of Technology, Atlanta, Georgia 30332; Sherrill, C. David

2014-11-28

Orbital-optimized MP2.5 [or simply “optimized MP2.5,” OMP2.5, for short] and its analytic energy gradients are presented. The cost of the presented method is as much as that of coupled-cluster singles and doubles (CCSD) [O(N{sup 6}) scaling] for energy computations. However, for analytic gradient computations the OMP2.5 method is only half as expensive as CCSD because there is no need to solve λ{sub 2}-amplitude equations for OMP2.5. The performance of the OMP2.5 method is compared with that of the standard second-order Møller–Plesset perturbation theory (MP2), MP2.5, CCSD, and coupled-cluster singles and doubles with perturbative triples (CCSD(T)) methods for equilibrium geometries, hydrogenmore » transfer reactions between radicals, and noncovalent interactions. For bond lengths of both closed and open-shell molecules, the OMP2.5 method improves upon MP2.5 and CCSD by 38%–43% and 31%–28%, respectively, with Dunning's cc-pCVQZ basis set. For complete basis set (CBS) predictions of hydrogen transfer reaction energies, the OMP2.5 method exhibits a substantially better performance than MP2.5, providing a mean absolute error of 1.1 kcal mol{sup −1}, which is more than 10 times lower than that of MP2.5 (11.8 kcal mol{sup −1}), and comparing to MP2 (14.6 kcal mol{sup −1}) there is a more than 12-fold reduction in errors. For noncovalent interaction energies (at CBS limits), the OMP2.5 method maintains the very good performance of MP2.5 for closed-shell systems, and for open-shell systems it significantly outperforms MP2.5 and CCSD, and approaches CCSD(T) quality. The MP2.5 errors decrease by a factor of 5 when the optimized orbitals are used for open-shell noncovalent interactions, and comparing to CCSD there is a more than 3-fold reduction in errors. Overall, the present application results indicate that the OMP2.5 method is very promising for open-shell noncovalent interactions and other chemical systems with difficult electronic structures.« less

On the Ionization and Ion Transmission Efficiencies of Different ESI-MS Interfaces

PubMed Central

Cox, Jonathan T.; Marginean, Ioan; Smith, Richard D.; Tang, Keqi

2014-01-01

The achievable sensitivity of electrospray ionization mass spectrometry (ESI-MS) is largely determined by the ionization efficiency in the ESI source and ion transmission efficiency through the ESI-MS interface. These performance characteristics are difficult to evaluate and compare across multiple platforms as it is difficult to correlate electrical current measurements to actual analyte ions reaching the detector of a mass spectrometer. We present an effective method to evaluate the overall ion utilization efficiency of an ESI-MS interface by measuring the total gas phase ion current transmitted through the interface and correlating it to the observed ion abundance measured in the corresponding mass spectrum. Using this method we systematically studied the ion transmission and ionization efficiencies of different ESI-MS interface configurations, including a single emitter/single inlet capillary, single emitter/multi-inlet capillary, and a subambient pressure ionization with nanoelectrospray (SPIN) MS interface with a single emitter and an emitter array, respectively. Our experimental results indicate that the overall ion utilization efficiency of SPIN-MS interface configurations exceeds that of the inlet capillary-based ESI-MS interface configurations. PMID:25267087

On the ionization and ion transmission efficiencies of different ESI-MS interfaces.

PubMed

Cox, Jonathan T; Marginean, Ioan; Smith, Richard D; Tang, Keqi

2015-01-01

The achievable sensitivity of electrospray ionization mass spectrometry (ESI-MS) is largely determined by the ionization efficiency in the ESI source and ion transmission efficiency through the ESI-MS interface. These performance characteristics are difficult to evaluate and compare across multiple platforms as it is difficult to correlate electrical current measurements to actual analyte ions reaching the detector of a mass spectrometer. We present an effective method to evaluate the overall ion utilization efficiency of an ESI-MS interface by measuring the total gas-phase ion current transmitted through the interface and correlating it to the observed ion abundance measured in the corresponding mass spectrum. Using this method, we systematically studied the ion transmission and ionization efficiencies of different ESI-MS interface configurations, including a single emitter/single inlet capillary, single emitter/multi-inlet capillary, and a subambient pressure ionization with nanoelectrospray (SPIN) MS interface with a single emitter and an emitter array, respectively. Our experimental results indicate that the overall ion utilization efficiency of SPIN-MS interface configurations exceeds that of the inlet capillary-based ESI-MS interface configurations.

An analytic model for acoustic scattering from an impedance cylinder placed normal to an impedance plane

NASA Astrophysics Data System (ADS)

Swearingen, Michelle E.

2004-04-01

An analytic model, developed in cylindrical coordinates, is described for the scattering of a spherical wave off a semi-infinite reight cylinder placed normal to a ground surface. The motivation for the research is to have a model with which one can simulate scattering from a single tree and which can be used as a fundamental element in a model for estimating the attenuation in a forest comprised of multiple tree trunks. Comparisons are made to the plane wave case, the transparent cylinder case, and the rigid and soft ground cases as a method of theoretically verifying the model for the contemplated range of model parameters. Agreement is regarded as excellent for these benchmark cases. Model sensitivity to five parameters is also explored. An experiment was performed to study the scattering from a cylinder normal to a ground surface. The data from the experiment is analyzed with a transfer function method to yield frequency and impulse responses, and calculations based on the analytic model are compared to the experimental data. Thesis advisor: David C. Swanson Copies of this thesis written in English can be obtained from

An analytical model for the celestial distribution of polarized light, accounting for polarization singularities, wavelength and atmospheric turbidity

NASA Astrophysics Data System (ADS)

Wang, Xin; Gao, Jun; Fan, Zhiguo; Roberts, Nicholas W.

2016-06-01

We present a computationally inexpensive analytical model for simulating celestial polarization patterns in variable conditions. We combine both the singularity theory of Berry et al (2004 New J. Phys. 6 162) and the intensity model of Perez et al (1993 Sol. Energy 50 235-245) such that our single model describes three key sets of data: (1) the overhead distribution of the degree of polarization as well as the existence of neutral points in the sky; (2) the change in sky polarization as a function of the turbidity of the atmosphere; and (3) sky polarization patterns as a function of wavelength, calculated in this work from the ultra-violet to the near infra-red. To verify the performance of our model we generate accurate reference data using a numerical radiative transfer model and statistical comparisons between these two methods demonstrate no significant difference in almost all situations. The development of our analytical model provides a novel method for efficiently calculating the overhead skylight polarization pattern. This provides a new tool of particular relevance for our understanding of animals that use the celestial polarization pattern as a source of visual information.

Multielemental Determination of As, Bi, Ge, Sb, and Sn in Agricultural Samples Using Hydride Generation Coupled to Microwave-Induced Plasma Optical Emission Spectrometry.

PubMed

Machado, Raquel C; Amaral, Clarice D B; Nóbrega, Joaquim A; Araujo Nogueira, Ana Rita

2017-06-14

A microwave-induced plasma optical emission spectrometer with N 2 -based plasma was combined with a multimode sample introduction system (MSIS) for hydride generation (HG) and multielemental determination of As, Bi, Ge, Sb, and Sn in samples of forage, bovine liver, powdered milk, agricultural gypsum, rice, and mineral fertilizer, using a single condition of prereduction and reduction. The accuracy of the developed analytical method was evaluated using certified reference materials of water and mineral fertilizer, and recoveries ranged from 95 to 106%. Addition and recovery experiments were carried out, and the recoveries varied from 85 to 117% for all samples evaluated. The limits of detection for As, Bi, Ge, Sb, and Sn were 0.46, 0.09, 0.19, 0.46, and 5.2 μg/L, respectively, for liquid samples, and 0.18, 0.04, 0.08, 0.19, and 2.1 mg/kg, respectively, for solid samples. The method proposed offers a simple, fast, multielemental, and robust alternative for successful determination of all five analytes in agricultural samples with low operational cost without compromising analytical performance.

Distribution of velocities and acceleration for a particle in Brownian correlated disorder: Inertial case

NASA Astrophysics Data System (ADS)

Le Doussal, Pierre; Petković, Aleksandra; Wiese, Kay Jörg

2012-06-01

We study the motion of an elastic object driven in a disordered environment in presence of both dissipation and inertia. We consider random forces with the statistics of random walks and reduce the problem to a single degree of freedom. It is the extension of the mean-field Alessandro-Beatrice- Bertotti-Montorsi (ABBM) model in presence of an inertial mass m. While the ABBM model can be solved exactly, its extension to inertia exhibits complicated history dependence due to oscillations and backward motion. The characteristic scales for avalanche motion are studied from numerics and qualitative arguments. To make analytical progress, we consider two variants which coincide with the original model whenever the particle moves only forward. Using a combination of analytical and numerical methods together with simulations, we characterize the distributions of instantaneous acceleration and velocity, and compare them in these three models. We show that for large driving velocity, all three models share the same large-deviation function for positive velocities, which is obtained analytically for small and large m, as well as for m=6/25. The effect of small additional thermal and quantum fluctuations can be treated within an approximate method.

Active noise attenuation in ventilation windows.

PubMed

Huang, Huahua; Qiu, Xiaojun; Kang, Jian

2011-07-01

The feasibility of applying active noise control techniques to attenuate low frequency noise transmission through a natural ventilation window into a room is investigated analytically and experimentally. The window system is constructed by staggering the opening sashes of a spaced double glazing window to allow ventilation and natural light. An analytical model based on the modal expansion method is developed to calculate the low frequency sound field inside the window and the room and to be used in the active noise control simulations. The effectiveness of the proposed analytical model is validated by using the finite element method. The performance of the active control system for a window with different source and receiver configurations are compared, and it is found that the numerical and experimental results are in good agreement and the best result is achieved when the secondary sources are placed in the center at the bottom of the staggered window. The extra attenuation at the observation points in the optimized window system is almost equivalent to the noise reduction at the error sensor and the frequency range of effective control is up to 390 Hz in the case of a single channel active noise control system. © 2011 Acoustical Society of America

Characterization of renal biomarkers for use in clinical trials: biomarker evaluation in healthy volunteers

PubMed Central

Brott, David A; Adler, Scott H; Arani, Ramin; Lovick, Susan C; Pinches, Mark; Furlong, Stephen T

2014-01-01

Background Several preclinical urinary biomarkers have been qualified and accepted by the health authorities (US Food and Drug Administration, European Medicines Agency, and Pharmaceuticals and Medical Devices Agency) for detecting drug-induced kidney injury during preclinical toxicologic testing. Validated human assays for many of these biomarkers have become commercially available, and this study was designed to characterize some of the novel clinical renal biomarkers. The objective of this study was to evaluate clinical renal biomarkers in a typical Phase I healthy volunteer population to determine confidence intervals (pilot reference intervals), intersubject and intrasubject variability, effects of food intake, effect of sex, and vendor assay comparisons. Methods Spot urine samples from 20 male and 19 female healthy volunteers collected on multiple days were analyzed using single analyte and multiplex assays. The following analytes were measured: α-1-microglobulin, β-2-microglobulin, calbindin, clusterin, connective tissue growth factor, creatinine, cystatin C, glutathione S-transferase-α, kidney injury marker-1, microalbumin, N-acetyl-β-(D) glucosaminidase, neutrophil gelatinase-associated lipocalin, osteopontin, Tamm-Horsfall urinary glycoprotein, tissue inhibitor of metalloproteinase 1, trefoil factor 3, and vascular endothelial growth factor. Results Confidence intervals were determined from the single analyte and multiplex assays. Intersubject and intrasubject variability ranged from 38% to 299% and from 29% to 82% for biomarker concentration, and from 24% to 331% and from 10% to 67% for biomarker concentration normalized to creatinine, respectively. There was no major effect of food intake or sex. Single analyte and multiplex assays correlated with r2≥0.700 for five of six biomarkers when evaluating biomarker concentration, but for only two biomarkers when evaluating concentration normalized to creatinine. Conclusion Confidence intervals as well as intersubject and intrasubject variability were determined for novel clinical renal biomarkers/assays, which should be considered for evaluation in the next steps of the qualification process. PMID:24611000

Developments in Analytical Chemistry: Acoustically Levitated Drop Reactors for Enzyme Reaction Kinetics and Single-Walled Carbon Nanotube-Based Sensors for Detection of Toxic Organic Phosphonates

ERIC Educational Resources Information Center

Field, Christopher Ryan

2009-01-01

Developments in analytical chemistry were made using acoustically levitated small volumes of liquid to study enzyme reaction kinetics and by detecting volatile organic compounds in the gas phase using single-walled carbon nanotubes. Experience gained in engineering, electronics, automation, and software development from the design and…

Reference materials for cellular therapeutics.

PubMed

Bravery, Christopher A; French, Anna

2014-09-01

The development of cellular therapeutics (CTP) takes place over many years, and, where successful, the developer will anticipate the product to be in clinical use for decades. Successful demonstration of manufacturing and quality consistency is dependent on the use of complex analytical methods; thus, the risk of process and method drift over time is high. The use of reference materials (RM) is an established scientific principle and as such also a regulatory requirement. The various uses of RM in the context of CTP manufacturing and quality are discussed, along with why they are needed for living cell products and the analytical methods applied to them. Relatively few consensus RM exist that are suitable for even common methods used by CTP developers, such as flow cytometry. Others have also identified this need and made proposals; however, great care will be needed to ensure any consensus RM that result are fit for purpose. Such consensus RM probably will need to be applied to specific standardized methods, and the idea that a single RM can have wide applicability is challenged. Written standards, including standardized methods, together with appropriate measurement RM are probably the most appropriate way to define specific starting cell types. The characteristics of a specific CTP will to some degree deviate from those of the starting cells; consequently, a product RM remains the best solution where feasible. Each CTP developer must consider how and what types of RM should be used to ensure the reliability of their own analytical measurements. Copyright © 2014 International Society for Cellular Therapy. Published by Elsevier Inc. All rights reserved.

Approximate Single-Diode Photovoltaic Model for Efficient I-V Characteristics Estimation

PubMed Central

Ting, T. O.; Zhang, Nan; Guan, Sheng-Uei; Wong, Prudence W. H.

2013-01-01

Precise photovoltaic (PV) behavior models are normally described by nonlinear analytical equations. To solve such equations, it is necessary to use iterative procedures. Aiming to make the computation easier, this paper proposes an approximate single-diode PV model that enables high-speed predictions for the electrical characteristics of commercial PV modules. Based on the experimental data, statistical analysis is conducted to validate the approximate model. Simulation results show that the calculated current-voltage (I-V) characteristics fit the measured data with high accuracy. Furthermore, compared with the existing modeling methods, the proposed model reduces the simulation time by approximately 30% in this work. PMID:24298205

Fractional discrete-time consensus models for single- and double-summator dynamics

NASA Astrophysics Data System (ADS)

Wyrwas, Małgorzata; Mozyrska, Dorota; Girejko, Ewa

2018-04-01

The leader-following consensus problem of fractional-order multi-agent discrete-time systems is considered. In the systems, interactions between opinions are defined like in Krause and Cucker-Smale models but the memory is included by taking the fractional-order discrete-time operator on the left-hand side of the nonlinear systems. In this paper, we investigate fractional-order models of opinions for the single- and double-summator dynamics of discrete-time by analytical methods as well as by computer simulations. The necessary and sufficient conditions for the leader-following consensus are formulated by proposing a consensus control law for tracking the virtual leader.

Effect of the qubit relaxation on transport properties of microwave photons

NASA Astrophysics Data System (ADS)

Sultanov, A. N.; Greenberg, Ya. S.

2017-11-01

In this work, using the non-Hermitian Hamiltonian method, the transmission of a single photon in a one-dimensional waveguide interacting with the cavity containing an arbitrary number of photons and the two-level artificial atom is studied with allowance for the relaxation of the latter. For transport factors, analytical expressions which explicitly take into account the qubit relaxation parameter have been obtained. The form of the transmission (reflection) coefficient when there is more than one photon in the cavity qualitatively differs from the single-photon cavity and contains the manifestation of the photon blockade effect. The qubit lifetime depends on the number of photons in the cavity.

A centroid molecular dynamics study of liquid para-hydrogen and ortho-deuterium.

PubMed

Hone, Tyler D; Voth, Gregory A

2004-10-01

Centroid molecular dynamics (CMD) is applied to the study of collective and single-particle dynamics in liquid para-hydrogen at two state points and liquid ortho-deuterium at one state point. The CMD results are compared with the results of classical molecular dynamics, quantum mode coupling theory, a maximum entropy analytic continuation approach, pair-product forward- backward semiclassical dynamics, and available experimental results. The self-diffusion constants are in excellent agreement with the experimental measurements for all systems studied. Furthermore, it is shown that the method is able to adequately describe both the single-particle and collective dynamics of quantum liquids. (c) 2004 American Institute of Physics

Chirped laser dispersion spectroscopy using a directly modulated quantum cascade laser

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

Hangauer, Andreas, E-mail: hangauer@princeton.edu; Nikodem, Michal; Wysocki, Gerard, E-mail: gwysocki@princeton.edu

2013-11-04

Chirped laser dispersion spectroscopy (CLaDS) utilizing direct modulation of a quantum cascade laser (QCL) is presented. By controlling the laser bias nearly single- and dual-sideband CLaDS operation can be realized in an extremely simplified optical setup with no external optical modulators. Capability of direct single-sideband modulation is a unique feature of QCLs that exhibit a low linewidth enhancement factor. The developed analytical model shows excellent agreement with the experimental, directly modulated CLaDS spectra. This method overcomes major technical limitations of mid-infrared CLaDS systems by allowing significantly higher modulation frequencies and eliminating optical fringes introduced by external modulators.

Microdose Induced Drain Leakage Effects in Power Trench MOSFETs: Experiment and Modeling

NASA Astrophysics Data System (ADS)

Zebrev, Gennady I.; Vatuev, Alexander S.; Useinov, Rustem G.; Emeliyanov, Vladimir V.; Anashin, Vasily S.; Gorbunov, Maxim S.; Turin, Valentin O.; Yesenkov, Kirill A.

