A simple three dimensional wide-angle beam propagation method

NASA Astrophysics Data System (ADS)

Ma, Changbao; van Keuren, Edward

2006-05-01

The development of three dimensional (3-D) waveguide structures for chip scale planar lightwave circuits (PLCs) is hampered by the lack of effective 3-D wide-angle (WA) beam propagation methods (BPMs). We present a simple 3-D wide-angle beam propagation method (WA-BPM) using Hoekstra’s scheme along with a new 3-D wave equation splitting method. The applicability, accuracy and effectiveness of our method are demonstrated by applying it to simulations of wide-angle beam propagation and comparing them with analytical solutions.

A simple three dimensional wide-angle beam propagation method.

PubMed

Ma, Changbao; Van Keuren, Edward

2006-05-29

The development of three dimensional (3-D) waveguide structures for chip scale planar lightwave circuits (PLCs) is hampered by the lack of effective 3-D wide-angle (WA) beam propagation methods (BPMs). We present a simple 3-D wide-angle beam propagation method (WA-BPM) using Hoekstra's scheme along with a new 3-D wave equation splitting method. The applicability, accuracy and effectiveness of our method are demonstrated by applying it to simulations of wide-angle beam propagation and comparing them with analytical solutions.

Keeping It Simple: Can We Estimate Malting Quality Potential Using an Isothermal Mashing Protocol and Common Laboratory Instrumentation?

USDA-ARS?s Scientific Manuscript database

Current methods for generating malting quality metrics have been developed largely to support commercial malting and brewing operations, providing accurate, reproducible analytical data to guide malting and brewing production. Infrastructure to support these analytical operations often involves sub...

Electrochemistry and analytical determination of lysergic acid diethylamide (LSD) via adsorptive stripping voltammetry.

PubMed

Merli, Daniele; Zamboni, Daniele; Protti, Stefano; Pesavento, Maria; Profumo, Antonella

2014-12-01

Lysergic acid diethylamide (LSD) is hardly detectable and quantifiable in biological samples because of its low active dose. Although several analytical tests are available, routine analysis of this drug is rarely performed. In this article, we report a simple and accurate method for the determination of LSD, based on adsorptive stripping voltammetry in DMF/tetrabutylammonium perchlorate, with a linear range of 1-90 ng L(-1) for deposition times of 50s. LOD of 1.4 ng L(-1) and LOQ of 4.3 ng L(-1) were found. The method can be also applied to biological samples after a simple extraction with 1-chlorobutane. Copyright © 2014 Elsevier B.V. All rights reserved.

A SIMPLE, EFFICIENT SOLUTION OF FLUX-PROFILE RELATIONSHIPS IN THE ATMOSPHERIC SURFACE LAYER

EPA Science Inventory

This note describes a simple scheme for analytical estimation of the surface layer similarity functions from state variables. What distinguishes this note from the many previous papers on this topic is that this method is specifically targeted for numerical models where simplici...

Analytical and multibody modeling for the power analysis of standing jumps.

PubMed

Palmieri, G; Callegari, M; Fioretti, S

2015-01-01

Two methods for the power analysis of standing jumps are proposed and compared in this article. The first method is based on a simple analytical formulation which requires as input the coordinates of the center of gravity in three specified instants of the jump. The second method is based on a multibody model that simulates the jumps processing the data obtained by a three-dimensional (3D) motion capture system and the dynamometric measurements obtained by the force platforms. The multibody model is developed with OpenSim, an open-source software which provides tools for the kinematic and dynamic analyses of 3D human body models. The study is focused on two of the typical tests used to evaluate the muscular activity of lower limbs, which are the counter movement jump and the standing long jump. The comparison between the results obtained by the two methods confirms that the proposed analytical formulation is correct and represents a simple tool suitable for a preliminary analysis of total mechanical work and the mean power exerted in standing jumps.

Stress Analysis of Beams with Shear Deformation of the Flanges

NASA Technical Reports Server (NTRS)

Kuhn, Paul

1937-01-01

This report discusses the fundamental action of shear deformation of the flanges on the basis of simplifying assumptions. The theory is developed to the point of giving analytical solutions for simple cases of beams and of skin-stringer panels under axial load. Strain-gage tests on a tension panel and on a beam corresponding to these simple cases are described and the results are compared with analytical results. For wing beams, an approximate method of applying the theory is given. As an alternative, the construction of a mechanical analyzer is advocated.

Prediction of thermal cycling induced matrix cracking

NASA Technical Reports Server (NTRS)

Mcmanus, Hugh L.

1992-01-01

Thermal fatigue has been observed to cause matrix cracking in laminated composite materials. A method is presented to predict transverse matrix cracks in composite laminates subjected to cyclic thermal load. Shear lag stress approximations and a simple energy-based fracture criteria are used to predict crack densities as a function of temperature. Prediction of crack densities as a function of thermal cycling is accomplished by assuming that fatigue degrades the material's inherent resistance to cracking. The method is implemented as a computer program. A simple experiment provides data on progressive cracking of a laminate with decreasing temperature. Existing data on thermal fatigue is also used. Correlations of the analytical predictions to the data are very good. A parametric study using the analytical method is presented which provides insight into material behavior under cyclical thermal loads.

Simple method for the determination of personal care product ingredients in lettuce by ultrasound-assisted extraction combined with solid-phase microextraction followed by GC-MS.

PubMed

Cabrera-Peralta, Jerónimo; Peña-Alvarez, Araceli

2018-05-01

A simple method for the simultaneous determination of personal care product ingredients: galaxolide, tonalide, oxybenzone, 4-methylbenzyliden camphor, padimate-o, 2-ethylhexyl methoxycinnamate, octocrylene, triclosan, and methyl triclosan in lettuce by ultrasound-assisted extraction combined with solid-phase microextraction followed by gas chromatography with mass spectrometry was developed. Lettuce was directly extracted by ultrasound-assisted extraction with methanol, this extract was combined with water, extracted by solid-phase microextraction in immersion mode, and analyzed by gas chromatography with mass spectrometry. Good linear relationships (25-250 ng/g, R 2  > 0.9702) and low detection limits (1.0-25 ng/g) were obtained for analytes along with acceptable precision for almost all analytes (RSDs < 20%). The validated method was applied for the determination of personal care product ingredients in commercial lettuce and lettuces grown in soil and irrigated with the analytes, identifying the target analytes in leaves and roots of the latter. This procedure is a miniaturized and environmentally friendly proposal which can be a useful tool for quality analysis in lettuce. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Improved Design of Tunnel Supports : Executive Summary

DOT National Transportation Integrated Search

1979-12-01

This report focuses on improvement of design methodologies related to the ground-structure interaction in tunneling. The design methods range from simple analytical and empirical methods to sophisticated finite element techniques as well as an evalua...

Phonon scattering in nanoscale systems: lowest order expansion of the current and power expressions

NASA Astrophysics Data System (ADS)

Paulsson, Magnus; Frederiksen, Thomas; Brandbyge, Mads

2006-04-01

We use the non-equilibrium Green's function method to describe the effects of phonon scattering on the conductance of nano-scale devices. Useful and accurate approximations are developed that both provide (i) computationally simple formulas for large systems and (ii) simple analytical models. In addition, the simple models can be used to fit experimental data and provide physical parameters.

Comparative Validation of the Determination of Sofosbuvir in Pharmaceuticals by Several Inexpensive Ecofriendly Chromatographic, Electrophoretic, and Spectrophotometric Methods.

PubMed

El-Yazbi, Amira F

2017-07-01

Sofosbuvir (SOFO) was approved by the U.S. Food and Drug Administration in 2013 for the treatment of hepatitis C virus infection with enhanced antiviral potency compared with earlier analogs. Notwithstanding, all current editions of the pharmacopeias still do not present any analytical methods for the quantification of SOFO. Thus, rapid, simple, and ecofriendly methods for the routine analysis of commercial formulations of SOFO are desirable. In this study, five accurate methods for the determination of SOFO in pharmaceutical tablets were developed and validated. These methods include HPLC, capillary zone electrophoresis, HPTLC, and UV spectrophotometric and derivative spectrometry methods. The proposed methods proved to be rapid, simple, sensitive, selective, and accurate analytical procedures that were suitable for the reliable determination of SOFO in pharmaceutical tablets. An analysis of variance test with P-value > 0.05 confirmed that there were no significant differences between the proposed assays. Thus, any of these methods can be used for the routine analysis of SOFO in commercial tablets.

Simultaneous determination of potassium guaiacolsulfonate, guaifenesin, diphenhydramine HCl and carbetapentane citrate in syrups by using HPLC-DAD coupled with partial least squares multivariate calibration.

PubMed

Dönmez, Ozlem Aksu; Aşçi, Bürge; Bozdoğan, Abdürrezzak; Sungur, Sidika

2011-02-15

A simple and rapid analytical procedure was proposed for the determination of chromatographic peaks by means of partial least squares multivariate calibration (PLS) of high-performance liquid chromatography with diode array detection (HPLC-DAD). The method is exemplified with analysis of quaternary mixtures of potassium guaiacolsulfonate (PG), guaifenesin (GU), diphenhydramine HCI (DP) and carbetapentane citrate (CP) in syrup preparations. In this method, the area does not need to be directly measured and predictions are more accurate. Though the chromatographic and spectral peaks of the analytes were heavily overlapped and interferents coeluted with the compounds studied, good recoveries of analytes could be obtained with HPLC-DAD coupled with PLS calibration. This method was tested by analyzing the synthetic mixture of PG, GU, DP and CP. As a comparison method, a classsical HPLC method was used. The proposed methods were applied to syrups samples containing four drugs and the obtained results were statistically compared with each other. Finally, the main advantage of HPLC-PLS method over the classical HPLC method tried to emphasized as the using of simple mobile phase, shorter analysis time and no use of internal standard and gradient elution. Copyright © 2010 Elsevier B.V. All rights reserved.

Use of Cdse/ZnS quantum dots for sensitive detection and quantification of paraquat in water samples.

PubMed

Durán, Gema M; Contento, Ana M; Ríos, Ángel

2013-11-01

Based on the highly sensitive fluorescence change of water-soluble CdSe/ZnS core-shell quantum dots (QD) by paraquat herbicide, a simple, rapid and reproducible methodology was developed to selectively determine paraquat (PQ) in water samples. The methodology enabled the use of simple pretreatment procedure based on the simple water solubilization of CdSe/ZnS QDs with hydrophilic heterobifunctional thiol ligands, such as 3-mercaptopropionic acid (3-MPA), using microwave irradiation. The resulting water-soluble QDs exhibit a strong fluorescence emission at 596 nm with a high and reproducible photostability. The proposed analytical method thus satisfies the need for a simple, sensible and rapid methodology to determine residues of paraquat in water samples, as required by the increasingly strict regulations for health protection introduced in recent years. The sensitivity of the method, expressed as detection limits, was as low as 3.0 ng L(-1). The lineal range was between 10-5×10(3) ng L(-1). RSD values in the range of 71-102% were obtained. The analytical applicability of proposed method was demonstrated by analyzing water samples from different procedence. Copyright © 2013 Elsevier B.V. All rights reserved.

1-D DC Resistivity Modeling and Interpretation in Anisotropic Media Using Particle Swarm Optimization

NASA Astrophysics Data System (ADS)

Pekşen, Ertan; Yas, Türker; Kıyak, Alper

2014-09-01

We examine the one-dimensional direct current method in anisotropic earth formation. We derive an analytic expression of a simple, two-layered anisotropic earth model. Further, we also consider a horizontally layered anisotropic earth response with respect to the digital filter method, which yields a quasi-analytic solution over anisotropic media. These analytic and quasi-analytic solutions are useful tests for numerical codes. A two-dimensional finite difference earth model in anisotropic media is presented in order to generate a synthetic data set for a simple one-dimensional earth. Further, we propose a particle swarm optimization method for estimating the model parameters of a layered anisotropic earth model such as horizontal and vertical resistivities, and thickness. The particle swarm optimization is a naturally inspired meta-heuristic algorithm. The proposed method finds model parameters quite successfully based on synthetic and field data. However, adding 5 % Gaussian noise to the synthetic data increases the ambiguity of the value of the model parameters. For this reason, the results should be controlled by a number of statistical tests. In this study, we use probability density function within 95 % confidence interval, parameter variation of each iteration and frequency distribution of the model parameters to reduce the ambiguity. The result is promising and the proposed method can be used for evaluating one-dimensional direct current data in anisotropic media.

Identifying Factors that Influence State-Specific Hunger Rates in the U.S.: A Simple Analytic Method for Understanding a Persistent Problem

ERIC Educational Resources Information Center

Edwards, Mark Evan; Weber, Bruce; Bernell, Stephanie

2007-01-01

An existing measure of food insecurity with hunger in the United States may serve as an effective indicator of quality of life. State level differences in that measure can reveal important differences in quality of life across places. In this study, we advocate and demonstrate two simple methods by which analysts can explore state-specific…

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

A computational method for optimizing fuel treatment locations

Treesearch

Mark A. Finney

2006-01-01

Modeling and experiments have suggested that spatial fuel treatment patterns can influence the movement of large fires. On simple theoretical landscapes consisting of two fuel types (treated and untreated) optimal patterns can be analytically derived that disrupt fire growth efficiently (i.e. with less area treated than random patterns). Although conceptually simple,...

A Comprehensive Analytical Solution of the Nonlinear Pendulum

ERIC Educational Resources Information Center

Ochs, Karlheinz

2011-01-01

In this paper, an analytical solution for the differential equation of the simple but nonlinear pendulum is derived. This solution is valid for any time and is not limited to any special initial instance or initial values. Moreover, this solution holds if the pendulum swings over or not. The method of approach is based on Jacobi elliptic functions…

Modern analytical chemistry in the contemporary world

NASA Astrophysics Data System (ADS)

Šíma, Jan

2016-12-01

Students not familiar with chemistry tend to misinterpret analytical chemistry as some kind of the sorcery where analytical chemists working as modern wizards handle magical black boxes able to provide fascinating results. However, this approach is evidently improper and misleading. Therefore, the position of modern analytical chemistry among sciences and in the contemporary world is discussed. Its interdisciplinary character and the necessity of the collaboration between analytical chemists and other experts in order to effectively solve the actual problems of the human society and the environment are emphasized. The importance of the analytical method validation in order to obtain the accurate and precise results is highlighted. The invalid results are not only useless; they can often be even fatal (e.g., in clinical laboratories). The curriculum of analytical chemistry at schools and universities is discussed. It is referred to be much broader than traditional equilibrium chemistry coupled with a simple description of individual analytical methods. Actually, the schooling of analytical chemistry should closely connect theory and practice.

A simple analytical platform based on thin-layer chromatography coupled with paper-based analytical device for determination of total capsaicinoids in chilli samples.

PubMed

Dawan, Phanphruk; Satarpai, Thiphol; Tuchinda, Patoomratana; Shiowatana, Juwadee; Siripinyanond, Atitaya

2017-01-01

A new analytical platform based on the use of thin-layer chromatography (TLC) coupled with paper-based analytical device (PAD) was developed for the determination of total capsaicinoids in chilli samples. This newly developed TLC-PAD is simple and low-cost without any requirement of special instrument or skillful person. The analysis consisted of two steps, i.e., extraction of capsaicinoids from chilli samples by using ethanol as solvent and separation of capsaicinoids by thin-layer chromatography (TLC) and elution of capsaicinoids from the TLC plate with in situ colorimetric detection of capsaicinoids on the PAD. For colorimetric detection, Folin-Ciocalteu reagent was used to detect phenolic functional group of capsaicinoids yielding the blue color. The blue color on the PAD was imaged by a scanner followed by evaluation of its grayscale intensity value by ImageJ program. This newly developed TLC-PAD method provided a linear range from 50 to 1000mgL -1 capsaicinoids with the limit of detection as low as 50mgL -1 capsaicinoids. The proposed method was applied to determine capsaicinoids in dried chilli and seasoning powder samples and the results were in good agreement with those obtained by HPLC method. Copyright © 2016 Elsevier B.V. All rights reserved.

A Review of Numerical Simulation and Analytical Modeling for Medical Devices Safety in MRI

PubMed Central

Kabil, J.; Belguerras, L.; Trattnig, S.; Pasquier, C.; Missoffe, A.

2016-01-01

Summary Objectives To review past and present challenges and ongoing trends in numerical simulation for MRI (Magnetic Resonance Imaging) safety evaluation of medical devices. Methods A wide literature review on numerical and analytical simulation on simple or complex medical devices in MRI electromagnetic fields shows the evolutions through time and a growing concern for MRI safety over the years. Major issues and achievements are described, as well as current trends and perspectives in this research field. Results Numerical simulation of medical devices is constantly evolving, supported by calculation methods now well-established. Implants with simple geometry can often be simulated in a computational human model, but one issue remaining today is the experimental validation of these human models. A great concern is to assess RF heating on implants too complex to be traditionally simulated, like pacemaker leads. Thus, ongoing researches focus on alternative hybrids methods, both numerical and experimental, with for example a transfer function method. For the static field and gradient fields, analytical models can be used for dimensioning simple implants shapes, but limited for complex geometries that cannot be studied with simplifying assumptions. Conclusions Numerical simulation is an essential tool for MRI safety testing of medical devices. The main issues remain the accuracy of simulations compared to real life and the studies of complex devices; but as the research field is constantly evolving, some promising ideas are now under investigation to take up the challenges. PMID:27830244

Approaching near real-time biosensing: microfluidic microsphere based biosensor for real-time analyte detection.

PubMed

Cohen, Noa; Sabhachandani, Pooja; Golberg, Alexander; Konry, Tania

2015-04-15

In this study we describe a simple lab-on-a-chip (LOC) biosensor approach utilizing well mixed microfluidic device and a microsphere-based assay capable of performing near real-time diagnostics of clinically relevant analytes such cytokines and antibodies. We were able to overcome the adsorption kinetics reaction rate-limiting mechanism, which is diffusion-controlled in standard immunoassays, by introducing the microsphere-based assay into well-mixed yet simple microfluidic device with turbulent flow profiles in the reaction regions. The integrated microsphere-based LOC device performs dynamic detection of the analyte in minimal amount of biological specimen by continuously sampling micro-liter volumes of sample per minute to detect dynamic changes in target analyte concentration. Furthermore we developed a mathematical model for the well-mixed reaction to describe the near real time detection mechanism observed in the developed LOC method. To demonstrate the specificity and sensitivity of the developed real time monitoring LOC approach, we applied the device for clinically relevant analytes: Tumor Necrosis Factor (TNF)-α cytokine and its clinically used inhibitor, anti-TNF-α antibody. Based on the reported results herein, the developed LOC device provides continuous sensitive and specific near real-time monitoring method for analytes such as cytokines and antibodies, reduces reagent volumes by nearly three orders of magnitude as well as eliminates the washing steps required by standard immunoassays. Copyright © 2014 Elsevier B.V. All rights reserved.

Validation and Application of a Simple UHPLC–MS-MS Method for the Enantiospecific Determination of Warfarin in Human Urine

PubMed Central

Alshogran, Osama Y.; Ocque, Andrew J.; Leblond, François A.; Pichette, Vincent; Nolin, Thomas D.

2016-01-01

A simple and rapid liquid chromatographic–tandem mass spectrometric method has been developed and validated for the enantiospecific determination of R- and S-warfarin in human urine. Warfarin enantiomers were extracted from urine using methyl tert-butyl ether. Chromatographic separation of warfarin enantiomers and the internal standard d5-warfarin was achieved using a Astec Chirobiotic V column with gradient mobile phase at a flow rate of 400 µL/min over 10 min. Detection was performed on a TSQ Quantum Ultra triple quadrupole mass spectrometer equipped with a heated electrospray ionization source. Analytes were detected in negative ionization mode using selected reaction monitoring. Calibration curves were linear with a correlation coefficient of ≥0.996 for both enantiomers over a concentration range of 5–500 ng/mL. The intra- and interday accuracy and precision for both analytes were within ±9.0%. Excellent extraction efficiency and negligible matrix effects were observed. The applicability of the method was demonstrated by successful measurement of warfarin enantiomers in urine of patients with kidney disease. The method is simple, accurate and reproducible and is currently being used to support warfarin pharmacokinetic studies. PMID:26657732

Finite Element Analysis of Simple Rectangular Microstrip Sensor for Determination Moisture Content of Hevea Rubber Latex

NASA Astrophysics Data System (ADS)

Yahaya, NZ; Ramli, MR; Razak, NNANA; Abbas, Z.

2018-04-01

The Finite Element Method, FEM has been successfully used to model a simple rectangular microstrip sensor to determine the moisture content of Hevea rubber latex. The FEM simulation of sensor and samples was implemented by using COMSOL Multiphysics software. The simulation includes the calculation of magnitude and phase of reflection coefficient and was compared to analytical method. The results show a good agreement in finding the magnitude and phase of reflection coefficient when compared with analytical results. Field distributions of both the unloaded sensor as well as the sensor loaded with different percentages of moisture content were visualized using FEM in conjunction with COMSOL software. The higher the amount of moisture content in the sample the more the electric loops were observed.

Entropy generation in Gaussian quantum transformations: applying the replica method to continuous-variable quantum information theory

NASA Astrophysics Data System (ADS)

Gagatsos, Christos N.; Karanikas, Alexandros I.; Kordas, Georgios; Cerf, Nicolas J.

2016-02-01

In spite of their simple description in terms of rotations or symplectic transformations in phase space, quadratic Hamiltonians such as those modelling the most common Gaussian operations on bosonic modes remain poorly understood in terms of entropy production. For instance, determining the quantum entropy generated by a Bogoliubov transformation is notably a hard problem, with generally no known analytical solution, while it is vital to the characterisation of quantum communication via bosonic channels. Here we overcome this difficulty by adapting the replica method, a tool borrowed from statistical physics and quantum field theory. We exhibit a first application of this method to continuous-variable quantum information theory, where it enables accessing entropies in an optical parametric amplifier. As an illustration, we determine the entropy generated by amplifying a binary superposition of the vacuum and a Fock state, which yields a surprisingly simple, yet unknown analytical expression.

Comparative Validation of the Determination of Sofosbuvir in Pharmaceuticals by Several Inexpensive Ecofriendly Chromatographic, Electrophoretic, and Spectrophotometric Methods.

PubMed

El-Yazbi, Amira F

2017-01-20

Sofosbuvir (SOFO) was approved by the U.S. Food and Drug Administration in 2013 for the treatment of hepatitis C virusinfection with enhanced antiviral potency compared with earlier analogs. Notwithstanding, all current editions of the pharmacopeias still do not present any analytical methods for the quantification of SOFO. Thus, rapid, simple, and ecofriendly methods for the routine analysis of commercial formulations of SOFO are desirable. In this study, five accurate methods for the determination of SOFO in pharmaceutical tablets were developed and validated. These methods include HPLC, capillary zone electrophoresis, HPTLC, and UV spectrophotometric and derivative spectrometry methods. The proposed methods proved to be rapid, simple, sensitive, selective, and accurate analytical procedures that were suitable for the reliable determination of SOFO in pharmaceutical tablets. An analysis of variance test with <em>P</em>-value &#x003E; 0.05 confirmed that there were no significant differences between the proposed assays. Thus, any of these methods can be used for the routine analysis of SOFO in commercial tablets.

Targeted Analyte Detection by Standard Addition Improves Detection Limits in MALDI Mass Spectrometry

PubMed Central

Eshghi, Shadi Toghi; Li, Xingde; Zhang, Hui

2014-01-01

Matrix-assisted laser desorption/ionization has proven an effective tool for fast and accurate determination of many molecules. However, the detector sensitivity and chemical noise compromise the detection of many invaluable low-abundance molecules from biological and clinical samples. To challenge this limitation, we developed a targeted analyte detection (TAD) technique. In TAD, the target analyte is selectively elevated by spiking a known amount of that analyte into the sample, thereby raising its concentration above the noise level, where we take advantage of the improved sensitivity to detect the presence of the endogenous analyte in the sample. We assessed TAD on three peptides in simple and complex background solutions with various exogenous analyte concentrations in two MALDI matrices. TAD successfully improved the limit of detection (LOD) of target analytes when the target peptides were added to the sample in a concentration close to optimum concentration. The optimum exogenous concentration was estimated through a quantitative method to be approximately equal to the original LOD for each target. Also, we showed that TAD could achieve LOD improvements on an average of 3-fold in a simple and 2-fold in a complex sample. TAD provides a straightforward assay to improve the LOD of generic target analytes without the need for costly hardware modifications. PMID:22877355

Targeted analyte detection by standard addition improves detection limits in matrix-assisted laser desorption/ionization mass spectrometry.

PubMed

Toghi Eshghi, Shadi; Li, Xingde; Zhang, Hui

2012-09-18

Matrix-assisted laser desorption/ionization (MALDI) has proven an effective tool for fast and accurate determination of many molecules. However, the detector sensitivity and chemical noise compromise the detection of many invaluable low-abundance molecules from biological and clinical samples. To challenge this limitation, we developed a targeted analyte detection (TAD) technique. In TAD, the target analyte is selectively elevated by spiking a known amount of that analyte into the sample, thereby raising its concentration above the noise level, where we take advantage of the improved sensitivity to detect the presence of the endogenous analyte in the sample. We assessed TAD on three peptides in simple and complex background solutions with various exogenous analyte concentrations in two MALDI matrices. TAD successfully improved the limit of detection (LOD) of target analytes when the target peptides were added to the sample in a concentration close to optimum concentration. The optimum exogenous concentration was estimated through a quantitative method to be approximately equal to the original LOD for each target. Also, we showed that TAD could achieve LOD improvements on an average of 3-fold in a simple and 2-fold in a complex sample. TAD provides a straightforward assay to improve the LOD of generic target analytes without the need for costly hardware modifications.

A simple formula for the effective complex conductivity of periodic fibrous composites with interfacial impedance and applications to biological tissues

NASA Astrophysics Data System (ADS)

Bisegna, Paolo; Caselli, Federica

2008-06-01

This paper presents a simple analytical expression for the effective complex conductivity of a periodic hexagonal arrangement of conductive circular cylinders embedded in a conductive matrix, with interfaces exhibiting a capacitive impedance. This composite material may be regarded as an idealized model of a biological tissue comprising tubular cells, such as skeletal muscle. The asymptotic homogenization method is adopted, and the corresponding local problem is solved by resorting to Weierstrass elliptic functions. The effectiveness of the present analytical result is proved by convergence analysis and comparison with finite-element solutions and existing models.

A new multi-step technique with differential transform method for analytical solution of some nonlinear variable delay differential equations.

PubMed

Benhammouda, Brahim; Vazquez-Leal, Hector

2016-01-01

This work presents an analytical solution of some nonlinear delay differential equations (DDEs) with variable delays. Such DDEs are difficult to treat numerically and cannot be solved by existing general purpose codes. A new method of steps combined with the differential transform method (DTM) is proposed as a powerful tool to solve these DDEs. This method reduces the DDEs to ordinary differential equations that are then solved by the DTM. Furthermore, we show that the solutions can be improved by Laplace-Padé resummation method. Two examples are presented to show the efficiency of the proposed technique. The main advantage of this technique is that it possesses a simple procedure based on a few straight forward steps and can be combined with any analytical method, other than the DTM, like the homotopy perturbation method.

Sensitive analytical method for simultaneous analysis of some vasoconstrictors with highly overlapped analytical signals

NASA Astrophysics Data System (ADS)

Nikolić, G. S.; Žerajić, S.; Cakić, M.

2011-10-01

Multivariate calibration method is a powerful mathematical tool that can be applied in analytical chemistry when the analytical signals are highly overlapped. The method with regression by partial least squares is proposed for the simultaneous spectrophotometric determination of adrenergic vasoconstrictors in decongestive solution containing two active components: phenyleprine hydrochloride and trimazoline hydrochloride. These sympathomimetic agents are that frequently associated in pharmaceutical formulations against the common cold. The proposed method, which is, simple and rapid, offers the advantages of sensitivity and wide range of determinations without the need for extraction of the vasoconstrictors. In order to minimize the optimal factors necessary to obtain the calibration matrix by multivariate calibration, different parameters were evaluated. The adequate selection of the spectral regions proved to be important on the number of factors. In order to simultaneously quantify both hydrochlorides among excipients, the spectral region between 250 and 290 nm was selected. A recovery for the vasoconstrictor was 98-101%. The developed method was applied to assay of two decongestive pharmaceutical preparations.

Comparative Chemometric Analysis for Classification of Acids and Bases via a Colorimetric Sensor Array.

PubMed

Kangas, Michael J; Burks, Raychelle M; Atwater, Jordyn; Lukowicz, Rachel M; Garver, Billy; Holmes, Andrea E

2018-02-01

With the increasing availability of digital imaging devices, colorimetric sensor arrays are rapidly becoming a simple, yet effective tool for the identification and quantification of various analytes. Colorimetric arrays utilize colorimetric data from many colorimetric sensors, with the multidimensional nature of the resulting data necessitating the use of chemometric analysis. Herein, an 8 sensor colorimetric array was used to analyze select acid and basic samples (0.5 - 10 M) to determine which chemometric methods are best suited for classification quantification of analytes within clusters. PCA, HCA, and LDA were used to visualize the data set. All three methods showed well-separated clusters for each of the acid or base analytes and moderate separation between analyte concentrations, indicating that the sensor array can be used to identify and quantify samples. Furthermore, PCA could be used to determine which sensors showed the most effective analyte identification. LDA, KNN, and HQI were used for identification of analyte and concentration. HQI and KNN could be used to correctly identify the analytes in all cases, while LDA correctly identified 95 of 96 analytes correctly. Additional studies demonstrated that controlling for solvent and image effects was unnecessary for all chemometric methods utilized in this study.

Modelling of nanoscale quantum tunnelling structures using algebraic topology method

NASA Astrophysics Data System (ADS)

Sankaran, Krishnaswamy; Sairam, B.

2018-05-01

We have modelled nanoscale quantum tunnelling structures using Algebraic Topology Method (ATM). The accuracy of ATM is compared to the analytical solution derived based on the wave nature of tunnelling electrons. ATM provides a versatile, fast, and simple model to simulate complex structures. We are currently expanding the method for modelling electrodynamic systems.

Experimental and analytical studies for the NASA carbon fiber risk assessment

NASA Technical Reports Server (NTRS)

1980-01-01

Various experimental and analytical studies performed for the NASA carbon fiber risk assessment program are described with emphasis on carbon fiber characteristics, sensitivity of electrical equipment and components to shorting or arcing by carbon fibers, attenuation effect of carbon fibers on aircraft landing aids, impact of carbon fibers on industrial facilities. A simple method of estimating damage from airborne carbon fibers is presented.