2014-08-01

We study experimentally and theoretically the micro-dose induced drain-source leakage current in the trench power MOSFETs under irradiation with high-LET heavy ions. We found experimentally that cumulative increase of leakage current occurs by means of stochastic spikes corresponding to a strike of single heavy ion into the MOSFET gate oxide. We simulate this effect with the proposed analytic model allowing to describe (including Monte Carlo methods) both the deterministic (cumulative dose) and stochastic (single event) aspects of the problem. Based on this model the survival probability assessment in space heavy ion environment with high LETs was proposed.

Highly sensitive and quantitative detection of rare pathogens through agarose droplet microfluidic emulsion PCR at the single-cell level.

PubMed

Zhu, Zhi; Zhang, Wenhua; Leng, Xuefei; Zhang, Mingxia; Guan, Zhichao; Lu, Jiangquan; Yang, Chaoyong James

2012-10-21

Genetic alternations can serve as highly specific biomarkers to distinguish fatal bacteria or cancer cells from their normal counterparts. However, these mutations normally exist in very rare amount in the presence of a large excess of non-mutated analogs. Taking the notorious pathogen E. coli O157:H7 as the target analyte, we have developed an agarose droplet-based microfluidic ePCR method for highly sensitive, specific and quantitative detection of rare pathogens in the high background of normal bacteria. Massively parallel singleplex and multiplex PCR at the single-cell level in agarose droplets have been successfully established. Moreover, we challenged the system with rare pathogen detection and realized the sensitive and quantitative analysis of a single E. coli O157:H7 cell in the high background of 100,000 excess normal K12 cells. For the first time, we demonstrated rare pathogen detection through agarose droplet microfluidic ePCR. Such a multiplex single-cell agarose droplet amplification method enables ultra-high throughput and multi-parameter genetic analysis of large population of cells at the single-cell level to uncover the stochastic variations in biological systems.

Multiplex single-molecule interaction profiling of DNA-barcoded proteins.

PubMed

Gu, Liangcai; Li, Chao; Aach, John; Hill, David E; Vidal, Marc; Church, George M

2014-11-27

In contrast with advances in massively parallel DNA sequencing, high-throughput protein analyses are often limited by ensemble measurements, individual analyte purification and hence compromised quality and cost-effectiveness. Single-molecule protein detection using optical methods is limited by the number of spectrally non-overlapping chromophores. Here we introduce a single-molecular-interaction sequencing (SMI-seq) technology for parallel protein interaction profiling leveraging single-molecule advantages. DNA barcodes are attached to proteins collectively via ribosome display or individually via enzymatic conjugation. Barcoded proteins are assayed en masse in aqueous solution and subsequently immobilized in a polyacrylamide thin film to construct a random single-molecule array, where barcoding DNAs are amplified into in situ polymerase colonies (polonies) and analysed by DNA sequencing. This method allows precise quantification of various proteins with a theoretical maximum array density of over one million polonies per square millimetre. Furthermore, protein interactions can be measured on the basis of the statistics of colocalized polonies arising from barcoding DNAs of interacting proteins. Two demanding applications, G-protein coupled receptor and antibody-binding profiling, are demonstrated. SMI-seq enables 'library versus library' screening in a one-pot assay, simultaneously interrogating molecular binding affinity and specificity.

Shell Corrections Stabilizing Superheavy Nuclei and Semi-spheroidal Atomic Clusters

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

Poenaru, Dorin N.

2008-01-24

The macroscopic-microscopic method is used to illustrate the shell effect stabilizing superheavy nuclei and to study the stability of semi-spheroidal clusters deposited on planar surfaces. The alpha decay of superheavy nuclei is calculated using three models: the analytical superasymmetric fission model; the universal curve, and the semiempirical formula taking into account the shell effects. Analytical relationships are obtained for the energy levels of the new semi-spheroidal harmonic oscillator (SSHO) single-particle model and for the surface and curvature energies of the semi-spheroidal clusters. The maximum degeneracy of the SSHO is reached at a super-deformed prolate shape for which the minimum ofmore » the liquid drop model energy is also attained.« less

Surface Analysis of Nerve Agent Degradation Products by ...

EPA Pesticide Factsheets

Report This sampling and analytical procedure was developed and applied by a single laboratory to investigate nerve agent degradation products, which may persist at a contaminated site, via surface wiping followed by analytical characterization. The performance data presented demonstrate the fitness-for-purpose regarding surface analysis in that single laboratory. Surfaces (laminate, glass, galvanized steel, vinyl tile, painted drywall and treated wood) were wiped with cotton gauze wipes, sonicated, extracted with distilled water, and filtered. Samples were analyzed with direct injection electrospray ionization liquid chromatography tandem mass spectrometry (ESI-LC/MS/MS) without derivatization. Detection limit data were generated for all analytes of interest on a laminate surface. Accuracy and precision data were generated from each surface fortified with these analytes.

Laser Ablation in situ (U-Th-Sm)/He and U-Pb Double-Dating of Apatite and Zircon: Techniques and Applications

NASA Astrophysics Data System (ADS)

McInnes, B.; Danišík, M.; Evans, N.; McDonald, B.; Becker, T.; Vermeesch, P.

2015-12-01

We present a new laser-based technique for rapid, quantitative and automated in situ microanalysis of U, Th, Sm, Pb and He for applications in geochronology, thermochronometry and geochemistry (Evans et al., 2015). This novel capability permits a detailed interrogation of the time-temperature history of rocks containing apatite, zircon and other accessory phases by providing both (U-Th-Sm)/He and U-Pb ages (+trace element analysis) on single crystals. In situ laser microanalysis offers several advantages over conventional bulk crystal methods in terms of safety, cost, productivity and spatial resolution. We developed and integrated a suite of analytical instruments including a 193 nm ArF excimer laser system (RESOlution M-50A-LR), a quadrupole ICP-MS (Agilent 7700s), an Alphachron helium mass spectrometry system and swappable flow-through and ultra-high vacuum analytical chambers. The analytical protocols include the following steps: mounting/polishing in PFA Teflon using methods similar to those adopted for fission track etching; laser He extraction and analysis using a 2 s ablation at 5 Hz and 2-3 J/cm2fluence; He pit volume measurement using atomic force microscopy, and U-Th-Sm-Pb (plus optional trace element) analysis using traditional laser ablation methods. The major analytical challenges for apatite include the low U, Th and He contents relative to zircon and the elevated common Pb content. On the other hand, apatite typically has less extreme and less complex zoning of parent isotopes (primarily U and Th). A freeware application has been developed for determining (U-Th-Sm)/He ages from the raw analytical data and Iolite software was used for U-Pb age and trace element determination. In situ double-dating has successfully replicated conventional U-Pb and (U-Th)/He age variations in xenocrystic zircon from the diamondiferous Ellendale lamproite pipe, Western Australia and increased zircon analytical throughput by a factor of 50 over conventional methods.Reference: Evans NJ, McInnes BIA, McDonald B, Becker T, Vermeesch P, Danisik M, Shelley M, Marillo-Sialer E and Patterson D. An in situ technique for (U-Th-Sm)/He and U-Pb double dating. J Analytical Atomic Spectrometry, 30, 1636 - 1645.

Benefits and Limitations of DNA Barcoding and Metabarcoding in Herbal Product Authentication

PubMed Central

Raclariu, Ancuta Cristina; Heinrich, Michael; Ichim, Mihael Cristin

2017-01-01

Abstract Introduction Herbal medicines play an important role globally in the health care sector and in industrialised countries they are often considered as an alternative to mono‐substance medicines. Current quality and authentication assessment methods rely mainly on morphology and analytical phytochemistry‐based methods detailed in pharmacopoeias. Herbal products however are often highly processed with numerous ingredients, and even if these analytical methods are accurate for quality control of specific lead or marker compounds, they are of limited suitability for the authentication of biological ingredients. Objective To review the benefits and limitations of DNA barcoding and metabarcoding in complementing current herbal product authentication. Method Recent literature relating to DNA based authentication of medicinal plants, herbal medicines and products are summarised to provide a basic understanding of how DNA barcoding and metabarcoding can be applied to this field. Results Different methods of quality control and authentication have varying resolution and usefulness along the value chain of these products. DNA barcoding can be used for authenticating products based on single herbal ingredients and DNA metabarcoding for assessment of species diversity in processed products, and both methods should be used in combination with appropriate hyphenated chemical methods for quality control. Conclusions DNA barcoding and metabarcoding have potential in the context of quality control of both well and poorly regulated supply systems. Standardisation of protocols for DNA barcoding and DNA sequence‐based identification are necessary before DNA‐based biological methods can be implemented as routine analytical approaches and approved by the competent authorities for use in regulated procedures. © 2017 The Authors. Phytochemical Analysis Published by John Wiley & Sons Ltd. PMID:28906059

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

PubMed

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

2007-12-01

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

A method for determining optimum phasing of a multiphase propulsion system for a single-stage vehicle with linearized inert weight

NASA Technical Reports Server (NTRS)

Martin, J. A.

1974-01-01

A general analytical treatment is presented of a single-stage vehicle with multiple propulsion phases. A closed-form solution for the cost and for the performance and a derivation of the optimal phasing of the propulsion are included. Linearized variations in the inert weight elements are included, and the function to be minimized can be selected. The derivation of optimal phasing results in a set of nonlinear algebraic equations for optimal fuel volumes, for which a solution method is outlined. Three specific example cases are analyzed: minimum gross lift-off weight, minimum inert weight, and a minimized general function for a two-phase vehicle. The results for the two-phase vehicle are applied to the dual-fuel rocket. Comparisons with single-fuel vehicles indicate that dual-fuel vehicles can have lower inert weight either by development of a dual-fuel engine or by parallel burning of separate engines from lift-off.

Single-cell topological RNA-Seq analysis reveals insights into cellular differentiation and development

PubMed Central

Rizvi, Abbas H.; Camara, Pablo G.; Kandror, Elena K.; Roberts, Thomas J.; Schieren, Ira; Maniatis, Tom; Rabadan, Raul

2017-01-01

Transcriptional programs control cellular lineage commitment and differentiation during development. Understanding cell fate has been advanced by studying single-cell RNA-seq, but is limited by the assumptions of current analytic methods regarding the structure of data. We present single-cell topological data analysis (scTDA), an algorithm for topology-based computational analyses to study temporal, unbiased transcriptional regulation. Compared to other methods, scTDA is a non-linear, model-independent, unsupervised statistical framework that can characterize transient cellular states. We applied scTDA to the analysis of murine embryonic stem cell (mESC) differentiation in vitro in response to inducers of motor neuron differentiation. scTDA resolved asynchrony and continuity in cellular identity over time, and identified four transient states (pluripotent, precursor, progenitor, and fully differentiated cells) based on changes in stage-dependent combinations of transcription factors, RNA-binding proteins and long non-coding RNAs. scTDA can be applied to study asynchronous cellular responses to either developmental cues or environmental perturbations. PMID:28459448

Basic forensic identification of artificial leather for hit-and-run cases.

PubMed

Sano, Tetsuya; Suzuki, Shinichi

2009-11-20

Single fibers retrieved from a victim's garments and adhered to the suspect's automobile have frequently been used to prove the relationship between victim and suspect's automobile. Identification method for single fiber discrimination has already been conducted. But, a case was encountered requiring discrimination of artificial leather fragments retrieved from the victim's bag and fused fibers from the bumper of the suspect's automobile. In this report, basic studies were conducted on identification of artificial leathers and single fibers from leather materials. Fiber morphology was observed using scanning electron microscopy (SEM), color of these leather sheets was evaluated by microspectrophotometry (MSP), the leather components were measured by infrared micro spectrometry (micro-FT-IR) and the inorganic contents were ascertained by micro-X-ray fluorescence spectrometry (micro-XRF). These two methods contribute to other analytical methods too, in the case of utilized single fiber analytical methods. The combination of these techniques showed high potential of discrimination ability in forensic examinations of these artificial leather samples. In regard with smooth surface artificial leather sheet samples, a total of 182 sheets were obtained, including 177 colored sheets directly from 10 of 24 manufacturers in Japan, and five of them were purchased at retail circulation products. Nine samples of suede-like artificial leather were obtained, 6 of them were supplied from 2 manufacturers and 3 sheets were purchased as retailing product. Single fibers from the smooth surface artificial leather sheets showed characteristic for surface markings, and XRF could effectively discriminate between these sheets. The combination of results of micro-FT-IR, color evaluation by MSP and the contained inorganic elements by XRF enabled to discriminate about 92% of 15,576 pairs comparison. Five smooth surface samples form retailing products were discriminated by their chemical composition into four categories, and in addition color information to this result, they were clearly distinguished. Suede-like artificial leather sheets showed characteristic extra-fine fibers on their surface by the observation of SEM imaging, providing high discriminating ability, in regard with suede-like artificial leather sheets were divided into three categories by micro-FT-IR, and the combination of these results and color evaluation information, it was possible to discriminate all the nine suede-like artificial leather sheets examined.

Developing a 'personalome' for precision medicine: emerging methods that compute interpretable effect sizes from single-subject transcriptomes.

PubMed

Vitali, Francesca; Li, Qike; Schissler, A Grant; Berghout, Joanne; Kenost, Colleen; Lussier, Yves A

2017-12-18

The development of computational methods capable of analyzing -omics data at the individual level is critical for the success of precision medicine. Although unprecedented opportunities now exist to gather data on an individual's -omics profile ('personalome'), interpreting and extracting meaningful information from single-subject -omics remain underdeveloped, particularly for quantitative non-sequence measurements, including complete transcriptome or proteome expression and metabolite abundance. Conventional bioinformatics approaches have largely been designed for making population-level inferences about 'average' disease processes; thus, they may not adequately capture and describe individual variability. Novel approaches intended to exploit a variety of -omics data are required for identifying individualized signals for meaningful interpretation. In this review-intended for biomedical researchers, computational biologists and bioinformaticians-we survey emerging computational and translational informatics methods capable of constructing a single subject's 'personalome' for predicting clinical outcomes or therapeutic responses, with an emphasis on methods that provide interpretable readouts. (i) the single-subject analytics of the transcriptome shows the greatest development to date and, (ii) the methods were all validated in simulations, cross-validations or independent retrospective data sets. This survey uncovers a growing field that offers numerous opportunities for the development of novel validation methods and opens the door for future studies focusing on the interpretation of comprehensive 'personalomes' through the integration of multiple -omics, providing valuable insights into individual patient outcomes and treatments. © The Author 2017. Published by Oxford University Press.

Piezoelectric sensors based on molecular imprinted polymers for detection of low molecular mass analytes.

PubMed

Uludağ, Yildiz; Piletsky, Sergey A; Turner, Anthony P F; Cooper, Matthew A

2007-11-01

Biomimetic recognition elements employed for the detection of analytes are commonly based on proteinaceous affibodies, immunoglobulins, single-chain and single-domain antibody fragments or aptamers. The alternative supra-molecular approach using a molecularly imprinted polymer now has proven utility in numerous applications ranging from liquid chromatography to bioassays. Despite inherent advantages compared with biochemical/biological recognition (which include robustness, storage endurance and lower costs) there are few contributions that describe quantitative analytical applications of molecularly imprinted polymers for relevant small molecular mass compounds in real-world samples. There is, however, significant literature describing the use of low-power, portable piezoelectric transducers to detect analytes in environmental monitoring and other application areas. Here we review the combination of molecularly imprinted polymers as recognition elements with piezoelectric biosensors for quantitative detection of small molecules. Analytes are classified by type and sample matrix presentation and various molecularly imprinted polymer synthetic fabrication strategies are also reviewed.

Analytic theory of alternate multilayer gratings operating in single-order regime.

PubMed

Yang, Xiaowei; Kozhevnikov, Igor V; Huang, Qiushi; Wang, Hongchang; Hand, Matthew; Sawhney, Kawal; Wang, Zhanshan

2017-07-10

Using the coupled wave approach (CWA), we introduce the analytical theory for alternate multilayer grating (AMG) operating in the single-order regime, in which only one diffraction order is excited. Differing from previous study analogizing AMG to crystals, we conclude that symmetrical structure, or equal thickness of the two multilayer materials, is not the optimal design for AMG and may result in significant reduction in diffraction efficiency. The peculiarities of AMG compared with other multilayer gratings are analyzed. An influence of multilayer structure materials on diffraction efficiency is considered. The validity conditions of analytical theory are also discussed.

High-performance liquid chromatographic method for guanylhydrazone compounds.

PubMed

Cerami, C; Zhang, X; Ulrich, P; Bianchi, M; Tracey, K J; Berger, B J

1996-01-12

A high-performance liquid chromatographic method has been developed for a series of aromatic guanylhydrazones that have demonstrated therapeutic potential as anti-inflammatory agents. The compounds were separated using octadecyl or diisopropyloctyl reversed-phase columns, with an acetonitrile gradient in water containing heptane sulfonate, tetramethylammonium chloride, and phosphoric acid. The method was used to reliably quantify levels of analyte as low as 785 ng/ml, and the detector response was linear to at least 50 micrograms/ml using a 100 microliters injection volume. The assay system was used to determine the basic pharmacokinetics of a lead compound, CNI-1493, from serum concentrations following a single intravenous injection in rats.

Opportunities for bead-based multiplex assays in veterinary diagnostic laboratories

USDA-ARS?s Scientific Manuscript database

Bead based multiplex assays (BBMA) also referred to as Luminex, MultiAnalyte Profiling or cytometric bead array (CBA) assays, are applicable for high throughput, simultaneous detection of multiple analytes in solution (from several, up to 50-500 analytes within a single, small sample volume). Curren...

Multi-residue method for the analysis of 85 current-use and legacy pesticides in bed and suspended sediments

USGS Publications Warehouse

Smalling, K.L.; Kuivila, K.M.

2008-01-01

A multi-residue method was developed for the simultaneous determination of 85 current-use and legacy organochlorine pesticides in a single sediment sample. After microwave-assisted extraction, clean-up of samples was optimized using gel permeation chromatography and either stacked carbon and alumina solid-phase extraction cartridges or a deactivated Florisil column. Analytes were determined by gas chromatography with ion-trap mass spectrometry and electron capture detection. Method detection limits ranged from 0.6 to 8.9 ??g/kg dry weight. Bed and suspended sediments from a variety of locations were analyzed to validate the method and 29 pesticides, including at least 1 from every class, were detected.