In-line micro-matrix solid-phase dispersion extraction for simultaneous separation and extraction of Sudan dyes in different spices.

PubMed

Rajabi, Maryam; Sabzalian, Sedigheh; Barfi, Behruz; Arghavani-Beydokhti, Somayeh; Asghari, Alireza

2015-12-18

A novel, simple, fast, and miniaturized method, termed in-line micro-matrix solid-phase dispersion (in-line MMSPD), coupled with high performance liquid chromatography (HPLC) was developed for the simultaneous extraction and determination of Sudan dyes (i.e. Sudan I-IV, Sudan orange G, Sudan black B, and Sudan red G) with the aid of an experimental design strategy. In this method, a matrix solid-phase dispersion (MSPD) column including a suitable mixture of polar sorbents was inserted in the mobile phase pathway, and while the interfering compounds were retained, the analytes were eluted and entered into the analytical column. In this way, the extraction, elution, and separation of the analytes were performed sequentially. Under the optimal experimental conditions (including the amount of sample, 0.0426g; amount of dispersant phase, 0.0216g of florisil, 0.0227g of silica, 0.0141g of alumina; and blending time, 112s), the limits of detection (LODs), limits of quantification, linear dynamic ranges, and recoveries were obtained to be 0.3-15.3μgkg(-1), 1-50μgkg(-1), 50-28,000μgkg(-1), and 94.5-99.1%, respectively. The results obtained showed that determination of the selected Sudan dyes in food samples using an enough sensitive and a simple analytically validated method like in-line MMSPD may offer a suitable screening method, which could be useful for food analysis and adulteration. Copyright © 2015 Elsevier B.V. All rights reserved.

Magnetic molecularly imprinted polymers for the determination of β-agonist residues in milk by ultra high performance liquid chromatography with tandem mass spectrometry.

PubMed

Liu, Hongcheng; Lin, Xin; Lin, Tao; Zhang, Yulong; Luo, Yinglan; Li, Qiwan

2016-09-01

A simple, accurate, and highly sensitive analytical method was developed in this study for the determination of nine β-agonists in milk. In this method, a new magnetic adsorbent of molecularly imprinted polymers/magnetic nanoparticles prepared by simple physical blending was adopted, which enabled magnetic solid-phase extraction. Thus, the resultant material can be separated from the solvent rapidly and conveniently by a magnet. Two kinds of molecularly imprinted polymer/magnetic nanoparticles materials were fabricated, and the characteristics of materials such as the ratio, pH, amount, desorption, and regeneration were investigated. The analytes were quantified by ultra high performance liquid chromatography coupled to an electrospray ionization tandem mass spectrometer operating in multiple reaction monitoring modes. The detection limit of the method was 0.003-0.3 μg/L, and the detection capability was 0.01-0.3 μg/L. The recoveries of these compounds were 65.7-114% at three spiked levels. Reproducibility represented by relative standard deviation was 11.2% or less. The method was successfully applied to the screening of real samples obtained from local markets and confirmation of the suspected target analytes. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Conservative Analytical Collision Probabilities for Orbital Formation Flying

NASA Technical Reports Server (NTRS)

Carpenter, J. Russell

2004-01-01

The literature offers a number of approximations for analytically and/or efficiently computing the probability of collision between two space objects. However, only one of these techniques is a completely analytical approximation that is suitable for use in the preliminary design phase, when it is more important to quickly analyze a large segment of the trade space than it is to precisely compute collision probabilities. Unfortunately, among the types of formations that one might consider, some combine a range of conditions for which this analytical method is less suitable. This work proposes a simple, conservative approximation that produces reasonable upper bounds on the collision probability in such conditions. Although its estimates are much too conservative under other conditions, such conditions are typically well suited for use of the existing method.

Conservative Analytical Collision Probability for Design of Orbital Formations

NASA Technical Reports Server (NTRS)

Carpenter, J. Russell

2004-01-01

The literature offers a number of approximations for analytically and/or efficiently computing the probability of collision between two space objects. However, only one of these techniques is a completely analytical approximation that is suitable for use in the preliminary design phase, when it is more important to quickly analyze a large segment of the trade space than it is to precisely compute collision probabilities. Unfortunately, among the types of formations that one might consider, some combine a range of conditions for which this analytical method is less suitable. This work proposes a simple, conservative approximation that produces reasonable upper bounds on the collision probability in such conditions. Although its estimates are much too conservative under other conditions, such conditions are typically well suited for use of the existing method.

A comparative review of optical surface contamination assessment techniques

NASA Technical Reports Server (NTRS)

Heaney, James B.

1987-01-01

This paper will review the relative sensitivities and practicalities of the common surface analytical methods that are used to detect and identify unwelcome adsorbants on optical surfaces. The compared methods include visual inspection, simple reflectometry and transmissiometry, ellipsometry, infrared absorption and attenuated total reflectance spectroscopy (ATR), Auger electron spectroscopy (AES), scanning electron microscopy (SEM), secondary ion mass spectrometry (SIMS), and mass accretion determined by quartz crystal microbalance (QCM). The discussion is biased toward those methods that apply optical thin film analytical techniques to spacecraft optical contamination problems. Examples are cited from both ground based and in-orbit experiments.

Development of a carbon-nanoparticle-coated stirrer for stir bar sorptive extraction by a simple carbon deposition in flame.

PubMed

Feng, Juanjuan; Sun, Min; Bu, Yanan; Luo, Chuannan

2016-03-01

Stir bar sorptive extraction is an environmentally friendly microextraction technique based on a stir bar with various sorbents. A commercial stirrer is a good support, but it has not been used in stir bar sorptive extraction due to difficult modification. A stirrer was modified with carbon nanoparticles by a simple carbon deposition process in flame and characterized by scanning electron microscopy and energy-dispersive X-ray spectrometry. A three-dimensional porous coating was formed with carbon nanoparticles. In combination with high-performance liquid chromatography, the stir bar was evaluated using five polycyclic aromatic hydrocarbons as model analytes. Conditions including extraction time and temperature, ionic strength, and desorption solvent were investigated by a factor-by-factor optimization method. The established method exhibited good linearity (0.01-10 μg/L) and low limits of quantification (0.01 μg/L). It was applied to detect model analytes in environmental water samples. No analyte was detected in river water, and five analytes were quantified in rain water. The recoveries of five analytes in two samples with spiked at 2 μg/L were in the range of 92.2-106% and 93.4-108%, respectively. The results indicated that the carbon nanoparticle-coated stirrer was an efficient stir bar for extraction analysis of some polycyclic aromatic hydrocarbons. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Validation and Application of a Simple UHPLC-MS-MS Method for the Enantiospecific Determination of Warfarin in Human Urine.

PubMed

Alshogran, Osama Y; Ocque, Andrew J; Leblond, François A; Pichette, Vincent; Nolin, Thomas D

2016-04-01

A simple and rapid liquid chromatographic-tandem mass spectrometric method has been developed and validated for the enantiospecific determination of R- and S-warfarin in human urine. Warfarin enantiomers were extracted from urine using methyl tert-butyl ether. Chromatographic separation of warfarin enantiomers and the internal standard d5-warfarin was achieved using a Astec Chirobiotic V column with gradient mobile phase at a flow rate of 400 µL/min over 10 min. Detection was performed on a TSQ Quantum Ultra triple quadrupole mass spectrometer equipped with a heated electrospray ionization source. Analytes were detected in negative ionization mode using selected reaction monitoring. Calibration curves were linear with a correlation coefficient of ≥0.996 for both enantiomers over a concentration range of 5-500 ng/mL. The intra- and interday accuracy and precision for both analytes were within ±9.0%. Excellent extraction efficiency and negligible matrix effects were observed. The applicability of the method was demonstrated by successful measurement of warfarin enantiomers in urine of patients with kidney disease. The method is simple, accurate and reproducible and is currently being used to support warfarin pharmacokinetic studies. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

A SIMPLE AND FAST EXTRACTION METHOD FOR ORGANOCHLORINE PESTICIDES AND POLYCHLORINATED BIPHENYLS IN SMALL VOLUMES OF AVIAN SERUM

EPA Science Inventory

A solid-phase extraction (SPE) method was developed using 8 M urea to desorb and extract organochlorine pesticides (OCs) and polychlorinated biphenyls (PCBs) from avian serum for analysis by capillary gas chromatography with electron capture detection (GC-ECD). The analytes were ...

Simple and Sensitive Paper-Based Device Coupling Electrochemical Sample Pretreatment and Colorimetric Detection.

PubMed

Silva, Thalita G; de Araujo, William R; Muñoz, Rodrigo A A; Richter, Eduardo M; Santana, Mário H P; Coltro, Wendell K T; Paixão, Thiago R L C

2016-05-17

We report the development of a simple, portable, low-cost, high-throughput visual colorimetric paper-based analytical device for the detection of procaine in seized cocaine samples. The interference of most common cutting agents found in cocaine samples was verified, and a novel electrochemical approach was used for sample pretreatment in order to increase the selectivity. Under the optimized experimental conditions, a linear analytical curve was obtained for procaine concentrations ranging from 5 to 60 μmol L(-1), with a detection limit of 0.9 μmol L(-1). The accuracy of the proposed method was evaluated using seized cocaine samples and an addition and recovery protocol.

Highly Accurate Analytical Approximate Solution to a Nonlinear Pseudo-Oscillator

NASA Astrophysics Data System (ADS)

Wu, Baisheng; Liu, Weijia; Lim, C. W.

2017-07-01

A second-order Newton method is presented to construct analytical approximate solutions to a nonlinear pseudo-oscillator in which the restoring force is inversely proportional to the dependent variable. The nonlinear equation is first expressed in a specific form, and it is then solved in two steps, a predictor and a corrector step. In each step, the harmonic balance method is used in an appropriate manner to obtain a set of linear algebraic equations. With only one simple second-order Newton iteration step, a short, explicit, and highly accurate analytical approximate solution can be derived. The approximate solutions are valid for all amplitudes of the pseudo-oscillator. Furthermore, the method incorporates second-order Taylor expansion in a natural way, and it is of significant faster convergence rate.

Simple determination of aflatoxins in rice by ultra-high performance liquid chromatography coupled to chemical post-column derivatization and fluorescence detection.

PubMed

Huertas-Pérez, José Fernando; Arroyo-Manzanares, Natalia; Hitzler, Dominik; Castro-Guerrero, Francisco Germán; Gámiz-Gracia, Laura; García-Campaña, Ana M

2018-04-15

A fast and simple analytical method was developed and characterized for the determination of aflatoxins (B 1 , B 2 , G 1 and G 2 ) in rice. The procedure is based on a simple solid-liquid extraction without further clean-up, and analysis by ultra-high performance liquid chromatography coupled with fluorescence detection. Fluorescence emission of aflatoxins B 1 and G 1 was enhanced by post-column chemical derivatization using pyridinium bromide perbromide. The analytical method was satisfactorily characterized in white and brown rice. Under optimum conditions, external calibration in solvent could be used for quantification purposes and limits of quantification were below the maximum contents established by the European Union regulation for these contaminants/commodity group combination (0.07-0.14 µg/kg for white rice and 0.20-0.28 µg/kg for brown rice). Recovery studies carried out at three different concentration levels (0.5, 2 and 5 µg/kg) showed values in the range of 84.5-105.3%, and RSDs ≤ 5%. Copyright © 2017 Elsevier Ltd. All rights reserved.

Analytical method for the fast time-domain reconstruction of fluorescent inclusions in vitro and in vivo.

PubMed

Han, Sung-Ho; Farshchi-Heydari, Salman; Hall, David J

2010-01-20

A novel time-domain optical method to reconstruct the relative concentration, lifetime, and depth of a fluorescent inclusion is described. We establish an analytical method for the estimations of these parameters for a localized fluorescent object directly from the simple evaluations of continuous wave intensity, exponential decay, and temporal position of the maximum of the fluorescence temporal point-spread function. Since the more complex full inversion process is not involved, this method permits a robust and fast processing in exploring the properties of a fluorescent inclusion. This method is confirmed by in vitro and in vivo experiments. Copyright 2010 Biophysical Society. Published by Elsevier Inc. All rights reserved.

Analytical Studies on the Synchronization of a Network of Linearly-Coupled Simple Chaotic Systems

NASA Astrophysics Data System (ADS)

Sivaganesh, G.; Arulgnanam, A.; Seethalakshmi, A. N.; Selvaraj, S.

2018-05-01

We present explicit generalized analytical solutions for a network of linearly-coupled simple chaotic systems. Analytical solutions are obtained for the normalized state equations of a network of linearly-coupled systems driven by a common chaotic drive system. Two parameter bifurcation diagrams revealing the various hidden synchronization regions, such as complete, phase and phase-lag synchronization are identified using the analytical results. The synchronization dynamics and their stability are studied using phase portraits and the master stability function, respectively. Further, experimental results for linearly-coupled simple chaotic systems are presented to confirm the analytical results. The synchronization dynamics of a network of chaotic systems studied analytically is reported for the first time.

Writing analytic element programs in Python.

PubMed

Bakker, Mark; Kelson, Victor A

2009-01-01

The analytic element method is a mesh-free approach for modeling ground water flow at both the local and the regional scale. With the advent of the Python object-oriented programming language, it has become relatively easy to write analytic element programs. In this article, an introduction is given of the basic principles of the analytic element method and of the Python programming language. A simple, yet flexible, object-oriented design is presented for analytic element codes using multiple inheritance. New types of analytic elements may be added without the need for any changes in the existing part of the code. The presented code may be used to model flow to wells (with either a specified discharge or drawdown) and streams (with a specified head). The code may be extended by any hydrogeologist with a healthy appetite for writing computer code to solve more complicated ground water flow problems. Copyright © 2009 The Author(s). Journal Compilation © 2009 National Ground Water Association.

An analytical approach to γ-ray self-shielding effects for radioactive bodies encountered nuclear decommissioning scenarios.

PubMed

Gamage, K A A; Joyce, M J

2011-10-01

A novel analytical approach is described that accounts for self-shielding of γ radiation in decommissioning scenarios. The approach is developed with plutonium-239, cobalt-60 and caesium-137 as examples; stainless steel and concrete have been chosen as the media for cobalt-60 and caesium-137, respectively. The analytical methods have been compared MCNPX 2.6.0 simulations. A simple, linear correction factor relates the analytical results and the simulated estimates. This has the potential to greatly simplify the estimation of self-shielding effects in decommissioning activities. Copyright © 2011 Elsevier Ltd. All rights reserved.

Ultimate Longitudinal Strength of Composite Ship Hulls

NASA Astrophysics Data System (ADS)

Zhang, Xiangming; Huang, Lingkai; Zhu, Libao; Tang, Yuhang; Wang, Anwen

2017-01-01

A simple analytical model to estimate the longitudinal strength of ship hulls in composite materials under buckling, material failure and ultimate collapse is presented in this paper. Ship hulls are regarded as assemblies of stiffened panels which idealized as group of plate-stiffener combinations. Ultimate strain of the plate-stiffener combination is predicted under buckling or material failure with composite beam-column theory. The effects of initial imperfection of ship hull and eccentricity of load are included. Corresponding longitudinal strengths of ship hull are derived in a straightforward method. A longitudinally framed ship hull made of symmetrically stacked unidirectional plies under sagging is analyzed. The results indicate that present analytical results have a good agreement with FEM method. The initial deflection of ship hull and eccentricity of load can dramatically reduce the bending capacity of ship hull. The proposed formulations provide a simple but useful tool for the longitudinal strength estimation in practical design.

Review of methods used for identification of biothreat agents in environmental protection and human health aspects.

PubMed

Mirski, Tomasz; Bartoszcze, Michał; Bielawska-Drózd, Agata; Cieślik, Piotr; Michalski, Aleksander J; Niemcewicz, Marcin; Kocik, Janusz; Chomiczewski, Krzysztof

2014-01-01

Modern threats of bioterrorism force the need to develop methods for rapid and accurate identification of dangerous biological agents. Currently, there are many types of methods used in this field of studies that are based on immunological or genetic techniques, or constitute a combination of both methods (immuno-genetic). There are also methods that have been developed on the basis of physical and chemical properties of the analytes. Each group of these analytical assays can be further divided into conventional methods (e.g. simple antigen-antibody reactions, classical PCR, real-time PCR), and modern technologies (e.g. microarray technology, aptamers, phosphors, etc.). Nanodiagnostics constitute another group of methods that utilize the objects at a nanoscale (below 100 nm). There are also integrated and automated diagnostic systems, which combine different methods and allow simultaneous sampling, extraction of genetic material and detection and identification of the analyte using genetic, as well as immunological techniques.

Development and Interlaboratory Validation of a Simple Screening Method for Genetically Modified Maize Using a ΔΔC(q)-Based Multiplex Real-Time PCR Assay.

PubMed

Noguchi, Akio; Nakamura, Kosuke; Sakata, Kozue; Sato-Fukuda, Nozomi; Ishigaki, Takumi; Mano, Junichi; Takabatake, Reona; Kitta, Kazumi; Teshima, Reiko; Kondo, Kazunari; Nishimaki-Mogami, Tomoko

2016-04-19

A number of genetically modified (GM) maize events have been developed and approved worldwide for commercial cultivation. A screening method is needed to monitor GM maize approved for commercialization in countries that mandate the labeling of foods containing a specified threshold level of GM crops. In Japan, a screening method has been implemented to monitor approved GM maize since 2001. However, the screening method currently used in Japan is time-consuming and requires generation of a calibration curve and experimental conversion factor (C(f)) value. We developed a simple screening method that avoids the need for a calibration curve and C(f) value. In this method, ΔC(q) values between the target sequences and the endogenous gene are calculated using multiplex real-time PCR, and the ΔΔC(q) value between the analytical and control samples is used as the criterion for determining analytical samples in which the GM organism content is below the threshold level for labeling of GM crops. An interlaboratory study indicated that the method is applicable independently with at least two models of PCR instruments used in this study.

Simultaneous determination of nikethamide and lidocaine in human blood and cerebrospinal fluid by high performance liquid chromatography.

PubMed

Chen, Lili; Liao, Linchuan; Zuo, Zhong; Yan, Youyi; Yang, Lin; Fu, Qiang; Chen, Yu; Hou, Junhong

2007-04-11

Nikethamide and lidocaine are often requested to be quantified simultaneously in forensic toxicological analysis. A simple reversed-phase high performance liquid chromatography (RP-HPLC) method has been developed for their simultaneous determination in human blood and cerebrospinal fluid. The method involves simple protein precipitation sample treatment followed by quantification of analytes using HPLC at 263 nm. Analytes were separated on a 5 microm Zorbax Dikema C18 column (150 mm x 4.60 mm, i.d.) with a mobile phase of 22:78 (v/v) mixture of methanol and a diethylamine-acetic acid buffer, pH 4.0. The mean recoveries were between 69.8 and 94.4% for nikethamide and between 78.9 and 97.2% for lidocaine. Limits of detection (LODs) for nikethamide and lidocaine were 0.008 and 0.16 microg/ml in plasma and 0.007 and 0.14 microg/ml in cerebrospinal fluid, respectively. The mean intra-assay and inter-assay coefficients of variation (CVs) for both analytes were less than 9.2 and 10.8%, respectively. The developed method was applied to blood sample analyses in eight forensic cases, where blood concentrations of lidocaine ranged from 0.68 to 34.4 microg/ml and nikethamide ranged from 1.25 to 106.8 microg/ml. In six cases cerebrospinal fluid analysis was requested. The values ranged from 20.3 to 185.6 microg/ml of lidocaine and 8.0 to 72.4 microg/ml of nikethamide. The method is simple and sensitive enough to be used in toxicological analysis for simultaneous determination of nikethamide and lidocaine in blood and cerebrospinal fluid.

A simple validated multi-analyte method for detecting drugs in oral fluid by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).

PubMed

Zheng, Yufang; Sparve, Erik; Bergström, Mats

2018-06-01

A UPLC-MS/MS method was developed to identify and quantitate 37 commonly abused drugs in oral fluid. Drugs of interest included amphetamines, benzodiazepines, cocaine, opiates, opioids, phencyclidine and tetrahydrocannabinol. Sample preparation and extraction are simple, and analysis times short. Validation showed satisfactory performance at relevant concentrations. The possibility of contaminated samples as well as the interpretation in relation to well-knows matrices, such as urine, will demand further study. Copyright © 2017 John Wiley & Sons, Ltd.

INTERNATIONAL CONFERENCE ON SEMICONDUCTOR INJECTION LASERS SELCO-87: Simple formula for the thermal conductivity of a quaternary solid solution

NASA Astrophysics Data System (ADS)

Nakwaski, W.

1988-11-01

An analysis is made of the thermal conductivity of quaternary solid solutions (alloys) allowing for their disordered structure on the basis of a phenomenological analysis proposed by Abeles. This method is applied to a quaternary solid solution In1 - xGaxAsyP1 - y. A simple analytic expression is derived for the thermal conductivity of this material.

Current distribution in a three-dimensional IC analyzed by a perturbation method. Part 1: A simple steady state theory

NASA Technical Reports Server (NTRS)

Edmonds, Larry D.

1987-01-01

The steady state current distribution in a three dimensional integrated circuit is presented. A device physics approach, based on a perturbation method rather than an equivalent lumped circuit approach, is used. The perturbation method allows the various currents to be expressed in terms of elementary solutions which are solutions to very simple boundary value problems. A Simple Steady State Theory is the subtitle because the most obvious limitation of the present version of the analysis is that all depletion region boundary surfaces are treated as equipotential surfaces. This may be an adequate approximation in some applications but it is an obvious weakness in the theory when applied to latched states. Examples that illustrate the use of these analytical methods are not given because they will be presented in detail in the future.

Simple column-switching ion chromatography method for determining eight monosaccharides and oligosaccharides in honeydew and nectar.

PubMed

Ni, Chengzhu; Zhu, Binhe; Wang, Nani; Wang, Muhua; Chen, Suqing; Zhang, Jiajie; Zhu, Yan

2016-03-01

Honeydew is excreted by aphids as a sweet waste and nectar is floral honey. Honeydew and nectar are complicated samples which consist of various sugars and amino acids. In this work, a simple ion chromatography with column-switching method was developed for the simultaneous analysis of 8 monosaccharides and oligosaccharides in honeydew and nectar. A reversed-phase column was used as a pretreatment column to eliminate organics on-line and sugars were eluted from a collection loop to analytical column by using column-switching technique. This method showed good linearity (r⩾0.9994) and afforded low limits of detection ranging from 1.55 to 10.17μgL(-1) for all the analytes. Recoveries ranged from 95% to 105% and repeatability results were acceptable with relative standard deviation of less than 3.21% (n=6). This method was successfully applied to quantification of these sugars in honeydew and nectar. These results showed honeydew had much more oligosaccharides than nectar. Copyright © 2015 Elsevier Ltd. All rights reserved.

Development and Validation of a Simple High Performance Liquid Chromatography/UV Method for Simultaneous Determination of Urinary Uric Acid, Hypoxanthine, and Creatinine in Human Urine.

PubMed

Wijemanne, Nimanthi; Soysa, Preethi; Wijesundara, Sulochana; Perera, Hemamali

2018-01-01

Uric acid and hypoxanthine are produced in the catabolism of purine. Abnormal urinary levels of these products are associated with many diseases and therefore it is necessary to have a simple and rapid method to detect them. Hence, we report a simple reverse phase high performance liquid chromatography (HPLC/UV) technique, developed and validated for simultaneous analysis of uric acid, hypoxanthine, and creatinine in human urine. Urine was diluted appropriately and eluted with C-18 column 100 mm × 4.6 mm with a C-18 precolumn 25 mm × 4.6 mm in series. Potassium phosphate buffer (20 mM, pH 7.25) at a flow rate of 0.40 mL/min was employed as the solvent and peaks were detected at 235 nm. Tyrosine was used as the internal standard. The experimental conditions offered a good separation of analytes without interference of endogenous substances. The calibration curves were linear for all test compounds with a regression coefficient, r 2 > 0.99. Uric acid, creatinine, tyrosine, and hypoxanthine were eluted at 5.2, 6.1, 7.2, and 8.3 min, respectively. Intraday and interday variability were less than 4.6% for all the analytes investigated and the recovery ranged from 98 to 102%. The proposed HPLC procedure is a simple, rapid, and low cost method with high accuracy with minimum use of organic solvents. This method was successfully applied for the determination of creatinine, hypoxanthine, and uric acid in human urine.

Determination of the transmission coefficients for quantum structures using FDTD method.

PubMed

Peng, Yangyang; Wang, Xiaoying; Sui, Wenquan

2011-12-01

The purpose of this work is to develop a simple method to incorporate quantum effect in traditional finite-difference time-domain (FDTD) simulators. Witch could make it possible to co-simulate systems include quantum structures and traditional components. In this paper, tunneling transmission coefficient is calculated by solving time-domain Schrödinger equation with a developed FDTD technique, called FDTD-S method. To validate the feasibility of the method, a simple resonant tunneling diode (RTD) structure model has been simulated using the proposed method. The good agreement between the numerical and analytical results proves its accuracy. The effectness and accuracy of this approach makes it a potential method for analysis and design of hybrid systems includes quantum structures and traditional components.

Genetics-based methods for detection of Salmonella spp. in foods.

PubMed

Mozola, Mark A

2006-01-01

Genetic methods are now at the forefront of foodborne pathogen testing. The sensitivity, specificity, and inclusivity advantages offered by deoxyribonucleic acid (DNA) probe technology have driven an intense effort in methods development over the past 20 years. DNA probe-based methods for Salmonella spp. and other pathogens have progressed from time-consuming procedures involving the use of radioisotopes to simple, high throughput, automated assays. The analytical sensitivity of nucleic acid amplification technology has facilitated a reduction in analysis time by allowing enriched samples to be tested for previously undetectable quantities of analyte. This article will trace the evolution of the development of genetic methods for detection of Salmonella in foods, review the basic assay formats and their advantages and limitations, and discuss method performance characteristics and considerations for selection of methods.

Development of a Terbium-Sensitized Fluorescence Method for Analysis of Silibinin.

PubMed

Ershadi, Saba; Jouyban, Abolghasem; Molavi, Ommoleila; Shayanfar, Ali

2017-05-01

Silibinin is a natural flavonoid with potent anticancer properties, as shown in both in vitro and in vivo experiments. Various methods have been used for silibinin analysis. Terbium-sensitized fluorescence methods have been widely used for the determination of drugs in pharmaceutical preparations and biological samples in recent years. The present work is aimed at providing a simple analytical method for the quantitative determination of silibinin in aqueous solutions based on the formation of a fluorescent complex with terbium ion. Terbium concentration, pH, and volume of buffer, the important effective parameters for the determination of silibinin by the proposed method, were optimized using response surface methodology. The fluorescence intensity of silibinin was measured at 545 nm using λex = 334 nm. The developed method was applied for the determination of silibinin in plasma samples after protein precipitation with acetone. Under optimum conditions, the method provided a linear range between 0.10 and 0.50 mg/L, with a coefficient of determination (R2) of 0.997. The LOD and LOQ were 0.034 and 0.112 mg/L, respectively. These results indicate that the developed method is a simple, low-cost, and suitable analytical method for the quantification of silibinin in aqueous solution and plasma samples.

Fokker-Planck Equations of Stochastic Acceleration: A Study of Numerical Methods

NASA Astrophysics Data System (ADS)

Park, Brian T.; Petrosian, Vahe

1996-03-01

Stochastic wave-particle acceleration may be responsible for producing suprathermal particles in many astrophysical situations. The process can be described as a diffusion process through the Fokker-Planck equation. If the acceleration region is homogeneous and the scattering mean free path is much smaller than both the energy change mean free path and the size of the acceleration region, then the Fokker-Planck equation reduces to a simple form involving only the time and energy variables. in an earlier paper (Park & Petrosian 1995, hereafter Paper 1), we studied the analytic properties of the Fokker-Planck equation and found analytic solutions for some simple cases. In this paper, we study the numerical methods which must be used to solve more general forms of the equation. Two classes of numerical methods are finite difference methods and Monte Carlo simulations. We examine six finite difference methods, three fully implicit and three semi-implicit, and a stochastic simulation method which uses the exact correspondence between the Fokker-Planck equation and the it5 stochastic differential equation. As discussed in Paper I, Fokker-Planck equations derived under the above approximations are singular, causing problems with boundary conditions and numerical overflow and underflow. We evaluate each method using three sample equations to test its stability, accuracy, efficiency, and robustness for both time-dependent and steady state solutions. We conclude that the most robust finite difference method is the fully implicit Chang-Cooper method, with minor extensions to account for the escape and injection terms. Other methods suffer from stability and accuracy problems when dealing with some Fokker-Planck equations. The stochastic simulation method, although simple to implement, is susceptible to Poisson noise when insufficient test particles are used and is computationally very expensive compared to the finite difference method.

Validation of Analytical Damping Ratio by Fatigue Stress Limit

NASA Astrophysics Data System (ADS)

Foong, Faruq Muhammad; Chung Ket, Thein; Beng Lee, Ooi; Aziz, Abdul Rashid Abdul

2018-03-01

The optimisation process of a vibration energy harvester is usually restricted to experimental approaches due to the lack of an analytical equation to describe the damping of a system. This study derives an analytical equation, which describes the first mode damping ratio of a clamp-free cantilever beam under harmonic base excitation by combining the transverse equation of motion of the beam with the damping-stress equation. This equation, as opposed to other common damping determination methods, is independent of experimental inputs or finite element simulations and can be solved using a simple iterative convergence method. The derived equation was determined to be correct for cases when the maximum bending stress in the beam is below the fatigue limit stress of the beam. However, an increasing trend in the error between the experiment and the analytical results were observed at high stress levels. Hence, the fatigue limit stress was used as a parameter to define the validity of the analytical equation.

Simultaneous determination of carotenoids, tocopherols, retinol and cholesterol in ovine lyophilised samples of milk, meat, and liver and in unprocessed/raw samples of fat.

PubMed

Bertolín, J R; Joy, M; Rufino-Moya, P J; Lobón, S; Blanco, M

2018-08-15

An accurate, fast, economic and simple method to determine carotenoids, tocopherols, retinol and cholesterol in lyophilised samples of ovine milk, muscle and liver and raw samples of fat, which are difficult to lyophilise, is sought. Those analytes have been studied in animal tissues to trace forage feeding and unhealthy contents. The sample treatment consisted of mild overnight saponification, liquid-liquid extraction, evaporation with vacuum evaporator and redissolution. The quantification of the different analytes was performed by the use of ultra-high performance liquid chromatography with diode-array detector for carotenoids, retinol and cholesterol and fluorescence detector for tocopherols. The retention times of the analytes were short and the resolution between analytes was very high. The limits of detection and quantification were very low. This method is suitable for all the matrices and analytes and could be adapted to other animal species with minor changes. Copyright © 2018 Elsevier Ltd. All rights reserved.

A simple and sensitive method for the determination of fibric acids in the liver by liquid chromatography.

PubMed

Karahashi, Minako; Fukuhara, Hiroto; Hoshina, Miki; Sakamoto, Takeshi; Yamazaki, Tohru; Mitsumoto, Atsushi; Kawashima, Yoichi; Kudo, Naomi

2014-01-01

Fibrates are used in biochemical and pharmacological studies as bioactive tools. Nevertheless, most studies have lacked information concerning the concentrations of fibric acids working inside tissues because a simple and sensitive method is not available for their quantitation. This study aimed to develop a simple and sensitive bioanalytical method for the quantitation of clofibric, bezafibric and fenofibric acids in samples of very small portions of tissues. Fibric acids were extracted into n-hexane-ethyl acetate from tissue homogenates (10 mg of liver, kidney or muscle) or serum (100 µL) and were derivatized with 4-bromomethyl-6,7-dimethoxycoumarin, followed by HPLC with fluorescence detection. These compounds were separated isocratically on a reversed phase with acetonitrile-water. Standard analytical curves were linear over the concentration range of 0.2-20 nmol/10 mg of liver. Precision and accuracy were within acceptable limits. Recovery from liver homogenates ranged from 93.03 to 112.29%. This method enabled the quantitation of fibric acids in 10 mg of liver from rats treated with clofibric acid, bezafibric acid or fenofibrate. From these analytical data, it became clear that there was no large difference in ratio of acyl-CoA oxidase 1 (Acox1) mRNA level to fibric acid content in the liver among the three fibric acids, suggesting that these three fibric acids have similar potency to increase expression of the Acox1 gene, which is a target of peroxisome proliferator-activated receptor α. Thus, the proposed method is a simple, sensitive and reliable tool for the quantitation of fibric acids working in vivo inside livers.

Recent advances in analytical methods for the determination of 4-alkylphenols and bisphenol A in solid environmental matrices: A critical review.

PubMed

Salgueiro-González, N; Castiglioni, S; Zuccato, E; Turnes-Carou, I; López-Mahía, P; Muniategui-Lorenzo, S

2018-09-18

The problem of endocrine disrupting compounds (EDCs) in the environment has become a worldwide concern in recent decades. Besides their toxicological effects at low concentrations and their widespread use in industrial and household applications, these pollutants pose a risk for non-target organisms and also for public safety. Analytical methods to determine these compounds at trace levels in different matrices are urgently needed. This review critically discusses trends in analytical methods for well-known EDCs like alkylphenols and bisphenol A in solid environmental matrices, including sediment and aquatic biological samples (from 2006 to 2018). Information about extraction, clean-up and determination is covered in detail, including analytical quality parameters (QA/QC). Conventional and novel analytical techniques are compared, with their advantages and drawbacks. Ultrasound assisted extraction followed by solid phase extraction clean-up is the most widely used procedure for sediment and aquatic biological samples, although softer extraction conditions have been employed for the latter. The use of liquid chromatography followed by tandem mass spectrometry has greatly increased in the last five years. The majority of these methods have been employed for the analysis of river sediments and bivalve molluscs because of their usefulness in aquatic ecosystem (bio)monitoring programs. Green, simple, fast analytical methods are now needed to determine these compounds in complex matrices. Copyright © 2018 Elsevier B.V. All rights reserved.

A pipette-based calibration system for fast-scan cyclic voltammetry with fast response times.

PubMed

Ramsson, Eric S

2016-01-01

Fast-scan cyclic voltammetry (FSCV) is an electrochemical technique that utilizes the oxidation and/or reduction of an analyte of interest to infer rapid changes in concentrations. In order to calibrate the resulting oxidative or reductive current, known concentrations of an analyte must be introduced under controlled settings. Here, I describe a simple and cost-effective method, using a Petri dish and pipettes, for the calibration of carbon fiber microelectrodes (CFMs) using FSCV.

Fabrication of plasmonic cavity arrays for SERS analysis

NASA Astrophysics Data System (ADS)

Li, Ning; Feng, Lei; Teng, Fei; Lu, Nan

2017-05-01

The plasmonic cavity arrays are ideal substrates for surface enhanced Raman scattering analysis because they can provide hot spots with large volume for analyte molecules. The large area increases the probability to make more analyte molecules on hot spots and leads to a high reproducibility. Therefore, to develop a simple method for creating cavity arrays is important. Herein, we demonstrate how to fabricate a V and W shape cavity arrays by a simple method based on self-assembly. Briefly, the V and W shape cavity arrays are respectively fabricated by taking KOH etching on a nanohole and a nanoring array patterned silicon (Si) slides. The nanohole array is generated by taking a reactive ion etching on a Si slide assembled with monolayer of polystyrene (PS) spheres. The nanoring array is generated by taking a reactive ion etching on a Si slide covered with a monolayer of octadecyltrichlorosilane before self-assembling PS spheres. Both plasmonic V and W cavity arrays can provide large hot area, which increases the probability for analyte molecules to deposit on the hot spots. Taking 4-Mercaptopyridine as analyte probe, the enhancement factor can reach 2.99 × 105 and 9.97 × 105 for plasmonic V cavity and W cavity array, respectively. The relative standard deviations of the plasmonic V and W cavity arrays are 6.5% and 10.2% respectively according to the spectra collected on 20 random spots.

Fabrication of plasmonic cavity arrays for SERS analysis.

PubMed

Li, Ning; Feng, Lei; Teng, Fei; Lu, Nan

2017-05-05

The plasmonic cavity arrays are ideal substrates for surface enhanced Raman scattering analysis because they can provide hot spots with large volume for analyte molecules. The large area increases the probability to make more analyte molecules on hot spots and leads to a high reproducibility. Therefore, to develop a simple method for creating cavity arrays is important. Herein, we demonstrate how to fabricate a V and W shape cavity arrays by a simple method based on self-assembly. Briefly, the V and W shape cavity arrays are respectively fabricated by taking KOH etching on a nanohole and a nanoring array patterned silicon (Si) slides. The nanohole array is generated by taking a reactive ion etching on a Si slide assembled with monolayer of polystyrene (PS) spheres. The nanoring array is generated by taking a reactive ion etching on a Si slide covered with a monolayer of octadecyltrichlorosilane before self-assembling PS spheres. Both plasmonic V and W cavity arrays can provide large hot area, which increases the probability for analyte molecules to deposit on the hot spots. Taking 4-Mercaptopyridine as analyte probe, the enhancement factor can reach 2.99 × 10 5 and 9.97 × 10 5 for plasmonic V cavity and W cavity array, respectively. The relative standard deviations of the plasmonic V and W cavity arrays are 6.5% and 10.2% respectively according to the spectra collected on 20 random spots.

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.

Simple HPLC method for detection of trace ephedrine and pseudoephedrine in high-purity methamphetamine.

PubMed

Makino, Yukiko

2012-03-01

A simple and sensitive HPLC technique was developed for the qualitative determination of ephedrine and pseudoephedrine (ephedrines), used as precursors of clandestine d-methamphetamine hydrochloride of high purity. Good separation of ephedrines from bulk d-methamphetamine was achieved, without any extraction or derivatization procedure on a CAPCELLPACK C18 MGII (250 × 4.6 mm) column. The mobile phase consisted of 50 mM KH2 PO4-acetonitrile (94:6 v/v %) using an isocratic pump system within 20 min for detecting two analytes. One run took about 50 min as it was necessary to wash out overloaded methamphetamine for column conditioning. The analytes were detected by UV absorbance measurement at 210 nm. A sample (20 mg) was simply dissolved in 1 mL of water, and a 50 μL aliquot of the solution was injected into the HPLC. The detection limits for ephedrine and pseudoephedrine in bulk d-methamphetamine were as low as 3 ppm each. This analytical separation technique made it possible to detect ephedrine and/or pseudoephedrine in seven samples of high-purity d-methamphetamine hydrochloride seized in Japan. The presence of trace ephedrines in illicit methamphetamine may strongly indicate a synthetic route via ephedrine in methamphetamine profiling. This method is simple and sensitive, requiring only commonly available equipment, and should be useful for high-purity methamphetamine profiling. Copyright © 2011 John Wiley & Sons, Ltd.

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...

Monte Carlo investigation of transient acoustic fields in partially or completely bounded medium. Ph.D. Thesis

NASA Technical Reports Server (NTRS)

Thanedar, B. D.

1972-01-01

A simple repetitive calculation was used to investigate what happens to the field in terms of the signal paths of disturbances originating from the energy source. The computation allowed the field to be reconstructed as a function of space and time on a statistical basis. The suggested Monte Carlo method is in response to the need for a numerical method to supplement analytical methods of solution which are only valid when the boundaries have simple shapes, rather than for a medium that is bounded. For the analysis, a suitable model was created from which was developed an algorithm for the estimation of acoustic pressure variations in the region under investigation. The validity of the technique was demonstrated by analysis of simple physical models with the aid of a digital computer. The Monte Carlo method is applicable to a medium which is homogeneous and is enclosed by either rectangular or curved boundaries.

Extension of rezoned Eulerian-Lagrangian method to astrophysical plasma applications

NASA Technical Reports Server (NTRS)

Song, M. T.; Wu, S. T.; Dryer, Murray

1993-01-01

The rezoned Eulerian-Lagrangian procedure developed by Brackbill and Pracht (1973), which is limited to simple configurations of the magnetic fields, is modified in order to make it applicable to astrophysical plasma. For this purpose, two specific methods are introduced, which make it possible to determine the initial field topology for which no analytical expressions are available. Numerical examples illustrating these methods are presented.

Analytical Assessment for Transient Stability Under Stochastic Continuous Disturbances

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

Ju, Ping; Li, Hongyu; Gan, Chun

Here, with the growing integration of renewable power generation, plug-in electric vehicles, and other sources of uncertainty, increasing stochastic continuous disturbances are brought to power systems. The impact of stochastic continuous disturbances on power system transient stability attracts significant attention. To address this problem, this paper proposes an analytical assessment method for transient stability of multi-machine power systems under stochastic continuous disturbances. In the proposed method, a probability measure of transient stability is presented and analytically solved by stochastic averaging. Compared with the conventional method (Monte Carlo simulation), the proposed method is many orders of magnitude faster, which makes itmore » very attractive in practice when many plans for transient stability must be compared or when transient stability must be analyzed quickly. Also, it is found that the evolution of system energy over time is almost a simple diffusion process by the proposed method, which explains the impact mechanism of stochastic continuous disturbances on transient stability in theory.« less

A facile fluorescent "turn-off" method for sensing paraquat based on pyranine-paraquat interaction

NASA Astrophysics Data System (ADS)

Zhao, Zuzhi; Zhang, Fengwei; Zhang, Zipin

2018-06-01

Development of a technically simple yet effective method for paraquat (PQ) detection is of great importance due to its high clinical and environmental relevance. In this study, we developed a pyranine-based fluorescent "turn-off" method for PQ sensing based on pyranine-PQ interaction. We investigated the dependence of analytical performance of this method on the experimental conditions, such as the ion strength, medium pH, and so on. Under the optimized conditions, the method is sensitive and selective, and could be used for PQ detection in real-world sample. This study essentially provides a readily accessible fluorescent system for PQ sensing which is cheap, robust, and technically simple, and it is envisaged to find more interesting clinical and environmental applications.

Screen-printed electrode-based electrochemical detector coupled with in-situ ionic-liquid-assisted dispersive liquid-liquid microextraction for determination of 2,4,6-trinitrotoluene.

PubMed

Fernández, Elena; Vidal, Lorena; Iniesta, Jesús; Metters, Jonathan P; Banks, Craig E; Canals, Antonio

2014-03-01

A novel method is reported, whereby screen-printed electrodes (SPELs) are combined with dispersive liquid-liquid microextraction. In-situ ionic liquid (IL) formation was used as an extractant phase in the microextraction technique and proved to be a simple, fast and inexpensive analytical method. This approach uses miniaturized systems both in sample preparation and in the detection stage, helping to develop environmentally friendly analytical methods and portable devices to enable rapid and onsite measurement. The microextraction method is based on a simple metathesis reaction, in which a water-immiscible IL (1-hexyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide, [Hmim][NTf2]) is formed from a water-miscible IL (1-hexyl-3-methylimidazolium chloride, [Hmim][Cl]) and an ion-exchange reagent (lithium bis[(trifluoromethyl)sulfonyl]imide, LiNTf2) in sample solutions. The explosive 2,4,6-trinitrotoluene (TNT) was used as a model analyte to develop the method. The electrochemical behavior of TNT in [Hmim][NTf2] has been studied in SPELs. The extraction method was first optimized by use of a two-step multivariate optimization strategy, using Plackett-Burman and central composite designs. The method was then evaluated under optimum conditions and a good level of linearity was obtained, with a correlation coefficient of 0.9990. Limits of detection and quantification were 7 μg L(-1) and 9 μg L(-1), respectively. The repeatability of the proposed method was evaluated at two different spiking levels (20 and 50 μg L(-1)), and coefficients of variation of 7 % and 5 % (n = 5) were obtained. Tap water and industrial wastewater were selected as real-world water samples to assess the applicability of the method.

Determination of dimethyltryptamine and β-carbolines (ayahuasca alkaloids) in plasma samples by LC-MS/MS.

PubMed

Oliveira, Carolina Dizioli Rodrigues; Okai, Guilherme Gonçalves; da Costa, José Luiz; de Almeida, Rafael Menck; Oliveira-Silva, Diogo; Yonamine, Mauricio

2012-07-01

Ayahuasca is a psychoactive plant beverage originally used by indigenous people throughout the Amazon Basin, long before its modern use by syncretic religious groups established in Brazil, the USA and European countries. The objective of this study was to develop a method for quantification of dimethyltryptamine and β-carbolines in human plasma samples. The analytes were extracted by means of C18 cartridges and injected into LC-MS/MS, operated in positive ion mode and multiple reaction monitoring. The LOQs obtained for all analytes were below 0.5 ng/ml. By using the weighted least squares linear regression, the accuracy of the analytical method was improved at the lower end of the calibration curve (from 0.5 to 100 ng/ml; r(2)> 0.98). The method proved to be simple, rapid and useful to estimate administered doses for further pharmacological and toxicological investigations of ayahuasca exposure.

Immunoanalysis Methods for the Detection of Dioxins and Related Chemicals

PubMed Central

Tian, Wenjing; Xie, Heidi Qunhui; Fu, Hualing; Pei, Xinhui; Zhao, Bin

2012-01-01

With the development of biotechnology, approaches based on antibodies, such as enzyme-linked immunosorbent assay (ELISA), active aryl hydrocarbon immunoassay (Ah-I) and other multi-analyte immunoassays, have been utilized as alternatives to the conventional techniques based on gas chromatography and mass spectroscopy for the analysis of dioxin and dioxin-like compounds in environmental and biological samples. These screening methods have been verified as rapid, simple and cost-effective. This paper provides an overview on the development and application of antibody-based approaches, such as ELISA, Ah-I, and multi-analyte immunoassays, covering the sample extraction and cleanup, antigen design, antibody preparation and immunoanalysis. However, in order to meet the requirements for on-site fast detection and relative quantification of dioxins in the environment, further optimization is needed to make these immuno-analytical methods more sensitive and easy to use. PMID:23443395

Calculated and measured fields in superferric wiggler magnets

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

Blum, E.B.; Solomon, L.

1995-02-01

Although Klaus Halbach is widely known and appreciated as the originator of the computer program POISSON for electromagnetic field calculation, Klaus has always believed that analytical methods can give much more insight into the performance of a magnet than numerical simulation. Analytical approximations readily show how the different aspects of a magnet`s design such as pole dimensions, current, and coil configuration contribute to the performance. These methods yield accuracies of better than 10%. Analytical methods should therefore be used when conceptualizing a magnet design. Computer analysis can then be used for refinement. A simple model is presented for the peakmore » on-axis field of an electro-magnetic wiggler with iron poles and superconducting coils. The model is applied to the radiator section of the superconducting wiggler for the BNL Harmonic Generation Free Electron Laser. The predictions of the model are compared to the measured field and the results from POISSON.« less

Application of the backward extrapolation method to pulsed neutron sources

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

Talamo, Alberto; Gohar, Yousry

We report particle detectors operated in pulse mode are subjected to the dead-time effect. When the average of the detector counts is constant over time, correcting for the dead-time effect is simple and can be accomplished by analytical formulas. However, when the average of the detector counts changes over time it is more difficult to take into account the dead-time effect. When a subcritical nuclear assembly is driven by a pulsed neutron source, simple analytical formulas cannot be applied to the measured detector counts to correct for the dead-time effect because of the sharp change of the detector counts overmore » time. This work addresses this issue by using the backward extrapolation method. The latter can be applied not only to a continuous (e.g. californium) external neutron source but also to a pulsed external neutron source (e.g. by a particle accelerator) driving a subcritical nuclear assembly. Finally, the backward extrapolation method allows to obtain from the measured detector counts both the dead-time value and the real detector counts.« less

Application of the backward extrapolation method to pulsed neutron sources

DOE PAGES

Talamo, Alberto; Gohar, Yousry

2017-09-23

We report particle detectors operated in pulse mode are subjected to the dead-time effect. When the average of the detector counts is constant over time, correcting for the dead-time effect is simple and can be accomplished by analytical formulas. However, when the average of the detector counts changes over time it is more difficult to take into account the dead-time effect. When a subcritical nuclear assembly is driven by a pulsed neutron source, simple analytical formulas cannot be applied to the measured detector counts to correct for the dead-time effect because of the sharp change of the detector counts overmore » time. This work addresses this issue by using the backward extrapolation method. The latter can be applied not only to a continuous (e.g. californium) external neutron source but also to a pulsed external neutron source (e.g. by a particle accelerator) driving a subcritical nuclear assembly. Finally, the backward extrapolation method allows to obtain from the measured detector counts both the dead-time value and the real detector counts.« less

3-D discrete analytical ridgelet transform.

PubMed

Helbert, David; Carré, Philippe; Andres, Eric

2006-12-01

In this paper, we propose an implementation of the 3-D Ridgelet transform: the 3-D discrete analytical Ridgelet transform (3-D DART). This transform uses the Fourier strategy for the computation of the associated 3-D discrete Radon transform. The innovative step is the definition of a discrete 3-D transform with the discrete analytical geometry theory by the construction of 3-D discrete analytical lines in the Fourier domain. We propose two types of 3-D discrete lines: 3-D discrete radial lines going through the origin defined from their orthogonal projections and 3-D planes covered with 2-D discrete line segments. These discrete analytical lines have a parameter called arithmetical thickness, allowing us to define a 3-D DART adapted to a specific application. Indeed, the 3-D DART representation is not orthogonal, It is associated with a flexible redundancy factor. The 3-D DART has a very simple forward/inverse algorithm that provides an exact reconstruction without any iterative method. In order to illustrate the potentiality of this new discrete transform, we apply the 3-D DART and its extension to the Local-DART (with smooth windowing) to the denoising of 3-D image and color video. These experimental results show that the simple thresholding of the 3-D DART coefficients is efficient.

Analysis of Bisphenol A, Alkylphenols, and Alkylphenol Ethoxylates in NIST SRM 2585 and Indoor House Dust by Gas Chromatography-Tandem Mass Spectrometry (GC/MS/MS).

PubMed

Fan, Xinghua; Kubwabo, Cariton; Wu, Fang; Rasmussen, Pat E

2018-06-26

Background: Ingestion of house dust has been demonstrated to be an important exposure pathway to several contaminants in young children. These compounds include bisphenol A (BPA), alkylphenols (APs), and alkylphenol ethoxylates (APEOs). Analysis of these compounds in house dust is challenging because of the complex composition of the sample matrix. Objective: The objective was to develop a simple and sensitive method to measure BPA, APs, and APEOs in indoor house dust. Methods: An integrated method that involved solvent extraction using sonication, sample cleanup by solid-phase extraction, derivatization by 2,2,2-trifluoro- N -methyl- N -(trimethylsilyl)acetamide, and analysis by GC coupled with tandem MS was developed for the simultaneous determination of BPA, APs, and APEOs in NIST Standard Reference Material (SRM) 2585 (Organic contaminants in house dust) and in settled house dust samples. Results: Target analytes included BPA, 4- tert -octylphenol (OP), OP monoethoxylate, OP diethoxylate, 4- n -nonylphenol (4 n NP), 4 n NP monoethoxylate (4 n NP 1 EO), branched nonylphenol (NP), NP monoethoxylate, NP diethoxylate, NP triethoxylate, and NP tetraethoxylate. The method was sensitive, with method detection limits ranging from 0.05 to 5.1 μg/g, and average recoveries between 82 and 115%. All target analytes were detected in SRM 2585 and house dust except 4 n NP and 4 n NP 1 EO. Conclusions: The method is simple and fast, with high sensitivity and good reproducibility. It is applicable to the analysis of target analytes in similar matrixes, such as sediments, soil, and biosolids. Highlights: Values measured in SRM 2585 will be useful for future research in method development and method comparison.

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.

Instrumental Surveillance of Water Quality.

ERIC Educational Resources Information Center

Miller, J. A.; And Others

The role analytical instrumentation performs in the surveillance and control of the quality of water resources is reviewed. Commonly performed analyses may range from simple tests for physical parameters to more highly sophisticated radiological or spectrophotometric methods. This publication explores many of these types of water quality analyses…

A SIMPLE COLORIMETRIC METHOD TO DETECT BIOLOGICAL EVIDENCE OF HUMAN EXPOSURE TO MICROCYSTINS

EPA Science Inventory

Toxic cyanobacteria are contaminants of surface waters worldwide. Microcystins are some of the most commonly detected toxins. Biological evidence of human exposure may be difficult to obtain due to limitations associated with cost, laboratory capacity, analytic support, and exp...

Rapid determination of minoxidil in human plasma using ion-pair HPLC.

PubMed

Zarghi, A; Shafaati, A; Foroutan, S M; Khoddam, A

2004-10-29

A rapid, simple and sensitive ion-pair high-performance liquid chromatography (HPLC) method has been developed for quantification of minoxidil in plasma. The assay enables the measurement of minoxidil for therapeutic drug monitoring with a minimum detectable limit of 0.5 ng ml(-1). The method involves simple, one-step extraction procedure and analytical recovery was complete. The separation was performed on an analytical 150 x 4.6 mm i.d. microbondapak C18 column. The wavelength was set at 281 nm. The mobile phase was a mixture of 0.01 M sodium dihydrogen phosphate buffer and acetonitrile (60:40, v/v) containing 2.5 mM sodium dodecyl sulphate adjusted to pH 3.5 at a flow rate of 1 ml/min. The column temperature was set at 50 degrees C. The calibration curve was linear over the concentration range 2-100 ng ml(-1). The coefficients of variation for inter-day and intra-day assay were found to be less than 8%.

Development and validation of a simple UHPLC-MS/MS method for the simultaneous determination of trimethylamine N-oxide, choline, and betaine in human plasma and urine.

PubMed

Ocque, Andrew J; Stubbs, Jason R; Nolin, Thomas D

2015-05-10

A simple, sensitive, and precise ultra-high performance liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous determination of trimethylamine N-oxide, choline, and betaine in human plasma and urine. Sample preparation involved protein precipitation with methanol containing internal standards. Chromatographic separation was achieved using an Acquity BEH Amide (2.1mm×50mm, 1.7μm) analytical column with gradient elution of solvent A (10mM ammonium formate, pH 3.5) and solvent B (acetonitrile). The flow rate was 0.4mL/min and the total run time was 5min. Detection of analytes was performed using heated electrospray ionization (positive mode) and selected reaction monitoring. Excellent linearity was observed over the standard curve concentration ranges of 0.010-5.00μg/mL (plasma) and 1.00-150μg/mL (urine) for all analytes. The intra- and inter-day accuracy and precision for all quality controls were within ±10%. Excellent recovery was observed. The method is rapid, accurate and reproducible, and was successfully applied to a pilot study of markers of atherosclerosis in patients with kidney disease who underwent successful kidney transplantation. Copyright © 2015 Elsevier B.V. All rights reserved.

Headspace-SPME-GC/MS as a simple cleanup tool for sensitive 2,6-diisopropylphenol analysis from lipid emulsions and adaptable to other matrices.

PubMed

Pickl, Karin E; Adamek, Viktor; Gorges, Roland; Sinner, Frank M

2011-07-15

Due to increased regulatory requirements, the interaction of active pharmaceutical ingredients with various surfaces and solutions during production and storage is gaining interest in the pharmaceutical research field, in particular with respect to development of new formulations, new packaging material and the evaluation of cleaning processes. Experimental adsorption/absorption studies as well as the study of cleaning processes require sophisticated analytical methods with high sensitivity for the drug of interest. In the case of 2,6-diisopropylphenol - a small lipophilic drug which is typically formulated as lipid emulsion for intravenous injection - a highly sensitive method in the concentration range of μg/l suitable to be applied to a variety of different sample matrices including lipid emulsions is needed. We hereby present a headspace-solid phase microextraction (HS-SPME) approach as a simple cleanup procedure for sensitive 2,6-diisopropylphenol quantification from diverse matrices choosing a lipid emulsion as the most challenging matrix with regard to complexity. By combining the simple and straight forward HS-SPME sample pretreatment with an optimized GC-MS quantification method a robust and sensitive method for 2,6-diisopropylphenol was developed. This method shows excellent sensitivity in the low μg/l concentration range (5-200μg/l), good accuracy (94.8-98.8%) and precision (intraday-precision 0.1-9.2%, inter-day precision 2.0-7.7%). The method can be easily adapted to other, less complex, matrices such as water or swab extracts. Hence, the presented method holds the potential to serve as a single and simple analytical procedure for 2,6-diisopropylphenol analysis in various types of samples such as required in, e.g. adsorption/absorption studies which typically deal with a variety of different surfaces (steel, plastic, glass, etc.) and solutions/matrices including lipid emulsions. Copyright © 2011 Elsevier B.V. All rights reserved.

Double-resolution electron holography with simple Fourier transform of fringe-shifted holograms.

PubMed

Volkov, V V; Han, M G; Zhu, Y

2013-11-01

We propose a fringe-shifting holographic method with an appropriate image wave recovery algorithm leading to exact solution of holographic equations. With this new method the complex object image wave recovered from holograms appears to have much less traditional artifacts caused by the autocorrelation band present practically in all Fourier transformed holograms. The new analytical solutions make possible a double-resolution electron holography free from autocorrelation band artifacts and thus push the limits for phase resolution. The new image wave recovery algorithm uses a popular Fourier solution of the side band-pass filter technique, while the fringe-shifting holographic method is simple to implement in practice. Published by Elsevier B.V.

An Improved Method for the Extraction and Thin-Layer Chromatography of Chlorophyll A and B from Spinach

ERIC Educational Resources Information Center

Quach, Hao T.; Steeper, Robert L.; Griffin, William G.

2004-01-01

A simple and fast method, which resolves chlorophyll a and b from spinach leaves on analytical plates while minimizing the appearance of chlorophyll degradation products is shown. An improved mobile phase for the Thin-layer chromatographic analysis of spinach extract that allows for the complete resolution of the common plant pigments found in…

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...

Which Method Is Most Precise; Which Is Most Accurate? An Undergraduate Experiment

ERIC Educational Resources Information Center

Jordan, A. D.

2007-01-01

A simple experiment, the determination of the density of a liquid by several methods, is presented. Since the concept of density is a familiar one, the experiment is suitable for the introductory laboratory period of a first- or second-year course in physical or analytical chemistry. The main objective of the experiment is to familiarize students…

Simultaneous determination of gabapentin, pregabalin, vigabatrin, and topiramate in plasma by HPLC with fluorescence detection.

PubMed

Martinc, Boštjan; Roškar, Robert; Grabnar, Iztok; Vovk, Tomaž

2014-07-01

Therapeutic drug monitoring (TDM) of antiepileptic drugs (AEDs) has been recognized as a useful tool in management of epilepsy. We developed a simple analytical method for simultaneous determination of four second generation AEDs, including gabapentin (GBP), pregabalin (PGB), vigabatrin (VGB), and topiramate (TOP). Analytes were extracted from human plasma using universal solid phase extraction, derivatized with 4-chloro-7-nitrobenzofurazan (NBD-Cl) and analyzed by HPLC with fluorescence detection. Using mass spectrometry we confirmed that NBD-Cl reacts with sulfamate group of TOP similarly as with amine group of the other three analytes. The method is linear (r(2)>0.998) across investigated analytical ranges (0.375-30.0μg/mL for GBP, PGB, and VGB; 0.50-20.0μg/mL for TOP). Intraday and interday precision do not exceed 9.40%. The accuracy is from 95.6% to 106%. The recovery is higher than 80.6%, and the lower limit of quantification is at least 0.5μg/mL. The method is selective and robust. For TOP determination the method was compared to a previously published method and the results obtained by the two methods were in good agreement. The developed method is suitable for routine TDM. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of urinary 2,5-hexanedione concentration by an improved analytical method as an index of exposure to n-hexane.

PubMed Central

Saito, I; Shibata, E; Huang, J; Hisanaga, N; Ono, Y; Takeuchi, Y

1991-01-01

2,5-Hexanedione is a main metabolite of n-hexane and is considered as the cause of n-hexane polyneuropathy. Therefore, it is useful to measure 2,5-hexanedione for biological monitoring of exposure to n-hexane. The analytical methods existing for n-hexane metabolites, however, were controversial and not established enough. Hence, a simple and precise method for determination of urinary 2,5-hexanedione has been developed. Five ml of urine was acidified to pH 0.5 with concentrated hydrochloric acid and heated for 30 minutes at 90-100 degrees C. After cooling in water, sodium chloride and dichloromethane containing internal standard were added. The sample was shaken and centrifuged. 2,5-Hexanedione concentration in an aliquot of dichloromethane extract was quantified by gas chromatography using a widebore column (DB-1701). Urinary concentration of 2,5-hexanedione showed a good correlation with exposure to n-hexane (n = 50, r = 0.973, p less than 0.001). This method is simple and precise for analysis of urinary 2,5-hexanedione as an index of exposure to n-hexane. PMID:1878315

Quantification of astaxanthin in shrimp waste hydrolysate by HPLC.