Optics-Integrated Microfluidic Platforms for Biomolecular Analyses

PubMed Central

Bates, Kathleen E.; Lu, Hang

2016-01-01

Compared with conventional optical methods, optics implemented on microfluidic chips provide small, and often much cheaper ways to interrogate biological systems from the level of single molecules up to small model organisms. The optical probing of single molecules has been used to investigate the mechanical properties of individual biological molecules; however, multiplexing of these measurements through microfluidics and nanofluidics confers many analytical advantages. Optics-integrated microfluidic systems can significantly simplify sample processing and allow a more user-friendly experience; alignments of on-chip optical components are predetermined during fabrication and many purely optical techniques are passively controlled. Furthermore, sample loss from complicated preparation and fluid transfer steps can be virtually eliminated, a particularly important attribute for biological molecules at very low concentrations. Excellent fluid handling and high surface area/volume ratios also contribute to faster detection times for low abundance molecules in small sample volumes. Although integration of optical systems with classical microfluidic analysis techniques has been limited, microfluidics offers a ready platform for interrogation of biophysical properties. By exploiting the ease with which fluids and particles can be precisely and dynamically controlled in microfluidic devices, optical sensors capable of unique imaging modes, single molecule manipulation, and detection of minute changes in concentration of an analyte are possible. PMID:27119629

Accurate analytic solution of chemical master equations for gene regulation networks in a single cell

NASA Astrophysics Data System (ADS)

Huang, Guan-Rong; Saakian, David B.; Hu, Chin-Kun

2018-01-01

Studying gene regulation networks in a single cell is an important, interesting, and hot research topic of molecular biology. Such process can be described by chemical master equations (CMEs). We propose a Hamilton-Jacobi equation method with finite-size corrections to solve such CMEs accurately at the intermediate region of switching, where switching rate is comparable to fast protein production rate. We applied this approach to a model of self-regulating proteins [H. Ge et al., Phys. Rev. Lett. 114, 078101 (2015), 10.1103/PhysRevLett.114.078101] and found that as a parameter related to inducer concentration increases the probability of protein production changes from unimodal to bimodal, then to unimodal, consistent with phenotype switching observed in a single cell.

Local orientational mobility in regular hyperbranched polymers.

PubMed

Dolgushev, Maxim; Markelov, Denis A; Fürstenberg, Florian; Guérin, Thomas

2016-07-01

We study the dynamics of local bond orientation in regular hyperbranched polymers modeled by Vicsek fractals. The local dynamics is investigated through the temporal autocorrelation functions of single bonds and the corresponding relaxation forms of the complex dielectric susceptibility. We show that the dynamic behavior of single segments depends on their remoteness from the periphery rather than on the size of the whole macromolecule. Remarkably, the dynamics of the core segments (which are most remote from the periphery) shows a scaling behavior that differs from the dynamics obtained after structural average. We analyze the most relevant processes of single segment motion and provide an analytic approximation for the corresponding relaxation times. Furthermore, we describe an iterative method to calculate the orientational dynamics in the case of very large macromolecular sizes.

Determination of fusarium mycotoxins in wheat, maize and animal feed using on-line clean-up with high resolution mass spectrometry.

PubMed

Ates, E; Mittendorf, K; Stroka, J; Senyuva, H

2013-01-01

An automated method involving on-line clean-up and analytical separation in a single run using TurboFlow™ reversed phase liquid chromatography coupled to a high resolution mass spectrometer has been developed for the simultaneous determination of deoxynivalenol, T2 toxin, HT2 toxin, zearalenone and fumonisins B1 and B2 in maize, wheat and animal feed. Detection was performed in full scan mode at a resolution of R = 100,000 full width at half maximum with high energy collision cell dissociation for the determination of fragment ions with a mass accuracy below 5 ppm. The extract from homogenised samples, after blending with a 0.1% aqueous mixture of 0.1% formic acid/acetonitrile (43:57) for 45 min, was injected directly onto the TurboFlow™ (TLX) column for automated on-line clean-up followed by analytical separation and accurate mass detection. The TurboFlow™ column enabled specific binding of target mycotoxins, whereas higher molecular weight compounds, like fats, proteins and other interferences with different chemical properties, were removed to waste. Single laboratory method validation was performed by spiking blank materials with mycotoxin standards. The recovery and repeatability was determined by spiking at three concentration levels (50, 100 and 200% of legislative limits) with six replicates. Average recovery, relative standard deviation and intermediate precision values were 71 to 120%, 1 to 19% and 4 to 19%, respectively. The method accuracy was confirmed with certified reference materials and participation in proficiency testing.

(Bio)Sensing Using Nanoparticle Arrays: On the Effect of Analyte Transport on Sensitivity.

PubMed

Lynn, N Scott; Homola, Jiří

2016-12-20

There has recently been an extensive amount of work regarding the development of optical, electrical, and mechanical (bio)sensors employing planar arrays of surface-bound nanoparticles. The sensor output for these systems is dependent on the rate at which analyte is transported to, and interacts with, each nanoparticle in the array. There has so far been little discussion on the relationship between the design parameters of an array and the interplay of convection, diffusion, and reaction. Moreover, current methods providing such information require extensive computational simulation. Here we demonstrate that the rate of analyte transport to a nanoparticle array can be quantified analytically. We show that such rates are bound by both the rate to a single NP and that to a planar surface (having equivalent size as the array), with the specific rate determined by the fill fraction: the ratio between the total surface area used for biomolecular capture with respect to the entire sensing area. We characterize analyte transport to arrays with respect to changes in numerous parameters relevant to experiment, including variation of the nanoparticle shape and size, packing density, flow conditions, and analyte diffusivity. We also explore how analyte capture is dependent on the kinetic parameters related to an affinity-based biosensor, and furthermore, we classify the conditions under which the array might be diffusion- or reaction-limited. The results obtained herein are applicable toward the design and optimization of all (bio)sensors based on nanoparticle arrays.

The contribution of lot-to-lot variation to the measurement uncertainty of an LC-MS-based multi-mycotoxin assay.

PubMed

Stadler, David; Sulyok, Michael; Schuhmacher, Rainer; Berthiller, Franz; Krska, Rudolf

2018-05-01

Multi-mycotoxin determination by LC-MS is commonly based on external solvent-based or matrix-matched calibration and, if necessary, the correction for the method bias. In everyday practice, the method bias (expressed as apparent recovery RA), which may be caused by losses during the recovery process and/or signal/suppression enhancement, is evaluated by replicate analysis of a single spiked lot of a matrix. However, RA may vary for different lots of the same matrix, i.e., lot-to-lot variation, which can result in a higher relative expanded measurement uncertainty (U r ). We applied a straightforward procedure for the calculation of U r from the within-laboratory reproducibility, which is also called intermediate precision, and the uncertainty of RA (u r,RA ). To estimate the contribution of the lot-to-lot variation to U r , the measurement results of one replicate of seven different lots of figs and maize and seven replicates of a single lot of these matrices, respectively, were used to calculate U r . The lot-to-lot variation was contributing to u r,RA and thus to U r for the majority of the 66 evaluated analytes in both figs and maize. The major contributions of the lot-to-lot variation to u r,RA were differences in analyte recovery in figs and relative matrix effects in maize. U r was estimated from long-term participation in proficiency test schemes with 58%. Provided proper validation, a fit-for-purpose U r of 50% was proposed for measurement results obtained by an LC-MS-based multi-mycotoxin assay, independent of the concentration of the analytes.

Quantification of 4 antidepressants and a metabolite by LC-MS for therapeutic drug monitoring.

PubMed

Choong, Eva; Rudaz, Serge; Kottelat, Astrid; Haldemann, Sophie; Guillarme, Davy; Veuthey, Jean-Luc; Eap, Chin B

2011-06-01

A liquid chromatography method coupled to mass spectrometry was developed for the quantification of bupropion, its metabolite hydroxy-bupropion, moclobemide, reboxetine and trazodone in human plasma. The validation of the analytical procedure was assessed according to Société Française des Sciences et Techniques Pharmaceutiques and the latest Food and Drug Administration guidelines. The sample preparation was performed with 0.5 mL of plasma extracted on a cation-exchange solid phase 96-well plate. The separation was achieved in 14 min on a C18 XBridge column (2.1 mm×100 mm, 3.5 μm) using a 50 mM ammonium acetate pH 9/acetonitrile mobile phase in gradient mode. The compounds of interest were analysed in the single ion monitoring mode on a single quadrupole mass spectrometer working in positive electrospray ionisation mode. Two ions were selected per molecule to increase the number of identification points and to avoid as much as possible any false positives. Since selectivity is always a critical point for routine therapeutic drug monitoring, more than sixty common comedications for the psychiatric population were tested. For each analyte, the analytical procedure was validated to cover the common range of concentrations measured in plasma samples: 1-400 ng/mL for reboxetine and bupropion, 2-2000 ng/mL for hydroxy-bupropion, moclobemide, and trazodone. For all investigated compounds, reliable performance in terms of accuracy, precision, trueness, recovery, selectivity and stability was obtained. One year after its implementation in a routine process, this method demonstrated a high robustness with accurate values over the wide concentration range commonly observed among a psychiatric population. Copyright © 2011 Elsevier B.V. All rights reserved.

Initialization and Simulation of Three-Dimensional Aircraft Wake Vortices

NASA Technical Reports Server (NTRS)

Ash, Robert L.; Zheng, Z. C.

1997-01-01

This paper studies the effects of axial velocity profiles on vortex decay, in order to properly initialize and simulate three-dimensional wake vortex flow. Analytical relationships are obtained based on a single vortex model and computational simulations are performed for a rather practical vortex wake, which show that the single vortex analytical relations can still be applicable at certain streamwise sections of three-dimensional wake vortices.

In situ single-atom array synthesis using dynamic holographic optical tweezers

PubMed Central

Kim, Hyosub; Lee, Woojun; Lee, Han-gyeol; Jo, Hanlae; Song, Yunheung; Ahn, Jaewook

2016-01-01

Establishing a reliable method to form scalable neutral-atom platforms is an essential cornerstone for quantum computation, quantum simulation and quantum many-body physics. Here we demonstrate a real-time transport of single atoms using holographic microtraps controlled by a liquid-crystal spatial light modulator. For this, an analytical design approach to flicker-free microtrap movement is devised and cold rubidium atoms are simultaneously rearranged with 2N motional degrees of freedom, representing unprecedented space controllability. We also accomplish an in situ feedback control for single-atom rearrangements with the high success rate of 99% for up to 10 μm translation. We hope this proof-of-principle demonstration of high-fidelity atom-array preparations will be useful for deterministic loading of N single atoms, especially on arbitrary lattice locations, and also for real-time qubit shuttling in high-dimensional quantum computing architectures. PMID:27796372

Rapid structural analysis of nanomaterials in aqueous solutions

NASA Astrophysics Data System (ADS)

Ryuzaki, Sou; Tsutsui, Makusu; He, Yuhui; Yokota, Kazumichi; Arima, Akihide; Morikawa, Takanori; Taniguchi, Masateru; Kawai, Tomoji

2017-04-01

Rapid structural analysis of nanoscale matter in a liquid environment represents innovative technologies that reveal the identities and functions of biologically important molecules. However, there is currently no method with high spatio-temporal resolution that can scan individual particles in solutions to gain structural information. Here we report the development of a nanopore platform realizing quantitative structural analysis for suspended nanomaterials in solutions with a high z-axis and xy-plane spatial resolution of 35.8 ± 1.1 and 12 nm, respectively. We used a low thickness-to-diameter aspect ratio pore architecture for achieving cross sectional areas of analyte (i.e. tomograms). Combining this with multiphysics simulation methods to translate ionic current data into tomograms, we demonstrated rapid structural analysis of single polystyrene (Pst) beads and single dumbbell-like Pst beads in aqueous solutions.

[Determination of five naphthaquinones in Arnebia euchroma by quantitative analysis multi-components with single-marker].

PubMed

Zhao, Wen-Wen; Wu, Zhi-Min; Wu, Xia; Zhao, Hai-Yu; Chen, Xiao-Qing

2016-10-01

This study is to determine five naphthaquinones (acetylshikonin, β-acetoxyisovalerylalkannin, isobutylshikonin, β,β'-dimethylacrylalkannin,α-methyl-n-butylshikonin） by quantitative analysis of multi-components with a single marker (QAMS). β,β'-Dimethylacrylalkannin was selected as the internal reference substance, and the relative correlation factors (RCFs) of acetylshikonin, β-acetoxyisovalerylalkannin, isobutylshikonin and α-methyl-n-butylshikonin were calculated. Then the ruggedness of relative correction factors was tested on different instruments and columns. Meanwhile, 16 batches of Arnebia euchroma were analyzed by external standard method (ESM) and QAMS, respectively. The peaks were identifited by LC-MS. The ruggedness of relative correction factors was good. And the analytical results calculated by ESM and QAMS showed no difference. The quantitative method established was feasible and suitable for the quality evaluation of A. euchroma. Copyright© by the Chinese Pharmaceutical Association.

Single-Laboratory Validation for the Determination of Flavonoids in Hawthorn Leaves and Finished Products by LC-UV.

PubMed

Mudge, Elizabeth M; Liu, Ying; Lund, Jensen A; Brown, Paula N

2016-11-01

Suitably validated analytical methods that can be used to quantify medicinally active phytochemicals in natural health products are required by regulators, manufacturers, and consumers. Hawthorn ( Crataegus ) is a botanical ingredient in natural health products used for the treatment of cardiovascular disorders. A method for the quantitation of vitexin-2″- O - rhamnoside, vitexin, isovitexin, rutin, and hyperoside in hawthorn leaf and flower raw materials and finished products was optimized and validated according to AOAC International guidelines. A two-level partial factorial study was used to guide the optimization of the sample preparation. The optimal conditions were found to be a 60-minute extraction using 50 : 48 : 2 methanol : water : acetic acid followed by a 25-minute separation using a reversed-phased liquid chromatography column with ultraviolet absorbance detection. The single-laboratory validation study evaluated method selectivity, accuracy, repeatability, linearity, limit of quantitation, and limit of detection. Individual flavonoid content ranged from 0.05 mg/g to 17.5 mg/g in solid dosage forms and raw materials. Repeatability ranged from 0.7 to 11.7 % relative standard deviation corresponding to HorRat ranges from 0.2 to 1.6. Calibration curves for each flavonoid were linear within the analytical ranges with correlation coefficients greater than 99.9 %. Herein is the first report of a validated method that is fit for the purpose of quantifying five major phytochemical marker compounds in both raw materials and finished products made from North American ( Crataegus douglasii ) and European ( Crataegus monogyna and Crataegus laevigata) hawthorn species. The method includes optimized extraction of samples without a prolonged drying process and reduced liquid chromatography separation time. Georg Thieme Verlag KG Stuttgart · New York.

Development and validation of a UPLC-MS method for the determination of galantamine in guinea pig plasma and its application to a pre-clinical bioavailability study of novel galantamine formulations.

PubMed

Wang, Jiang; Pavurala, Naresh; Xu, Xiaoming; Krishnaiah, Yellela S R; Faustino, Patrick J

2018-05-04

To evaluate the bioavailability and pharmacokinetic profiles of two novel galantamine formulations as medical countermeasure products, an ultra-performance liquid chromatography-single quadrupole mass spectrometry (UPLC-MS) method was developed and validated for quantifying galantamine in guinea pig plasma using solid-phase extraction with a mixed mode strong cation exchange reversed-phase cartridge. Chromatographic separation was achieved on a Waters Acquity UPLC BEH C 18 column maintained at 40°C. The mobile phases were solution A, acetonitrile-water, 5:95 (v/v) and solution B, acetonitrile-water 90:10 (v/v), both containing 2 mM ammonium formate and 0.2% formic acid. The mobile phase was delivered utilizing a 3 min gradient program start with 95%A-5%B at a flow rate of 0.6 mL/min. The analyte and internal standard, galantamine-d3, were detected by selected ion monitoring mode on a Waters 3100 single quadrupole mass spectrometer with positive electrospray ionization. The method was validated according to the US Food and Drug Administration bioanalytical guidance. The method was selective and was linear over the analytical range of 2-2000 ng/mL. Accuracy and precision were acceptable with intra- and inter-day accuracies between 96.8 and 101% and precisions (RSD) <4.88%. The method was successfully implemented to measure galantamine plasma levels in a series of pre-clinical bioavailability studies for the evaluation of novel galantamine formulations. Published 2018. This article is a U.S. Government work and is in the public domain in the USA.

Liquid chromatographic tandem mass spectrometric assay for quantification of 97/78 and its metabolite 97/63: a promising trioxane antimalarial in monkey plasma.

PubMed

Singh, R P; Sabarinath, S; Gautam, N; Gupta, R C; Singh, S K

2009-07-15

The present manuscript describes development and validation of LC-MS/MS assay for the simultaneous quantitation of 97/78 and its active in-vivo metabolite 97/63 in monkey plasma using alpha-arteether as internal standard (IS). The method involves a single step protein precipitation using acetonitrile as extraction method. The analytes were separated on a Columbus C(18) (50 mm x 2 mm i.d., 5 microm particle size) column by isocratic elution with acetonitrile:ammonium acetate buffer (pH 4, 10 mM) (80:20 v/v) at a flow rate of 0.45 mL/min, and analyzed by mass spectrometry in multiple reaction-monitoring (MRM) positive ion mode. The chromatographic run time was 4.0 min and the weighted (1/x(2)) calibration curves were linear over a range of 1.56-200 ng/mL. The method was linear for both the analytes with correlation coefficients >0.995. The intra-day and inter-day accuracy (% bias) and precisions (% RSD) of the assay were less than 6.27%. Both analytes were stable after three freeze-thaw cycles (% deviation <8.2) and also for 30 days in plasma (% deviation <6.7). The absolute recoveries of 97/78, 97/63 and internal standard (IS), from spiked plasma samples were >90%. The validated assay method, described here, was successfully applied to the pharmacokinetic study of 97/78 and its active in-vivo metabolite 97/63 in Rhesus monkeys.

Carbon nanohorn sensitized electrochemical immunosensor for rapid detection of microcystin-LR.