PubMed

López-Cervantes, J; Sánchez-Machado, D I; Gutiérrez-Coronado, M A; Ríos-Vázquez, N J

2006-10-01

In the present study, a simple and rapid reversed-phase HPLC method for the determination of astaxanthin in shrimp waste hydrolysate has been developed and validated. The analytical procedure involves the direct extraction of astaxanthin from the lipid fraction with methanol. The analytical column, SS Exil ODS, was operated at 25C. The mobile phase consisted of a mixture of water:methanol:dichloromethane:acetonitrile (4.5:28:22:45.5 v/v/v/v) at a flow rate of 1.0 mL/min. Detection and identification were performed using a photodiode array detector (lambda(detection) = 476 nm). The proposed HPLC method showed adequate linearity, repeatability and accuracy.

Food adulteration analysis without laboratory prepared or determined reference food adulterant values.

PubMed

Kalivas, John H; Georgiou, Constantinos A; Moira, Marianna; Tsafaras, Ilias; Petrakis, Eleftherios A; Mousdis, George A

2014-04-01

Quantitative analysis of food adulterants is an important health and economic issue that needs to be fast and simple. Spectroscopy has significantly reduced analysis time. However, still needed are preparations of analyte calibration samples matrix matched to prediction samples which can be laborious and costly. Reported in this paper is the application of a newly developed pure component Tikhonov regularization (PCTR) process that does not require laboratory prepared or reference analysis methods, and hence, is a greener calibration method. The PCTR method requires an analyte pure component spectrum and non-analyte spectra. As a food analysis example, synchronous fluorescence spectra of extra virgin olive oil samples adulterated with sunflower oil is used. Results are shown to be better than those obtained using ridge regression with reference calibration samples. The flexibility of PCTR allows including reference samples and is generic for use with other instrumental methods and food products. Copyright © 2013 Elsevier Ltd. All rights reserved.

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

PubMed

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

2006-04-21

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

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

PubMed

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

2018-01-01

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

Sensitive sub-Doppler nonlinear spectroscopy for hyperfine-structure analysis using simple atomizers

NASA Astrophysics Data System (ADS)

Mickadeit, Fritz K.; Kemp, Helen; Schafer, Julia; Tong, William M.

1998-05-01

Laser wave-mixing spectroscopy is presented as a sub-Doppler method that offers not only high spectral resolution, but also excellent detection sensitivity. It offers spectral resolution suitable for hyperfine structure analysis and isotope ratio measurements. In a non-planar backward- scattering four-wave mixing optical configuration, two of the three input beams counter propagate and the Doppler broadening is minimized, and hence, spectral resolution is enhanced. Since the signal is a coherent beam, optical collection is efficient and signal detection is convenient. This simple multi-photon nonlinear laser method offers un usually sensitive detection limits that are suitable for trace-concentration isotope analysis using a few different types of simple analytical atomizers. Reliable measurement of hyperfine structures allows effective determination of isotope ratios for chemical analysis.

New analytic results for speciation times in neutral models.

PubMed

Gernhard, Tanja

2008-05-01

In this paper, we investigate the standard Yule model, and a recently studied model of speciation and extinction, the "critical branching process." We develop an analytic way-as opposed to the common simulation approach-for calculating the speciation times in a reconstructed phylogenetic tree. Simple expressions for the density and the moments of the speciation times are obtained. Methods for dating a speciation event become valuable, if for the reconstructed phylogenetic trees, no time scale is available. A missing time scale could be due to supertree methods, morphological data, or molecular data which violates the molecular clock. Our analytic approach is, in particular, useful for the model with extinction, since simulations of birth-death processes which are conditioned on obtaining n extant species today are quite delicate. Further, simulations are very time consuming for big n under both models.

Validation of the replica trick for simple models

NASA Astrophysics Data System (ADS)

Shinzato, Takashi

2018-04-01

We discuss the replica analytic continuation using several simple models in order to prove mathematically the validity of the replica analysis, which is used in a wide range of fields related to large-scale complex systems. While replica analysis consists of two analytical techniques—the replica trick (or replica analytic continuation) and the thermodynamical limit (and/or order parameter expansion)—we focus our study on replica analytic continuation, which is the mathematical basis of the replica trick. We apply replica analysis to solve a variety of analytical models, and examine the properties of replica analytic continuation. Based on the positive results for these models we propose that replica analytic continuation is a robust procedure in replica analysis.

Preliminary Upper Estimate of Peak Currents in Transcranial Magnetic Stimulation at Distant Locations from a TMS Coil

PubMed Central

Makarov, Sergey N.; Yanamadala, Janakinadh; Piazza, Matthew W.; Helderman, Alex M.; Thang, Niang S.; Burnham, Edward H.; Pascual-Leone, Alvaro

2016-01-01

Goals Transcranial magnetic stimulation (TMS) is increasingly used as a diagnostic and therapeutic tool for numerous neuropsychiatric disorders. The use of TMS might cause whole-body exposure to undesired induced currents in patients and TMS operators. The aim of the present study is to test and justify a simple analytical model known previously, which may be helpful as an upper estimate of eddy current density at a particular distant observation point for any body composition and any coil setup. Methods We compare the analytical solution with comprehensive adaptive mesh refinement-based FEM simulations of a detailed full-body human model, two coil types, five coil positions, about 100,000 observation points, and two distinct pulse rise times, thus providing a representative number of different data sets for comparison, while also using other numerical data. Results Our simulations reveal that, after a certain modification, the analytical model provides an upper estimate for the eddy current density at any location within the body. In particular, it overestimates the peak eddy currents at distant locations from a TMS coil by a factor of 10 on average. Conclusion The simple analytical model tested in the present study may be valuable as a rapid method to safely estimate levels of TMS currents at different locations within a human body. Significance At present, safe limits of general exposure to TMS electric and magnetic fields are an open subject, including fetal exposure for pregnant women. PMID:26685221

A simple method for the small scale synthesis and solid-phase extraction purification of steroid sulfates.

PubMed

Waller, Christopher C; McLeod, Malcolm D

2014-12-01

Steroid sulfates are a major class of steroid metabolite that are of growing importance in fields such as anti-doping analysis, the detection of residues in agricultural produce or medicine. Despite this, many steroid sulfate reference materials may have limited or no availability hampering the development of analytical methods. We report simple protocols for the rapid synthesis and purification of steroid sulfates that are suitable for adoption by analytical laboratories. Central to this approach is the use of solid-phase extraction (SPE) for purification, a technique routinely used for sample preparation in analytical laboratories around the world. The sulfate conjugates of sixteen steroid compounds encompassing a wide range of steroid substitution patterns and configurations are prepared, including the previously unreported sulfate conjugates of the designer steroids furazadrol (17β-hydroxyandrostan[2,3-d]isoxazole), isofurazadrol (17β-hydroxyandrostan[3,2-c]isoxazole) and trenazone (17β-hydroxyestra-4,9-dien-3-one). Structural characterization data, together with NMR and mass spectra are reported for all steroid sulfates, often for the first time. The scope of this approach for small scale synthesis is highlighted by the sulfation of 1μg of testosterone (17β-hydroxyandrost-4-en-3-one) as monitored by liquid chromatography-mass spectrometry (LCMS). Copyright © 2014 Elsevier Inc. All rights reserved.

A simple fabrication of plasmonic surface-enhanced Raman scattering (SERS) substrate for pesticide analysis via the immobilization of gold nanoparticles on UF membrane

NASA Astrophysics Data System (ADS)

Hong, Jangho; Kawashima, Ayato; Hamada, Noriaki

2017-06-01

In this study, we developed a facile fabrication method to access a highly reproducible plasmonic surface enhanced Raman scattering substrate via the immobilization of gold nanoparticles on an Ultrafiltration (UF) membrane using a suction technique. This was combined with a simple and rapid analyte concentration and detection method utilizing portable Raman spectroscopy. The minimum detectable concentrations for aqueous thiabendazole standard solution and thiabendazole in orange extract are 0.01 μg/mL and 0.125 μg/g, respectively. The partial least squares (PLS) regression plot shows a good linear relationship between 0.001 and 100 μg/mL of analyte, with a root mean square error of prediction (RMSEP) of 0.294 and a correlation coefficient (R2) of 0.976 for the thiabendazole standard solution. Meanwhile, the PLS plot also shows a good linear relationship between 0.0 and 2.5 μg/g of analyte, with an RMSEP value of 0.298 and an R2 value of 0.993 for the orange peel extract. In addition to the detection of other types of pesticides in agricultural products, this highly uniform plasmonic substrate has great potential for application in various environmentally-related areas.

An Economical Semi-Analytical Orbit Theory for Retarded Satellite Motion About an Oblate Planet

NASA Technical Reports Server (NTRS)

Gordon, R. A.

1980-01-01

Brouwer and Brouwer-Lyddanes' use of the Von Zeipel-Delaunay method is employed to develop an efficient analytical orbit theory suitable for microcomputers. A succinctly simple pseudo-phenomenologically conceptualized algorithm is introduced which accurately and economically synthesizes modeling of drag effects. The method epitomizes and manifests effortless efficient computer mechanization. Simulated trajectory data is employed to illustrate the theory's ability to accurately accommodate oblateness and drag effects for microcomputer ground based or onboard predicted orbital representation. Real tracking data is used to demonstrate that the theory's orbit determination and orbit prediction capabilities are favorably adaptable to and are comparable with results obtained utilizing complex definitive Cowell method solutions on satellites experiencing significant drag effects.

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.

A simple one-step ultrasonic-assisted extraction and derivatization method coupling to high-performance liquid chromatographyfor the determination of ε-aminocaproic acid and amino acids in cosmetics.

PubMed

Du, Yuanqi; Xia, Ling; Xiao, Xiaohua; Li, Gongke; Chen, Xiaoguang

2018-06-15

Nowadays, the safety of cosmetics is a widespread concern. Amines are common cosmetic additives. Some of them such as amino acids are beneficial. Another kind of amines, however, ε-aminocaproic acid (EACA) is prohibited to add into cosmetics for its adverse reactions. In this study, a simple, rapid, sensitive and eco-friendly one-step ultrasonic-assisted extraction and derivatization (UAE-D) method was developed for determination of EACA and amino acids in cosmetics by coupling with high-performance liquid chromatography (HPLC). By using this sample preparation method, extraction and derivatization of EACA and amino acids were finished in one step in ultrasound field. During this procedure, 4-fluoro-7-nitrobenzofurazan (NBD-F)was applied as derivatization reagent. The extraction conditions including the amount of NBD-F, extraction and derivatization temperature, the ultrasonic vibration time and pH value of the aqueous phase were evaluated. Meanwhile, the extraction mechanism was investigated. Under optimized conditions, the method detection limits were 0.086-0.15 μg/L, and method quantitation limits were 0.29-0.47 μg/L with RSDs less than 3.7% (n = 3). The recoveries of EACA and amino acids obtained from cosmetic samples were in range from 76.9% to 122.3%. Amino acids were found in all selected samples and quantified in range from 1.9 ± 0.9 to 677.2 ± 17.9 μg/kg. And EACA was found and quantified with the contents of 1284.3 ± 22.1 μg/kg in a toner sample. This UAE-D-HPLC method shortened and simplified the sample pretreatment as well as enhanced the sensitivity of analytical method. In our record, only 10 min was needed for the total sample preparation process. And the method detection limits were two orders of magnitude less than literature reports. Furthermore, we reduced the consumption of solvent and minimized the usage of organic solvents, which made our method moving towards green analytical chemistry. In brief, our UAE-D-HPLC method is a simple, rapid, sensitive and eco-friendly analytical method for the determination of EACA and amino acids in cosmetics. Copyright © 2018 Elsevier B.V. All rights reserved.

A simple and effective method for detecting precipitated proteins in MALDI-TOF MS.

PubMed

Oshikane, Hiroyuki; Watabe, Masahiko; Nakaki, Toshio

2018-04-01

MALDI-TOF MS has developed rapidly into an essential analytical tool for the life sciences. Cinnamic acid derivatives are generally employed in routine molecular weight determinations of intact proteins using MALDI-TOF MS. However, a protein of interest may precipitate when mixed with matrix solution, perhaps preventing MS detection. We herein provide a simple approach to enable the MS detection of such precipitated protein species by means of a "direct deposition method" -- loading the precipitant directly onto the sample plate. It is thus expected to improve routine MS analysis of intact proteins. Copyright © 2018. Published by Elsevier Inc.

A Requirements-Driven Optimization Method for Acoustic Liners Using Analytic Derivatives

NASA Technical Reports Server (NTRS)

Berton, Jeffrey J.; Lopes, Leonard V.

2017-01-01

More than ever, there is flexibility and freedom in acoustic liner design. Subject to practical considerations, liner design variables may be manipulated to achieve a target attenuation spectrum. But characteristics of the ideal attenuation spectrum can be difficult to know. Many multidisciplinary system effects govern how engine noise sources contribute to community noise. Given a hardwall fan noise source to be suppressed, and using an analytical certification noise model to compute a community noise measure of merit, the optimal attenuation spectrum can be derived using multidisciplinary systems analysis methods. In a previous paper on this subject, a method deriving the ideal target attenuation spectrum that minimizes noise perceived by observers on the ground was described. A simple code-wrapping approach was used to evaluate a community noise objective function for an external optimizer. Gradients were evaluated using a finite difference formula. The subject of this paper is an application of analytic derivatives that supply precise gradients to an optimization process. Analytic derivatives improve the efficiency and accuracy of gradient-based optimization methods and allow consideration of more design variables. In addition, the benefit of variable impedance liners is explored using a multi-objective optimization.

Freeze-thaw approach: A practical sample preparation strategy for residue analysis of multi-class veterinary drugs in chicken muscle.

PubMed

Zhang, Meiyu; Li, Erfen; Su, Yijuan; Song, Xuqin; Xie, Jingmeng; Zhang, Yingxia; He, Limin

2018-06-01

Seven drugs from different classes, namely, fluoroquinolones (enrofloxacin, ciprofloxacin, sarafloxacin), sulfonamides (sulfadimidine, sulfamonomethoxine), and macrolides (tilmicosin, tylosin), were used as test compounds in chickens by oral administration, a simple extraction step after cryogenic freezing might allow the effective extraction of multi-class veterinary drug residues from minced chicken muscles by mix vortexing. On basis of the optimized freeze-thaw approach, a convenient, selective, and reproducible liquid chromatography with tandem mass spectrometry method was developed. At three spiking levels in blank chicken and medicated chicken muscles, average recoveries of the analytes were in the range of 71-106 and 63-119%, respectively. All the relative standard deviations were <20%. The limits of quantification of analytes were 0.2-5.0 ng/g. Regardless of the chicken levels, there were no significant differences (P > 0.05) in the average contents of almost any of the analytes in medicated chickens between this method and specific methods in the literature for the determination of specific analytes. Finally, the developed method was successfully extended to the monitoring of residues of 55 common veterinary drugs in food animal muscles. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Numerical simulation for solution of space-time fractional telegraphs equations with local fractional derivatives via HAFSTM

NASA Astrophysics Data System (ADS)

Pandey, Rishi Kumar; Mishra, Hradyesh Kumar

2017-11-01

In this paper, the semi-analytic numerical technique for the solution of time-space fractional telegraph equation is applied. This numerical technique is based on coupling of the homotopy analysis method and sumudu transform. It shows the clear advantage with mess methods like finite difference method and also with polynomial methods similar to perturbation and Adomian decomposition methods. It is easily transform the complex fractional order derivatives in simple time domain and interpret the results in same meaning.

Analytical method for lipoperoxidation relevant reactive aldehydes in human sera by high-performance liquid chromatography-fluorescence detection.

PubMed

El-Maghrabey, Mahmoud H; Kishikawa, Naoya; Ohyama, Kaname; Kuroda, Naotaka

2014-11-01

A validated, simple and sensitive HPLC method was developed for the simultaneous determination of lipoperoxidation relevant reactive aldehydes: glyoxal (GO), acrolein (ACR), malondialdehyde (MDA), and 4-hydroxy-2-nonenal (HNE) in human serum. The studied aldehydes were reacted with 2,2'-furil to form fluorescent difurylimidazole derivatives that were separated on a C18 column using gradient elution and fluorescence detection at excitation and emission wavelengths of 250 and 355nm, respectively. The method showed good linearity over the concentration ranges of 0.100-5.00, 0.200-10.0, 0.200-40.0, and 0.400-10.0nmol/mL for GO, ACR, HNE, and MDA, respectively, with detection limits ranging from 0.030 to 0.11nmol/mL. The percentage RSD of intraday and interday precision did not exceed 5.0 and 6.2%, respectively, and the accuracy (%found) ranged from 95.5 to 103%. The proposed method was applied for monitoring the four aldehydes in sera of healthy, diabetic, and rheumatic human subjects with simple pretreatment steps and without interference from endogenous components. By virtue of its high sensitivity and accuracy, our method enabled detection of differences between analytes concentrations in sera of human subjects under different clinical conditions. Copyright © 2014 Elsevier Inc. All rights reserved.

Separation-oriented derivatization of native fluorescent compounds through fluorous labeling followed by liquid chromatography with fluorous-phase.

PubMed

Sakaguchi, Yohei; Yoshida, Hideyuki; Todoroki, Kenichiro; Nohta, Hitoshi; Yamaguchi, Masatoshi

2009-06-15

We have developed a new and simple method based on "fluorous derivatization" for LC of native fluorescent compounds. This method involves the use of a column with a fluorous stationary phase. Native fluorescent analytes with target functional groups are precolumn derivatized with a nonfluorescent fluorous tag, and the fluorous-labeled analytes are retained in the column, whereas underivatized substances are not. Only the retained fluorescent analytes are detected fluorometrically at appropriate retention times, and retained substrates without fluorophores are not detected. In this study, biologically important carboxylic acids (homovanillic acid, vanillylmandelic acid, and 5-hydroxyindoleacetic acid) and drugs (naproxen, felbinac, flurbiprofen, and etodolac) were used as model native fluorescent compounds. Experimental results indicate that the fluorous-phase column can selectively retain fluorous compounds including fluorous-labeled analytes on the basis of fluorous separation. We believe that separation-oriented derivatization presented here is the first step toward the introduction of fluorous derivatization in quantitative LC analysis.

A brief introduction to computer-intensive methods, with a view towards applications in spatial statistics and stereology.

PubMed

Mattfeldt, Torsten

2011-04-01

Computer-intensive methods may be defined as data analytical procedures involving a huge number of highly repetitive computations. We mention resampling methods with replacement (bootstrap methods), resampling methods without replacement (randomization tests) and simulation methods. The resampling methods are based on simple and robust principles and are largely free from distributional assumptions. Bootstrap methods may be used to compute confidence intervals for a scalar model parameter and for summary statistics from replicated planar point patterns, and for significance tests. For some simple models of planar point processes, point patterns can be simulated by elementary Monte Carlo methods. The simulation of models with more complex interaction properties usually requires more advanced computing methods. In this context, we mention simulation of Gibbs processes with Markov chain Monte Carlo methods using the Metropolis-Hastings algorithm. An alternative to simulations on the basis of a parametric model consists of stochastic reconstruction methods. The basic ideas behind the methods are briefly reviewed and illustrated by simple worked examples in order to encourage novices in the field to use computer-intensive methods. © 2010 The Authors Journal of Microscopy © 2010 Royal Microscopical Society.

A Guide to Job Analysis for the Preparation of Job Training Programmes.

ERIC Educational Resources Information Center

Ceramics, Glass, and Mineral Products Industry Training Board, Harrow (England).

The paper deals with job analysis for the preparation of job training programs. The analytical approach involves five steps: enlisting support, examining the job, describing the job, analyzing training requirements, and planning the programs. Appendixes include methods of producing training schemes--the simple job breakdown, straightforward…

Multiple Contact Dates and SARS Incubation Periods

PubMed Central

2004-01-01

Many severe acute respiratory syndrome (SARS) patients have multiple possible incubation periods due to multiple contact dates. Multiple contact dates cannot be used in standard statistical analytic techniques, however. I present a simple spreadsheet-based method that uses multiple contact dates to calculate the possible incubation periods of SARS. PMID:15030684

Implementation and Use of the Reference Analytics Module of LibAnswers

ERIC Educational Resources Information Center

Flatley, Robert; Jensen, Robert Bruce

2012-01-01

Academic libraries have traditionally collected reference statistics using hash marks on paper. Although efficient and simple, this method is not an effective way to capture the complexity of reference transactions. Several electronic tools are now available to assist libraries with collecting often elusive reference data--among them homegrown…

Deciphering mRNA Sequence Determinants of Protein Production Rate

NASA Astrophysics Data System (ADS)

Szavits-Nossan, Juraj; Ciandrini, Luca; Romano, M. Carmen

2018-03-01

One of the greatest challenges in biophysical models of translation is to identify coding sequence features that affect the rate of translation and therefore the overall protein production in the cell. We propose an analytic method to solve a translation model based on the inhomogeneous totally asymmetric simple exclusion process, which allows us to unveil simple design principles of nucleotide sequences determining protein production rates. Our solution shows an excellent agreement when compared to numerical genome-wide simulations of S. cerevisiae transcript sequences and predicts that the first 10 codons, which is the ribosome footprint length on the mRNA, together with the value of the initiation rate, are the main determinants of protein production rate under physiological conditions. Finally, we interpret the obtained analytic results based on the evolutionary role of the codons' choice for regulating translation rates and ribosome densities.

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

PubMed

G Archana; Dhodapkar, Rita; Kumar, Anupama

2016-09-01

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

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.

Pre-concentration technique for reduction in "Analytical instrument requirement and analysis"

NASA Astrophysics Data System (ADS)

Pal, Sangita; Singha, Mousumi; Meena, Sher Singh

2018-04-01

Availability of analytical instruments for a methodical detection of known and unknown effluents imposes a serious hindrance in qualification and quantification. Several analytical instruments such as Elemental analyzer, ICP-MS, ICP-AES, EDXRF, ion chromatography, Electro-analytical instruments which are not only expensive but also time consuming, required maintenance, damaged essential parts replacement which are of serious concern. Move over for field study and instant detection installation of these instruments are not convenient to each and every place. Therefore, technique such as pre-concentration of metal ions especially for lean stream elaborated and justified. Chelation/sequestration is the key of immobilization technique which is simple, user friendly, most effective, least expensive, time efficient; easy to carry (10g - 20g vial) to experimental field/site has been demonstrated.

Penning Ionization Electron Spectroscopy in Glow Discharge: A New Dimension for Gas Chromatography Detectors

NASA Technical Reports Server (NTRS)

Sheverev, V. A.; Khromov, N. A.; Kojiro, D. R.; Fonda, Mark (Technical Monitor)

2002-01-01

Admixtures to helium of 100 ppm and 5 ppm of nitrogen, and 100 ppm and 10 ppm of carbon monoxide were identified and measured in the helium discharge afterglow using an electrical probe placed into the plasma. For nitrogen and carbon monoxide gases, the measured electron energy spectra display distinct characteristic peaks (fingerprints). Location of the peaks on the energy scale is determined by the ionization energies of the analyte molecules. Nitrogen and carbon monoxide fingerprints were also observed in a binary mixture of these gases in helium, and the relative concentration analytes has been predicted. The technically simple and durable method is considered a good candidate for a number of analytical applications, and in particular, in GC and for analytical flight instrumentation.

Ultra-high Performance Liquid Chromatography Tandem Mass-Spectrometry for Simple and Simultaneous Quantification of Cannabinoids

PubMed Central

Jamwal, Rohitash; Topletz, Ariel R.; Ramratnam, Bharat; Akhlaghi, Fatemeh

2017-01-01

Cannabis is used widely in the United States, both recreationally and for medical purposes. Current methods for analysis of cannabinoids in human biological specimens rely on complex extraction process and lengthy analysis time. We established a rapid and simple assay for quantification of Δ9-tetrahydrocannabinol (THC), cannabidiol (CBD), 11-hydroxy Δ9-tetrahydrocannabinol (11-OH THC) and 11-nor-9-carboxy-Δ9-tetrahydrocannbinol (THC-COOH) in human plasma by U-HPLC-MS/MS using Δ9-tetrahydrocannabinol-D3 as the internal standard. Chromatographic separation was achieved on an Acquity BEH C18 column using a gradient comprising of water (0.1% formic acid) and methanol (0.1% formic acid) over a 6 min run-time. Analytes from 200 µL plasma were extracted using acetonitrile (containing 1% formic acid and THC-D3). Mass spectrometry was performed in positive ionization mode, and total ion chromatogram was used for quantification of analytes. The assay was validated according to guidelines set forth by Food and Drug Administration of United States. An eight-point calibration curve was fitted with quadratic regression (r2>0.99) from 1.56 to 100 ng mL−1 and a lower limit of quantification (LLOQ) of 1.56 ng mL−1 was achieved. Accuracy and precision calculated from six calibration curves was between 85 to 115% while the mean extraction recovery was >90% for all the analytes. Several plasma phospholipids eluted after the analytes thus did not interfere with the assay. Bench-top, freeze-thaw, auto-sampler and short-term stability ranged from 92.7 to 106.8% of nominal values. Application of the method was evaluated by quantification of analytes in human plasma from six subjects. PMID:28192758

A simple microplate-based method for the determination of α-amylase activity using the glucose assay kit (GOD method).

PubMed

Visvanathan, Rizliya; Jayathilake, Chathuni; Liyanage, Ruvini

2016-11-15

For the first time, a reliable, simple, rapid and high-throughput analytical method for the detection and quantification of α-amylase inhibitory activity using the glucose assay kit was developed. The new method facilitates rapid screening of a large number of samples, reduces labor, time and reagents and is also suitable for kinetic studies. This method is based on the reaction of maltose with glucose oxidase (GOD) and the development of a red quinone. The test is done in microtitre plates with a total volume of 260μL and an assay time of 40min including the pre-incubation steps. The new method is tested for linearity, sensitivity, precision, reproducibility and applicability. The new method is also compared with the most commonly used 3,5-dinitrosalicylic acid (DNSA) method for determining α-amylase activity. Copyright © 2016 Elsevier Ltd. All rights reserved.

Cisapride a green analytical reagent for rapid and sensitive determination of bromate in drinking water, bread and flour additives by oxidative coupling spectrophotometric methods

NASA Astrophysics Data System (ADS)

Al Okab, Riyad Ahmed

2013-02-01

Green analytical methods using Cisapride (CPE) as green analytical reagent was investigated in this work. Rapid, simple, and sensitive spectrophotometric methods for the determination of bromate in water sample, bread and flour additives were developed. The proposed methods based on the oxidative coupling between phenoxazine and Cisapride in the presence of bromate to form red colored product with max at 520 nm. Phenoxazine and Cisapride and its reaction products were found to be environmentally friendly under the optimum experimental condition. The method obeys beers law in concentration range 0.11-4.00 g ml-1 and molar absorptivity 1.41 × 104 L mol-1 cm-1. All variables have been optimized and the presented reaction sequences were applied to the analysis of bromate in water, bread and flour additive samples. The performance of these method was evaluated in terms of Student's t-test and variance ratio F-test to find out the significance of proposed methods over the reference method. The combination of pharmaceutical drugs reagents with low concentration create some unique green chemical analyses.

Computational methods and traveling wave solutions for the fourth-order nonlinear Ablowitz-Kaup-Newell-Segur water wave dynamical equation via two methods and its applications

NASA Astrophysics Data System (ADS)

Ali, Asghar; Seadawy, Aly R.; Lu, Dianchen

2018-05-01

The aim of this article is to construct some new traveling wave solutions and investigate localized structures for fourth-order nonlinear Ablowitz-Kaup-Newell-Segur (AKNS) water wave dynamical equation. The simple equation method (SEM) and the modified simple equation method (MSEM) are applied in this paper to construct the analytical traveling wave solutions of AKNS equation. The different waves solutions are derived by assigning special values to the parameters. The obtained results have their importance in the field of physics and other areas of applied sciences. All the solutions are also graphically represented. The constructed results are often helpful for studying several new localized structures and the waves interaction in the high-dimensional models.

Cloud point extraction thermospray flame quartz furnace atomic absorption spectrometry for determination of ultratrace cadmium in water and urine

NASA Astrophysics Data System (ADS)

Wu, Peng; Zhang, Yunchang; Lv, Yi; Hou, Xiandeng

2006-12-01

A simple, low cost and highly sensitive method based on cloud point extraction (CPE) for separation/preconcentration and thermospray flame quartz furnace atomic absorption spectrometry was proposed for the determination of ultratrace cadmium in water and urine samples. The analytical procedure involved the formation of analyte-entrapped surfactant micelles by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution and a Triton X-114 solution. When the temperature of the system was higher than the cloud point of Triton X-114, the complex of cadmium-PDC entered the surfactant-rich phase and thus separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, the limit of detection was 0.04 μg/L for cadmium with a sample volume of 10 mL. The analytical results of cadmium in water and urine samples agreed well with those by ICP-MS.

Analytical application of solid contact ion-selective electrodes for determination of copper and nitrate in various food products and drinking water.

PubMed

Wardak, Cecylia; Grabarczyk, Malgorzata

2016-08-02

A simple, fast and cheap method for monitoring copper and nitrate in drinking water and food products using newly developed solid contact ion-selective electrodes is proposed. Determination of copper and nitrate was performed by application of multiple standard additions technique. The reliability of the obtained results was assessed by comparing them using the anodic stripping voltammetry or spectrophotometry for the same samples. In each case, satisfactory agreement of the results was obtained, which confirms the analytical usefulness of the constructed electrodes.

Comment on "Classification of aerosol properties derived from AERONET direct sun data" by Gobbi et al. (2007)

NASA Astrophysics Data System (ADS)

O'Neill, N. T.

2010-10-01

It is pointed out that the graphical, aerosol classification method of Gobbi et al. (2007) can be interpreted as a manifestation of fundamental analytical relations whose existance depends on the simple assumption that the optical effects of aerosols are essentially bimodal in nature. The families of contour lines in their "Ada" curvature space are essentially empirical and discretized illustrations of analytical parabolic forms in (α, α') space (the space formed by the continuously differentiable Angstrom exponent and its spectral derivative).

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

PubMed

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

2018-02-20

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

Multi-band transmission color filters for multi-color white LEDs based visible light communication

NASA Astrophysics Data System (ADS)

Wang, Qixia; Zhu, Zhendong; Gu, Huarong; Chen, Mengzhu; Tan, Qiaofeng

2017-11-01

Light-emitting diodes (LEDs) based visible light communication (VLC) can provide license-free bands, high data rates, and high security levels, which is a promising technique that will be extensively applied in future. Multi-band transmission color filters with enough peak transmittance and suitable bandwidth play a pivotal role for boosting signal-noise-ratio in VLC systems. In this paper, multi-band transmission color filters with bandwidth of dozens nanometers are designed by a simple analytical method. Experiment results of one-dimensional (1D) and two-dimensional (2D) tri-band color filters demonstrate the effectiveness of the multi-band transmission color filters and the corresponding analytical method.

Experimental investigation and numerical simulation of 3He gas diffusion in simple geometries: implications for analytical models of 3He MR lung morphometry.

PubMed

Parra-Robles, J; Ajraoui, S; Deppe, M H; Parnell, S R; Wild, J M

2010-06-01

Models of lung acinar geometry have been proposed to analytically describe the diffusion of (3)He in the lung (as measured with pulsed gradient spin echo (PGSE) methods) as a possible means of characterizing lung microstructure from measurement of the (3)He ADC. In this work, major limitations in these analytical models are highlighted in simple diffusion weighted experiments with (3)He in cylindrical models of known geometry. The findings are substantiated with numerical simulations based on the same geometry using finite difference representation of the Bloch-Torrey equation. The validity of the existing "cylinder model" is discussed in terms of the physical diffusion regimes experienced and the basic reliance of the cylinder model and other ADC-based approaches on a Gaussian diffusion behaviour is highlighted. The results presented here demonstrate that physical assumptions of the cylinder model are not valid for large diffusion gradient strengths (above approximately 15 mT/m), which are commonly used for (3)He ADC measurements in human lungs. (c) 2010 Elsevier Inc. All rights reserved.

An Approximate Solution to the Equation of Motion for Large-Angle Oscillations of the Simple Pendulum with Initial Velocity

ERIC Educational Resources Information Center

Johannessen, Kim

2010-01-01

An analytic approximation of the solution to the differential equation describing the oscillations of a simple pendulum at large angles and with initial velocity is discussed. In the derivation, a sinusoidal approximation has been applied, and an analytic formula for the large-angle period of the simple pendulum is obtained, which also includes…

A simple and green analytical method for determination of glyphosate in commercial formulations and water by diffuse reflectance spectroscopy

NASA Astrophysics Data System (ADS)

da Silva, Aline Santana; Fernandes, Flávio Cesar Bedatty; Tognolli, João Olímpio; Pezza, Leonardo; Pezza, Helena Redigolo

2011-09-01

This article describes a simple, inexpensive, and environmentally friendly method for the monitoring of glyphosate using diffuse reflectance spectroscopy. The proposed method is based on reflectance measurements of the colored compound produced from the spot test reaction between glyphosate and p-dimethylaminocinnamaldehyde ( p-DAC) in acid medium, using a filter paper as solid support. Experimental designs were used to optimize the analytical conditions. All reflectance measurements were carried out at 495 nm. Under optimal conditions, the glyphosate calibration graphs obtained by plotting the optical density of the reflectance signal (A R) against the concentration were linear in the range 50-500 μg mL -1, with a correlation coefficient of 0.9987. The limit of detection (LOD) for glyphosate was 7.28 μg mL -1. The technique was successfully applied to the direct determination of glyphosate in commercial formulations, as well as in water samples (river water, pure water and mineral drinking water) after a previous clean-up or pre-concentration step. Recoveries were in the ranges 93.2-102.6% and 91.3-102.9% for the commercial formulations and water samples, respectively.

A simple and green analytical method for determination of glyphosate in commercial formulations and water by diffuse reflectance spectroscopy.

PubMed

da Silva, Aline Santana; Fernandes, Flávio Cesar Bedatty; Tognolli, João Olímpio; Pezza, Leonardo; Pezza, Helena Redigolo

2011-09-01

This article describes a simple, inexpensive, and environmentally friendly method for the monitoring of glyphosate using diffuse reflectance spectroscopy. The proposed method is based on reflectance measurements of the colored compound produced from the spot test reaction between glyphosate and p-dimethylaminocinnamaldehyde (p-DAC) in acid medium, using a filter paper as solid support. Experimental designs were used to optimize the analytical conditions. All reflectance measurements were carried out at 495 nm. Under optimal conditions, the glyphosate calibration graphs obtained by plotting the optical density of the reflectance signal (AR) against the concentration were linear in the range 50-500 μg mL(-1), with a correlation coefficient of 0.9987. The limit of detection (LOD) for glyphosate was 7.28 μg mL(-1). The technique was successfully applied to the direct determination of glyphosate in commercial formulations, as well as in water samples (river water, pure water and mineral drinking water) after a previous clean-up or pre-concentration step. Recoveries were in the ranges 93.2-102.6% and 91.3-102.9% for the commercial formulations and water samples, respectively. Copyright © 2011 Elsevier B.V. All rights reserved.

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.

Solvent microextraction-flame atomic absorption spectrometry (SME-FAAS) for determination of ultratrace amounts of cadmium in meat and fish samples.

PubMed

Goudarzi, Nasser

2009-02-11

A simple, low cost and highly sensitive method based on solvent microextraction (SME) for separation/preconcentration and flame atomic absorption spectrometry (FAAS) was proposed for the determination of ultratrace amounts of cadmium in meat and fish samples. The analytical procedure involved the formation of a hydrophobic complex by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution. In suitable conditions, the complex of cadmium-APDC entered the micro organic phase, and thus, separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, a detection limit (3 sigma) of 0.8 ng L(-1) and an enrichment factor of 93 were achieved. The relative standard deviation for the method was found to be 2.2% for Cd. The interference effects of some anions and cations were also investigated. The developed method has been applied to the determination of trace Cd in meat and fish samples.

Method development and qualification of capillary zone electrophoresis for investigation of therapeutic monoclonal antibody quality.

PubMed

Suba, Dávid; Urbányi, Zoltán; Salgó, András

2016-10-01

Capillary electrophoresis techniques are widely used in the analytical biotechnology. Different electrophoretic techniques are very adequate tools to monitor size-and charge heterogenities of protein drugs. Method descriptions and development studies of capillary zone electrophoresis (CZE) have been described in literature. Most of them are performed based on the classical one-factor-at-time (OFAT) approach. In this study a very simple method development approach is described for capillary zone electrophoresis: a "two-phase-four-step" approach is introduced which allows a rapid, iterative method development process and can be a good platform for CZE method. In every step the current analytical target profile and an appropriate control strategy were established to monitor the current stage of development. A very good platform was established to investigate intact and digested protein samples. Commercially available monoclonal antibody was chosen as model protein for the method development study. The CZE method was qualificated after the development process and the results were presented. The analytical system stability was represented by the calculated RSD% value of area percentage and migration time of the selected peaks (<0.8% and <5%) during the intermediate precision investigation. Copyright © 2016 Elsevier B.V. All rights reserved.

Three-Dimensional Dynamic Deformation Measurements Using Stereoscopic Imaging and Digital Speckle Photography

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

Prentice, H. J.; Proud, W. G.

2006-07-28

A technique has been developed to determine experimentally the three-dimensional displacement field on the rear surface of a dynamically deforming plate. The technique combines speckle analysis with stereoscopy, using a modified angular-lens method: this incorporates split-frame photography and a simple method by which the effective lens separation can be adjusted and calibrated in situ. Whilst several analytical models exist to predict deformation in extended or semi-infinite targets, the non-trivial nature of the wave interactions complicates the generation and development of analytical models for targets of finite depth. By interrogating specimens experimentally to acquire three-dimensional strain data points, both analytical andmore » numerical model predictions can be verified more rigorously. The technique is applied to the quasi-static deformation of a rubber sheet and dynamically to Mild Steel sheets of various thicknesses.« less

Development and validation of a method for the simultaneous extraction and separate measurement of oxytetracycline, florfenicol, oxolinic acid and flumequine from marine sediments.

PubMed

Norambuena, Luis; Gras, Nuri; Contreras, Sergio

2013-08-15

A simple and rapid method for the detection and extraction of oxolinic acid, flumequine, florfenicol and oxytetracycline from marine sediments was developed and validated. The analytes were extracted from the marine sediment using a solution of oxalic acid diluted in methanol with sonication before detection by HPLC using a diode-array detector (florfenicol and oxytetracycline) and fluorescence (oxolinic acid and flumequine). The quantification limits (QL) were 100 ng/g for oxytetracycline and florfenicol and 5 ng/g for oxolinic acid and flumequine. The coefficients of variation of the repeatability and intermediate precision were less than 10% in all of the analytes. The calibration curves were linear between 50 and 500 ng/ml for oxytetracycline and florfenicol and 1 and 20 ng/ml for oxolinic acid and flumequine. The recuperation rate for the analytes was above 86%. Copyright © 2013 Elsevier Ltd. All rights reserved.

Validation of the analytical method for the simultaneous determination of selected polybrominated diphenyl ethers, polychlorinated biphenyls and organochlorine pesticides in human blood serum by gas chromatography with microelectron capture detector.

PubMed

Matuszak, Małgorzata; Minorczyk, Maria; Góralczyk, Katarzyna; Hernik, Agnieszka; Struciński, Paweł; Liszewska, Monika; Czaja, Katarzyna; Korcz, Wojciech; Łyczewska, Monika; Ludwicki, Jan K

2016-01-01

Polybrominated diphenyl ethers (PBDEs) as other persistent organic pollutants like polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) pose a significant hazard to human health, mainly due to interference with the endocrine system and carcinogenetic effects. Humans are exposed to these substances mainly through a food of animal origin. These pollutants are globally detected in human matrices which requires to dispose reliable and simple analytical method that would enable further studies to assess the exposure of specific human populations to these compounds. The purpose of this study was to modify and validate of the analytical procedure for the simultaneous determination of selected PBDEs, PCBs and OCPs in human blood serum samples. The analytical measurement was performed by GC-µECD following preparation of serum samples (denaturation, multiple extraction, lipid removal). Identity of the compounds was confirmed by GC-MS. The method was characterised by the appropriate linearity, good repeatability (CV below 20%). The recoveries ranged from 52.9 to 125.0% depending on compound and level of fortification. The limit of quantification was set at 0.03 ng mL(-1) of serum. The modified analytical method proved to be suitable for the simultaneous determination of selected PBDEs, PCBs and OCPs in human blood serum by GC-µECD with good precision.

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

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.

Evaluation of generalized degrees of freedom for sparse estimation by replica method

NASA Astrophysics Data System (ADS)

Sakata, A.

2016-12-01

We develop a method to evaluate the generalized degrees of freedom (GDF) for linear regression with sparse regularization. The GDF is a key factor in model selection, and thus its evaluation is useful in many modelling applications. An analytical expression for the GDF is derived using the replica method in the large-system-size limit with random Gaussian predictors. The resulting formula has a universal form that is independent of the type of regularization, providing us with a simple interpretation. Within the framework of replica symmetric (RS) analysis, GDF has a physical meaning as the effective fraction of non-zero components. The validity of our method in the RS phase is supported by the consistency of our results with previous mathematical results. The analytical results in the RS phase are calculated numerically using the belief propagation algorithm.

A simple and highly sensitive UPLC-ESI-MS/MS method for the simultaneous quantification of nicotine, cotinine, and the tobacco-specific carcinogens N'-nitrosonornicotine and 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone in serum samples.

PubMed

Loukotková, Lucie; VonTungeln, Linda S; Vanlandingham, Michelle; da Costa, Gonçalo Gamboa

2018-01-01

According to the World Health Organization, the consumption of tobacco products is the single largest cause of preventable deaths in the world, exceeding the total aggregated number of deaths caused by diseases such as AIDS, tuberculosis, and malaria. An important element in the evaluation of the health risks associated with the consumption of tobacco products is the assessment of the internal exposure to the tobacco constituents responsible for their addictive (e.g. nicotine) and carcinogenic (e.g. N-nitrosamines such as NNN and NNK) properties. However, the assessment of the serum levels of these compounds is often challenging from an analytical standpoint, in particular when limited sample volumes are available and low detection limits are required. Currently available analytical methods often rely on complex multi-step sample preparation procedures, which are prone to low analyte recoveries and ex-vivo contamination due to the ubiquitous nature of these compounds as background contaminants. In order to circumvent these problems, we report a facile and highly sensitive method for the simultaneous quantification of nicotine, cotinine, NNN, and NNK in serum samples. The method relies on a simple "one pot" liquid-liquid extraction procedure and isotope dilution ultra-high pressure (UPLC) hydrophilic interaction liquid chromatography (HILIC) coupled with tandem mass spectrometry. The method requires only 10μL of serum and presents a limit of quantification of 0.02nmol (3000pg/mL) nicotine, 0.6pmol (100pg/mL) cotinine, 0.05pmol NNK (10pg/mL), and 0.06pmol NNN (10pg/mL), making it appropriate for pharmacokinetic evaluations. Published by Elsevier B.V.

Simple apparatus for polarization sensing of analytes

NASA Astrophysics Data System (ADS)

Gryczynski, Zygmunt; Gryczynski, Ignacy; Lakowicz, Joseph R.

2000-09-01

We describe a simple device for fluorescence sensing based on an unexpansive light source, a dual photocell and a Watson bridge. The emission is detected from two fluorescent samples, one of which changes intensity in response to the analyte. The emission from these two samples is observed through two orthogonally oriented polarizers and an analyzer polarizer. The latter polarizer is rotated to yield equal intensities from both sides of the dual photocell, as determined by a zero voltage from the Watson bridge. Using this device, we are able to measure fluorescein concentration to an accuracy near 2% at 1 (mu) M fluorescein, and pH values accurate to +/- 0.02 pH units. We also use this approach with a UV hand lamp and a glucose-sensitive protein to measure glucose concentrations near 2 (mu) M to an accuracy of +/- 0.1 (mu) M. This approach requires only simple electronics, which can be battery powered. Additionally, the method is generic, and can be applied with any fluorescent sample that displays a change in intensity. One can imagine this approach being used to develop portable point-of-care clinical devices.

SU-FF-T-668: A Simple Algorithm for Range Modulation Wheel Design in Proton Therapy

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

Nie, X; Nazaryan, Vahagn; Gueye, Paul

2009-06-01

Purpose: To develop a simple algorithm in designing the range modulation wheel to generate a very smooth Spread-Out Bragg peak (SOBP) for proton therapy.Method and Materials: A simple algorithm has been developed to generate the weight factors in corresponding pristine Bragg peaks which composed a smooth SOBP in proton therapy. We used a modified analytical Bragg peak function based on Monte Carol simulation tool-kits of Geant4 as pristine Bragg peaks input in our algorithm. A simple METLAB(R) Quad Program was introduced to optimize the cost function in our algorithm. Results: We found out that the existed analytical function of Braggmore » peak can't directly use as pristine Bragg peak dose-depth profile input file in optimization of the weight factors since this model didn't take into account of the scattering factors introducing from the range shifts in modifying the proton beam energies. We have done Geant4 simulations for proton energy of 63.4 MeV with a 1.08 cm SOBP for variation of pristine Bragg peaks which composed this SOBP and modified the existed analytical Bragg peak functions for their peak heights, ranges of R{sub 0}, and Gaussian energies {sigma}{sub E}. We found out that 19 pristine Bragg peaks are enough to achieve a flatness of 1.5% of SOBP which is the best flatness in the publications. Conclusion: This work develops a simple algorithm to generate the weight factors which is used to design a range modulation wheel to generate a smooth SOBP in protonradiation therapy. We have found out that a medium number of pristine Bragg peaks are enough to generate a SOBP with flatness less than 2%. It is potential to generate data base to store in the treatment plan to produce a clinic acceptable SOBP by using our simple algorithm.« less

Exploring the Dynamics of Cell Processes through Simulations of Fluorescence Microscopy Experiments

PubMed Central

Angiolini, Juan; Plachta, Nicolas; Mocskos, Esteban; Levi, Valeria

2015-01-01

Fluorescence correlation spectroscopy (FCS) methods are powerful tools for unveiling the dynamical organization of cells. For simple cases, such as molecules passively moving in a homogeneous media, FCS analysis yields analytical functions that can be fitted to the experimental data to recover the phenomenological rate parameters. Unfortunately, many dynamical processes in cells do not follow these simple models, and in many instances it is not possible to obtain an analytical function through a theoretical analysis of a more complex model. In such cases, experimental analysis can be combined with Monte Carlo simulations to aid in interpretation of the data. In response to this need, we developed a method called FERNET (Fluorescence Emission Recipes and Numerical routines Toolkit) based on Monte Carlo simulations and the MCell-Blender platform, which was designed to treat the reaction-diffusion problem under realistic scenarios. This method enables us to set complex geometries of the simulation space, distribute molecules among different compartments, and define interspecies reactions with selected kinetic constants, diffusion coefficients, and species brightness. We apply this method to simulate single- and multiple-point FCS, photon-counting histogram analysis, raster image correlation spectroscopy, and two-color fluorescence cross-correlation spectroscopy. We believe that this new program could be very useful for predicting and understanding the output of fluorescence microscopy experiments. PMID:26039162

Fast and Simple Analytical Method for Direct Determination of Total Chlorine Content in Polyglycerol by ICP-MS.

PubMed

Jakóbik-Kolon, Agata; Milewski, Andrzej; Dydo, Piotr; Witczak, Magdalena; Bok-Badura, Joanna

2018-02-23

The fast and simple method for total chlorine determination in polyglycerols using low resolution inductively coupled plasma mass spectrometry (ICP-MS) without the need for additional equipment and time-consuming sample decomposition was evaluated. Linear calibration curve for 35 Cl isotope in the concentration range 20-800 µg/L was observed. Limits of detection and quantification equaled to 15 µg/L and 44 µg/L, respectively. This corresponds to possibility of detection 3 µg/g and determination 9 µg/g of chlorine in polyglycerol using studied conditions (0.5% matrix-polyglycerol samples diluted or dissolved with water to an overall concentration of 0.5%). Matrix effects as well as the effect of chlorine origin have been evaluated. The presence of 0.5% (m/m) of matrix species similar to polyglycerol (polyethylene glycol-PEG) did not influence the chlorine determination for PEGs with average molecular weights (MW) up to 2000 Da. Good precision and accuracy of the chlorine content determination was achieved regardless on its origin (inorganic/organic). High analyte recovery level and low relative standard deviation values were observed for real polyglycerol samples spiked with chloride. Additionally, the Combustion Ion Chromatography System was used as a reference method. The results confirmed high accuracy and precision of the tested method.

Data as the Driver

ERIC Educational Resources Information Center

Bechler, Kent L.

2013-01-01

In the book "Moneyball: The Art of Winning an Unfair Game," author Michael Lewis describes how the Oakland Athletics, one of the poorest teams in Major League Baseball, became one of the most successful teams by using simple analytical methods that had existed for years but had been largely ignored by the baseball executives. "Moneyball"…

Making and Using a Sensing Polymeric Material for Cu[superscript 2+

ERIC Educational Resources Information Center

Paddock, Jean R.; Maghasi, Anne T.; Heineman, William R.; Seliskar, Carl J.

2005-01-01

A simple chemical sensor-related experiment rooted in the synthesis of polymeric materials for use in either an advanced high-school or undergraduate college laboratory is presented. Students are introduced to and combine to the concepts of the chemical sensor, polymer chemistry, spectroscopy, metal chelates, and quantitative analytical methods.

Simple, rapid, and environmentally friendly method for the separation of isoflavones using ultra-high performance supercritical fluid chromatography.

PubMed

Wu, Wenjie; Zhang, Yuan; Wu, Hanqiu; Zhou, Weie; Cheng, Yan; Li, Hongna; Zhang, Chuanbin; Li, Lulu; Huang, Ying; Zhang, Feng

2017-07-01

Isoflavones are natural substances that exhibit hormone-like pharmacological activities. The separation of isoflavones remains an analytical challenge because of their similar structures. We show that ultra-high performance supercritical fluid chromatography can be an appropriate tool to achieve the fast separation of 12 common dietary isoflavones. Among the five tested columns the Torus DEA column was found to be the most effective column for the separation of these isoflavones. The impact of individual parameters on the retention time and separation factor was evaluated. These parameters were optimized to develop a simple, rapid, and green method for the separation of the 12 target analytes. It only took 12.91 min using gradient elution with methanol as an organic modifier and formic acid as an additive. These isoflavones were determined with limit of quantitation ranging from 0.10 to 0.50 μg/mL, which was sufficient for reliable determination of various matrixes. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Dynamics of a parametrically excited simple pendulum

NASA Astrophysics Data System (ADS)

Depetri, Gabriela I.; Pereira, Felipe A. C.; Marin, Boris; Baptista, Murilo S.; Sartorelli, J. C.

2018-03-01

The dynamics of a parametric simple pendulum submitted to an arbitrary angle of excitation ϕ was investigated experimentally by simulations and analytically. Analytical calculations for the loci of saddle-node bifurcations corresponding to the creation of resonant orbits were performed by applying Melnikov's method. However, this powerful perturbative method cannot be used to predict the existence of odd resonances for a vertical excitation within first order corrections. Yet, we showed that period-3 resonances indeed exist in such a configuration. Two degenerate attractors of different phases, associated with the same loci of saddle-node bifurcations in parameter space, are reported. For tilted excitation, the degeneracy is broken due to an extra torque, which was confirmed by the calculation of two distinct loci of saddle-node bifurcations for each attractor. This behavior persists up to ϕ≈7 π/180 , and for inclinations larger than this, only one attractor is observed. Bifurcation diagrams were constructed experimentally for ϕ=π/8 to demonstrate the existence of self-excited resonances (periods smaller than three) and hidden oscillations (for periods greater than three).

Dynamics of a parametrically excited simple pendulum.

PubMed

Depetri, Gabriela I; Pereira, Felipe A C; Marin, Boris; Baptista, Murilo S; Sartorelli, J C

2018-03-01

The dynamics of a parametric simple pendulum submitted to an arbitrary angle of excitation ϕ was investigated experimentally by simulations and analytically. Analytical calculations for the loci of saddle-node bifurcations corresponding to the creation of resonant orbits were performed by applying Melnikov's method. However, this powerful perturbative method cannot be used to predict the existence of odd resonances for a vertical excitation within first order corrections. Yet, we showed that period-3 resonances indeed exist in such a configuration. Two degenerate attractors of different phases, associated with the same loci of saddle-node bifurcations in parameter space, are reported. For tilted excitation, the degeneracy is broken due to an extra torque, which was confirmed by the calculation of two distinct loci of saddle-node bifurcations for each attractor. This behavior persists up to ϕ≈7π/180, and for inclinations larger than this, only one attractor is observed. Bifurcation diagrams were constructed experimentally for ϕ=π/8 to demonstrate the existence of self-excited resonances (periods smaller than three) and hidden oscillations (for periods greater than three).

Extension of the Helmholtz-Smoluchowski velocity to the hydrophobic microchannels with velocity slip.

PubMed

Park, H M; Kim, T W

2009-01-21

Electrokinetic flows through hydrophobic microchannels experience velocity slip at the microchannel wall, which affects volumetric flow rate and solute retention time. The usual method of predicting the volumetric flow rate and velocity profile for hydrophobic microchannels is to solve the Navier-Stokes equation and the Poisson-Boltzmann equation for the electric potential with the boundary condition of velocity slip expressed by the Navier slip coefficient, which is computationally demanding and defies analytic solutions. In the present investigation, we have devised a simple method of predicting the velocity profiles and volumetric flow rates of electrokinetic flows by extending the concept of the Helmholtz-Smoluchowski velocity to microchannels with Navier slip. The extended Helmholtz-Smoluchowski velocity is simple to use and yields accurate results as compared to the exact solutions. Employing the extended Helmholtz-Smoluchowski velocity, the analytical expressions for volumetric flow rate and velocity profile for electrokinetic flows through rectangular microchannels with Navier slip have been obtained at high values of zeta potential. The range of validity of the extended Helmholtz-Smoluchowski velocity is also investigated.

A New Unified Analysis of Estimate Errors by Model-Matching Phase-Estimation Methods for Sensorless Drive of Permanent-Magnet Synchronous Motors and New Trajectory-Oriented Vector Control, Part II

NASA Astrophysics Data System (ADS)

Shinnaka, Shinji

This paper presents a new unified analysis of estimate errors by model-matching extended-back-EMF estimation methods for sensorless drive of permanent-magnet synchronous motors. Analytical solutions about estimate errors, whose validity is confirmed by numerical experiments, are rich in universality and applicability. As an example of universality and applicability, a new trajectory-oriented vector control method is proposed, which can realize directly quasi-optimal strategy minimizing total losses with no additional computational loads by simply orienting one of vector-control coordinates to the associated quasi-optimal trajectory. The coordinate orientation rule, which is analytically derived, is surprisingly simple. Consequently the trajectory-oriented vector control method can be applied to a number of conventional vector control systems using model-matching extended-back-EMF estimation methods.

Bounded Linear Stability Analysis - A Time Delay Margin Estimation Approach for Adaptive Control

NASA Technical Reports Server (NTRS)

Nguyen, Nhan T.; Ishihara, Abraham K.; Krishnakumar, Kalmanje Srinlvas; Bakhtiari-Nejad, Maryam

2009-01-01

This paper presents a method for estimating time delay margin for model-reference adaptive control of systems with almost linear structured uncertainty. The bounded linear stability analysis method seeks to represent the conventional model-reference adaptive law by a locally bounded linear approximation within a small time window using the comparison lemma. The locally bounded linear approximation of the combined adaptive system is cast in a form of an input-time-delay differential equation over a small time window. The time delay margin of this system represents a local stability measure and is computed analytically by a matrix measure method, which provides a simple analytical technique for estimating an upper bound of time delay margin. Based on simulation results for a scalar model-reference adaptive control system, both the bounded linear stability method and the matrix measure method are seen to provide a reasonably accurate and yet not too conservative time delay margin estimation.

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.

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

Meeks, Kelsey; Pantoya, Michelle L.; Green, Micah

For dispersions containing a single type of particle, it has been observed that the onset of percolation coincides with a critical value of volume fraction. When the volume fraction is calculated based on excluded volume, this critical percolation threshold is nearly invariant to particle shape. The critical threshold has been calculated to high precision for simple geometries using Monte Carlo simulations, but this method is slow at best, and infeasible for complex geometries. This article explores an analytical approach to the prediction of percolation threshold in polydisperse mixtures. Specifically, this paper suggests an extension of the concept of excluded volume,more » and applies that extension to the 2D binary disk system. The simple analytical expression obtained is compared to Monte Carlo results from the literature. In conclusion, the result may be computed extremely rapidly and matches key parameters closely enough to be useful for composite material design.« less

Paper-based microfluidic approach for surface-enhanced raman spectroscopy and highly reproducible detection of proteins beyond picomolar concentration.

PubMed

Saha, Arindam; Jana, Nikhil R

2015-01-14

Although microfluidic approach is widely used in various point of care diagnostics, its implementation in surface enhanced Raman spectroscopy (SERS)-based detection is challenging. This is because SERS signal depends on plasmonic nanoparticle aggregation induced generation of stable electromagnetic hot spots and in currently available microfluidic platform this condition is difficult to adapt. Here we show that SERS can be adapted using simple paper based microfluidic system where both the plasmonic nanomaterials and analyte are used in mobile phase. This approach allows analyte induced controlled particle aggregation and electromagnetic hot spot generation inside the microfluidic channel with the resultant SERS signal, which is highly reproducible and sensitive. This approach has been used for reproducible detection of protein in the pico to femtomolar concentration. Presented approach is simple, rapid, and cost-effective, and requires low sample volume. Method can be extended for SERS-based detection of other biomolecules.

Simultaneous determination of glucose, triglycerides, urea, cholesterol, albumin and total protein in human plasma by Fourier transform infrared spectroscopy: direct clinical biochemistry without reagents.

PubMed

Jessen, Torben E; Höskuldsson, Agnar T; Bjerrum, Poul J; Verder, Henrik; Sørensen, Lars; Bratholm, Palle S; Christensen, Bo; Jensen, Lene S; Jensen, Maria A B

2014-09-01

Direct measurement of chemical constituents in complex biologic matrices without the use of analyte specific reagents could be a step forward toward the simplification of clinical biochemistry. Problems related to reagents such as production errors, improper handling, and lot-to-lot variations would be eliminated as well as errors occurring during assay execution. We describe and validate a reagent free method for direct measurement of six analytes in human plasma based on Fourier-transform infrared spectroscopy (FTIR). Blood plasma is analyzed without any sample preparation. FTIR spectrum of the raw plasma is recorded in a sampling cuvette specially designed for measurement of aqueous solutions. For each analyte, a mathematical calibration process is performed by a stepwise selection of wavelengths giving the optimal least-squares correlation between the measured FTIR signal and the analyte concentration measured by conventional clinical reference methods. The developed calibration algorithms are subsequently evaluated for their capability to predict the concentration of the six analytes in blinded patient samples. The correlation between the six FTIR methods and corresponding reference methods were 0.87

Optimized theory for simple and molecular fluids.

PubMed

Marucho, M; Montgomery Pettitt, B

2007-03-28

An optimized closure approximation for both simple and molecular fluids is presented. A smooth interpolation between Perkus-Yevick and hypernetted chain closures is optimized by minimizing the free energy self-consistently with respect to the interpolation parameter(s). The molecular version is derived from a refinement of the method for simple fluids. In doing so, a method is proposed which appropriately couples an optimized closure with the variant of the diagrammatically proper integral equation recently introduced by this laboratory [K. M. Dyer et al., J. Chem. Phys. 123, 204512 (2005)]. The simplicity of the expressions involved in this proposed theory has allowed the authors to obtain an analytic expression for the approximate excess chemical potential. This is shown to be an efficient tool to estimate, from first principles, the numerical value of the interpolation parameters defining the aforementioned closure. As a preliminary test, representative models for simple fluids and homonuclear diatomic Lennard-Jones fluids were analyzed, obtaining site-site correlation functions in excellent agreement with simulation data.

Erratum: A Simple, Analytical Model of Collisionless Magnetic Reconnection in a Pair Plasma

NASA Technical Reports Server (NTRS)

Hesse, Michael; Zenitani, Seiji; Kuznetsova, Masha; Klimas, Alex

2011-01-01

The following describes a list of errata in our paper, "A simple, analytical model of collisionless magnetic reconnection in a pair plasma." It supersedes an earlier erratum. We recently discovered an error in the derivation of the outflow-to-inflow density ratio.

Evaluation of analytical performance based on partial order methodology.

PubMed

Carlsen, Lars; Bruggemann, Rainer; Kenessova, Olga; Erzhigitov, Erkin

2015-01-01

Classical measurements of performances are typically based on linear scales. However, in analytical chemistry a simple scale may be not sufficient to analyze the analytical performance appropriately. Here partial order methodology can be helpful. Within the context described here, partial order analysis can be seen as an ordinal analysis of data matrices, especially to simplify the relative comparisons of objects due to their data profile (the ordered set of values an object have). Hence, partial order methodology offers a unique possibility to evaluate analytical performance. In the present data as, e.g., provided by the laboratories through interlaboratory comparisons or proficiency testings is used as an illustrative example. However, the presented scheme is likewise applicable for comparison of analytical methods or simply as a tool for optimization of an analytical method. The methodology can be applied without presumptions or pretreatment of the analytical data provided in order to evaluate the analytical performance taking into account all indicators simultaneously and thus elucidating a "distance" from the true value. In the present illustrative example it is assumed that the laboratories analyze a given sample several times and subsequently report the mean value, the standard deviation and the skewness, which simultaneously are used for the evaluation of the analytical performance. The analyses lead to information concerning (1) a partial ordering of the laboratories, subsequently, (2) a "distance" to the Reference laboratory and (3) a classification due to the concept of "peculiar points". Copyright © 2014 Elsevier B.V. All rights reserved.