PubMed

Zhang, Jing; Lei, Jianping; Xu, Chuanlai; Ding, Lin; Ju, Huangxian

2010-02-01

A sensitive electrochemical immunosensor was proposed by functionalizing single-walled carbon nanohorns (SWNHs) with analyte for microcystin-LR (MC-LR) detection. The functionalization of SWNHs was performed by covalently binding MC-LR to the abundant carboxylic groups on the cone-shaped tips of SWNHs in the presence of linkage reagents and characterized with Raman spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscopy, and a transmission electron micrograph. Compared with single-walled carbon nanotubes, SWNHs as immobilization matrixes showed a better sensitizing effect. Using home-prepared horseradish peroxidase-labeled MC-LR antibody for the competitive immunoassay, under optimal conditions, the immunosensor exhibited a wide linear response to MC-LR ranging from 0.05 to 20 microg/L with a detection limit of 0.03 microg/L at a signal-to-noise of 3. This method showed good accuracy, acceptable precision, and reproducibility. The assay results of MC-LR in polluted water were in a good agreement with the reference values. The proposed strategy provided a biocompatible immobilization and sensitized recognition platform for analytes as small antigens and possessed promising application in food and environmental monitoring.

PACS—Realization of an adaptive concept using pressure actuated cellular structures

NASA Astrophysics Data System (ADS)

Gramüller, B.; Boblenz, J.; Hühne, C.

2014-10-01

A biologically inspired concept is investigated which can be utilized to develop energy efficient, lightweight and applicational flexible adaptive structures. Building a real life morphing unit is an ambitious task as the numerous works in the particular field show. Summarizing fundamental demands and barriers regarding shape changing structures, the basic challenges of designing morphing structures are listed. The concept of Pressure Actuated Cellular Structures (PACS) is arranged within the recent morphing activities and it is shown that it complies with the underlying demands. Systematically divided into energy-related and structural subcomponents the working principle is illuminated and relationships between basic design parameters are expressed. The analytical background describing the physical mechanisms of PACS is presented in concentrated manner. This work focuses on the procedure of dimensioning, realizing and experimental testing of a single cell and a single row cantilever made of PACS. The experimental outcomes as well as the results from the FEM computations are used for evaluating the analytical methods. The functionality of the basic principle is thus validated and open issues are determined pointing the way ahead.

Computer program for analysis of high speed, single row, angular contact, spherical roller bearing, SASHBEAN. Volume 2: Mathematical formulation and analysis

NASA Technical Reports Server (NTRS)

Aggarwal, Arun K.

1993-01-01

Spherical roller bearings have typically been used in applications with speeds limited to about 5000 rpm and loads limited for operation at less than about 0.25 million DN. However, spherical roller bearings are now being designed for high load and high speed applications including aerospace applications. A computer program, SASHBEAN, was developed to provide an analytical tool to design, analyze, and predict the performance of high speed, single row, angular contact (including zero contact angle), spherical roller bearings. The material presented is the mathematical formulation and analytical methods used to develop computer program SASHBEAN. For a given set of operating conditions, the program calculates the bearings ring deflections (axial and radial), roller deflections, contact areas stresses, depth and magnitude of maximum shear stresses, axial thrust, rolling element and cage rotational speeds, lubrication parameters, fatigue lives, and rates of heat generation. Centrifugal forces and gyroscopic moments are fully considered. The program is also capable of performing steady-state and time-transient thermal analyses of the bearing system.

N-of-1-pathways MixEnrich: advancing precision medicine via single-subject analysis in discovering dynamic changes of transcriptomes.

PubMed

Li, Qike; Schissler, A Grant; Gardeux, Vincent; Achour, Ikbel; Kenost, Colleen; Berghout, Joanne; Li, Haiquan; Zhang, Hao Helen; Lussier, Yves A

2017-05-24

Transcriptome analytic tools are commonly used across patient cohorts to develop drugs and predict clinical outcomes. However, as precision medicine pursues more accurate and individualized treatment decisions, these methods are not designed to address single-patient transcriptome analyses. We previously developed and validated the N-of-1-pathways framework using two methods, Wilcoxon and Mahalanobis Distance (MD), for personal transcriptome analysis derived from a pair of samples of a single patient. Although, both methods uncover concordantly dysregulated pathways, they are not designed to detect dysregulated pathways with up- and down-regulated genes (bidirectional dysregulation) that are ubiquitous in biological systems. We developed N-of-1-pathways MixEnrich, a mixture model followed by a gene set enrichment test, to uncover bidirectional and concordantly dysregulated pathways one patient at a time. We assess its accuracy in a comprehensive simulation study and in a RNA-Seq data analysis of head and neck squamous cell carcinomas (HNSCCs). In presence of bidirectionally dysregulated genes in the pathway or in presence of high background noise, MixEnrich substantially outperforms previous single-subject transcriptome analysis methods, both in the simulation study and the HNSCCs data analysis (ROC Curves; higher true positive rates; lower false positive rates). Bidirectional and concordant dysregulated pathways uncovered by MixEnrich in each patient largely overlapped with the quasi-gold standard compared to other single-subject and cohort-based transcriptome analyses. The greater performance of MixEnrich presents an advantage over previous methods to meet the promise of providing accurate personal transcriptome analysis to support precision medicine at point of care.

Benefits and Limitations of DNA Barcoding and Metabarcoding in Herbal Product Authentication.

PubMed

Raclariu, Ancuta Cristina; Heinrich, Michael; Ichim, Mihael Cristin; de Boer, Hugo

2018-03-01

Herbal medicines play an important role globally in the health care sector and in industrialised countries they are often considered as an alternative to mono-substance medicines. Current quality and authentication assessment methods rely mainly on morphology and analytical phytochemistry-based methods detailed in pharmacopoeias. Herbal products however are often highly processed with numerous ingredients, and even if these analytical methods are accurate for quality control of specific lead or marker compounds, they are of limited suitability for the authentication of biological ingredients. To review the benefits and limitations of DNA barcoding and metabarcoding in complementing current herbal product authentication. Recent literature relating to DNA based authentication of medicinal plants, herbal medicines and products are summarised to provide a basic understanding of how DNA barcoding and metabarcoding can be applied to this field. Different methods of quality control and authentication have varying resolution and usefulness along the value chain of these products. DNA barcoding can be used for authenticating products based on single herbal ingredients and DNA metabarcoding for assessment of species diversity in processed products, and both methods should be used in combination with appropriate hyphenated chemical methods for quality control. DNA barcoding and metabarcoding have potential in the context of quality control of both well and poorly regulated supply systems. Standardisation of protocols for DNA barcoding and DNA sequence-based identification are necessary before DNA-based biological methods can be implemented as routine analytical approaches and approved by the competent authorities for use in regulated procedures. © 2017 The Authors. Phytochemical Analysis Published by John Wiley & Sons Ltd. © 2017 The Authors. Phytochemical Analysis Published by John Wiley & Sons Ltd.

Development of a highly sensitive methodology for quantitative determination of fexofenadine in a microdose study by multiple injection method using ultra-high performance liquid chromatography with tandem mass spectrometry.

PubMed

Tanaka, Yukari; Yoshikawa, Yutaka; Yasui, Hiroyuki

2012-01-01

An ultra high-sensitivity method for quantifying fexofenadine concentration in rat plasma samples by multiple injection method (MIM) was developed for a microdose study. In this study, MIM involved continuous injections of multiple samples containing the single compound into a column of the ultra-HPLC (UHPLC) system, and then, temporary trapping of the analyte at the column head. This was followed by elution of the compound from the column and detection by mass spectrometer. Fexofenadine, used as a model compound in this study, was extracted from the plasma samples by a protein precipitation method. Chromatographic separation was achieved on a reversed-phase C18 column by using a gradient method with 0.1% formic acid and 0.1% formic acid in acetonitrile as the mobile phase. The analyte was quantified in the positive-ion electrospray ionization mode using selected reaction monitoring. In this study, the analytical time per fexofenadine sample was approximately 2 min according to the UHPLC system. The method exhibited the linear dynamic ranges of 5-5000 pg/mL for fexofenadine in rat plasma. The intra-day precisions were from 3.2 to 8.7% and the accuracy range was 95.2-99.3%. The inter-day precisions and accuracies ranged from 3.5 to 8.4% and from 98.6 to 102.6%, respectively. The validated MIM was successfully applied to a microdose study in the rats that received oral administration of 100 µg/kg fexofenadine. We suggest that this method might be beneficial for the quantification of fexofenadine concentrations in a microdose clinical study.

Analytical Method Validation of High-Performance Liquid Chromatography and Stability-Indicating Study of Medroxyprogesterone Acetate Intravaginal Sponges

PubMed Central

Batrawi, Nidal; Wahdan, Shorouq; Abualhasan, Murad

2017-01-01

Medroxyprogesterone acetate is widely used in veterinary medicine as intravaginal dosage for the synchronization of breeding cycle in ewes and goats. The main goal of this study was to develop reverse-phase high-performance liquid chromatography method for the quantification of medroxyprogesterone acetate in veterinary vaginal sponges. A single high-performance liquid chromatography/UV isocratic run was used for the analytical assay of the active ingredient medroxyprogesterone. The chromatographic system consisted of a reverse-phase C18 column as the stationary phase and a mixture of 60% acetonitrile and 40% potassium dihydrogen phosphate buffer as the mobile phase; the pH was adjusted to 5.6. The method was validated according to the International Council for Harmonisation (ICH) guidelines. Forced degradation studies were also performed to evaluate the stability-indicating properties and specificity of the method. Medroxyprogesterone was eluted at 5.9 minutes. The linearity of the method was confirmed in the range of 0.0576 to 0.1134 mg/mL (R2 > 0.999). The limit of quantification was shown to be 3.9 µg/mL. Precision and accuracy ranges were found to be %RSD <0.2 and 98% to 102%, respectively. Medroxyprogesterone capacity factor value of 2.1, tailing factor value of 1.03, and resolution value of 3.9 were obtained in accordance with ICH guidelines. Based on the obtained results, a rapid, precise, accurate, sensitive, and cost-effective analysis procedure was proposed for quantitative determination of medroxyprogesterone in vaginal sponges. This analytical method is the only available method to analyse medroxyprogesterone in veterinary intravaginal dosage form. PMID:28469407

Satellite attitude motion models for capture and retrieval investigations

NASA Technical Reports Server (NTRS)

Cochran, John E., Jr.; Lahr, Brian S.

1986-01-01

The primary purpose of this research is to provide mathematical models which may be used in the investigation of various aspects of the remote capture and retrieval of uncontrolled satellites. Emphasis has been placed on analytical models; however, to verify analytical solutions, numerical integration must be used. Also, for satellites of certain types, numerical integration may be the only practical or perhaps the only possible method of solution. First, to provide a basis for analytical and numerical work, uncontrolled satellites were categorized using criteria based on: (1) orbital motions, (2) external angular momenta, (3) internal angular momenta, (4) physical characteristics, and (5) the stability of their equilibrium states. Several analytical solutions for the attitude motions of satellite models were compiled, checked, corrected in some minor respects and their short-term prediction capabilities were investigated. Single-rigid-body, dual-spin and multi-rotor configurations are treated. To verify the analytical models and to see how the true motion of a satellite which is acted upon by environmental torques differs from its corresponding torque-free motion, a numerical simulation code was developed. This code contains a relatively general satellite model and models for gravity-gradient and aerodynamic torques. The spacecraft physical model for the code and the equations of motion are given. The two environmental torque models are described.

Green aspects, developments and perspectives of liquid phase microextraction techniques.

PubMed

Spietelun, Agata; Marcinkowski, Łukasz; de la Guardia, Miguel; Namieśnik, Jacek

2014-02-01

Determination of analytes at trace levels in complex samples (e.g. biological or contaminated water or soils) are often required for the environmental assessment and monitoring as well as for scientific research in the field of environmental pollution. A limited number of analytical techniques are sensitive enough for the direct determination of trace components in samples and, because of that, a preliminary step of the analyte isolation/enrichment prior to analysis is required in many cases. In this work the newest trends and innovations in liquid phase microextraction, like: single-drop microextraction (SDME), hollow fiber liquid-phase microextraction (HF-LPME), and dispersive liquid-liquid microextraction (DLLME) have been discussed, including their critical evaluation and possible application in analytical practice. The described modifications of extraction techniques deal with system miniaturization and/or automation, the use of ultrasound and physical agitation, and electrochemical methods. Particular attention was given to pro-ecological aspects therefore the possible use of novel, non-toxic extracting agents, inter alia, ionic liquids, coacervates, surfactant solutions and reverse micelles in the liquid phase microextraction techniques has been evaluated in depth. Also, new methodological solutions and the related instruments and devices for the efficient liquid phase micoextraction of analytes, which have found application at the stage of procedure prior to chromatographic determination, are presented. © 2013 Published by Elsevier B.V.

Strategies for Dealing with Missing Data in Clinical Trials: From Design to Analysis

PubMed Central

Dziura, James D.; Post, Lori A.; Zhao, Qing; Fu, Zhixuan; Peduzzi, Peter

2013-01-01

Randomized clinical trials are the gold standard for evaluating interventions as randomized assignment equalizes known and unknown characteristics between intervention groups. However, when participants miss visits, the ability to conduct an intent-to-treat analysis and draw conclusions about a causal link is compromised. As guidance to those performing clinical trials, this review is a non-technical overview of the consequences of missing data and a prescription for its treatment beyond the typical analytic approaches to the entire research process. Examples of bias from incorrect analysis with missing data and discussion of the advantages/disadvantages of analytic methods are given. As no single analysis is definitive when missing data occurs, strategies for its prevention throughout the course of a trial are presented. We aim to convey an appreciation for how missing data influences results and an understanding of the need for careful consideration of missing data during the design, planning, conduct, and analytic stages. PMID:24058309

Development and analytical performance evaluation of FREND-SAA and FREND-Hp

NASA Astrophysics Data System (ADS)

Choi, Eunha; Seong, Jihyun; Lee, Seiyoung; Han, Sunmi

2017-07-01

The FREND System is a portable cartridge reader, quantifying analytes by measuring laser-induced fluorescence in a single-use reagent cartridge. The objective of this study was to evaluate FREND-SAA and FREND-Hp assays. The FREND-SAA and Hp assays were standardized to the WHO and IFCC reference materials. Analytical performance studies of Precision, Linearity, Limits of Detections, Interferences, and Method Comparisons for both assays were performed according to the CLSI guidelines. Both assays demonstrated acceptable imprecision of %CV in three different levels of samples. The linearity of the assays was found to be acceptable (SAA 5 150 mg/L, Hp 30 400 mg/dL). The detection limits were 3.8 mg/L (SAA) and 10.2 mg/dL (Hp). No significant interference and no significant deviation from linearity was found in the both comparison studies. In conclusion, NanoEnTek's FREND-SAA and Hp assays represent rapid, accurate and convenient means to quantify SAA and Hp in human serum on FREND system.

Simultaneous determination of nitroimidazoles, benzimidazoles, and chloramphenicol components in bovine milk by ultra-high performance liquid chromatography-tandem mass spectrometry.

PubMed

Wang, Yuanyuan; Li, Xiaowei; Zhang, Zhiwen; Ding, Shuangyang; Jiang, Haiyang; Li, Jiancheng; Shen, Jianzhong; Xia, Xi

2016-02-01

A sensitive, confirmatory ultra-high performance liquid chromatography-tandem mass spectrometric method was developed and validated to detect 23 veterinary drugs and metabolites (nitroimidazoles, benzimidazoles, and chloramphenicol components) in bovine milk. Compounds of interest were sequentially extracted from milk with acetonitrile and basified acetonitrile using sodium chloride to induce liquid-liquid partition. The extract was purified on a mixed mode solid-phase extraction cartridge. Using rapid polarity switching in electrospray ionization, a single injection was capable of detecting both positively and negatively charged analytes in a 9 min chromatography run time. Recoveries based on matrix-matched calibrations and isotope labeled internal standards for milk ranged from 51.7% to 101.8%. The detection limits and quantitation limits of the analytical method were found to be within the range of 2-20 ng/kg and 5-50 ng/kg, respectively. The recommended method is simple, specific, and reliable for the routine monitoring of nitroimidazoles, benzimidazoles, and chloramphenicol components in bovine milk samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

A stochastic Markov chain approach for tennis: Monte Carlo simulation and modeling

NASA Astrophysics Data System (ADS)

Aslam, Kamran

This dissertation describes the computational formulation of probability density functions (pdfs) that facilitate head-to-head match simulations in tennis along with ranking systems developed from their use. A background on the statistical method used to develop the pdfs , the Monte Carlo method, and the resulting rankings are included along with a discussion on ranking methods currently being used both in professional sports and in other applications. Using an analytical theory developed by Newton and Keller in [34] that defines a tennis player's probability of winning a game, set, match and single elimination tournament, a computational simulation has been developed in Matlab that allows further modeling not previously possible with the analytical theory alone. Such experimentation consists of the exploration of non-iid effects, considers the concept the varying importance of points in a match and allows an unlimited number of matches to be simulated between unlikely opponents. The results of these studies have provided pdfs that accurately model an individual tennis player's ability along with a realistic, fair and mathematically sound platform for ranking them.

Determination of supplemental feeding needs for astaxanthin and canthaxanthin in salmonids by supramolecular solvent-based microextraction and liquid chromatography-UV/VIS spectroscopy.

PubMed

Caballo, Carmen; Costi, Esther María; Sicilia, María Dolores; Rubio, Soledad

2012-09-15

Development of simple and rapid analytical methods for predicting supplemental feeding requirements in aquaculture is a need to reduce production costs. In this article, a supramolecular solvent (SUPRAS) made up of decanoic acid (DeA) assemblies was proposed to simplify sample treatment in the total and individual determination of carotenoids (red-pink pigments) in farmed salmonids. The analytes were quantitatively extracted in a single step that spends a few minutes using a small volume of SUPRAS (i.e. 800 μL) and directly determined in extracts without the interference from fats or other matrix components. The methods based on the combination of microextraction with SUPRAS and photometry or HPLC-UV/VIS spectroscopy were developed for the determination of total and individual carotenoids, respectively. The applicability of the methods was demonstrated by analysing non-fortified and fortified samples of farmed Atlantic salmons and rainbow trouts. Recoveries obtained by photometry and HPLC-UV/VIS spectroscopy were within the intervals 98-104% and 94-106%, respectively. Copyright © 2012 Elsevier Ltd. All rights reserved.