A numerical test of the topographic bias

NASA Astrophysics Data System (ADS)

Sjöberg, L. E.; Joud, M. S. S.

2018-02-01

In 1962 A. Bjerhammar introduced the method of analytical continuation in physical geodesy, implying that surface gravity anomalies are downward continued into the topographic masses down to an internal sphere (the Bjerhammar sphere). The method also includes analytical upward continuation of the potential to the surface of the Earth to obtain the quasigeoid. One can show that also the common remove-compute-restore technique for geoid determination includes an analytical continuation as long as the complete density distribution of the topography is not known. The analytical continuation implies that the downward continued gravity anomaly and/or potential are/is in error by the so-called topographic bias, which was postulated by a simple formula of L E Sjöberg in 2007. Here we will numerically test the postulated formula by comparing it with the bias obtained by analytical downward continuation of the external potential of a homogeneous ellipsoid to an inner sphere. The result shows that the postulated formula holds: At the equator of the ellipsoid, where the external potential is downward continued 21 km, the computed and postulated topographic biases agree to less than a millimetre (when the potential is scaled to the unit of metre).

A simple analytical method to estimate all exit parameters of a cross-flow air dehumidifier using liquid desiccant.

PubMed

Bassuoni, M M

2014-03-01

The dehumidifier is a key component in liquid desiccant air-conditioning systems. Analytical solutions have more advantages than numerical solutions in studying the dehumidifier performance parameters. This paper presents the performance results of exit parameters from an analytical model of an adiabatic cross-flow liquid desiccant air dehumidifier. Calcium chloride is used as desiccant material in this investigation. A program performing the analytical solution is developed using the engineering equation solver software. Good accuracy has been found between analytical solution and reliable experimental results with a maximum deviation of +6.63% and -5.65% in the moisture removal rate. The method developed here can be used in the quick prediction of the dehumidifier performance. The exit parameters from the dehumidifier are evaluated under the effects of variables such as air temperature and humidity, desiccant temperature and concentration, and air to desiccant flow rates. The results show that hot humid air and desiccant concentration have the greatest impact on the performance of the dehumidifier. The moisture removal rate is decreased with increasing both air inlet temperature and desiccant temperature while increases with increasing air to solution mass ratio, inlet desiccant concentration, and inlet air humidity ratio.

Determination of Three Corticosteroids in the Biologic Matrix of Vitreous Humor by HPLC-tandem Mass Spectrometry: Method Development and Validation.

PubMed

Prieto, Esther; Vispe, Eugenio; Otín-Mallada, Sofía; Garcia-Martin, Elena; Polo-Llorens, Vicente; Fraile, José M; Pablo, Luis E; Mayoral, José A

2017-02-01

To develop a simple, specific, and rapid method to determine corticosteroid concentrations in vitreous humor. An analytical method based on high-pressure liquid chromatography-tandem mass spectrometry (HPLC-MS) with a simple extraction procedure was developed. New Zealand albino rabbits (n = 54) received a single (0.1 mL) intravitreal injection of dexamethasone (DXM, 0.1 mg), methylprednisolone (MP, 2 mg), or triamcinolone acetonide (TA, 10 mg). Eyes were enucleated and mean vitreous steroid levels were quantified at 12 h and 1, 2, 3, 7, and 14 days. Corticosteroids were extracted from the vitreous with acetonitrile, and TA was extracted with ethyl acetate, yielding high protein precipitation and clean solution samples. Vitreous samples were analyzed by isocratic HPLC-MS with mobile phase comprising acetonitrile and 2 mM ammonium formate buffer in water, pH 3.5. The linear range was 50-100,000 ng/g with a lower quantification limit of 45 ng/g for DXM and MP, and 50 ng/g for TA. Vitreous levels of DXM and MP were not detectable 14 days post-administration. Vitreous levels of TA were positive and stable throughout the study in both injected and control eyes. The HPLC-MS analytical method is an alternative to HPLC-MS/MS methods, sensitive enough for identifying and quantifying steroids in vitreous humor at a therapeutic dosage scale.

A simple method to produce 2D and 3D microfluidic paper-based analytical devices for clinical analysis.

PubMed

de Oliveira, Ricardo A G; Camargo, Fiamma; Pesquero, Naira C; Faria, Ronaldo Censi

2017-03-08

This paper describes the fabrication of 2D and 3D microfluidic paper-based analytical devices (μPADs) for monitoring glucose, total protein, and nitrite in blood serum and artificial urine. A new method of cutting and sealing filter paper to construct μPADs was demonstrated. Using an inexpensive home cutter printer soft cellulose-based filter paper was easily and precisely cut to produce pattern hydrophilic microchannels. 2D and 3D μPADs were designed with three detection zones each for the colorimetric detection of the analytes. A small volume of samples was added to the μPADs, which was photographed after 15 min using a digital camera. Both μPADs presented an excellent analytical performance for all analytes. The 2D device was applied in artificial urine samples and reached limits of detection (LODs) of 0.54 mM, 5.19 μM, and 2.34 μM for glucose, protein, and nitrite, respectively. The corresponding LODs of the 3D device applied for detecting the same analytes in artificial blood serum were 0.44 mM, 1.26 μM, and 4.35 μM. Copyright © 2017 Elsevier B.V. All rights reserved.

A Ricin Forensic Profiling Approach Based on a Complex Set of Biomarkers

DOE PAGES

Fredriksson, Sten-Ake; Wunschel, David S.; Lindstrom, Susanne Wiklund; ...

2018-03-28

A forensic method for the retrospective determination of preparation methods used for illicit ricin toxin production was developed. The method was based on a complex set of biomarkers, including carbohydrates, fatty acids, seed storage proteins, in combination with data on ricin and Ricinus communis agglutinin. The analyses were performed on samples prepared from four castor bean plant (R. communis) cultivars by four different sample preparation methods (PM1 – PM4) ranging from simple disintegration of the castor beans to multi-step preparation methods including different protein precipitation methods. Comprehensive analytical data was collected by use of a range of analytical methods andmore » robust orthogonal partial least squares-discriminant analysis- models (OPLS-DA) were constructed based on the calibration set. By the use of a decision tree and two OPLS-DA models, the sample preparation methods of test set samples were determined. The model statistics of the two models were good and a 100% rate of correct predictions of the test set was achieved.« less

A Ricin Forensic Profiling Approach Based on a Complex Set of Biomarkers

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

Fredriksson, Sten-Ake; Wunschel, David S.; Lindstrom, Susanne Wiklund

A forensic method for the retrospective determination of preparation methods used for illicit ricin toxin production was developed. The method was based on a complex set of biomarkers, including carbohydrates, fatty acids, seed storage proteins, in combination with data on ricin and Ricinus communis agglutinin. The analyses were performed on samples prepared from four castor bean plant (R. communis) cultivars by four different sample preparation methods (PM1 – PM4) ranging from simple disintegration of the castor beans to multi-step preparation methods including different protein precipitation methods. Comprehensive analytical data was collected by use of a range of analytical methods andmore » robust orthogonal partial least squares-discriminant analysis- models (OPLS-DA) were constructed based on the calibration set. By the use of a decision tree and two OPLS-DA models, the sample preparation methods of test set samples were determined. The model statistics of the two models were good and a 100% rate of correct predictions of the test set was achieved.« less

Observability during planetary approach navigation

NASA Technical Reports Server (NTRS)

Bishop, Robert H.; Burkhart, P. Daniel; Thurman, Sam W.

1993-01-01

The objective of the research is to develop an analytic technique to predict the relative navigation capability of different Earth-based radio navigation measurements. In particular, the problem is to determine the relative ability of geocentric range and Doppler measurements to detect the effects of the target planet gravitational attraction on the spacecraft during the planetary approach and near-encounter mission phases. A complete solution to the two-dimensional problem has been developed. Relatively simple analytic formulas are obtained for range and Doppler measurements which describe the observability content of the measurement data along the approach trajectories. An observability measure is defined which is based on the observability matrix for nonlinear systems. The results show good agreement between the analytic observability analysis and the computational batch processing method.

Similarity solution of the Boussinesq equation

NASA Astrophysics Data System (ADS)

Lockington, D. A.; Parlange, J.-Y.; Parlange, M. B.; Selker, J.

Similarity transforms of the Boussinesq equation in a semi-infinite medium are available when the boundary conditions are a power of time. The Boussinesq equation is reduced from a partial differential equation to a boundary-value problem. Chen et al. [Trans Porous Media 1995;18:15-36] use a hodograph method to derive an integral equation formulation of the new differential equation which they solve by numerical iteration. In the present paper, the convergence of their scheme is improved such that numerical iteration can be avoided for all practical purposes. However, a simpler analytical approach is also presented which is based on Shampine's transformation of the boundary value problem to an initial value problem. This analytical approximation is remarkably simple and yet more accurate than the analytical hodograph approximations.

Quantum decay model with exact explicit analytical solution

NASA Astrophysics Data System (ADS)

Marchewka, Avi; Granot, Er'El

2009-01-01

A simple decay model is introduced. The model comprises a point potential well, which experiences an abrupt change. Due to the temporal variation, the initial quantum state can either escape from the well or stay localized as a new bound state. The model allows for an exact analytical solution while having the necessary features of a decay process. The results show that the decay is never exponential, as classical dynamics predicts. Moreover, at short times the decay has a fractional power law, which differs from perturbation quantum method predictions. At long times the decay includes oscillations with an envelope that decays algebraically. This is a model where the final state can be either continuous or localized, and that has an exact analytical solution.

Liquid chromatography method to determine polyamines in thermosetting polymers.

PubMed

Dopico-García, M S; López-Vilariño, J M; Fernández-Martínez, G; González-Rodríguez, M V

2010-05-14

A simple, robust and sensitive analytical method to determine three polyamines commonly used as hardeners in epoxy resin systems and in the manufacture of polyurethane is reported. The studied polyamines are: one tetramine, TETA (triethylenetetramine), and two diamines, IPDA (Isophorone diamine) and TCD-diamine (4,7-methano-1H-indene-5,?-dimethanamine, octahydro-). The latter has an incompletely defined structure, and, as far as we know, has not been previously determined by other methods. All three polyamines contain primary amines; TETA also contains secondary amines. The analytical method involves derivatization with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate, used for the first time for these compounds, followed by high performance liquid chromatography (HPLC) analysis with a fluorescence (FL) detector (lambda excitation 248nm, lambda emision 395nm). The HPLC-DAD-LTQ Orbitrap MS was used in order to provide structural information about the obtained derivatized compounds. The hybrid linear ion trap LTQ Orbitrap mass spectrometer has been introduced in recent years and provides a high mass accuracy. The structures of the derivatized analytes were identified from the protonated molecular ions [M+H](+) and corresponded to the fully labelled analytes. The following analytical parameters were determined for the method using the HPLC-FL: linearity, precision (2.5-10%), instrumental precision intraday (0.8-1.5%) and interday (2.9-6.3%), and detection limits (0.02-0.14mgL(-1)). The stability of stock solutions and derivatized compounds was also investigated. The method was applied to determine the amine free content in epoxy resin dust collected in workplaces. Copyright 2010 Elsevier B.V. All rights reserved.

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

Hoenig, M.; Elsen, Y.V.; Cauter, R.V.

The progressive degradation of the pyrolytic graphite surface of atomizers provides variable and misleading results of molybdenum peak-height measurements. The changes in the peak shapes produce no analytical problems during the lifetime of the atomizer (approx.300 firings) when integrated absorbance (A.s signals) is considered and the possible base-line drifts are controlled. This was demonstrated on plant samples mineralized by simple digestion with a mixture of HNO/sub 3/ and H/sub 2/O/sub 2/. The value of this method was assessed by comparison with a standard dry oxidation method and by molybdenum determination in National Bureau of Standards reference plant samples. The relativemore » standard deviations (n = 5) of the full analytical procedure do not exceed 7%. 13 references, 3 figures, 3 tables.« less

Quantum State Tomography via Linear Regression Estimation

PubMed Central

Qi, Bo; Hou, Zhibo; Li, Li; Dong, Daoyi; Xiang, Guoyong; Guo, Guangcan

2013-01-01

A simple yet efficient state reconstruction algorithm of linear regression estimation (LRE) is presented for quantum state tomography. In this method, quantum state reconstruction is converted into a parameter estimation problem of a linear regression model and the least-squares method is employed to estimate the unknown parameters. An asymptotic mean squared error (MSE) upper bound for all possible states to be estimated is given analytically, which depends explicitly upon the involved measurement bases. This analytical MSE upper bound can guide one to choose optimal measurement sets. The computational complexity of LRE is O(d4) where d is the dimension of the quantum state. Numerical examples show that LRE is much faster than maximum-likelihood estimation for quantum state tomography. PMID:24336519

Distributed Parameter Analysis of Pressure and Flow Disturbances in Rocket Propellant Feed Systems

NASA Technical Reports Server (NTRS)

Dorsch, Robert G.; Wood, Don J.; Lightner, Charlene

1966-01-01

A digital distributed parameter model for computing the dynamic response of propellant feed systems is formulated. The analytical approach used is an application of the wave-plan method of analyzing unsteady flow. Nonlinear effects are included. The model takes into account locally high compliances at the pump inlet and at the injector dome region. Examples of the calculated transient and steady-state periodic responses of a simple hypothetical propellant feed system to several types of disturbances are presented. Included are flow disturbances originating from longitudinal structural motion, gimbaling, throttling, and combustion-chamber coupling. The analytical method can be employed for analyzing developmental hardware and offers a flexible tool for the calculation of unsteady flow in these systems.

Rapid screening of mixed edible oils and gutter oils by matrix-assisted laser desorption/ionization mass spectrometry.

PubMed

Ng, Tsz-Tsun; So, Pui-Kin; Zheng, Bo; Yao, Zhong-Ping

2015-07-16

Authentication of edible oils is a long-term issue in food safety, and becomes particularly important with the emergence and wide spread of gutter oils in recent years. Due to the very high analytical demand and diversity of gutter oils, a high throughput analytical method and a versatile strategy for authentication of mixed edible oils and gutter oils are highly desirable. In this study, an improved matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) method has been developed for direct analysis of edible oils. This method involved on-target sample loading, automatic data acquisition and simple data processing. MALDI-MS spectra with high quality and high reproducibility have been obtained using this method, and a preliminary spectral database of edible oils has been set up. The authenticity of an edible oil sample can be determined by comparing its MALDI-MS spectrum and principal component analysis (PCA) results with those of its labeled oil in the database. This method is simple and the whole process only takes several minutes for analysis of one oil sample. We demonstrated that the method was sensitive to change in oil compositions and can be used for measuring compositions of mixed oils. The capability of the method for determining mislabeling enables it for rapid screening of gutter oils since fraudulent mislabeling is a common feature of gutter oils. Copyright © 2015 Elsevier B.V. All rights reserved.

Quantitative determination of carcinogenic mycotoxins in human and animal biological matrices and animal-derived foods using multi-mycotoxin and analyte-specific high performance liquid chromatography-tandem mass spectrometric methods.

PubMed

Cao, Xiaoqin; Li, Xiaofei; Li, Jian; Niu, Yunhui; Shi, Lu; Fang, Zhenfeng; Zhang, Tao; Ding, Hong

2018-01-15

A sensitive and reliable multi-mycotoxin-based method was developed to identify and quantify several carcinogenic mycotoxins in human blood and urine, as well as edible animal tissues, including muscle and liver tissue from swine and chickens, using liquid chromatography-tandem mass spectrometry (LC-MS/MS). For the toxicokinetic studies with individual mycotoxins, highly sensitive analyte-specific LC-MS/MS methods were developed for rat plasma and urine. Sample purification consisted of a rapid 'dilute and shoot' approach in urine samples, a simple 'dilute, evaporate and shoot' approach in plasma samples and a 'QuEChERS' procedure in edible animal tissues. The multi-mycotoxin and analyte-specific methods were validated in-house: The limits of detection (LOD) for the multi-mycotoxin and analyte-specific methods ranged from 0.02 to 0.41 μg/kg (μg/L) and 0.01 to 0.19 μg/L, respectively, and limits of quantification (LOQ) between 0.10 to 1.02 μg/kg (μg/L) and 0.09 to 0.47 μg/L, respectively. Apparent recoveries of the samples spiked with 0.25 to 4 μg/kg (μg/L) ranged from 60.1% to 109.8% with relative standard deviations below 15%. The methods were successfully applied to real samples. To the best of our knowledge, this is the first study carried out using a small group of patients from the Chinese population with hepatocellular carcinoma to assess their exposure to carcinogenic mycotoxins using biomarkers. Finally, the multi-mycotoxin method is a useful analytical method for assessing exposure to mycotoxins edible in animal tissues. The analyte-specific methods could be useful during toxicokinetic and toxicological studies. Copyright © 2017. Published by Elsevier B.V.

Approximate analytical relationships for linear optimal aeroelastic flight control laws

NASA Astrophysics Data System (ADS)

Kassem, Ayman Hamdy

1998-09-01

This dissertation introduces new methods to uncover functional relationships between design parameters of a contemporary control design technique and the resulting closed-loop properties. Three new methods are developed for generating such relationships through analytical expressions: the Direct Eigen-Based Technique, the Order of Magnitude Technique, and the Cost Function Imbedding Technique. Efforts concentrated on the linear-quadratic state-feedback control-design technique applied to an aeroelastic flight control task. For this specific application, simple and accurate analytical expressions for the closed-loop eigenvalues and zeros in terms of basic parameters such as stability and control derivatives, structural vibration damping and natural frequency, and cost function weights are generated. These expressions explicitly indicate how the weights augment the short period and aeroelastic modes, as well as the closed-loop zeros, and by what physical mechanism. The analytical expressions are used to address topics such as damping, nonminimum phase behavior, stability, and performance with robustness considerations, and design modifications. This type of knowledge is invaluable to the flight control designer and would be more difficult to formulate when obtained from numerical-based sensitivity analysis.

From analytical solutions of solute transport equations to multidimensional time-domain random walk (TDRW) algorithms

NASA Astrophysics Data System (ADS)

Bodin, Jacques

2015-03-01

In this study, new multi-dimensional time-domain random walk (TDRW) algorithms are derived from approximate one-dimensional (1-D), two-dimensional (2-D), and three-dimensional (3-D) analytical solutions of the advection-dispersion equation and from exact 1-D, 2-D, and 3-D analytical solutions of the pure-diffusion equation. These algorithms enable the calculation of both the time required for a particle to travel a specified distance in a homogeneous medium and the mass recovery at the observation point, which may be incomplete due to 2-D or 3-D transverse dispersion or diffusion. The method is extended to heterogeneous media, represented as a piecewise collection of homogeneous media. The particle motion is then decomposed along a series of intermediate checkpoints located on the medium interface boundaries. The accuracy of the multi-dimensional TDRW method is verified against (i) exact analytical solutions of solute transport in homogeneous media and (ii) finite-difference simulations in a synthetic 2-D heterogeneous medium of simple geometry. The results demonstrate that the method is ideally suited to purely diffusive transport and to advection-dispersion transport problems dominated by advection. Conversely, the method is not recommended for highly dispersive transport problems because the accuracy of the advection-dispersion TDRW algorithms degrades rapidly for a low Péclet number, consistent with the accuracy limit of the approximate analytical solutions. The proposed approach provides a unified methodology for deriving multi-dimensional time-domain particle equations and may be applicable to other mathematical transport models, provided that appropriate analytical solutions are available.

A sensitive LC-MS/MS method for simultaneous determination of amygdalin and paeoniflorin in human plasma and its application.

PubMed

Li, Xiaobing; Shi, Fuguo; Gu, Pan; Liu, Lingye; He, Hua; Ding, Li

2014-04-01

A simple and sensitive HPLC-MS/MS method was developed and fully validated for the simultaneous determination of amygdalin (AD) and paeoniflorin (PF) in human plasma. For both analytes, the method exhibited high sensitivity (LLOQs of 0.6ng/mL) by selecting the ammonium adduct ions ([M+NH4](+)) as the precursor ions and good linearity over the concentration range of 0.6-2000ng/mL with the correlation coefficients>0.9972. The intra- and inter-day precision was lower than 10% in relation to relative standard deviation, while accuracy was within ±2.3% in terms of relative error for both analytes. The developed method was successfully applied to a pilot pharmacokinetic study of AD and PF in healthy volunteers after intravenous infusion administration of Huoxue-Tongluo lyophilized powder for injection. Copyright © 2014 Elsevier B.V. All rights reserved.

Mathematical modeling and pharmaceutical pricing: analyses used to inform in-licensing and developmental go/No-Go decisions.

PubMed

Vernon, John A; Hughen, W Keener; Johnson, Scott J

2005-05-01

In the face of significant real healthcare cost inflation, pressured budgets, and ongoing launches of myriad technology of uncertain value, payers have formalized new valuation techniques that represent a barrier to entry for drugs. Cost-effectiveness analysis predominates among these methods, which involves differencing a new technological intervention's marginal costs and benefits with a comparator's, and comparing the resulting ratio to a payer's willingness-to-pay threshold. In this paper we describe how firms are able to model the feasible range of future product prices when making in-licensing and developmental Go/No-Go decisions by considering payers' use of the cost-effectiveness method. We illustrate this analytic method with a simple deterministic example and then incorporate stochastic assumptions using both analytic and simulation methods. Using this strategic approach, firms may reduce product development and in-licensing risk.

Methods to Assess Bioavailability of Hydrophobic Organic Contaminants: Principles, Operations, and Limitations

PubMed Central

Cui, Xinyi; Mayer, Philipp; Gan, Jay

2013-01-01

Many important environmental contaminants are hydrophobic organic contaminants (HOCs), which include PCBs, PAHs, PBDEs, DDT and other chlorinated insecticides, among others. Owing to their strong hydrophobicity, HOCs have their final destination in soil or sediment, where their ecotoxicological effects are closely regulated by sorption and thus bioavailability. The last two decades has seen a dramatic increase in research efforts in developing and applying partitioning based methods and biomimetic extractions for measuring HOC bioavailability. However, the many variations of both analytical methods and associated measurement endpoints are often a source of confusion for users. In this review, we distinguish the most commonly used analytical approaches based on their measurement objectives, and illustrate their practical operational steps, strengths and limitations using simple flowcharts. This review may serve as guidance for new users on the selection and use of established methods, and a reference for experienced investigators to identify potential topics for further research. PMID:23064200

Q-controlled amplitude modulation atomic force microscopy in liquids: An analysis

NASA Astrophysics Data System (ADS)

Hölscher, H.; Schwarz, U. D.

2006-08-01

An analysis of amplitude modulation atomic force microscopy in liquids is presented with respect to the application of the Q-Control technique. The equation of motion is solved by numerical and analytic methods with and without Q-Control in the presence of a simple model interaction force adequate for many liquid environments. In addition, the authors give an explicit analytical formula for the tip-sample indentation showing that higher Q factors reduce the tip-sample force. It is found that Q-Control suppresses unwanted deformations of the sample surface, leading to the enhanced image quality reported in several experimental studies.

Multidisciplinary optimization in aircraft design using analytic technology models

NASA Technical Reports Server (NTRS)

Malone, Brett; Mason, W. H.

1991-01-01

An approach to multidisciplinary optimization is presented which combines the Global Sensitivity Equation method, parametric optimization, and analytic technology models. The result is a powerful yet simple procedure for identifying key design issues. It can be used both to investigate technology integration issues very early in the design cycle, and to establish the information flow framework between disciplines for use in multidisciplinary optimization projects using much more computational intense representations of each technology. To illustrate the approach, an examination of the optimization of a short takeoff heavy transport aircraft is presented for numerous combinations of performance and technology constraints.

Bio-analytical method development and validation of Rasagiline by high performance liquid chromatography tandem mass spectrometry detection and its application to pharmacokinetic study

PubMed Central

Konda, Ravi Kumar; Chandu, Babu Rao; Challa, B.R.; Kothapalli, Chandrasekhar B.

2012-01-01

The most suitable bio-analytical method based on liquid–liquid extraction has been developed and validated for quantification of Rasagiline in human plasma. Rasagiline-13C3 mesylate was used as an internal standard for Rasagiline. Zorbax Eclipse Plus C18 (2.1 mm×50 mm, 3.5 μm) column provided chromatographic separation of analyte followed by detection with mass spectrometry. The method involved simple isocratic chromatographic condition and mass spectrometric detection in the positive ionization mode using an API-4000 system. The total run time was 3.0 min. The proposed method has been validated with the linear range of 5–12000 pg/mL for Rasagiline. The intra-run and inter-run precision values were within 1.3%–2.9% and 1.6%–2.2% respectively for Rasagiline. The overall recovery for Rasagiline and Rasagiline-13C3 mesylate analog was 96.9% and 96.7% respectively. This validated method was successfully applied to the bioequivalence and pharmacokinetic study of human volunteers under fasting condition. PMID:29403764

Determination of glycerophosphate and other anions in dentifrices by ion chromatography.

PubMed

Chen, Yongxin; Ye, Mingli; Cui, Hairong; Wu, Feiyan; Zhu, Yan; Fritz, James S

2006-06-16

Simple, reliable and sensitive analytical methods to determine the anions, such as fluoride, monofluorophaosphate, glycerophosphate related to anticaries are necessary for basic investigations of anticaries and quality control of dentifrices. A method for the simultaneous determination of organic acids, organic anions and inorganic anions in the sample of commercial toothpaste is proposed. Nine anions (fluoride, chloride, nitrite, nitrate, sulfate, phosphate, monofluorophaosphate, glycerophosphate and oxalic acid) were analyzed by means of ion chromatography using a gradient elution with KOH as mobile phase, IonPac AS18 as the separation column and suppressed conductivity detection. Optimized analytical conditions were further validated in terms of accuracy, precision and total uncertainty and the results showed the reliability of the IC method. The relative standard deviations (RSD) of the retention time and peak area of all species were less than 0.170 and 1.800%, respectively. The correlation coefficients for target analytes ranged from 0.9985 to 0.9996. The detection limit (signal to noise ratio of 3:1) of this method was at low ppb level (<15 ppb). The spiked recoveries for the anions were 96-103%. The method was applied to toothpaste without interferences.

Electrolyte system strategies for anionic ITP with ESI-MS detection. 3. The ITP spacer technique in moving-boundary systems and configurations with two self-maintained ITP subsystems.

PubMed

Gebauer, Petr; Malá, Zdena; Boček, Petr

2014-03-01

This contribution is the third part of the project on strategies used in the selection and tuning of electrolyte systems for anionic ITP with ESI-MS detection. The strategy presented here is based on the creation of self-maintained ITP subsystems in moving-boundary systems and describes two new principal approaches offering physical separation of analyte zones from their common ITP stack and/or simultaneous selective stacking of two different analyte groups. Both strategic directions are based on extending the number of components forming the electrolyte system by adding a third suitable anion. The first method is the application of the spacer technique to moving-boundary anionic ITP systems, the second method is a technique utilizing a moving-boundary ITP system in which two ITP subsystems exist and move with mutually different velocities. It is essential for ESI detection that both methods can be based on electrolyte systems containing only several simple chemicals, such as simple volatile organic acids (formic and acetic) and their ammonium salts. The properties of both techniques are defined theoretically and discussed from the viewpoint of their applicability to trace analysis by ITP-ESI-MS. Examples of system design for selected model separations of preservatives and pharmaceuticals illustrate the validity of the theoretical model and application potential of the proposed techniques by both computer simulations and experiments. Both new methods enhance the application range of ITP-MS and may be beneficial particularly for complex multicomponent samples or for analytes with identical molecular mass. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ultrasound-assisted extraction of azadirachtin from dried entire fruits of Azadirachta indica A. Juss. (Meliaceae) and its determination by a validated HPLC-PDA method.

PubMed

de Paula, Joelma Abadia Marciano; Brito, Lucas Ferreira; Caetano, Karen Lorena Ferreira Neves; de Morais Rodrigues, Mariana Cristina; Borges, Leonardo Luiz; da Conceição, Edemilson Cardoso

2016-01-01

Azadirachta indica A. Juss., also known as neem, is a Meliaceae family tree from India. It is globally known for the insecticidal properties of its limonoid tetranortriterpenoid derivatives, such as azadirachtin. This work aimed to optimize the azadirachtin ultrasound-assisted extraction (UAE) and validate the HPLC-PDA analytical method for the measurement of this marker in neem dried fruit extracts. Box-Behnken design and response surface methodology (RSM) were used to investigate the effect of process variables on the UAE. Three independent variables, including ethanol concentration (%, w/w), temperature (°C), and material-to-solvent ratio (gmL(-1)), were studied. The azadirachtin content (µgmL(-1)), i.e., dependent variable, was quantified by the HPLC-PDA analytical method. Isocratic reversed-phase chromatography was performed using acetonitrile/water (40:60), a flow of 1.0mLmin(-1), detection at 214nm, and C18 column (250×4.6mm(2), 5µm). The primary validation parameters were determined according to ICH guidelines and Brazilian legislation. The results demonstrated that the optimal UAE condition was obtained with ethanol concentration range of 75-80% (w/w), temperature of 30°C, and material-to-solvent ratio of 0.55gmL(-1). The HPLC-PDA analytical method proved to be simple, selective, linear, precise, accurate and robust. The experimental values of azadirachtin content under optimal UAE conditions were in good agreement with the RSM predicted values and were superior to the azadirachtin content of percolated extract. Such findings suggest that UAE is a more efficient extractive process in addition to being simple, fast, and inexpensive. Copyright © 2015 Elsevier B.V. All rights reserved.

Simultaneous quantification of fentanyl, sufentanil, cefazolin, doxapram and keto-doxapram in plasma using liquid chromatography - tandem mass spectrometry.