Effect of processing on recovery and variability associated with immunochemical analytical methods for multiple allergens in a single matrix: sugar cookies.

PubMed

Khuda, Sefat; Slate, Andrew; Pereira, Marion; Al-Taher, Fadwa; Jackson, Lauren; Diaz-Amigo, Carmen; Bigley, Elmer C; Whitaker, Thomas; Williams, Kristina M

2012-05-02

Among the major food allergies, peanut, egg, and milk are the most common. The immunochemical detection of food allergens depends on various factors, such as the food matrix and processing method, which can affect allergen conformation and extractability. This study aimed to (1) develop matrix-specific incurred reference materials for allergen testing, (2) determine whether multiple allergens in the same model food can be simultaneously detected, and (3) establish the effect of processing on reference material stability and allergen detection. Defatted peanut flour, whole egg powder, and spray-dried milk were added to cookie dough at seven incurred levels before baking. Allergens were measured using five commercial enzyme-linked immunosorbent assay (ELISA) kits. All kits showed decreased recovery of all allergens after baking. Analytical coefficients of variation for most kits increased with baking time, but decreased with incurred allergen level. Thus, food processing negatively affects the recovery and variability of peanut, egg, and milk detection in a sugar cookie matrix when using immunochemical methods.

Rapid screening of drugs of abuse and their metabolites by gas chromatography/mass spectrometry: application to urinalysis.

PubMed

Strano-Rossi, Sabina; Molaioni, Francesco; Rossi, Francesca; Botrè, Francesco

2005-01-01

This paper describes a rapid gas chromatographic/mass spectrometric (GC/MS) screening method for the detection of drugs of abuse and/or their metabolites in urine. Synthetic stimulants, opiates, cocaine metabolites, cannabinoids--and specifically the acid metabolite of tetrahydrocannabinol (THC-COOH)--can be simultaneously extracted by a single liquid/liquid separation step, at alkaline pH, and assayed as trimethylsilyl derivatives by GC/MS in SIM (selected ion monitoring) mode. All the analytes show a good linearity (R2 > 0.99 for most of the considered substances) in the range 25-1000 ng/mL, with a good reproducibility of both the retention times (CV% <0.7) and the relative abundances of the characteristic diagnostic ions (CV% <13). The limit of detection (LOD) of the method is 25 ng/mL of target compound in human urine for most of the substances investigated, 3 ng/mL for THC-COOH, and 10 ng/mL for norbuprenorphine. Validation of the method allows its application to different fields of forensic analytical toxicology, including antidoping analysis.

The analytic structure of conformal blocks and the generalized Wilson-Fisher fixed points

DOE PAGES

Gliozzi, Ferdinando; Guerrieri, Andrea L.; Petkou, Anastasios C.; ...

2017-04-11

Here, we describe in detail the method used in our previous work arXiv:1611.10344 to study the Wilson-Fisher critical points nearby generalized free CFTs, exploiting the analytic structure of conformal blocks as functions of the conformal dimension of the exchanged operator. Our method is equivalent to the mechanism of conformal multiplet recombination set up by null states. We also compute, to the first non-trivial order in the ε-expansion, the anomalous dimensions and the OPE coefficients of infinite classes of scalar local operators using just CFT data. We study single-scalar and O(N)-invariant theories, as well as theories with multiple deformations. When availablemore » we agree with older results, but we also produce a wealth of new ones. Furthermore, unitarity and crossing symmetry are not used in our approach and we are able to apply our method to non-unitary theories as well. Some implications of our results for the study of the non-unitary theories containing partially conserved higher-spin currents are briefly mentioned.« less

Dynamic leaching and fractionation of trace elements from environmental solids exploiting a novel circulating-flow platform.

PubMed

Mori, Masanobu; Nakano, Koji; Sasaki, Masaya; Shinozaki, Haruka; Suzuki, Shiho; Okawara, Chitose; Miró, Manuel; Itabashi, Hideyuki

2016-02-01

A dynamic flow-through microcolumn extraction system based on extractant re-circulation is herein proposed as a novel analytical approach for simplification of bioaccessibility tests of trace elements in sediments. On-line metal leaching is undertaken in the format of all injection (AI) analysis, which is a sequel of flow injection analysis, but involving extraction under steady-state conditions. The minimum circulation times and flow rates required to determine the maximum bioaccessible pools of target metals (viz., Cu, Zn, Cd, and Pb) from lake and river sediment samples were estimated using Tessier's sequential extraction scheme and an acid single extraction test. The on-line AIA method was successfully validated by mass balance studies of CRM and real sediment samples. Tessier's test in on-line AI format demonstrated to be carried out by one third of extraction time (6h against more than 17 h by the conventional method), with better analytical precision (<9.2% against >15% by the conventional method) and significant decrease in blank readouts as compared with the manual batch counterpart. Copyright © 2015 Elsevier B.V. All rights reserved.

NOTE: Solving the ECG forward problem by means of a meshless finite element method

NASA Astrophysics Data System (ADS)

Li, Z. S.; Zhu, S. A.; He, Bin

2007-07-01

The conventional numerical computational techniques such as the finite element method (FEM) and the boundary element method (BEM) require laborious and time-consuming model meshing. The new meshless FEM only uses the boundary description and the node distribution and no meshing of the model is required. This paper presents the fundamentals and implementation of meshless FEM and the meshless FEM method is adapted to solve the electrocardiography (ECG) forward problem. The method is evaluated on a single-layer torso model, in which the analytical solution exists, and tested in a realistic geometry homogeneous torso model, with satisfactory results being obtained. The present results suggest that the meshless FEM may provide an alternative for ECG forward solutions.

Methods for Synthesizing Findings on Moderation Effects Across Multiple Randomized Trials

PubMed Central

Brown, C Hendricks; Sloboda, Zili; Faggiano, Fabrizio; Teasdale, Brent; Keller, Ferdinand; Burkhart, Gregor; Vigna-Taglianti, Federica; Howe, George; Masyn, Katherine; Wang, Wei; Muthén, Bengt; Stephens, Peggy; Grey, Scott; Perrino, Tatiana

2011-01-01

This paper presents new methods for synthesizing results from subgroup and moderation analyses across different randomized trials. We demonstrate that such a synthesis generally results in additional power to detect significant moderation findings above what one would find in a single trial. Three general methods for conducting synthesis analyses are discussed, with two methods, integrative data analysis, and parallel analyses, sharing a large advantage over traditional methods available in meta-analysis. We present a broad class of analytic models to examine moderation effects across trials that can be used to assess their overall effect and explain sources of heterogeneity, and present ways to disentangle differences across trials due to individual differences, contextual level differences, intervention, and trial design. PMID:21360061

Methods for synthesizing findings on moderation effects across multiple randomized trials.

PubMed

Brown, C Hendricks; Sloboda, Zili; Faggiano, Fabrizio; Teasdale, Brent; Keller, Ferdinand; Burkhart, Gregor; Vigna-Taglianti, Federica; Howe, George; Masyn, Katherine; Wang, Wei; Muthén, Bengt; Stephens, Peggy; Grey, Scott; Perrino, Tatiana

2013-04-01

This paper presents new methods for synthesizing results from subgroup and moderation analyses across different randomized trials. We demonstrate that such a synthesis generally results in additional power to detect significant moderation findings above what one would find in a single trial. Three general methods for conducting synthesis analyses are discussed, with two methods, integrative data analysis and parallel analyses, sharing a large advantage over traditional methods available in meta-analysis. We present a broad class of analytic models to examine moderation effects across trials that can be used to assess their overall effect and explain sources of heterogeneity, and present ways to disentangle differences across trials due to individual differences, contextual level differences, intervention, and trial design.

A multi-purpose tool for food inspection: Simultaneous determination of various classes of preservatives and biogenic amines in meat and fish products by LC-MS.

PubMed

Molognoni, Luciano; Daguer, Heitor; de Sá Ploêncio, Leandro Antunes; De Dea Lindner, Juliano

2018-02-01

This paper describes an innovative fast and multipurpose method for the chemical inspection of meat and fish products by liquid chromatography-tandem mass spectrometry. Solid-liquid extraction and low temperature partitioning were applied to 17 analytes, which included large bacteriocins (3.5kDa) and small molecules (organic acids, heterocyclic compounds, polyene macrolides, alkyl esters of the p-hydroxybenzoic acid, aromatic, and aliphatic biogenic amines and polyamines). Chromatographic separation was achieved in 10min, using stationary phase of di-isopropyl-3-aminopropyl silane bound to hydroxylated silica. Method validation was in accordance to Commission Decision 657/2002/CE. Linear ranges were among 1.25-10.0mgkg -1 (natamycin and parabens), 2.50-10.0mgkg -1 (sorbate and nisin), 25.0-200mgkg -1 (biogenic amines, hexamethylenetetramine, benzoic and lactic acids), and 50.0-400mgkg -1 (citric acid). Expanded measurement uncertainty (U) was estimated by single laboratory validation combined to modeling in two calculation approaches: internal (U = 5%) and external standardization (U = 24%). Method applicability was checked on 89 real samples among raw, cooked, dry fermented and cured products, yielding acceptable recoveries. Many regulatory issues were revealed, corroborating the need for enhancement of the current analytical methods. This simple execution method dispenses the use of additional procedures of extraction and, therefore, reduces costs over time. It is suitable for routine analysis as a screening or confirmatory tool for both qualitative and quantitative results, replacing many time consuming analytical procedures. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

Analytical quality by design: a tool for regulatory flexibility and robust analytics.

PubMed

Peraman, Ramalingam; Bhadraya, Kalva; Padmanabha Reddy, Yiragamreddy

2015-01-01

Very recently, Food and Drug Administration (FDA) has approved a few new drug applications (NDA) with regulatory flexibility for quality by design (QbD) based analytical approach. The concept of QbD applied to analytical method development is known now as AQbD (analytical quality by design). It allows the analytical method for movement within method operable design region (MODR). Unlike current methods, analytical method developed using analytical quality by design (AQbD) approach reduces the number of out-of-trend (OOT) results and out-of-specification (OOS) results due to the robustness of the method within the region. It is a current trend among pharmaceutical industry to implement analytical quality by design (AQbD) in method development process as a part of risk management, pharmaceutical development, and pharmaceutical quality system (ICH Q10). Owing to the lack explanatory reviews, this paper has been communicated to discuss different views of analytical scientists about implementation of AQbD in pharmaceutical quality system and also to correlate with product quality by design and pharmaceutical analytical technology (PAT).

Analytical Quality by Design: A Tool for Regulatory Flexibility and Robust Analytics

PubMed Central

Bhadraya, Kalva; Padmanabha Reddy, Yiragamreddy

2015-01-01

Very recently, Food and Drug Administration (FDA) has approved a few new drug applications (NDA) with regulatory flexibility for quality by design (QbD) based analytical approach. The concept of QbD applied to analytical method development is known now as AQbD (analytical quality by design). It allows the analytical method for movement within method operable design region (MODR). Unlike current methods, analytical method developed using analytical quality by design (AQbD) approach reduces the number of out-of-trend (OOT) results and out-of-specification (OOS) results due to the robustness of the method within the region. It is a current trend among pharmaceutical industry to implement analytical quality by design (AQbD) in method development process as a part of risk management, pharmaceutical development, and pharmaceutical quality system (ICH Q10). Owing to the lack explanatory reviews, this paper has been communicated to discuss different views of analytical scientists about implementation of AQbD in pharmaceutical quality system and also to correlate with product quality by design and pharmaceutical analytical technology (PAT). PMID:25722723

Cavity radiation model for solar central receivers

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

Lipps, F.W.

1981-01-01

The Energy Laboratory of the University of Houston has developed a computer simulation program called CREAM (i.e., Cavity Radiations Exchange Analysis Model) for application to the solar central receiver system. The zone generating capability of CREAM has been used in several solar re-powering studies. CREAM contains a geometric configuration factor generator based on Nusselt's method. A formulation of Nusselt's method provides support for the FORTRAN subroutine NUSSELT. Numerical results from NUSSELT are compared to analytic values and values from Sparrow's method. Sparrow's method is based on a double contour integral and its reduction to a single integral which is approximatedmore » by Guassian methods. Nusselt's method is adequate for the intended engineering applications, but Sparrow's method is found to be an order of magnitude more efficient in many situations.« less

Energy thresholds of discrete breathers in thermal equilibrium and relaxation processes.

PubMed

Ming, Yi; Ling, Dong-Bo; Li, Hui-Min; Ding, Ze-Jun

2017-06-01

So far, only the energy thresholds of single discrete breathers in nonlinear Hamiltonian systems have been analytically obtained. In this work, the energy thresholds of discrete breathers in thermal equilibrium and the energy thresholds of long-lived discrete breathers which can remain after a long time relaxation are analytically estimated for nonlinear chains. These energy thresholds are size dependent. The energy thresholds of discrete breathers in thermal equilibrium are the same as the previous analytical results for single discrete breathers. The energy thresholds of long-lived discrete breathers in relaxation processes are different from the previous results for single discrete breathers but agree well with the published numerical results known to us. Because real systems are either in thermal equilibrium or in relaxation processes, the obtained results could be important for experimental detection of discrete breathers.

Synthesis-identification integration: One-pot hydrothermal preparation of fluorescent nitrogen-doped carbon nanodots for differentiating nucleobases with the aid of multivariate chemometrics analysis.

PubMed

Zhuang, Qianfen; Cao, Wei; Ni, Yongnian; Wang, Yong

2018-08-01

Most of the conventional multidimensional differential sensors currently need at least two-step fabrication, namely synthesis of probe(s) and identification of multiple analytes by mixing of analytes with probe(s), and were conducted using multiple sensing elements or several devices. In the study, we chose five different nucleobases (adenine, cytosine, guanine, thymine, and uracil) as model analytes, and found that under hydrothermal conditions, sodium citrate could react directly with various nucleobases to yield different nitrogen-doped carbon nanodots (CDs). The CDs synthesized from different nucleobases exhibited different fluorescent properties, leading to their respective characteristic fluorescence spectra. Hence, we combined the fluorescence spectra of the CDs with advanced chemometrics like principle component analysis (PCA), hierarchical cluster analysis (HCA), K-nearest neighbor (KNN) and soft independent modeling of class analogy (SIMCA), to present a conceptually novel "synthesis-identification integration" strategy to construct a multidimensional differential sensor for nucleobase discrimination. Single-wavelength excitation fluorescence spectral data, single-wavelength emission fluorescence spectral data, and fluorescence Excitation-Emission Matrices (EEMs) of the CDs were respectively used as input data of the differential sensor. The results showed that the discrimination ability of the multidimensional differential sensor with EEM data set as input data was superior to those with single-wavelength excitation/emission fluorescence data set, suggesting that increasing the number of the data input could improve the discrimination power. Two supervised pattern recognition methods, namely KNN and SIMCA, correctly identified the five nucleobases with a classification accuracy of 100%. The proposed "synthesis-identification integration" strategy together with a multidimensional array of experimental data holds great promise in the construction of differential sensors. Copyright © 2018 Elsevier B.V. All rights reserved.

Method for measuring lead concentrations in blood

DOEpatents

Nogar, Nicholas S.

2001-01-01

Method for measuring lead concentrations in blood. The present invention includes the use of resonant laser ablation to analyze .ltoreq.1 .mu.L (or equivalent mass) samples of blood for lead content. A typical finger prick, for example, yields about 10 .mu.L. Solid samples may also readily be analyzed by resonant laser ablation. The sample is placed on a lead-free, electrically conducting substrate and irradiated with a single, focused laser beam which simultaneously vaporizes, atomizes, and resonantly ionizes an analyte of interest in a sample. The ions are then sorted, collected and detected using a mass spectrometer.

Selection of reference standard during method development using the analytical hierarchy process.

PubMed

Sun, Wan-yang; Tong, Ling; Li, Dong-xiang; Huang, Jing-yi; Zhou, Shui-ping; Sun, Henry; Bi, Kai-shun

2015-03-25

Reference standard is critical for ensuring reliable and accurate method performance. One important issue is how to select the ideal one from the alternatives. Unlike the optimization of parameters, the criteria of the reference standard are always immeasurable. The aim of this paper is to recommend a quantitative approach for the selection of reference standard during method development based on the analytical hierarchy process (AHP) as a decision-making tool. Six alternative single reference standards were assessed in quantitative analysis of six phenolic acids from Salvia Miltiorrhiza and its preparations by using ultra-performance liquid chromatography. The AHP model simultaneously considered six criteria related to reference standard characteristics and method performance, containing feasibility to obtain, abundance in samples, chemical stability, accuracy, precision and robustness. The priority of each alternative was calculated using standard AHP analysis method. The results showed that protocatechuic aldehyde is the ideal reference standard, and rosmarinic acid is about 79.8% ability as the second choice. The determination results successfully verified the evaluation ability of this model. The AHP allowed us comprehensive considering the benefits and risks of the alternatives. It was an effective and practical tool for optimization of reference standards during method development. Copyright © 2015 Elsevier B.V. All rights reserved.

Temperature dependence of single-event burnout in n-channel power MOSFET's

NASA Astrophysics Data System (ADS)

Johnson, G. H.; Schrimpf, R. D.; Galloway, K. F.; Koga, R.

1994-03-01

The temperature dependence of single-event burnout (SEB) in n-channel power metal-oxide-semiconductor field effect transistors (MOSFET's) is investigated experimentally and analytically. Experimental data are presented which indicate that the SEB susceptibility of the power MOSFET decreases with increasing temperature. A previously reported analytical model that describes the SEB mechanism is updated to include temperature variations. This model is shown to agree with the experimental trends.

Microchip-Based Single-Cell Functional Proteomics for Biomedical Applications

PubMed Central

Lu, Yao; Yang, Liu; Wei, Wei; Shi, Qihui

2017-01-01

Cellular heterogeneity has been widely recognized but only recently have single cell tools become available that allow characterizing heterogeneity at the genomic and proteomic levels. We review the technological advances in microchip-based toolkits for single-cell functional proteomics. Each of these tools has distinct advantages and limitations, and a few have advanced toward being applied to address biological or clinical problems that fail to be addressed by traditional population-based methods. High-throughput single-cell proteomic assays generate high-dimensional data sets that contain new information and thus require developing new analytical framework to extract new biology. In this review article, we highlight a few biological and clinical applications in which the microchip-based single-cell proteomic tools provide unique advantages. The examples include resolving functional heterogeneity and dynamics of immune cells, dissecting cell-cell interaction by creating well-contolled on-chip microenvironment, capturing high-resolution snapshots of immune system functions in patients for better immunotherapy and elucidating phosphoprotein signaling networks in cancer cells for guiding effective molecularly targeted therapies. PMID:28280819

Analytical Method for the Detection of Residual Active Ingredients Found in Neutralized Suspensions of Antimicrobial Products.

PubMed

Kamel, Alaa; Tomasino, Stephen F

2017-03-01

An analytical method for determining the presence and levels of residual active ingredients found in neutralized suspensions of phenolic and quaternary ammonium salt-based antimicrobial products was developed using solid-phase extraction in combination with LC-tandem MS. A single-laboratory validation of the method was performed at three concentration levels for the quaternary ammonium compounds (also referred to as benzalkonium chlorides or BACs) and the phenols in the presence of letheen broth neutralizer at 2.5 and 2.75 μg/mL, respectively, as well as at dilutions of 1:10 and 1:100 in those concentrations. The method's lowest LODs were 0.005 μg/g for BACs and 0.006 μg/g for phenols. The average recovery of the fortified samples for both active ingredients ranged between 80 and 124%, and RSDs were generally <20%. In a related study, the effectiveness of letheen broth with and without sodium thiosulfate was evaluated as a neutralizer for sodium hypochlorite. The results showed that letheen broth without sodium thiosulfate neutralizes chlorine concentrations up to 60 ppm, and that 200 μg sodium thiosulfate are required to neutralize a 72 ppm concentrated chlorine solution in letheen broth.

Experimental and analytical transonic flutter characteristics of a geared-elevator configuration

NASA Technical Reports Server (NTRS)

Ruhlin, C. L.; Doggett, R. V., Jr.; Gregory, R. A.

1980-01-01

The flutter model represented the aft fuselage and empennage of a proposed supersonic transport airplane and had an all movable horizontal tail with a geared elevator. It was tested mounted from a sting in the transonic dynamics tunnel. Symmetric flutter boundaries were determined experimentally at Mach numbers from 0.7 to 1.14 for a geared elevator configuration (gear ratio of 2.8 to 1.0) and an ungeared elevator configuration (gear ratio of 1.0 to 1.0). Gearing the elevator increased the experimental flutter dynamic pressures about 20 percent. Flutter calculations were made for the geared elevator configuration by using two analytical methods based on subsonic lifting surface theory. Both methods analyzed the stabilizer and elevator as a single, deforming surface, but one method also allowed the elevator to be analyzed as hinged from the stabilizer. All analyses predicted lower flutter dynamic pressures than experiment with best agreement (within 12 percent) for the hinged elevator method. Considering the model as mounted from a flexible rather than rigid sting in the analyses, had only a slight effect on the flutter results but was significant in that a sting related vibration mode was identified as a potentially flutter critical mode.

The Development and Single-Laboratory Validation of a Method for the Determination of Steroid Residues in Fish and Fish Products.

PubMed

Watson, Lynn; Potter, Ross; Murphy, Cory; Gibbs, Ryan

2015-01-01

Due to potential use in aquacultured fish products, the Canadian Food Inspection Agency has identified residue testing for steroids as a priority. These compounds are used in aquaculture primarily to direct sexual differentiation with both androgens and estrogens applied depending on the desired outcome. Published research is lacking with respect to steroid residue testing in fish; however, recent studies in other matrixes provided transferable cleanup techniques. A simple, rapid, and sensitive method was developed and validated for use in monitoring aquacultured fish products for the presence of methyltestosterone, nandrolone, epi-nandrolone, boldenone, and epi-boldenone residues. The developed method consists of solvent extraction followed by cleanup using hexane and dual cartridge SPE with analysis by ultra-HPLC-MS/MS. The method is capable of detecting and confirming steroid residue levels ranging from 0.05 to 25 ng/g in salmon and tilapia, depending on the analyte. Recoveries ranged from 88 to 130% for the analytes. Instrument repeatability was less than 13% for all compounds, while intermediate precision ranged from 5 to 25% RSD. HorRat values were within acceptable ranges.

Review of Processing and Analytical Methods for Francisella ...

EPA Pesticide Factsheets

Journal Article The etiological agent of tularemia, Francisella tularensis, is a resilient organism within the environment and can be acquired many ways (infectious aerosols and dust, contaminated food and water, infected carcasses, and arthropod bites). However, isolating F. tularensis from environmental samples can be challenging due to its nutritionally fastidious and slow-growing nature. In order to determine the current state of the science regarding available processing and analytical methods for detection and recovery of F. tularensis from water and soil matrices, a review of the literature was conducted. During the review, analysis via culture, immunoassays, and genomic identification were the most commonly found methods for F. tularensis detection within environmental samples. Other methods included combined culture and genomic analysis for rapid quantification of viable microorganisms and use of one assay to identify multiple pathogens from a single sample. Gaps in the literature that were identified during this review suggest that further work to integrate culture and genomic identification would advance our ability to detect and to assess the viability of Francisella spp. The optimization of DNA extraction, whole genome amplification with inhibition-resistant polymerases, and multiagent microarray detection would also advance biothreat detection.

7 CFR 94.303 - Analytical methods.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 3 2011-01-01 2011-01-01 false Analytical methods. 94.303 Section 94.303 Agriculture... POULTRY AND EGG PRODUCTS Processed Poultry Products § 94.303 Analytical methods. The analytical methods... latest edition of the Official Methods of Analysis of AOAC INTERNATIONAL, Suite 500, 481 North Frederick...

7 CFR 94.303 - Analytical methods.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 94.303 Section 94.303 Agriculture... POULTRY AND EGG PRODUCTS Processed Poultry Products § 94.303 Analytical methods. The analytical methods... latest edition of the Official Methods of Analysis of AOAC INTERNATIONAL, Suite 500, 481 North Frederick...

7 CFR 94.303 - Analytical methods.

Code of Federal Regulations, 2012 CFR

2012-01-01

... 7 Agriculture 3 2012-01-01 2012-01-01 false Analytical methods. 94.303 Section 94.303 Agriculture... POULTRY AND EGG PRODUCTS Processed Poultry Products § 94.303 Analytical methods. The analytical methods... latest edition of the Official Methods of Analysis of AOAC INTERNATIONAL, Suite 500, 481 North Frederick...

7 CFR 94.303 - Analytical methods.

Code of Federal Regulations, 2013 CFR

2013-01-01

... 7 Agriculture 3 2013-01-01 2013-01-01 false Analytical methods. 94.303 Section 94.303 Agriculture... POULTRY AND EGG PRODUCTS Processed Poultry Products § 94.303 Analytical methods. The analytical methods... latest edition of the Official Methods of Analysis of AOAC INTERNATIONAL, Suite 500, 481 North Frederick...

7 CFR 94.303 - Analytical methods.

Code of Federal Regulations, 2014 CFR

2014-01-01

... 7 Agriculture 3 2014-01-01 2014-01-01 false Analytical methods. 94.303 Section 94.303 Agriculture... POULTRY AND EGG PRODUCTS Processed Poultry Products § 94.303 Analytical methods. The analytical methods... latest edition of the Official Methods of Analysis of AOAC INTERNATIONAL, Suite 500, 481 North Frederick...

Stochastic chaos induced by diffusion processes with identical spectral density but different probability density functions.

PubMed

Lei, Youming; Zheng, Fan

2016-12-01

Stochastic chaos induced by diffusion processes, with identical spectral density but different probability density functions (PDFs), is investigated in selected lightly damped Hamiltonian systems. The threshold amplitude of diffusion processes for the onset of chaos is derived by using the stochastic Melnikov method together with a mean-square criterion. Two quasi-Hamiltonian systems, namely, a damped single pendulum and damped Duffing oscillator perturbed by stochastic excitations, are used as illustrative examples. Four different cases of stochastic processes are taking as the driving excitations. It is shown that in such two systems the spectral density of diffusion processes completely determines the threshold amplitude for chaos, regardless of the shape of their PDFs, Gaussian or otherwise. Furthermore, the mean top Lyapunov exponent is employed to verify analytical results. The results obtained by numerical simulations are in accordance with the analytical results. This demonstrates that the stochastic Melnikov method is effective in predicting the onset of chaos in the quasi-Hamiltonian systems.

Meta-analytic framework for sparse K-means to identify disease subtypes in multiple transcriptomic studies

PubMed Central

Huo, Zhiguang; Ding, Ying; Liu, Silvia; Oesterreich, Steffi; Tseng, George

2016-01-01

Disease phenotyping by omics data has become a popular approach that potentially can lead to better personalized treatment. Identifying disease subtypes via unsupervised machine learning is the first step towards this goal. In this paper, we extend a sparse K-means method towards a meta-analytic framework to identify novel disease subtypes when expression profiles of multiple cohorts are available. The lasso regularization and meta-analysis identify a unique set of gene features for subtype characterization. An additional pattern matching reward function guarantees consistent subtype signatures across studies. The method was evaluated by simulations and leukemia and breast cancer data sets. The identified disease subtypes from meta-analysis were characterized with improved accuracy and stability compared to single study analysis. The breast cancer model was applied to an independent METABRIC dataset and generated improved survival difference between subtypes. These results provide a basis for diagnosis and development of targeted treatments for disease subgroups. PMID:27330233

Meta-analytic framework for sparse K-means to identify disease subtypes in multiple transcriptomic studies.

PubMed

Huo, Zhiguang; Ding, Ying; Liu, Silvia; Oesterreich, Steffi; Tseng, George

Disease phenotyping by omics data has become a popular approach that potentially can lead to better personalized treatment. Identifying disease subtypes via unsupervised machine learning is the first step towards this goal. In this paper, we extend a sparse K -means method towards a meta-analytic framework to identify novel disease subtypes when expression profiles of multiple cohorts are available. The lasso regularization and meta-analysis identify a unique set of gene features for subtype characterization. An additional pattern matching reward function guarantees consistent subtype signatures across studies. The method was evaluated by simulations and leukemia and breast cancer data sets. The identified disease subtypes from meta-analysis were characterized with improved accuracy and stability compared to single study analysis. The breast cancer model was applied to an independent METABRIC dataset and generated improved survival difference between subtypes. These results provide a basis for diagnosis and development of targeted treatments for disease subgroups.

SAM Radiochemical Methods Query

EPA Pesticide Factsheets

Laboratories measuring target radiochemical analytes in environmental samples can use this online query tool to identify analytical methods in EPA's Selected Analytical Methods for Environmental Remediation and Recovery for select radiochemical analytes.

Simultaneous quantification of four metabolites of sulfur mustard in urine samples by ultra-high performance liquid chromatography-tandem mass spectrometry after solid phase extraction.

PubMed

Liu, Chang-Cai; Liu, Shi-Lei; Xi, Hai-Ling; Yu, Hui-Lan; Zhou, Shi-Kun; Huang, Gui-Lan; Liang, Long-Hui; Liu, Jing-Quan

2017-04-07

Four HD urinary metabolites including hydrolysis metabolite thiodiglycol (TDG), glutathione-derived metabolite 1,1'-sulfonylbis[2-S-(N-acetylcysteinyl)ethane] (SBSNAE), as well as the β-lyase metabolites 1,1'-sulfonylbis[2-(methylsulfinyl)ethane] (SBMSE) and 1-methylsulfinyl-2-[2-(methylthio) ethylsulfonyl]ethane (MSMTESE) are considered as important biomarkers for short-term retrospective detection of HD exposure. In this study, a single method for simultaneous quantification of the four HD metabolites in urine samples was developed using ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The four urinary metabolites were simultaneously extracted from urinary samples using a solid phase extraction (SPE) method with high extraction recoveries for all four metabolites varied in the range of 71.1-103% followed by UHPLC-MS/MS analysis. The SPE is simple and high effective only requiring 0.1mL of urinary samples and 0.5h time consuming. The problem of previous co-elution of TDG and SBSNAE in UHPLC was well solved, and complete separation of TDG, SBSNAE, SBMSE and MSMTESE from SPE-processed urine matrix was obtained to increase specificity and sensitivity. A full method validation was performed for each analyte in urine matrix. The linear range of calibration curves for the four analytes were respectively from 0.50-500ngmL -1 for TDG and SBSNAE, 0.05-500ngmL -1 for SBMSE and MSMTESE with coefficient of determination value (R 2 ) ≥0.990. The limit of detection was 0.25ngmL -1 for TDG and SBSNAE, 0.01ngmL -1 for SBMSE and MSMTESE spiked in normal urine. The intra/inter-day precision for each analyte at three QC levels had relative standard deviation (%RSD) of ≤10.3%, and the intra/inter-day accuracy ranged between 88.0-108%. This developed method allows for simultaneous and trace measurement of four HD urinary metabolites within one single determination with the lowest usage amount of urine samples over all previous methods This study provides a useful tool for early diagnosis and monitoring of HD poisoning for medical treatment with high confidence, avoiding the need for application of several analysis methods. Copyright © 2017 Elsevier B.V. All rights reserved.

Stationary and moving solitons in spin-orbit-coupled spin-1 Bose-Einstein condensates

NASA Astrophysics Data System (ADS)

Li, Yu-E.; Xue, Ju-Kui

2018-04-01

We investigate the matter-wave solitons in a spin-orbit-coupled spin-1 Bose-Einstein condensate using a multiscale perturbation method. Beginning with the one-dimensional spin-orbit-coupled threecomponent Gross-Pitaevskii equations, we derive a single nonlinear Schrödinger equation, which allows determination of the analytical soliton solutions of the system. Stationary and moving solitons in the system are derived. In particular, a parameter space for different existing soliton types is provided. It is shown that there exist only dark or bright solitons when the spin-orbit coupling is weak, with the solitons depending on the atomic interactions. However, when the spin-orbit coupling is strong, both dark and bright solitons exist, being determined by the Raman coupling. Our analytical solutions are confirmed by direct numerical simulations.

DNA-Encoded Raman-Active Anisotropic Nanoparticles for microRNA Detection.

PubMed

Qi, Lin; Xiao, Mingshu; Wang, Xiwei; Wang, Cheng; Wang, Lihua; Song, Shiping; Qu, Xiangmeng; Li, Li; Shi, Jiye; Pei, Hao

2017-09-19

The development of highly sensitive and selective methods for the detection of microRNA (miRNA) has attracted tremendous attention because of its importance in fundamental biological studies and diagnostic applications. In this work, we develop DNA-encoded Raman-active anisotropic nanoparticles modified origami paper analytical devices (oPADs) for rapid, highly sensitive, and specific miRNA detection. The Raman-active anisotropic nanoparticles were prepared using 10-mer oligo-A, -T, -C, and -G to mediate the growth of Ag cubic seeds into Ag nanoparticles (AgNPs) with different morphologies. The resulting AgNPs were further encoded with DNA probes to serve as effective surface-enhanced Raman scattering (SERS) probes. The analytical device was then fabricated on a single piece of SERS probes loaded paper-based substrate and assembled based on the principles of origami. The addition of the target analyte amplifies the Raman signals on DNA-encoded AgNPs through a target-dependent, sequence specific DNA hybridization assembly. This simple and low-cost analytical device is generic and applicable to a variety of miRNAs, allowing detection sensitivity down to 1 pM and assay time within 15 min, and therefore holds promising applications in point-of-care diagnostics.

Cytometry standards continuum

NASA Astrophysics Data System (ADS)

Leif, Robert C.; Spidlen, Josef; Brinkman, Ryan R.

2008-02-01

Introduction: The International Society for Analytical Cytology, ISAC, is developing a new combined flow and image Analytical Cytometry Standard (ACS). This standard needs to serve both the research and clinical communities. The clinical medicine and clinical research communities have a need to exchange information with hospital and other clinical information systems. Methods: 1) Prototype the standard by creating CytometryML and a RAW format for binary data. 2) Join the ISAC Data Standards Task Force. 3) Create essential project documentation. 4) Cooperate with other groups by assisting in the preparation of the DICOM Supplement 122: Specimen Module and Pathology Service-Object Pair Classes. Results: CytometryML has been created and serves as a prototype and source of experience for the following: the Analytical Cytometry Standard (ACS) 1.0, the ACS container, Minimum Information about a Flow Cytometry Experiment (MIFlowCyt), and Requirements for a Data File Standard Format to Describe Flow Cytometry and Related Analytical Cytology Data. These requirements provide a means to judge the appropriateness of design elements and to develop tests for the final ACS. The requirements include providing the information required for understanding and reproducing a cytometry experiment or clinical measurement, and for a single standard for both flow and digital microscopic cytometry. Schemas proposed by other members of the ISAC Data Standards Task Force (e.g, Gating-ML) have been independently validated and have been integrated with CytometryML. The use of netCDF as an element of the ACS container has been proposed by others and a suggested method of its use is proposed.

Characterization of titanium dioxide nanoparticles in food products: analytical methods to define nanoparticles.

PubMed

Peters, Ruud J B; van Bemmel, Greet; Herrera-Rivera, Zahira; Helsper, Hans P F G; Marvin, Hans J P; Weigel, Stefan; Tromp, Peter C; Oomen, Agnes G; Rietveld, Anton G; Bouwmeester, Hans

2014-07-09

Titanium dioxide (TiO2) is a common food additive used to enhance the white color, brightness, and sometimes flavor of a variety of food products. In this study 7 food grade TiO2 materials (E171), 24 food products, and 3 personal care products were investigated for their TiO2 content and the number-based size distribution of TiO2 particles present in these products. Three principally different methods have been used to determine the number-based size distribution of TiO2 particles: electron microscopy, asymmetric flow field-flow fractionation combined with inductively coupled mass spectrometry, and single-particle inductively coupled mass spectrometry. The results show that all E171 materials have similar size distributions with primary particle sizes in the range of 60-300 nm. Depending on the analytical method used, 10-15% of the particles in these materials had sizes below 100 nm. In 24 of the 27 foods and personal care products detectable amounts of titanium were found ranging from 0.02 to 9.0 mg TiO2/g product. The number-based size distributions for TiO2 particles in the food and personal care products showed that 5-10% of the particles in these products had sizes below 100 nm, comparable to that found in the E171 materials. Comparable size distributions were found using the three principally different analytical methods. Although the applied methods are considered state of the art, they showed practical size limits for TiO2 particles in the range of 20-50 nm, which may introduce a significant bias in the size distribution because particles <20 nm are excluded. This shows the inability of current state of the art methods to support the European Union recommendation for the definition of nanomaterials.