PubMed

Flint, Robert B; Bahmany, Soma; van der Nagel, Bart C H; Koch, Birgit C P

2018-05-16

A simple and specific UPLC-MS/MS method was developed and validated for simultaneous quantification of fentanyl, sufentanil, cefazolin, doxapram and its active metabolite keto-doxapram. The internal standard was fentanyl-d5 for all analytes. Chromatographic separation was achieved with a reversed phase Acquity UPLC HSS T3 column with a run-time of only 5.0 minutes per injected sample. Gradient elution was performed with a mobile phase consisting of ammonium acetate, formic acid in Milli-Q ultrapure water or in methanol with a total flow rate of 0.4 mL minute -1 . A plasma volume of only 50 μL was required to achieve both adequate accuracy and precision. Calibration curves of all 5 analytes were linear. All analytes were stable for at least 48 hours in the autosampler. The method was validated according to US Food and Drug Administration guidelines. This method allows quantification of fentanyl, sufentanil, cefazolin, doxapram and keto-doxapram, which serves purposes for research, as well as therapeutic drug monitoring, if applicable. The strength of this method is the combination of a small sample volume, a short run-time, a deuterated internal standard, an easy sample preparation method and the ability to simultaneously quantify all analytes in one run. This article is protected by copyright. All rights reserved.

Determination of tocopherols and sitosterols in seeds and nuts by QuEChERS-liquid chromatography.

PubMed

Delgado-Zamarreño, M Milagros; Fernández-Prieto, Cristina; Bustamante-Rangel, Myriam; Pérez-Martín, Lara

2016-02-01

In the present work a simple, reliable and affordable sample treatment method for the simultaneous analysis of tocopherols and free phytosterols in nuts was developed. Analyte extraction was carried out using the QuEChERS methodology and analyte separation and detection were accomplished using HPLC-DAD. The use of this methodology for the extraction of natural occurring substances provides advantages such as speed, simplicity and ease of use. The parameters evaluated for the validation of the method developed included the linearity of the calibration plots, the detection and quantification limits, repeatability, reproducibility and recovery. The proposed method was successfully applied to the analysis of tocopherols and free phytosterols in samples of almonds, cashew nuts, hazelnuts, peanuts, tiger nuts, sun flower seeds and pistachios. Copyright © 2015 Elsevier Ltd. All rights reserved.

Understanding Business Analytics

DTIC Science & Technology

2015-01-05

analytics have been used in organizations for a variety of reasons for quite some time; ranging from the simple (generating and understanding business analytics...process. understanding business analytics 3 How well these two components are orchestrated will determine the level of success an organization has in

Supersymmetric quantum mechanics method for the Fokker-Planck equation with applications to protein folding dynamics

NASA Astrophysics Data System (ADS)

Polotto, Franciele; Drigo Filho, Elso; Chahine, Jorge; Oliveira, Ronaldo Junio de

2018-03-01

This work developed analytical methods to explore the kinetics of the time-dependent probability distributions over thermodynamic free energy profiles of protein folding and compared the results with simulation. The Fokker-Planck equation is mapped onto a Schrödinger-type equation due to the well-known solutions of the latter. Through a semi-analytical description, the supersymmetric quantum mechanics formalism is invoked and the time-dependent probability distributions are obtained with numerical calculations by using the variational method. A coarse-grained structure-based model of the two-state protein Tm CSP was simulated at a Cα level of resolution and the thermodynamics and kinetics were fully characterized. Analytical solutions from non-equilibrium conditions were obtained with the simulated double-well free energy potential and kinetic folding times were calculated. It was found that analytical folding time as a function of temperature agrees, quantitatively, with simulations and experiments from the literature of Tm CSP having the well-known 'U' shape of the Chevron Plots. The simple analytical model developed in this study has a potential to be used by theoreticians and experimentalists willing to explore, quantitatively, rates and the kinetic behavior of their system by informing the thermally activated barrier. The theory developed describes a stochastic process and, therefore, can be applied to a variety of biological as well as condensed-phase two-state systems.

Approximate analytical solution for induction heating of solid cylinders

DOE PAGES

Jankowski, Todd Andrew; Pawley, Norma Helen; Gonzales, Lindsey Michal; ...

2015-10-20

An approximate solution to the mathematical model for induction heating of a solid cylinder in a cylindrical induction coil is presented here. The coupled multiphysics model includes equations describing the electromagnetic field in the heated object, a heat transfer simulation to determine temperature of the heated object, and an AC circuit simulation of the induction heating power supply. A multiple-scale perturbation method is used to solve the multiphysics model. The approximate analytical solution yields simple closed-form expressions for the electromagnetic field and heat generation rate in the solid cylinder, for the equivalent impedance of the associated tank circuit, and formore » the frequency response of a variable frequency power supply driving the tank circuit. The solution developed here is validated by comparing predicted power supply frequency to both experimental measurements and calculated values from finite element analysis for heating of graphite cylinders in an induction furnace. The simple expressions from the analytical solution clearly show the functional dependence of the power supply frequency on the material properties of the load and the geometrical characteristics of the furnace installation. In conclusion, the expressions developed here provide physical insight into observations made during load signature analysis of induction heating.« less

The magnetic particle in a box: Analytic and micromagnetic analysis of probe-localized spin wave modes

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

Adur, Rohan, E-mail: adur@physics.osu.edu; Du, Chunhui; Manuilov, Sergei A.

2015-05-07

The dipole field from a probe magnet can be used to localize a discrete spectrum of standing spin wave modes in a continuous ferromagnetic thin film without lithographic modification to the film. Obtaining the resonance field for a localized mode is not trivial due to the effect of the confined and inhomogeneous magnetization precession. We compare the results of micromagnetic and analytic methods to find the resonance field of localized modes in a ferromagnetic thin film, and investigate the accuracy of these methods by comparing with a numerical minimization technique that assumes Bessel function modes with pinned boundary conditions. Wemore » find that the micromagnetic technique, while computationally more intensive, reveals that the true magnetization profiles of localized modes are similar to Bessel functions with gradually decaying dynamic magnetization at the mode edges. We also find that an analytic solution, which is simple to implement and computationally much faster than other methods, accurately describes the resonance field of localized modes when exchange fields are negligible, and demonstrating the accessibility of localized mode analysis.« less

Simultaneous determination of fluoride, chloride, sulfate, phosphate, monofluorophosphate, glycerophosphate, sorbate, and saccharin in gargles by ion chromatography*

PubMed Central

Zhang, Yan-zhen; Zhou, Yan-chun; Liu, Li; Zhu, Yan

2007-01-01

Simple, reliable and sensitive analytical methods to determine anticariogenic agents, preservatives, and artificial sweeteners contained in commercial gargles are necessary for evaluating their effectiveness, safety, and quality. An ion chromatography (IC) method has been described to analyze simultaneously eight anions including fluoride, chloride, sulfate, phosphate, monofluorophosphate, glycerophosphate (anticariogenic agents), sorbate (a preservative), and saccharin (an artificial sweetener) in gargles. In this IC system, we applied a mobile phased gradient elution with KOH, separation by IonPac AS18 columns, and suppressed conductivity detection. Optimized analytical conditions were further evaluated for accuracy. The relative standard deviations (RSDs) of the inter-day’s retention time and peak area of all species were less than 0.938% and 8.731%, respectively, while RSDs of 5-day retention time and peak area were less than 1.265% and 8.934%, respectively. The correlation coefficients for targeted analytes ranged from 0.999 7 to 1.000 0. The spiked recoveries for the anions were 90%~102.5%. We concluded that the method can be applied for comprehensive evaluation of commercial gargles. PMID:17610331

Simultaneous determination of fluoride, chloride, sulfate, phosphate, monofluorophosphate, glycerophosphate, sorbate, and saccharin in gargles by ion chromatography.

PubMed

Zhang, Yan-zhen; Zhou, Yan-chun; Liu, Li; Zhu, Yan

2007-07-01

Simple, reliable and sensitive analytical methods to determine anticariogenic agents, preservatives, and artificial sweeteners contained in commercial gargles are necessary for evaluating their effectiveness, safety, and quality. An ion chromatography (IC) method has been described to analyze simultaneously eight anions including fluoride, chloride, sulfate, phosphate, monofluorophosphate, glycerophosphate (anticariogenic agents), sorbate (a preservative), and saccharin (an artificial sweetener) in gargles. In this IC system, we applied a mobile phased gradient elution with KOH, separation by IonPac AS18 columns, and suppressed conductivity detection. Optimized analytical conditions were further evaluated for accuracy. The relative standard deviations (RSDs) of the inter-day's retention time and peak area of all species were less than 0.938% and 8.731%, respectively, while RSDs of 5-day retention time and peak area were less than 1.265% and 8.934%, respectively. The correlation coefficients for targeted analytes ranged from 0.999 7 to 1.000 0. The spiked recoveries for the anions were 90% approximately 102.5%. We concluded that the method can be applied for comprehensive evaluation of commercial gargles.

Simple and accurate methods for quantifying deformation, disruption, and development in biological tissues

PubMed Central

Boyle, John J.; Kume, Maiko; Wyczalkowski, Matthew A.; Taber, Larry A.; Pless, Robert B.; Xia, Younan; Genin, Guy M.; Thomopoulos, Stavros

2014-01-01

When mechanical factors underlie growth, development, disease or healing, they often function through local regions of tissue where deformation is highly concentrated. Current optical techniques to estimate deformation can lack precision and accuracy in such regions due to challenges in distinguishing a region of concentrated deformation from an error in displacement tracking. Here, we present a simple and general technique for improving the accuracy and precision of strain estimation and an associated technique for distinguishing a concentrated deformation from a tracking error. The strain estimation technique improves accuracy relative to other state-of-the-art algorithms by directly estimating strain fields without first estimating displacements, resulting in a very simple method and low computational cost. The technique for identifying local elevation of strain enables for the first time the successful identification of the onset and consequences of local strain concentrating features such as cracks and tears in a highly strained tissue. We apply these new techniques to demonstrate a novel hypothesis in prenatal wound healing. More generally, the analytical methods we have developed provide a simple tool for quantifying the appearance and magnitude of localized deformation from a series of digital images across a broad range of disciplines. PMID:25165601

Simple method for self-referenced and lable-free biosensing by using a capillary sensing element.

PubMed

Liu, Yun; Chen, Shimeng; Liu, Qiang; Liu, Zigeng; Wei, Peng

2017-05-15

We demonstrated a simple method for self-reference and label free biosensing based on a capillary sensing element and common optoelectronic devices. The capillary sensing element is illuminated by a light-emitting diode (LED) light source and detected by a webcam. Part of gold film that deposited on the tubing wall is functionalized to carry on the biological information in the excited SPR modes. The end face of the capillary was monitored and separate regions of interest (ROIs) were selected as the measurement channel and the reference channel. In the ROIs, the biological information can be accurately extracted from the image by simple image processing. Moreover, temperature fluctuation, bulk RI fluctuation, light source fluctuation and other factors can be effectively compensated during detection. Our biosensing device has a sensitivity of 1145%/RIU and a resolution better than 5.287 × 10 -4 RIU, considering a 0.79% noise level. We apply it for concanavalin A (Con A) biological measurement, which has an approximately linear response to the specific analyte concentration. This simple method provides a new approach for multichannel SPR sensing and reference-compensated calibration of SPR signal for label-free detection.

Prediction of Sound Waves Propagating Through a Nozzle Without/With a Shock Wave Using the Space-Time CE/SE Method

NASA Technical Reports Server (NTRS)

Wang, Xiao-Yen; Chang, Sin-Chung; Jorgenson, Philip C. E.

2000-01-01

The benchmark problems in Category 1 (Internal Propagation) of the third Computational Aeroacoustics (CAA) Work-shop sponsored by NASA Glenn Research Center are solved using the space-time conservation element and solution element (CE/SE) method. The first problem addresses the propagation of sound waves through a nearly choked transonic nozzle. The second one concerns shock-sound interaction in a supersonic nozzle. A quasi one-dimension CE/SE Euler solver for a nonuniform mesh is developed and employed to solve both problems. Numerical solutions are compared with the analytical solution for both problems. It is demonstrated that the CE/SE method is capable of solving aeroacoustic problems with/without shock waves in a simple way. Furthermore, the simple nonreflecting boundary condition used in the CE/SE method which is not based on the characteristic theory works very well.

Trends in tungsten coil atomic spectrometry

NASA Astrophysics Data System (ADS)

Donati, George L.

Renewed interest in electrothermal atomic spectrometric methods based on tungsten coil atomizers is a consequence of a world wide increasing demand for fast, inexpensive, sensitive, and portable analytical methods for trace analysis. In this work, tungsten coil atomic absorption spectrometry (WCAAS) and tungsten coil atomic emission spectrometry (WCAES) are used to determine several different metals and even a non-metal at low levels in different samples. Improvements in instrumentation and new strategies to reduce matrix effects and background signals are presented. Investigation of the main factors affecting both WCAAS and WCAES analytical signals points to the importance of a reducing, high temperature gas phase in the processes leading to atomic cloud generation. Some more refractory elements such as V and Ti were determined for the first time by double tungsten coil atomic emission spectrometry (DWCAES). The higher temperatures provided by two atomizers in DWCAES also allowed the detection of Ag, Cu and Sn emission signals for the first time. Simultaneous determination of several elements by WCAES in relatively complex sample matrices was possible after a simple acid extraction. The results show the potential of this method as an alternative to more traditional, expensive methods for fast, more effective analyses and applications in the field. The development of a new metallic atomization cell is also presented. Lower limits of detection in both WCAAS and WCAES determinations were obtained due to factors such as better control of background signal, smaller, more isothermal system, with atomic cloud concentration at the optical path for a longer period of time. Tungsten coil-based methods are especially well suited to applications requiring low sample volume, low cost, sensitivity and portability. Both WCAAS and WCAES have great commercial potential in fields as diverse as archeology and industrial quality control. They are simple, inexpensive, effective methods for trace metal determinations in several different samples, representing an important asset in today's analytical chemistry.

A new method for flight test determination of propulsive efficiency and drag coefficient

NASA Technical Reports Server (NTRS)

Bull, G.; Bridges, P. D.

1983-01-01

A flight test method is described from which propulsive efficiency as well as parasite and induced drag coefficients can be directly determined using relatively simple instrumentation and analysis techniques. The method uses information contained in the transient response in airspeed for a small power change in level flight in addition to the usual measurement of power required for level flight. Measurements of pitch angle and longitudinal and normal acceleration are eliminated. The theoretical basis for the method, the analytical techniques used, and the results of application of the method to flight test data are presented.

Analysis and Experimental Investigation of Optimum Design of Thermoelectric Cooling/Heating System for Car Seat Climate Control (CSCC)

NASA Astrophysics Data System (ADS)

Elarusi, Abdulmunaem; Attar, Alaa; Lee, HoSung

2018-02-01

The optimum design of a thermoelectric system for application in car seat climate control has been modeled and its performance evaluated experimentally. The optimum design of the thermoelectric device combining two heat exchangers was obtained by using a newly developed optimization method based on the dimensional technique. Based on the analytical optimum design results, commercial thermoelectric cooler and heat sinks were selected to design and construct the climate control heat pump. This work focuses on testing the system performance in both cooling and heating modes to ensure accurate analytical modeling. Although the analytical performance was calculated using the simple ideal thermoelectric equations with effective thermoelectric material properties, it showed very good agreement with experiment for most operating conditions.

WHAEM: PROGRAM DOCUMENTATION FOR THE WELLHEAD ANALYTIC ELEMENT MODEL

EPA Science Inventory

The Wellhead Analytic Element Model (WhAEM) demonstrates a new technique for the definition of time-of-travel capture zones in relatively simple geohydrologic settings. he WhAEM package includes an analytic element model that uses superposition of (many) analytic solutions to gen...

Environmental monitoring of phenolic pollutants in water by cloud point extraction prior to micellar electrokinetic chromatography.

PubMed

Stege, Patricia W; Sombra, Lorena L; Messina, Germán A; Martinez, Luis D; Silva, María F

2009-05-01

Many aromatic compounds can be found in the environment as a result of anthropogenic activities and some of them are highly toxic. The need to determine low concentrations of pollutants requires analytical methods with high sensitivity, selectivity, and resolution for application to soil, sediment, water, and other environmental samples. Complex sample preparation involving analyte isolation and enrichment is generally necessary before the final analysis. The present paper outlines a novel, simple, low-cost, and environmentally friendly method for the simultaneous determination of p-nitrophenol (PNP), p-aminophenol (PAP), and hydroquinone (HQ) by micellar electrokinetic capillary chromatography after preconcentration by cloud point extraction. Enrichment factors of 180 to 200 were achieved. The limits of detection of the analytes for the preconcentration of 50-ml sample volume were 0.10 microg L(-1) for PNP, 0.20 microg L(-1) for PAP, and 0.16 microg L(-1) for HQ. The optimized procedure was applied to the determination of phenolic pollutants in natural waters from San Luis, Argentina.

Microchip electrophoresis with electrochemical detection for the determination of analytes in the dopamine metabolic pathway

PubMed Central

Saylor, Rachel A.; Reid, Erin A.; Lunte, Susan M.

2016-01-01

A method for the separation and detection of analytes in the dopamine metabolic pathway was developed using microchip electrophoresis with electrochemical detection. The microchip consisted of a 5 cm PDMS separation channel in a simple-t configuration. Analytes in the dopamine metabolic pathway were separated using a background electrolyte composed of 15 mM phosphate at pH 7.4, 15 mM SDS, and 2.5 mM boric acid. Two different microchip substrates using different electrode materials were compared for the analysis: a PDMS/PDMS device with a carbon fiber electrode and a PDMS/glass hybrid device with a pyrolyzed photoresist film carbon electrode. While the PDMS/PDMS device generated high separation efficiencies and good resolution, more reproducible migration times were obtained with the PDMS/glass hybrid device, making it a better choice for biological applications. Lastly, the optimized method was used to monitor L-DOPA metabolism in a rat brain slice. PMID:25958983

Development of a point-kinetic verification scheme for nuclear reactor applications

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

Demazière, C., E-mail: demaz@chalmers.se; Dykin, V.; Jareteg, K.

In this paper, a new method that can be used for checking the proper implementation of time- or frequency-dependent neutron transport models and for verifying their ability to recover some basic reactor physics properties is proposed. This method makes use of the application of a stationary perturbation to the system at a given frequency and extraction of the point-kinetic component of the system response. Even for strongly heterogeneous systems for which an analytical solution does not exist, the point-kinetic component follows, as a function of frequency, a simple analytical form. The comparison between the extracted point-kinetic component and its expectedmore » analytical form provides an opportunity to verify and validate neutron transport solvers. The proposed method is tested on two diffusion-based codes, one working in the time domain and the other working in the frequency domain. As long as the applied perturbation has a non-zero reactivity effect, it is demonstrated that the method can be successfully applied to verify and validate time- or frequency-dependent neutron transport solvers. Although the method is demonstrated in the present paper in a diffusion theory framework, higher order neutron transport methods could be verified based on the same principles.« less

Use of LC-HRMS in full scan-XIC mode for multi-analyte urine drug testing - a step towards a 'black-box' solution?

PubMed

Stephanson, N N; Signell, P; Helander, A; Beck, O

2017-08-01

The influx of new psychoactive substances (NPS) has created a need for improved methods for drug testing in toxicology laboratories. The aim of this work was to design, validate and apply a multi-analyte liquid chromatography-high-resolution mass spectrometry (LC-HRMS) method for screening of 148 target analytes belonging to the NPS class, plant alkaloids and new psychoactive therapeutic drugs. The analytical method used a fivefold dilution of urine with nine deuterated internal standards and injection of 2 μl. The LC system involved a 2.0 μm 100 × 2.0 mm YMC-UltraHT Hydrosphere-C 18 column and gradient elution with a flow rate of 0.5 ml/min and a total analysis time of 6.0 min. Solvent A consisted of 10 mmol/l ammonium formate and 0.005% formic acid, pH 4.8, and Solvent B was methanol with 10 mmol/l ammonium formate and 0.005% formic acid. The HRMS (Q Exactive, Thermo Scientific) used a heated electrospray interface and was operated in positive mode with 70 000 resolution. The scan range was 100-650 Da, and data for extracted ion chromatograms used ± 10 ppm tolerance. Product ion monitoring was applied for confirmation analysis and for some selected analytes also for screening. Method validation demonstrated limited influence from urine matrix, linear response within the measuring range (typically 0.1-1.0 μg/ml) and acceptable imprecision in quantification (CV <15%). A few analytes were found to be unstable in urine upon storage. The method was successfully applied for routine drug testing of 17 936 unknown samples, of which 2715 (15%) contained 52 of the 148 analytes. It is concluded that the method design based on simple dilution of urine and using LC-HRMS in extracted ion chromatogram mode may offer an analytical system for urine drug testing that fulfils the requirement of a 'black box' solution and can replace immunochemical screening applied on autoanalyzers. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Development and Validation of a Fast Procedure to Analyze Amoxicillin in River Waters by Direct-Injection LC-MS/MS

ERIC Educational Resources Information Center

Homem, Vera; Alves, Arminda; Santos, Lu´cia

2014-01-01

A laboratory application with a strong component in analytical chemistry was designed for undergraduate students, in order to introduce a current problem in the environmental science field, the water contamination by antibiotics. Therefore, a simple and rapid method based on direct injection and high performance liquid chromatography-tandem mass…

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…

Multi-class method for determination of veterinary drug residues and other contaminants in infant formula by ultra performance liquid chromatography-tandem mass spectrometry.

PubMed

Zhan, Jia; Zhong, Ying-ying; Yu, Xue-jun; Peng, Jin-feng; Chen, Shubing; Yin, Ju-yi; Zhang, Jia-Jie; Zhu, Yan

2013-06-01

A rapid, simple and generic analytical method which was able to simultaneously determine 220 undesirable chemical residues in infant formula had been developed. The method comprised of extraction with acetonitrile, clean-up by low temperature and water precipitation, and analysis by ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS-MS) using multiple reaction monitoring (MRM) mode. Most fat materials in acetonitrile extract were eliminated by low temperature clean-up. The water precipitation, providing a necessary and supplementary cleanup, could avoid losses of hydrophobic analytes (avermectins, ionophores). Average recoveries for spiked infant formula were in the range from 57% to 147% with associated RSD values between 1% and 28%. For over 80% of the analytes, the recoveries were between 70% and 120% with RSD values in the range of 1-15%. The limits of quantification (LOQs) were from 0.01 to 5 μg/kg, which were usually sufficient to verify the compliance of products with legal tolerances. Application of this method in routine monitoring programs would imply a drastic reduction of both effort and time. Copyright © 2012 Elsevier Ltd. All rights reserved.

Development of a temperature gradient focusing method for in situ extraterrestrial biomarker analysis.

PubMed

Danger, Grégoire; Ross, David

2008-08-01

Scanning temperature gradient focusing (TGF) is a recently described technique for the simultaneous concentration and separation of charged analytes. It allows for high analyte peak capacities and low LODs in microcolumn electrophoretic separations. In this paper, we present the application of scanning TGF for chiral separations of amino acids. Using a mixture of seven carboxyfluorescein succinimidyl ester-labeled amino acids (including five chiral amino acids) which constitute the Mars7 standard, we show that scanning TGF is a very simple and efficient method for chiral separations. The modulation of TGF separation parameters (temperature window, pressure scan rate, temperature range, and chiral selector concentration) allows optimization of peak efficiencies and analyte resolutions. The use of hydroxypropyl-beta-CD at low concentration (1-5 mmol/L) as a chiral selector, with an appropriate pressure scan rate ( -0.25 Pa/s) and with a low temperature range (3-25 degrees C over 1 cm) provided high resolution between enantiomers (Rs >1.5 for each pair of enantiomers) using a short, 4 cm long capillary. With these new results, the scanning TGF method appears to be a viable method for in situ trace biomarker analysis for future missions to Mars or other solar system bodies.

Improving the treatment of coarse-grain electrostatics: CVCEL.

PubMed

Ceres, N; Lavery, R

2015-12-28

We propose an analytic approach for calculating the electrostatic energy of proteins or protein complexes in aqueous solution. This method, termed CVCEL (Circular Variance Continuum ELectrostatics), is fitted to Poisson calculations and is able to reproduce the corresponding energies for different choices of solute dielectric constant. CVCEL thus treats both solute charge interactions and charge self-energies, and it can also deal with salt solutions. Electrostatic damping notably depends on the degree of solvent exposure of the charges, quantified here in terms of circular variance, a measure that reflects the vectorial distribution of the neighbors around a given center. CVCEL energies can be calculated rapidly and have simple analytical derivatives. This approach avoids the need for calculating effective atomic volumes or Born radii. After describing how the method was developed, we present test results for coarse-grain proteins of different shapes and sizes, using different internal dielectric constants and different salt concentrations and also compare the results with those from simple distance-dependent models. We also show that the CVCEL approach can be used successfully to calculate the changes in electrostatic energy associated with changes in protein conformation or with protein-protein binding.

Experimental and CFD evidence of multiple solutions in a naturally ventilated building.

PubMed

Heiselberg, P; Li, Y; Andersen, A; Bjerre, M; Chen, Z

2004-02-01

This paper considers the existence of multiple solutions to natural ventilation of a simple one-zone building, driven by combined thermal and opposing wind forces. The present analysis is an extension of an earlier analytical study of natural ventilation in a fully mixed building, and includes the effect of thermal stratification. Both computational and experimental investigations were carried out in parallel with an analytical investigation. When flow is dominated by thermal buoyancy, it was found experimentally that there is thermal stratification. When the flow is wind-dominated, the room is fully mixed. Results from all three methods have shown that the hysteresis phenomena exist. Under certain conditions, two different stable steady-state solutions are found to exist by all three methods for the same set of parameters. As shown by both the computational fluid dynamics (CFD) and experimental results, one of the solutions can shift to another when there is a sufficient perturbation. These results have probably provided the strongest evidence so far for the conclusion that multiple states exist in natural ventilation of simple buildings. Different initial conditions in the CFD simulations led to different solutions, suggesting that caution must be taken when adopting the commonly used 'zero initialization'.

Simultaneous separation and determination of eleven nucleosides and bases in beer, herring sperm DNA and RNA soft capsule by high-performance liquid chromatography.

PubMed

Hou, Shengjie; Ding, Mingyu

2010-01-01

A simple and rapid high-performance liquid chromatography method was developed for the determination of eleven nucleosides and bases in beer, herring sperm DNA and RNA soft capsules. The separation was carried out on an Agilent extend-C(18) column with a simple gradient elution of acetonitrile and water as the mobile phase. Good linear relationships between the peak areas and the concentrations of the analytes were obtained. The detection limits for eleven analytes were in the range of 0.007-0.037 mg/L by UV detection at 260 nm. The relative standard deviations (RSDs) of the retention times were in the range of 0.78-1.85% for intra-day and 0.87-1.94% for inter-day, respectively. The RSDs of the peak areas were in the range of 2.71-3.22% for intra-day and 3.03-3.39% for inter-day, respectively. This method has been successfully applied to simultaneous determination of eleven nucleosides and bases in beer, herring sperm DNA and RNA soft capsules with the recoveries in the range of 93.7-108.3%.

Evaluation of available analytical techniques for monitoring the quality of space station potable water

NASA Technical Reports Server (NTRS)

Geer, Richard D.

1989-01-01

To assure the quality of potable water (PW) on the Space Station (SS) a number of chemical and physical tests must be conducted routinely. After reviewing the requirements for potable water, both direct and indirect analytical methods are evaluated that could make the required tests and improvements compatible with the Space Station operation. A variety of suggestions are made to improve the analytical techniques for SS operation. The most important recommendations are: (1) the silver/silver chloride electrode (SB) method of removing I sub 2/I (-) biocide from the water, since it may interfere with analytical procedures for PW and also its end uses; (2) the orbital reactor (OR) method of carrying out chemistry and electrochemistry in microgravity by using a disk shaped reactor on an orbital table to impart artificial G force to the contents, allowing solution mixing and separation of gases and liquids; and (3) a simple ultra low volume highly sensitive electrochemical/conductivity detector for use with a capillary zone electrophoresis apparatus. It is also recommended, since several different conductivity and resistance measurements are made during the analysis of PW, that the bipolar pulse measuring circuit be used in all these applications for maximum compatibility and redundancy of equipment.

Plate and butt-weld stresses beyond elastic limit, material and structural modeling

NASA Technical Reports Server (NTRS)

Verderaime, V.

1991-01-01

Ultimate safety factors of high performance structures depend on stress behavior beyond the elastic limit, a region not too well understood. An analytical modeling approach was developed to gain fundamental insights into inelastic responses of simple structural elements. Nonlinear material properties were expressed in engineering stresses and strains variables and combined with strength of material stress and strain equations similar to numerical piece-wise linear method. Integrations are continuous which allows for more detailed solutions. Included with interesting results are the classical combined axial tension and bending load model and the strain gauge conversion to stress beyond the elastic limit. Material discontinuity stress factors in butt-welds were derived. This is a working-type document with analytical methods and results applicable to all industries of high reliability structures.

Determination of diacylhydrazines-type insect growth regulator JS-118 residues in cabbage and soil by high performance liquid chromatography with DAD detection.

PubMed

Hu, J-Y; Deng, Z-B; Qin, D-M

2009-12-01

JS-118 is a diacylhydrazines-type insect growth regulator used extensively in China now. An analytical method for residues determination of JS-118 in cabbage and soil samples by high performance liquid chromatography with DAD detection was established and optimized. Primary secondary amine solid phase extraction cartridge was used for sample preparation. Mean recoveries for the analyte ranged from 96.6% to 107.0% with CV value less than 4.7%. The limit of quantification is 0.01 mg/kg. Direct confirmation of JS-118 residues in samples was realized by high performance liquid chromatography-mass spectrometry. The proposed method is simple, rapid and reliable to perform and could be utilized for monitoring of pesticides residues.

On the line-shape analysis of Compton profiles and its application to neutron scattering

NASA Astrophysics Data System (ADS)

Romanelli, G.; Krzystyniak, M.

2016-05-01

Analytical properties of Compton profiles are used in order to simplify the analysis of neutron Compton scattering experiments. In particular, the possibility to fit the difference of Compton profiles is discussed as a way to greatly decrease the level of complexity of the data treatment, making the analysis easier, faster and more robust. In the context of the novel method proposed, two mathematical models describing the shapes of differenced Compton profiles are discussed: the simple Gaussian approximation for harmonic and isotropic local potential, and an analytical Gauss-Hermite expansion for an anharmonic or anisotropic potential. The method is applied to data collected by VESUVIO spectrometer at ISIS neutron and muon pulsed source (UK) on Copper and Aluminium samples at ambient and low temperatures.