Simultaneous in situ derivatization and ultrasound-assisted dispersive magnetic solid phase extraction for thiamine determination by spectrofluorimetry.

PubMed

Tarigh, Ghazale Daneshvar; Shemirani, Farzaneh

2014-06-01

A simple and rapid method for the simultaneous in situ derivatizaion, preconcentration and extraction of thiamine (vitamin B1) as a model analyte was developed by a novel quantitative method, namely ultrasound-assisted dispersive magnetic solid phase extraction spectrofluorimetry (USA-DMSPE-FL) from different real samples. This method consists of sample preparation, in situ derivatization, exhaustive extraction and clean up by a single process. High extraction efficiency and in situ derivatization in a short period of time is the main advantages of this procedure. For this purpose, the reusable magnetic multi-wall carbon nanotube (MMWCNT) nanocomposite was used as an adsorbent for preconcentration and determination of thiamine. Thiamine was, simultaneously, in situ derivatized as thiochrome by potassium hexacyanoferrate (III) and adsorbed on MMWCNT in an ultrasonic water bath. The MMWCNTs were then collected using an external magnetic field. Subsequently, the extracted thiochrome was washed from the surface of the adsorbent and determined by spectrofluorimetry. The developed method, which has been analytically characterized under its optimal operating conditions, allows the detection of the analyte in the samples with method detection limits of 0.37 µg L(-1). The repeatability of the method, expressed as the relative standard deviation (RSD, n=6), varies between 2.0% and 4.8% in different real samples, while the enhancement factor is 197. The proposed procedure has been applied for the determination of thiamine in biological (serum and urine), pharmaceutical (multivitamin tablet and B complex syrup) and foodstuff samples (cereal, wheat flour, banana and honey) with the good recoveries in the range from 90% to 105%. Copyright © 2014 Elsevier B.V. All rights reserved.

Analytical study of the effects of clouds on the light produced by lightning

NASA Technical Reports Server (NTRS)

Phanord, Dieudonne D.

1990-01-01

Researchers consider the scattering of visible and infrared light due to lightning by cubic, cylindrical and spherical clouds. The researchers extend to cloud physics the work by Twersky for single and multiple scattering of electromagnetic waves. They solve the interior problem separately to obtain the bulk parameters for the scatterer equivalent to the ensemble of spherical droplets. With the interior solution or the equivalent medium approach, the multiple scattering problem is reduced to that of a single scatterer in isolation. Hence, the computing methods of Wiscombe or Bohren specialized to Mie scattering with the possibility for absorption were used to generate numerical results in short computer time.

7 CFR 98.4 - Analytical methods.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 3 2011-01-01 2011-01-01 false Analytical methods. 98.4 Section 98.4 Agriculture....4 Analytical methods. (a) The majority of analytical methods used by the USDA laboratories to perform analyses of meat, meat food products and MRE's are listed as follows: (1) Official Methods of...

7 CFR 93.4 - Analytical methods.

Code of Federal Regulations, 2013 CFR

2013-01-01

... 7 Agriculture 3 2013-01-01 2013-01-01 false Analytical methods. 93.4 Section 93.4 Agriculture... PROCESSED FRUITS AND VEGETABLES Citrus Juices and Certain Citrus Products § 93.4 Analytical methods. (a) The majority of analytical methods for citrus products are found in the Official Methods of Analysis of AOAC...

7 CFR 98.4 - Analytical methods.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 98.4 Section 98.4 Agriculture....4 Analytical methods. (a) The majority of analytical methods used by the USDA laboratories to perform analyses of meat, meat food products and MRE's are listed as follows: (1) Official Methods of...

7 CFR 93.4 - Analytical methods.

Code of Federal Regulations, 2014 CFR

2014-01-01

... 7 Agriculture 3 2014-01-01 2014-01-01 false Analytical methods. 93.4 Section 93.4 Agriculture... PROCESSED FRUITS AND VEGETABLES Citrus Juices and Certain Citrus Products § 93.4 Analytical methods. (a) The majority of analytical methods for citrus products are found in the Official Methods of Analysis of AOAC...

7 CFR 93.4 - Analytical methods.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 93.4 Section 93.4 Agriculture... PROCESSED FRUITS AND VEGETABLES Citrus Juices and Certain Citrus Products § 93.4 Analytical methods. (a) The majority of analytical methods for citrus products are found in the Official Methods of Analysis of AOAC...

7 CFR 98.4 - Analytical methods.

Code of Federal Regulations, 2012 CFR

2012-01-01

... 7 Agriculture 3 2012-01-01 2012-01-01 false Analytical methods. 98.4 Section 98.4 Agriculture....4 Analytical methods. (a) The majority of analytical methods used by the USDA laboratories to perform analyses of meat, meat food products and MRE's are listed as follows: (1) Official Methods of...

7 CFR 98.4 - Analytical methods.

Code of Federal Regulations, 2013 CFR

2013-01-01

... 7 Agriculture 3 2013-01-01 2013-01-01 false Analytical methods. 98.4 Section 98.4 Agriculture....4 Analytical methods. (a) The majority of analytical methods used by the USDA laboratories to perform analyses of meat, meat food products and MRE's are listed as follows: (1) Official Methods of...

7 CFR 98.4 - Analytical methods.

Code of Federal Regulations, 2014 CFR

2014-01-01

... 7 Agriculture 3 2014-01-01 2014-01-01 false Analytical methods. 98.4 Section 98.4 Agriculture... Analytical methods. (a) The majority of analytical methods used by the USDA laboratories to perform analyses of meat, meat food products and MREs are listed as follows: (1) Official Methods of Analysis of AOAC...

7 CFR 93.4 - Analytical methods.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 3 2011-01-01 2011-01-01 false Analytical methods. 93.4 Section 93.4 Agriculture... PROCESSED FRUITS AND VEGETABLES Citrus Juices and Certain Citrus Products § 93.4 Analytical methods. (a) The majority of analytical methods for citrus products are found in the Official Methods of Analysis of AOAC...

7 CFR 93.4 - Analytical methods.

Code of Federal Regulations, 2012 CFR

2012-01-01

... 7 Agriculture 3 2012-01-01 2012-01-01 false Analytical methods. 93.4 Section 93.4 Agriculture... PROCESSED FRUITS AND VEGETABLES Citrus Juices and Certain Citrus Products § 93.4 Analytical methods. (a) The majority of analytical methods for citrus products are found in the Official Methods of Analysis of AOAC...

Rapid analysis of the essential oil components of dried Zanthoxylum bungeanum Maxim by Fe2O3-magnetic-microsphere-assisted microwave distillation and simultaneous headspace single-drop microextraction followed by GC-MS.

PubMed

Ye, Qing

2013-06-01

In this work, microwave distillation assisted by Fe2 O3 magnetic microspheres (FMMS) and headspace single-drop microextraction were combined, and developed for determination of essential oil compounds in dried Zanthoxylum bungeanum Maxim (ZBM). The FMMS were used as microwave absorption solid medium for dry distillation of dried ZBM. Using the proposed method, isolation, extraction, and concentration of essential oil compounds can be carried out in a single step. The experimental parameters including extraction solvent, solvent volume, microwave power, irradiation time, and the amount of added FMMS, were studied. The optimal analytical conditions were: 2.0 μL decane as the extraction solvent, microwave power of 300 W, irradiation time of 2 min, and the addition of 0.1 g FMMS to ZBM. The method precision was from 4 to 10%. A total of 52 compounds were identified by the proposed method. The conventional steam distillation method was also used for the analysis of essential oil in dried ZBM and only 31 compounds were identified by steam distillation method. It was found that the proposed method is a simple, rapid, reliable, and solvent-free technique for the determination of volatile compounds in Chinese herbs. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Nonlinear Analysis of Bonded Composite Single-LAP Joints

NASA Technical Reports Server (NTRS)

Oterkus, E.; Barut, A.; Madenci, E.; Smeltzer, S. S.; Ambur, D. R.

2004-01-01

This study presents a semi-analytical solution method to analyze the geometrically nonlinear response of bonded composite single-lap joints with tapered adherend edges under uniaxial tension. The solution method provides the transverse shear and normal stresses in the adhesive and in-plane stress resultants and bending moments in the adherends. The method utilizes the principle of virtual work in conjunction with von Karman s nonlinear plate theory to model the adherends and the shear lag model to represent the kinematics of the thin adhesive layer between the adherends. Furthermore, the method accounts for the bilinear elastic material behavior of the adhesive while maintaining a linear stress-strain relationship in the adherends. In order to account for the stiffness changes due to thickness variation of the adherends along the tapered edges, their in-plane and bending stiffness matrices are varied as a function of thickness along the tapered region. The combination of these complexities results in a system of nonlinear governing equilibrium equations. This approach represents a computationally efficient alternative to finite element method. Comparisons are made with corresponding results obtained from finite-element analysis. The results confirm the validity of the solution method. The numerical results present the effects of taper angle, adherend overlap length, and the bilinear adhesive material on the stress fields in the adherends, as well as the adhesive, of a single-lap joint

Experiences with Probabilistic Analysis Applied to Controlled Systems

NASA Technical Reports Server (NTRS)

Kenny, Sean P.; Giesy, Daniel P.

2004-01-01

This paper presents a semi-analytic method for computing frequency dependent means, variances, and failure probabilities for arbitrarily large-order closed-loop dynamical systems possessing a single uncertain parameter or with multiple highly correlated uncertain parameters. The approach will be shown to not suffer from the same computational challenges associated with computing failure probabilities using conventional FORM/SORM techniques. The approach is demonstrated by computing the probabilistic frequency domain performance of an optimal feed-forward disturbance rejection scheme.

Measured effects of coolant injection on the performance of a film cooled turbine

NASA Technical Reports Server (NTRS)

Mcdonel, J. D.; Eiswerth, J. E.

1977-01-01

Tests have been conducted on a 20-inch diameter single-stage air-cooled turbine designed to evaluate the effects of film cooling air on turbine aerodynamic performance. The present paper reports the results of five test configurations, including two different cooling designs and three combinations of cooled and solid airfoils. A comparison is made of the experimental results with a previously published analytical method of evaluating coolant injection effects on turbine performance.

Micromechanics of Interfaces in High Temperature Composites

DTIC Science & Technology

1992-05-30

the development of analytical solutions to solve the eigenstrain problem of both a single fiber (treated as a cylindrical inclusion) in an elastic... eigenstrain in a half space by using Green’s functions. Green’s functions were obtained for problems of an elastic half space with a free surface or rigidly...normal to the crack surface, the eigenstrain £3, for the equivalent inclusion method is introduced to simulate the bridged crack. Specially £33 in DO

An Overview of Grain Growth Theories for Pure Single Phase Systems,

DTIC Science & Technology

1986-10-01

the fundamental causes for these distributions. This Blanc and Mocellin (1979) and Carnal and Mocellin (1981j set out to do. 7.1 Monte-Carlo Simulations...termed event B) (in 2-D) of 3-sided grains. (2) Neighbour-switching (termed event C). Blanc and Mocellin (1979) dealt with 2-D sections through...Kurtz and Carpay (1980a). 7.2 Analytical Method to Obtain fn Carnal and Mocellin (1981) obtained the distribution of grain coordination numbers in

Determination of Total Biotin by Liquid Chromatography Coupled with Immunoaffinity Column Cleanup Extraction: Multilaboratory Testing, Final Action 2016.02.

PubMed

Joseph, George; Devi, Ranjani; Marley, Elaine C; Leeman, David

2018-05-01

Single- and multilaboratory testing data have provided systematic scientific evidence that a simple, selective, accurate, and precise method can be used as a potential candidate reference method for dispute resolution in determining total biotin in all forms of infant, adult, and/or pediatric formula. Using LC coupled with immunoaffinity column cleanup extraction, the method fully meets the intended purpose and applicability statement in AOAC Standard Method Performance Requirement 2014.005. The method was applied to a cross-section of infant formula and adult nutritional matrixes, and acceptable precision and accuracy were established. The analytical platform is inexpensive, and the method can be used in almost any laboratory worldwide with basic facilities. The immunoaffinity column cleanup extraction is the key step to successful analysis.

Simultaneous quantification of five steroid saponins from Dioscorea zingiberensis C.H.Wright in rat plasma by HPLC-MS/MS and its application to the pharmacokinetic studies

PubMed Central

Zhang, Xinxin; Li, Jing; Ito, Yoichiro; Sun, Wenji

2014-01-01

A simple, reliable and sensitive high-performance liquid chromatography tandem mass spectrometry method (HPLC-MS/MS) was established for simultaneous analyses of the following 5 steroid saponins in rat plasma after the single dose administration of total steroid saponins extracted from the rhizome of Dioscorea zingiberensis C.H.Wright for the first time. Protodioscin, huangjiangsu A, zingiberensis new saponin, dioscin, and gracillin were quantified using ginsenoside Rb1 as the internal standard (IS). The plasma samples were pretreated by a single step acetonitrile-mediated protein precipitation. The chromatographic separation was performed on an Inersil ODS-3 C18 column (250 mm × 4.6 mm, 5 μm) with the mobile phase composed of acetonitrile and water containing 0.1% formic acid under a gradient elution mode at 0.2 mL min−1 using a microsplit after the eluent from the HPLC apparatus. The quantification was accomplished on a triple quadrupole tandem mass spectrometer using the multiple reaction monitoring (MRM) in the positive ionization mode. The above five analytes were stable under sample storage and preparation conditions applied in the present study. The linearity, precision, accuracy, and recoveries of the analysis confirmed the requirements for quality-control purposes. After validation, this proposed method was successfully adopted to investigate the pharmacokinetic parameters of these five analytes. PMID:25201262

Nanostructured Tip-Shaped Biosensors: Application of Six Sigma Approach for Enhanced Manufacturing.

PubMed

Kahng, Seong-Joong; Kim, Jong-Hoon; Chung, Jae-Hyun

2016-12-23

Nanostructured tip-shaped biosensors have drawn attention for biomolecule detection as they are promising for highly sensitive and specific detection of a target analyte. Using a nanostructured tip, the sensitivity is increased to identify individual molecules because of the high aspect ratio structure. Various detection methods, such as electrochemistry, fluorescence microcopy, and Raman spectroscopy, have been attempted to enhance the sensitivity and the specificity. Due to the confined path of electrons, electrochemical measurement using a nanotip enables the detection of single molecules. When an electric field is combined with capillary action and fluid flow, target molecules can be effectively concentrated onto a nanotip surface for detection. To enhance the concentration efficacy, a dendritic nanotip rather than a single tip could be used to detect target analytes, such as nanoparticles, cells, and DNA. However, reproducible fabrication with relation to specific detection remains a challenge due to the instability of a manufacturing method, resulting in inconsistent shape. In this paper, nanostructured biosensors are reviewed with our experimental results using dendritic nanotips for sequence specific detection of DNA. By the aid of the Six Sigma approach, the fabrication yield of dendritic nanotips increases from 20.0% to 86.6%. Using the nanotips, DNA is concentrated and detected in a sequence specific way with the detection limit equivalent to 1000 CFU/mL. The pros and cons of a nanotip biosensor are evaluated in conjunction with future prospects.

Propulsion System Modeling and Simulation

NASA Technical Reports Server (NTRS)

Tai, Jimmy C. M.; McClure, Erin K.; Mavris, Dimitri N.; Burg, Cecile

2002-01-01

The Aerospace Systems Design Laboratory at the School of Aerospace Engineering in Georgia Institute of Technology has developed a core competency that enables propulsion technology managers to make technology investment decisions substantiated by propulsion and airframe technology system studies. This method assists the designer/manager in selecting appropriate technology concepts while accounting for the presence of risk and uncertainty as well as interactions between disciplines. This capability is incorporated into a single design simulation system that is described in this paper. This propulsion system design environment is created with a commercially available software called iSIGHT, which is a generic computational framework, and with analysis programs for engine cycle, engine flowpath, mission, and economic analyses. iSIGHT is used to integrate these analysis tools within a single computer platform and facilitate information transfer amongst the various codes. The resulting modeling and simulation (M&S) environment in conjunction with the response surface method provides the designer/decision-maker an analytical means to examine the entire design space from either a subsystem and/or system perspective. The results of this paper will enable managers to analytically play what-if games to gain insight in to the benefits (and/or degradation) of changing engine cycle design parameters. Furthermore, the propulsion design space will be explored probabilistically to show the feasibility and viability of the propulsion system integrated with a vehicle.

Molecularly imprinted solid phase extraction for simultaneous determination of Δ9-tetrahydrocannabinol and its main metabolites by gas chromatography-mass spectrometry in urine samples.

PubMed

Nestić, Marina; Babić, Sandra; Pavlović, Dragana Mutavdžić; Sutlović, Davorka

2013-09-10

In presented paper analytical method based on solid-phase extraction using molecularly imprinted polymer and gas chromatography-mass spectrometry has been developed and validated for the confirmation of THC, THC-OH and THC-COOH in urine samples. Non-covalent molecularly imprinted polymers of THC-OH were prepared using different functional monomers (methacrylic acid, 4-vinylpyridine, and 2-hydroxyethyl methacrylate), ethylene glycol dimethacrylate as a cross-linker and 2,2'-azobis-isobutyronitrile as an initiator of radical polymerization. Analytes were extracted from urine samples using prepared polymer sorbent with highest binding selectivity and capability. Before extraction, urine samples were hydrolyzed with alkaline. Elution was performed with chloroform:ethyl acetate (60:40, v/v). Dry extracts were silylated with BSTFA+1% TMCS. Detection and quantification were performed using gas chromatography-mass spectrometry in single ion recording mode. The developed method was linear over the range from LOQ to 150 ng mL(-1) for all three analytes. For THC, THC-OH and THC-COOH LOD was 2.5, 1 and 1 ng mL(-1), and LOQ was 3, 2 and 2 ng mL(-1), respectively. The precision, accuracy, recovery and matrix effect were investigated at 5, 25 and 50 ng mL(-1). In the investigated concentration range recoveries were 71.9% for THC, 78.6% for THC-OH and 75.2% for THC-COOH. Matrix effect was not significant (<10%) for all analytes in the concentration range from 5 ng mL(-1) to 50 ng mL(-1). Extraction recovery on non-imprinted polymer was relatively high indicating high non-specific binding. Optimized and validated method was applied to 15 post-mortem urine samples. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

A Multiomics Approach to Identify Genes Associated with Childhood Asthma Risk and Morbidity.

PubMed

Forno, Erick; Wang, Ting; Yan, Qi; Brehm, John; Acosta-Perez, Edna; Colon-Semidey, Angel; Alvarez, Maria; Boutaoui, Nadia; Cloutier, Michelle M; Alcorn, John F; Canino, Glorisa; Chen, Wei; Celedón, Juan C

2017-10-01

Childhood asthma is a complex disease. In this study, we aim to identify genes associated with childhood asthma through a multiomics "vertical" approach that integrates multiple analytical steps using linear and logistic regression models. In a case-control study of childhood asthma in Puerto Ricans (n = 1,127), we used adjusted linear or logistic regression models to evaluate associations between several analytical steps of omics data, including genome-wide (GW) genotype data, GW methylation, GW expression profiling, cytokine levels, asthma-intermediate phenotypes, and asthma status. At each point, only the top genes/single-nucleotide polymorphisms/probes/cytokines were carried forward for subsequent analysis. In step 1, asthma modified the gene expression-protein level association for 1,645 genes; pathway analysis showed an enrichment of these genes in the cytokine signaling system (n = 269 genes). In steps 2-3, expression levels of 40 genes were associated with intermediate phenotypes (asthma onset age, forced expiratory volume in 1 second, exacerbations, eosinophil counts, and skin test reactivity); of those, methylation of seven genes was also associated with asthma. Of these seven candidate genes, IL5RA was also significant in analytical steps 4-8. We then measured plasma IL-5 receptor α levels, which were associated with asthma age of onset and moderate-severe exacerbations. In addition, in silico database analysis showed that several of our identified IL5RA single-nucleotide polymorphisms are associated with transcription factors related to asthma and atopy. This approach integrates several analytical steps and is able to identify biologically relevant asthma-related genes, such as IL5RA. It differs from other methods that rely on complex statistical models with various assumptions.

Analytical results for a conditional phase shift between single-photon pulses in a nonlocal nonlinear medium

NASA Astrophysics Data System (ADS)

Viswanathan, Balakrishnan; Gea-Banacloche, Julio

2017-04-01

We analyze a recent scheme proposed by Xia et al. to induce a conditional phase shift between two single-photon pulses by having them propagate at different speeds through a nonlinear medium with a nonlocal response. We have obtained an analytical solution for the case they considered, which supports their claim that a π phase shift with unit fidelity is possible in principle. We discuss the conditions that have to be met and the challenges and opportunities that this might present to the realization of a single-photon conditional phase gate.

Controlling the angular radiation of single emitters using dielectric patch nanoantennas

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

Yang, Yuanqing; Li, Qiang; Qiu, Min, E-mail: minqiu@zju.edu.cn

2015-07-20

Dielectric nanoantennas have generated much interest in recent years owing to their low loss and optically induced electric and magnetic resonances. In this paper, we investigate the coupling between a single emitter and dielectric patch nanoantennas. For the coupled system involving non-spherical structures, analytical Mie theory is no longer applicable. A semi-analytical model is proposed instead to interpret the coupling mechanism and the radiation characteristics of the system. Based on the presented model, we demonstrate that the angular emission of the single emitter can be not only enhanced but also rotated using the dielectric patch nanoantennas.

40 CFR 161.180 - Enforcement analytical method.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 25 2012-07-01 2012-07-01 false Enforcement analytical method. 161.180... DATA REQUIREMENTS FOR REGISTRATION OF ANTIMICROBIAL PESTICIDES Product Chemistry Data Requirements § 161.180 Enforcement analytical method. An analytical method suitable for enforcement purposes must be...

Nonlinear Analysis of Bonded Composite Tubular Lap Joints

NASA Technical Reports Server (NTRS)

Oterkus, E.; Madenci, E.; Smeltzer, S. S., III; Ambur, D. R.

2005-01-01

The present study describes a semi-analytical solution method for predicting the geometrically nonlinear response of a bonded composite tubular single-lap joint subjected to general loading conditions. The transverse shear and normal stresses in the adhesive as well as membrane stress resultants and bending moments in the adherends are determined using this method. The method utilizes the principle of virtual work in conjunction with nonlinear thin-shell theory to model the adherends and a cylindrical shear lag model to represent the kinematics of the thin adhesive layer between the adherends. The kinematic boundary conditions are imposed by employing the Lagrange multiplier method. In the solution procedure, the displacement components for the tubular joint are approximated in terms of non-periodic and periodic B-Spline functions in the longitudinal and circumferential directions, respectively. The approach presented herein represents a rapid-solution alternative to the finite element method. The solution method was validated by comparison against a previously considered tubular single-lap joint. The steep variation of both peeling and shearing stresses near the adhesive edges was successfully captured. The applicability of the present method was also demonstrated by considering tubular bonded lap-joints subjected to pure bending and torsion.

An evaluation of four single element airfoil analytic methods

NASA Technical Reports Server (NTRS)

Freuler, R. J.; Gregorek, G. M.

1979-01-01

A comparison of four computer codes for the analysis of two-dimensional single element airfoil sections is presented for three classes of section geometries. Two of the computer codes utilize vortex singularities methods to obtain the potential flow solution. The other two codes solve the full inviscid potential flow equation using finite differencing techniques, allowing results to be obtained for transonic flow about an airfoil including weak shocks. Each program incorporates boundary layer routines for computing the boundary layer displacement thickness and boundary layer effects on aerodynamic coefficients. Computational results are given for a symmetrical section represented by an NACA 0012 profile, a conventional section illustrated by an NACA 65A413 profile, and a supercritical type section for general aviation applications typified by a NASA LS(1)-0413 section. The four codes are compared and contrasted in the areas of method of approach, range of applicability, agreement among each other and with experiment, individual advantages and disadvantages, computer run times and memory requirements, and operational idiosyncrasies.

Finite element modeling of borehole heat exchanger systems. Part 1. Fundamentals

NASA Astrophysics Data System (ADS)

Diersch, H.-J. G.; Bauer, D.; Heidemann, W.; Rühaak, W.; Schätzl, P.

2011-08-01

Single borehole heat exchanger (BHE) and arrays of BHE are modeled by using the finite element method. The first part of the paper derives the fundamental equations for BHE systems and their finite element representations, where the thermal exchange between the borehole components is modeled via thermal transfer relations. For this purpose improved relationships for thermal resistances and capacities of BHE are introduced. Pipe-to-grout thermal transfer possesses multiple grout points for double U-shape and single U-shape BHE to attain a more accurate modeling. The numerical solution of the final 3D problems is performed via a widely non-sequential (essentially non-iterative) coupling strategy for the BHE and porous medium discretization. Four types of vertical BHE are supported: double U-shape (2U) pipe, single U-shape (1U) pipe, coaxial pipe with annular (CXA) and centred (CXC) inlet. Two computational strategies are used: (1) The analytical BHE method based on Eskilson and Claesson's (1988) solution, (2) numerical BHE method based on Al-Khoury et al.'s (2005) solution. The second part of the paper focusses on BHE meshing aspects, the validation of BHE solutions and practical applications for borehole thermal energy store systems.

The trap DOS in small molecule organic semiconductors: A quantitative comparison of thin-film transistors with single crystals

NASA Astrophysics Data System (ADS)

Kalb, Wolfgang; Haas, Simon; Pernstich, Kurt; Mathis, Thomas; Batlogg, Bertram

2010-03-01

Our study shows that it is possible to reach one of the ultimate goals of organic electronics: organic field-effect transistors can be produced with trap densities as low as in the bulk of single crystals. Several analytical methods to calculate the spectral density of localized states in the band gap (trap DOS) from measured data were used to clarify, if the different methods lead to similar results. We then compared quantitatively trap DOS information from the literature, correcting for differences due to different calculation methods. In the bulk of single crystals the trap DOS is lower by several orders of magnitude than in thin films. The compilation of all data strongly suggests that structural defects at grain boundaries are the main cause of ``fast'' traps in TFT's made with vacuum-evaporated pentacene. For high-performance transistors made with small molecule semiconductors such as rubrene it is essential to reduce the dipolar disorder caused by water adsorbed on the gate dielectric. We will discuss to what degree band broadening due to the thermal fluctuations of the intermolecular transfer integral is reflected in the trap DOS very close (<0.15 eV) to the mobility edge.

Rapid analysis of pharmaceuticals and personal care products in fish plasma micro-aliquots using liquid chromatography tandem mass spectrometry.

PubMed

Chen, Fangfang; Gong, Zhiyuan; Kelly, Barry C

2015-02-27

A sensitive analytical method based on liquid-liquid extraction (LLE) and liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed for rapid analysis of 11 pharmaceuticals and personal care products (PPCPs) in fish plasma micro-aliquots (∼20μL). Target PPCPs included, bisphenol A, carbamazepine, diclofenac, fluoxetine, gemfibrozil, ibuprofen, naproxen, risperidone, sertraline, simvastatin and triclosan. A relatively quicker and cheaper LLE procedure exhibited comparable analyte recoveries with solid-phase extraction. Rapid separation and analysis of target compounds in fish plasma extracts was achieved by employing a high efficiency C-18 HPLC column (Agilent Poroshell 120 SB-C18, 2.1mm×50mm, 2.7μm) and fast polarity switching, enabling effective monitoring of positive and negative ions in a single 9min run. With the exception of bisphenol A, which exhibited relatively high background contamination, method detection limits of individual PPCPs ranged between 0.15 and 0.69pg/μL, while method quantification limits were between 0.05 and 2.3pg/μL. Mean matrix effect (ME) values ranged between 65 and 156% for the various target analytes. Isotope dilution quantification using isotopically labelled internal surrogates was utilized to correct for signal suppression or enhancement and analyte losses during sample preparation. The method was evaluated by analysis of 20μL plasma micro-aliquots collected from zebrafish (Danio rerio) from a laboratory bioaccumulation study, which included control group fish (no exposure), as well as fish exposed to environmentally relevant concentrations of PPCPs. Using the developed LC-MS/MS based method, concentrations of the studied PPCPs were consistently detected in the low pg/μL (ppb) range. The method may be useful for investigations requiring fast, reliable concentration measurements of PPCPs in fish plasma. In particular, the method may be applicable for in situ contaminant biomonitoring, as well as bioaccumulation and toxicology studies employing small fishes with low blood compartment volumes. Copyright © 2015 Elsevier B.V. All rights reserved.

Analysis of intracellular and extracellular microcystin variants in sediments and pore waters by accelerated solvent extraction and high performance liquid chromatography-tandem mass spectrometry.

PubMed

Zastepa, Arthur; Pick, Frances R; Blais, Jules M; Saleem, Ammar

2015-05-04

The fate and persistence of microcystin cyanotoxins in aquatic ecosystems remains poorly understood in part due to the lack of analytical methods for microcystins in sediments. Existing methods have been limited to the extraction of a few extracellular microcystins of similar chemistry. We developed a single analytical method, consisting of accelerated solvent extraction, hydrophilic-lipophilic balance solid phase extraction, and reversed phase high performance liquid chromatography-tandem mass spectrometry, suitable for the extraction and quantitation of both intracellular and extracellular cyanotoxins in sediments as well as pore waters. Recoveries of nine microcystins, representing the chemical diversity of microcystins, and nodularin (a marine analogue) ranged between 75 and 98% with one, microcystin-RR (MC-RR), at 50%. Chromatographic separation of these analytes was achieved within 7.5 min and the method detection limits were between 1.1 and 2.5 ng g(-1) dry weight (dw). The robustness of the method was demonstrated on sediment cores collected from seven Canadian lakes of diverse geography and trophic states. Individual microcystin variants reached a maximum concentration of 829 ng g(-1) dw on sediment particles and 132 ng mL(-1) in pore waters and could be detected in sediments as deep as 41 cm (>100 years in age). MC-LR, -RR, and -LA were more often detected while MC-YR, -LY, -LF, and -LW were less common. The analytical method enabled us to estimate sediment-pore water distribution coefficients (K(d)), MC-RR had the highest affinity for sediment particles (log K(d)=1.3) while MC-LA had the lowest affinity (log K(d)=-0.4), partitioning mainly into pore waters. Our findings confirm that sediments serve as a reservoir for microcystins but suggest that some variants may diffuse into overlying water thereby constituting a new route of exposure following the dissipation of toxic blooms. The method is well suited to determine the fate and persistence of different microcystins in aquatic systems. Copyright © 2015 Elsevier B.V. All rights reserved.

Development of two step liquid-liquid extraction tandem UHPLC-MS/MS method for the simultaneous determination of Ginkgo flavonoids, terpene lactones and nimodipine in rat plasma: Application to the pharmacokinetic study of the combination of Ginkgo biloba dispersible tablets and Nimodipine tablets.

PubMed

Xiao, Jie; Wang, Tianyang; Li, Pei; Liu, Ran; Li, Qing; Bi, Kaishun

2016-08-15

A sensitive, reliable and accurate UHPLC-MS/MS method has been firstly established and validated for the simultaneous quantification of ginkgo flavonoids, terpene lactones and nimodipine in rat plasma after oral administration of Ginkgo biloba dispersible tablets, Nimodipine tablets and the combination of the both, respectively. The plasma samples were extracted by two step liquid-liquid extraction, nimodipine was extracted by hexane-ether (3:1, v/v) at the first step, after that ginkgo flavonoids and terpene lactones were extracted by ethyl acetate. Then the analytes were successfully separated by running gradient elution with the mobile phase consisting of 0.1% formic acid in water and methanol at a flow rate of 0.6mL/min. The detection of the analytes was performed on a UHPLC-MS/MS system with turbo ion spray source in the negative ion and multiple reaction monitoring (MRM) mode. The calibration curves for the determination of all the analytes showed good linearity (R(2)>0.99), and the lower limits of quantification were 0.50-4.00ng/mL. Intra-day and inter-day precisions were in the range of 3.6%-9.2% and 3.2%-13.1% for all the analytes. The mean extraction recoveries of the analytes were within 69.82%-103.5% and the matrix were within 82.8%-110.0%. The validated method had been successfully applied to compare the pharmacokinetic parameters of ginkgo flavonoids, terpene lactones and nimodipine in rat plasma after oral administration of Ginkgo biloba dispersible tablets, Nimodipine tablets with the combination of the both. There were no statistically significant differences on the pharmacokinetic behaviors of all the analytes between the combined and single administration groups. Results showed that the combination of the two agents may avoid dosage adjustments in clinic and the combination is more convenient as well as efficient on different pathogenesis of cerebral ischemia. Copyright © 2016 Elsevier B.V. All rights reserved.

Quantitative SIMS Imaging of Agar-Based Microbial Communities.

PubMed

Dunham, Sage J B; Ellis, Joseph F; Baig, Nameera F; Morales-Soto, Nydia; Cao, Tianyuan; Shrout, Joshua D; Bohn, Paul W; Sweedler, Jonathan V

2018-05-01

After several decades of widespread use for mapping elemental ions and small molecular fragments in surface science, secondary ion mass spectrometry (SIMS) has emerged as a powerful analytical tool for molecular imaging in biology. Biomolecular SIMS imaging has primarily been used as a qualitative technique; although the distribution of a single analyte can be accurately determined, it is difficult to map the absolute quantity of a compound or even to compare the relative abundance of one molecular species to that of another. We describe a method for quantitative SIMS imaging of small molecules in agar-based microbial communities. The microbes are cultivated on a thin film of agar, dried under nitrogen, and imaged directly with SIMS. By use of optical microscopy, we show that the area of the agar is reduced by 26 ± 2% (standard deviation) during dehydration, but the overall biofilm morphology and analyte distribution are largely retained. We detail a quantitative imaging methodology, in which the ion intensity of each analyte is (1) normalized to an external quadratic regression curve, (2) corrected for isomeric interference, and (3) filtered for sample-specific noise and lower and upper limits of quantitation. The end result is a two-dimensional surface density image for each analyte. The sample preparation and quantitation methods are validated by quantitatively imaging four alkyl-quinolone and alkyl-quinoline N-oxide signaling molecules (including Pseudomonas quinolone signal) in Pseudomonas aeruginosa colony biofilms. We show that the relative surface densities of the target biomolecules are substantially different from values inferred through direct intensity comparison and that the developed methodologies can be used to quantitatively compare as many ions as there are available standards.

Fabrication strategies, sensing modes and analytical applications of ratiometric electrochemical biosensors.

PubMed

Jin, Hui; Gui, Rijun; Yu, Jianbo; Lv, Wei; Wang, Zonghua

2017-05-15

Previously developed electrochemical biosensors with single-electric signal output are probably affected by intrinsic and extrinsic factors. In contrast, the ratiometric electrochemical biosensors (RECBSs) with dual-electric signal outputs have an intrinsic built-in correction to the effects from system or background electric signals, and therefore exhibit a significant potential to improve the accuracy and sensitivity in electrochemical sensing applications. In this review, we systematically summarize the fabrication strategies, sensing modes and analytical applications of RECBSs. First, the different fabrication strategies of RECBSs were introduced, referring to the analytes-induced single- and dual-dependent electrochemical signal strategies for RECBSs. Second, the different sensing modes of RECBSs were illustrated, such as differential pulse voltammetry, square wave voltammetry, cyclic voltammetry, alternating current voltammetry, electrochemiluminescence, and so forth. Third, the analytical applications of RECBSs were discussed based on the types of target analytes. Finally, the forthcoming development and future prospects in the research field of RECBSs were also highlighted. Copyright © 2017 Elsevier B.V. All rights reserved.