Analytical solution for the transient wave propagation of a buried cylindrical P-wave line source in a semi-infinite elastic medium with a fluid surface layer

NASA Astrophysics Data System (ADS)

Shan, Zhendong; Ling, Daosheng

2018-02-01

This article develops an analytical solution for the transient wave propagation of a cylindrical P-wave line source in a semi-infinite elastic solid with a fluid layer. The analytical solution is presented in a simple closed form in which each term represents a transient physical wave. The Scholte equation is derived, through which the Scholte wave velocity can be determined. The Scholte wave is the wave that propagates along the interface between the fluid and solid. To develop the analytical solution, the wave fields in the fluid and solid are defined, their analytical solutions in the Laplace domain are derived using the boundary and interface conditions, and the solutions are then decomposed into series form according to the power series expansion method. Each item of the series solution has a clear physical meaning and represents a transient wave path. Finally, by applying Cagniard's method and the convolution theorem, the analytical solutions are transformed into the time domain. Numerical examples are provided to illustrate some interesting features in the fluid layer, the interface and the semi-infinite solid. When the P-wave velocity in the fluid is higher than that in the solid, two head waves in the solid, one head wave in the fluid and a Scholte wave at the interface are observed for the cylindrical P-wave line source.

A New Unified Analysis of Estimate Errors by Model-Matching Phase-Estimation Methods for Sensorless Drive of Permanent-Magnet Synchronous Motors and New Trajectory-Oriented Vector Control, Part I

NASA Astrophysics Data System (ADS)

Shinnaka, Shinji; Sano, Kousuke

This paper presents a new unified analysis of estimate errors by model-matching phase-estimation methods such as rotor-flux state-observers, back EMF state-observers, and back EMF disturbance-observers, for sensorless drive of permanent-magnet synchronous motors. Analytical solutions about estimate errors, whose validity is confirmed by numerical experiments, are rich in universality and applicability. As an example of universality and applicability, a new trajectory-oriented vector control method is proposed, which can realize directly quasi-optimal strategy minimizing total losses with no additional computational loads by simply orienting one of vector-control coordinates to the associated quasi-optimal trajectory. The coordinate orientation rule, which is analytically derived, is surprisingly simple. Consequently the trajectory-oriented vector control method can be applied to a number of conventional vector control systems using one of the model-matching phase-estimation methods.

A simple method for the enrichment of bisphenols using boron nitride.

PubMed

Fischnaller, Martin; Bakry, Rania; Bonn, Günther K

2016-03-01

A simple solid-phase extraction method for the enrichment of 5 bisphenol derivatives using hexagonal boron nitride (BN) was developed. BN was applied to concentrate bisphenol derivatives in spiked water samples and the compounds were analyzed using HPLC coupled to fluorescence detection. The effect of pH and organic solvents on the extraction efficiency was investigated. An enrichment factor up to 100 was achieved without evaporation and reconstitution. The developed method was applied for the determination of bisphenol A migrated from some polycarbonate plastic products. Furthermore, bisphenol derivatives were analyzed in spiked and non-spiked canned food and beverages. None of the analyzed samples exceeded the migration limit set by the European Union of 0.6mg/kg food. The method showed good recovery rates ranging from 80% to 110%. Validation of the method was performed in terms of accuracy and precision. The applied method is robust, fast, efficient and easily adaptable to different analytical problems. Copyright © 2015 Elsevier Ltd. All rights reserved.

Air sampling with solid phase microextraction

NASA Astrophysics Data System (ADS)

Martos, Perry Anthony

There is an increasing need for simple yet accurate air sampling methods. The acceptance of new air sampling methods requires compatibility with conventional chromatographic equipment, and the new methods have to be environmentally friendly, simple to use, yet with equal, or better, detection limits, accuracy and precision than standard methods. Solid phase microextraction (SPME) satisfies the conditions for new air sampling methods. Analyte detection limits, accuracy and precision of analysis with SPME are typically better than with any conventional air sampling methods. Yet, air sampling with SPME requires no pumps, solvents, is re-usable, extremely simple to use, is completely compatible with current chromatographic equipment, and requires a small capital investment. The first SPME fiber coating used in this study was poly(dimethylsiloxane) (PDMS), a hydrophobic liquid film, to sample a large range of airborne hydrocarbons such as benzene and octane. Quantification without an external calibration procedure is possible with this coating. Well understood are the physical and chemical properties of this coating, which are quite similar to those of the siloxane stationary phase used in capillary columns. The log of analyte distribution coefficients for PDMS are linearly related to chromatographic retention indices and to the inverse of temperature. Therefore, the actual chromatogram from the analysis of the PDMS air sampler will yield the calibration parameters which are used to quantify unknown airborne analyte concentrations (ppb v to ppm v range). The second fiber coating used in this study was PDMS/divinyl benzene (PDMS/DVB) onto which o-(2,3,4,5,6- pentafluorobenzyl) hydroxylamine (PFBHA) was adsorbed for the on-fiber derivatization of gaseous formaldehyde (ppb v range), with and without external calibration. The oxime formed from the reaction can be detected with conventional gas chromatographic detectors. Typical grab sampling times were as small as 5 seconds. With 300 seconds sampling, the formaldehyde detection limit was 2.1 ppbv, better than any other 5 minute sampling device for formaldehyde. The first-order rate constant for product formation was used to quantify formaldehyde concentrations without a calibration curve. This spot sampler was used to sample the headspace of hair gel, particle board, plant material and coffee grounds for formaldehyde, and other carbonyl compounds, with extremely promising results. The SPME sampling devices were also used for time- weighted average sampling (30 minutes to 16 hours). Finally, the four new SPME air sampling methods were field tested with side-by-side comparisons to standard air sampling methods, showing a tremendous use of SPME as an air sampler.

A simple analytical method to estimate all exit parameters of a cross-flow air dehumidifier using liquid desiccant

PubMed Central

Bassuoni, M.M.

2013-01-01

The dehumidifier is a key component in liquid desiccant air-conditioning systems. Analytical solutions have more advantages than numerical solutions in studying the dehumidifier performance parameters. This paper presents the performance results of exit parameters from an analytical model of an adiabatic cross-flow liquid desiccant air dehumidifier. Calcium chloride is used as desiccant material in this investigation. A program performing the analytical solution is developed using the engineering equation solver software. Good accuracy has been found between analytical solution and reliable experimental results with a maximum deviation of +6.63% and −5.65% in the moisture removal rate. The method developed here can be used in the quick prediction of the dehumidifier performance. The exit parameters from the dehumidifier are evaluated under the effects of variables such as air temperature and humidity, desiccant temperature and concentration, and air to desiccant flow rates. The results show that hot humid air and desiccant concentration have the greatest impact on the performance of the dehumidifier. The moisture removal rate is decreased with increasing both air inlet temperature and desiccant temperature while increases with increasing air to solution mass ratio, inlet desiccant concentration, and inlet air humidity ratio. PMID:25685485

Simultaneous determination of water-soluble vitamins in selected food matrices by liquid chromatography/electrospray ionization tandem mass spectrometry.

PubMed

Gentili, Alessandra; Caretti, Fulvia; D'Ascenzo, Giuseppe; Marchese, Stefano; Perret, Daniela; Di Corcia, Daniele; Rocca, Lucia Mainero

2008-07-01

A rapid, simple and sensitive method based on liquid chromatography/tandem mass spectrometry (LC/MS/MS) with an electrospray ionization (ESI) source for the simultaneous analysis of fourteen water-soluble vitamins (B1, B2, two B3 vitamers, B5, five B6 vitamers, B8, B9, B12 and C) in various food matrices, i.e. maize flour, green and golden kiwi and tomato pulp, is presented here. Analytes were separated by ion-suppression reversed-phase liquid chromatography in less than 10 min and detected in positive ion mode. Sensitivity and specificity of this method allowed two important results to be achieved: (i) limits of detection of the analytes at ng g(-1) levels (except for vitamin C); (ii) development of a rapid sample treatment that minimizes analyte exposition to light, air and heat, eliminating any step of extract concentration. Analyte recovery depended on the type of matrix. In particular, recovery of the analytes in maize flour was > or =70%, with the exception of vitamin C, pyridoxal-5'-phosphate and vitamin B9 (ca 40%); with tomato pulp, recovery was > or =64%, except for vitamin C (41%); with kiwi, recovery was > or =73%, except for nicotinamide (ca. 30%).

Improved HPLC method for determination of four PPIs, omeprazole, pantoprazole, lansoprazole and rabeprazole in human plasma.

PubMed

Noubarani, Maryam; Keyhanfar, Fariborz; Motevalian, Manijeh; Mahmoudian, Masoud

2010-01-01

To develop a simple and rapid HPLC method for measuring of four proton-pump inhibitors (PPIs), omeprazole (OPZ), pantoprazole (PPZ), lansoprazole (LPZ) and rabeprazole (RPZ) concentrations in human plasma. Following a single step liquid-liquid extraction analytes along with an internal standard (IS) were separated using an isocratic mobile phase of phosphate buffer (10 mM)/acetonitrile (53/47, v/v adjusted pH to 7.3 with triethylamine) at flow rate of 1 mL/min on reverse phase TRACER EXCEL 120 ODS-A column at room temperature. Total analytical run time for selected PPIs was 10 min. The assays exhibited good linearity (r(2)>0.99) over the studied range of 20 to 2500 ng/mL for OPZ, 20 to 4000 ng/mL for PPZ, 20 to 3000 ng/mL for LPZ and 20 to 1500 ng/mL for RPZ. The recovery of method was equal or greater than 80% and lower limit of quantification (LLOQ) was 20 ng/mL for four PPIs. Coefficient of variation and error at all of the intra-day and inter-day assessment were less than 9.2% for all compounds. The results indicated that this method is a simple, rapid, precise and accurate assay for determination of four PPIs concentrations in human plasma. This validated method is sensitive and reproducible enough to be used in pharmacokinetic studies and also is time- and cost-benefit when selected PPIs are desired to be analyzed.

Simple quasi-analytical holonomic homogenization model for the non-linear analysis of in-plane loaded masonry panels: Part 1, meso-scale

NASA Astrophysics Data System (ADS)

Milani, G.; Bertolesi, E.

2017-07-01

A simple quasi analytical holonomic homogenization approach for the non-linear analysis of masonry walls in-plane loaded is presented. The elementary cell (REV) is discretized with 24 triangular elastic constant stress elements (bricks) and non-linear interfaces (mortar). A holonomic behavior with softening is assumed for mortar. It is shown how the mechanical problem in the unit cell is characterized by very few displacement variables and how homogenized stress-strain behavior can be evaluated semi-analytically.

Development of a selective and sensitive flotation method for determination of trace amounts of cobalt, nickel, copper and iron in environmental samples.

PubMed

Karimi, H; Ghaedi, M; Shokrollahi, A; Rajabi, H R; Soylak, M; Karami, B

2008-02-28

A simple, selective and rapid flotation method for the separation-preconcentration of trace amounts of cobalt, nickel, iron and copper ions using phenyl 2-pyridyl ketone oxime (PPKO) has been developed prior to their flame atomic absorption spectrometric determinations. The influence of pH, amount of PPKO as collector, type and amount of eluting agent, type and amount of surfactant as floating agent and ionic strength was evaluated on the recoveries of analytes. The influences of the concomitant ions on the recoveries of the analyte ions were also examined. The enrichment factor was 93. The detection limits based on 3 sigma for Cu, Ni, Co and Fe were 0.7, 0.7, 0.8, and 0.7 ng mL(-1), respectively. The method has been successfully applied for determination of trace amounts of ions in various real samples.

Detection of heavy metal by paper-based microfluidics.

PubMed

Lin, Yang; Gritsenko, Dmitry; Feng, Shaolong; Teh, Yi Chen; Lu, Xiaonan; Xu, Jie

2016-09-15

Heavy metal pollution has shown great threat to the environment and public health worldwide. Current methods for the detection of heavy metals require expensive instrumentation and laborious operation, which can only be accomplished in centralized laboratories. Various microfluidic paper-based analytical devices have been developed recently as simple, cheap and disposable alternatives to conventional ones for on-site detection of heavy metals. In this review, we first summarize current development of paper-based analytical devices and discuss the selection of paper substrates, methods of device fabrication, and relevant theories in these devices. We then compare and categorize recent reports on detection of heavy metals using paper-based microfluidic devices on the basis of various detection mechanisms, such as colorimetric, fluorescent, and electrochemical methods. To finalize, the future development and trend in this field are discussed. Copyright © 2016 Elsevier B.V. All rights reserved.

High Sensitivity Analysis of Nanoliter Volumes of Volatile and Nonvolatile Compounds using Matrix Assisted Ionization (MAI) Mass Spectrometry

NASA Astrophysics Data System (ADS)

Hoang, Khoa; Pophristic, Milan; Horan, Andrew J.; Johnston, Murray V.; McEwen, Charles N.

2016-10-01

First results are reported using a simple, fast, and reproducible matrix-assisted ionization (MAI) sample introduction method that provides substantial improvements relative to previously published MAI methods. The sensitivity of the new MAI methods, which requires no laser, high voltage, or nebulizing gas, is comparable to those reported for MALDI-TOF and n-ESI. High resolution full acquisition mass spectra having low chemical background are acquired from low nanoliters of solution using only a few femtomoles of analyte. The limit-of-detection for angiotensin II is less than 50 amol on an Orbitrap Exactive mass spectrometer. Analysis of peptides, including a bovine serum albumin digest, and drugs, including drugs in urine without a purification step, are reported using a 1 μL zero dead volume syringe in which only the analyte solution wetting the walls of the syringe needle is used in the analysis.

Temperature-controlled micro-TLC: a versatile green chemistry and fast analytical tool for separation and preliminary screening of steroids fraction from biological and environmental samples.

PubMed

Zarzycki, Paweł K; Slączka, Magdalena M; Zarzycka, Magdalena B; Bartoszuk, Małgorzata A; Włodarczyk, Elżbieta; Baran, Michał J

2011-11-01

This paper is a continuation of our previous research focusing on development of micro-TLC methodology under temperature-controlled conditions. The main goal of present paper is to demonstrate separation and detection capability of micro-TLC technique involving simple analytical protocols without multi-steps sample pre-purification. One of the advantages of planar chromatography over its column counterpart is that each TLC run can be performed using non-previously used stationary phase. Therefore, it is possible to fractionate or separate complex samples characterized by heavy biological matrix loading. In present studies components of interest, mainly steroids, were isolated from biological samples like fish bile using single pre-treatment steps involving direct organic liquid extraction and/or deproteinization by freeze-drying method. Low-molecular mass compounds with polarity ranging from estetrol to progesterone derived from the environmental samples (lake water, untreated and treated sewage waters) were concentrated using optimized solid-phase extraction (SPE). Specific bands patterns for samples derived from surface water of the Middle Pomerania in northern part of Poland can be easily observed on obtained micro-TLC chromatograms. This approach can be useful as simple and non-expensive complementary method for fast control and screening of treated sewage water discharged by the municipal wastewater treatment plants. Moreover, our experimental results show the potential of micro-TLC as an efficient tool for retention measurements of a wide range of steroids under reversed-phase (RP) chromatographic conditions. These data can be used for further optimalization of SPE or HPLC systems working under RP conditions. Furthermore, we also demonstrated that micro-TLC based analytical approach can be applied as an effective method for the internal standard (IS) substance search. Generally, described methodology can be applied for fast fractionation or screening of the whole range of target substances as well as chemo-taxonomic studies and fingerprinting of complex mixtures, which are present in biological or environmental samples. Due to low consumption of eluent (usually 0.3-1mL/run) mainly composed of water-alcohol binary mixtures, this method can be considered as environmentally friendly and green chemistry focused analytical tool, supplementary to analytical protocols involving column chromatography or planar micro-fluidic devices. Copyright © 2011 Elsevier Ltd. All rights reserved.

Extending the excluded volume for percolation threshold estimates in polydisperse systems: The binary disk system

DOE PAGES

Meeks, Kelsey; Pantoya, Michelle L.; Green, Micah; ...

2017-06-01

For dispersions containing a single type of particle, it has been observed that the onset of percolation coincides with a critical value of volume fraction. When the volume fraction is calculated based on excluded volume, this critical percolation threshold is nearly invariant to particle shape. The critical threshold has been calculated to high precision for simple geometries using Monte Carlo simulations, but this method is slow at best, and infeasible for complex geometries. This article explores an analytical approach to the prediction of percolation threshold in polydisperse mixtures. Specifically, this paper suggests an extension of the concept of excluded volume,more » and applies that extension to the 2D binary disk system. The simple analytical expression obtained is compared to Monte Carlo results from the literature. In conclusion, the result may be computed extremely rapidly and matches key parameters closely enough to be useful for composite material design.« less

Accurate Estimate of Some Propagation Characteristics for the First Higher Order Mode in Graded Index Fiber with Simple Analytic Chebyshev Method

NASA Astrophysics Data System (ADS)

Dutta, Ivy; Chowdhury, Anirban Roy; Kumbhakar, Dharmadas

2013-03-01

Using Chebyshev power series approach, accurate description for the first higher order (LP11) mode of graded index fibers having three different profile shape functions are presented in this paper and applied to predict their propagation characteristics. These characteristics include fractional power guided through the core, excitation efficiency and Petermann I and II spot sizes with their approximate analytic formulations. We have shown that where two and three Chebyshev points in LP11 mode approximation present fairly accurate results, the values based on our calculations involving four Chebyshev points match excellently with available exact numerical results.

Brownian systems with spatially inhomogeneous activity

NASA Astrophysics Data System (ADS)

Sharma, A.; Brader, J. M.

2017-09-01

We generalize the Green-Kubo approach, previously applied to bulk systems of spherically symmetric active particles [J. Chem. Phys. 145, 161101 (2016), 10.1063/1.4966153], to include spatially inhomogeneous activity. The method is applied to predict the spatial dependence of the average orientation per particle and the density. The average orientation is given by an integral over the self part of the Van Hove function and a simple Gaussian approximation to this quantity yields an accurate analytical expression. Taking this analytical result as input to a dynamic density functional theory approximates the spatial dependence of the density in good agreement with simulation data. All theoretical predictions are validated using Brownian dynamics simulations.

Analytic descriptions of cylindrical electromagnetic waves in a nonlinear medium

PubMed Central

Xiong, Hao; Si, Liu-Gang; Yang, Xiaoxue; Wu, Ying

2015-01-01

A simple but highly efficient approach for dealing with the problem of cylindrical electromagnetic waves propagation in a nonlinear medium is proposed based on an exact solution proposed recently. We derive an analytical explicit formula, which exhibiting rich interesting nonlinear effects, to describe the propagation of any amount of cylindrical electromagnetic waves in a nonlinear medium. The results obtained by using the present method are accurately concordant with the results of using traditional coupled-wave equations. As an example of application, we discuss how a third wave affects the sum- and difference-frequency generation of two waves propagation in the nonlinear medium. PMID:26073066

Investigating the causes of low detectability of pesticides in fruits and vegetables analysed by high-performance liquid chromatography - Time-of-flight.

PubMed

Muehlwald, S; Buchner, N; Kroh, L W

2018-03-23

Because of the high number of possible pesticide residues and their chemical complexity, it is necessary to develop methods which cover a broad range of pesticides. In this work, a qualitative multi-screening method for pesticides was developed by use of HPLC-ESI-Q-TOF. 110 pesticides were chosen for the creation of a personal compound database and library (PCDL). The MassHunter Qualitative Analysis software from Agilent Technologies was used to identify the analytes. The software parameter settings were optimised to produce a low number of false positive as well as false negative results. The method was validated for 78 selected pesticides. However, the validation criteria were not fulfilled for 45 analytes. Due to this result, investigations were started to elucidate reasons for the low detectability. It could be demonstrated that the three main causes of the signal suppression were the co-eluting matrix (matrix effect), the low sensitivity of the analyte in standard solution and the fragmentation of the analyte in the ion source (in-source collision-induced dissociation). In this paper different examples are discussed showing that the impact of these three causes is different for each analyte. For example, it is possible that an analyte with low signal intensity and an intense fragmentation in the ion source is detectable in a difficult matrix, whereas an analyte with a high sensitivity and a low fragmentation is not detectable in a simple matrix. Additionally, it could be shown that in-source fragments are a helpful tool for an unambiguous identification. Copyright © 2018 Elsevier B.V. All rights reserved.

A miniaturized capacitively coupled plasma microtorch optical emission spectrometer and a Rh coiled-filament as small-sized electrothermal vaporization device for simultaneous determination of volatile elements from liquid microsamples: spectral and analytical characterization.

PubMed

Frentiu, Tiberiu; Darvasi, Eugen; Butaciu, Sinziana; Ponta, Michaela; Petreus, Dorin; Mihaltan, Alin I; Frentiu, Maria

2014-11-01

A low power and low argon consumption (13.56 MHz, 15 W, 150 ml min(-1)) capacitively coupled plasma microtorch interfaced with a low-resolution microspectrometer and a small-sized electrothermal vaporization Rh coiled-filament as liquid microsample introduction device into the plasma was investigated for the simultaneous determination of several volatile elements of interest for environment. Constructive details, spectral and analytical characteristics, and optimum operating conditions of the laboratory equipment for the simultaneous determination of Ag, Cd, Cu, Pb and Zn requiring low vaporization power are provided. The method involves drying of 10 μl sample at 100°C, vaporization at 1500°C and emission measurement by capture of 20 successive spectral episodes each at an integration time of 500 ms. Experiments showed that emission of elements and plasma background were disturbed by the presence of complex matrix and hot Ar flow transporting the microsample into plasma. The emission spectrum of elements is simple, dominated by the resonance lines. The analytical system provided detection limits in the ng ml(-1) range: 0.5(Ag); 1.5(Cd); 5.6(Cu); 20(Pb) and 3(Zn) and absolute detection limits of the order of pg: 5(Ag); 15(Cd); 56(Cu); 200(Pb) and 30(Zn). It was demonstrated the utility and capability of the miniaturized analytical system in the simultaneous determination of elements in soil and water sediment using the standard addition method to compensate for the non-spectral effects of alkali and earth alkaline elements. The analysis of eight certified reference materials exhibited reliable results with recovery in the range of 95-108% and precision of 0.5-9.0% for the five examined elements. The proposed miniaturized analytical system is attractive due to the simple construction of the electrothermal vaporization device and microtorch, low costs associated to plasma generation, high analytical sensitivity and easy-to-run for simultaneous multielemental analysis of liquid microsamples. Copyright © 2014. Published by Elsevier B.V.

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.

Absorption into fluorescence. A method to sense biologically relevant gas molecules

NASA Astrophysics Data System (ADS)

Strianese, Maria; Varriale, Antonio; Staiano, Maria; Pellecchia, Claudio; D'Auria, Sabato

2011-01-01

In this work we present an innovative optical sensing methodology based on the use of biomolecules as molecular gating nano-systems. Here, as an example, we report on the detection ofanalytes related to climate change. In particular, we focused our attention on the detection ofnitric oxide (NO) and oxygen (O2). Our methodology builds on the possibility of modulating the excitation intensity of a fluorescent probe used as a transducer and a sensor molecule whose absorption is strongly affected by the binding of an analyte of interest used as a filter. The two simple conditions that have to be fulfilled for the method to work are: (a) the absorption spectrum of the sensor placed inside the cuvette, and acting as the recognition element for the analyte of interest, should strongly change upon the binding of the analyte and (b) the fluorescence dye transducer should exhibit an excitation band which overlaps with one or more absorption bands of the sensor. The absorption band of the sensor affected by the binding of the specific analyte should overlap with the excitation band of the transducer. The high sensitivity of fluorescence detection combined with the use of proteins as highly selective sensors makes this method a powerful basis for the development of a new generation of analytical assays. Proof-of-principle results showing that cytochrome c peroxidase (CcP) for NO detection and myoglobin (Mb) for O2 detection can be successfully used by exploiting our new methodology are reported. The proposed technology can be easily expanded to the determination of different target analytes.

Fast screening of analytes for chemical reactions by reactive low-temperature plasma ionization mass spectrometry.

PubMed

Zhang, Wei; Huang, Guangming

2015-11-15

Approaches for analyte screening have been used to aid in the fine-tuning of chemical reactions. Herein, we present a simple and straightforward analyte screening method for chemical reactions via reactive low-temperature plasma ionization mass spectrometry (reactive LTP-MS). Solution-phase reagents deposited on sample substrates were desorbed into the vapor phase by action of the LTP and by thermal desorption. Treated with LTP, both reagents reacted through a vapor phase ion/molecule reaction to generate the product. Finally, protonated reagents and products were identified by LTP-MS. Reaction products from imine formation reaction, Eschweiler-Clarke methylation and the Eberlin reaction were detected via reactive LTP-MS. Products from the imine formation reaction with reagents substituted with different functional groups (26 out of 28 trials) were successfully screened in a time of 30 s each. Besides, two short-lived reactive intermediates of Eschweiler-Clarke methylation were also detected. LTP in this study serves both as an ambient ionization source for analyte identification (including reagents, intermediates and products) and as a means to produce reagent ions to assist gas-phase ion/molecule reactions. The present reactive LTP-MS method enables fast screening for several analytes from several chemical reactions, which possesses good reagent compatibility and the potential to perform high-throughput analyte screening. In addition, with the detection of various reactive intermediates (intermediates I and II of Eschweiler-Clarke methylation), the present method would also contribute to revealing and elucidating reaction mechanisms. Copyright © 2015 John Wiley & Sons, Ltd.

A rapid method for the determination of some antihypertensive and antipyretic drugs by thermometric titrimetry.

PubMed

Abbasi, U M; Chand, F; Bhanger, M I; Memon, S A

1986-02-01

A simple and rapid method is described for the direct thermometric determination of milligram amounts of methyl dopa, propranolol hydrochloride, 1-phenyl-3-methylpyrazolone (MPP) and 2,3-dimethyl-1-phenylpyrazol-5-one (phenazone) in the presence of excipients. The compounds are reacted with N'-bromosuccinimide and the heat of reaction is used to determine the end-point of the titration. The time required is approximately 2 min, and the accuracy is analytically acceptable.

Gain Switching for a Detection System to Accommodate a Newly Developed MALDI-Based Quantification Method

NASA Astrophysics Data System (ADS)

Ahn, Sung Hee; Hyeon, Taeghwan; Kim, Myung Soo; Moon, Jeong Hee

2017-09-01

In matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF), matrix-derived ions are routinely deflected away to avoid problems with ion detection. This, however, limits the use of a quantification method that utilizes the analyte-to-matrix ion abundance ratio. In this work, we will show that it is possible to measure this ratio by a minor instrumental modification of a simple form of MALDI-TOF. This involves detector gain switching. [Figure not available: see fulltext.

Gauge-independent decoherence models for solids in external fields

NASA Astrophysics Data System (ADS)

Wismer, Michael S.; Yakovlev, Vladislav S.

2018-04-01

We demonstrate gauge-invariant modeling of an open system of electrons in a periodic potential interacting with an optical field. For this purpose, we adapt the covariant derivative to the case of mixed states and put forward a decoherence model that has simple analytical forms in the length and velocity gauges. We demonstrate our methods by calculating harmonic spectra in the strong-field regime and numerically verifying the equivalence of the deterministic master equation to the stochastic Monte Carlo wave-function method.

A ricin forensic profiling approach based on a complex set of biomarkers.

PubMed

Fredriksson, Sten-Åke; Wunschel, David S; Lindström, Susanne Wiklund; Nilsson, Calle; Wahl, Karen; Åstot, Crister

2018-08-15

A forensic method for the retrospective determination of preparation methods used for illicit ricin toxin production was developed. The method was based on a complex set of biomarkers, including carbohydrates, fatty acids, seed storage proteins, in combination with data on ricin and Ricinus communis agglutinin. The analyses were performed on samples prepared from four castor bean plant (R. communis) cultivars by four different sample preparation methods (PM1-PM4) ranging from simple disintegration of the castor beans to multi-step preparation methods including different protein precipitation methods. Comprehensive analytical data was collected by use of a range of analytical methods and robust orthogonal partial least squares-discriminant analysis- models (OPLS-DA) were constructed based on the calibration set. By the use of a decision tree and two OPLS-DA models, the sample preparation methods of test set samples were determined. The model statistics of the two models were good and a 100% rate of correct predictions of the test set was achieved. Copyright © 2018 Elsevier B.V. All rights reserved.

The dynamics of coastal models

USGS Publications Warehouse

Hearn, Clifford J.

2008-01-01

Coastal basins are defined as estuaries, lagoons, and embayments. This book deals with the science of coastal basins using simple models, many of which are presented in either analytical form or Microsoft Excel or MATLAB. The book introduces simple hydrodynamics and its applications, from the use of simple box and one-dimensional models to flow over coral reefs. The book also emphasizes models as a scientific tool in our understanding of coasts, and introduces the value of the most modern flexible mesh combined wave-current models. Examples from shallow basins around the world illustrate the wonders of the scientific method and the power of simple dynamics. This book is ideal for use as an advanced textbook for graduate students and as an introduction to the topic for researchers, especially those from other fields of science needing a basic understanding of the basic ideas of the dynamics of coastal basins.

Designing stellarator coils by a modified Newton method using FOCUS

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

Zhu, Caoxiang; Hudson, Stuart R.; Song, Yuntao

To find the optimal coils for stellarators, nonlinear optimization algorithms are applied in existing coil design codes. However, none of these codes have used the information from the second-order derivatives. In this paper, we present a modified Newton method in the recently developed code FOCUS. The Hessian matrix is calculated with analytically derived equations. Its inverse is approximated by a modified Cholesky factorization and applied in the iterative scheme of a classical Newton method. Using this method, FOCUS is able to recover the W7-X modular coils starting from a simple initial guess. Results demonstrate significant advantages.

Designing stellarator coils by a modified Newton method using FOCUS

NASA Astrophysics Data System (ADS)

Zhu, Caoxiang; Hudson, Stuart R.; Song, Yuntao; Wan, Yuanxi

2018-06-01

To find the optimal coils for stellarators, nonlinear optimization algorithms are applied in existing coil design codes. However, none of these codes have used the information from the second-order derivatives. In this paper, we present a modified Newton method in the recently developed code FOCUS. The Hessian matrix is calculated with analytically derived equations. Its inverse is approximated by a modified Cholesky factorization and applied in the iterative scheme of a classical Newton method. Using this method, FOCUS is able to recover the W7-X modular coils starting from a simple initial guess. Results demonstrate significant advantages.

Designing stellarator coils by a modified Newton method using FOCUS

DOE PAGES

Zhu, Caoxiang; Hudson, Stuart R.; Song, Yuntao; ...

2018-03-22

To find the optimal coils for stellarators, nonlinear optimization algorithms are applied in existing coil design codes. However, none of these codes have used the information from the second-order derivatives. In this paper, we present a modified Newton method in the recently developed code FOCUS. The Hessian matrix is calculated with analytically derived equations. Its inverse is approximated by a modified Cholesky factorization and applied in the iterative scheme of a classical Newton method. Using this method, FOCUS is able to recover the W7-X modular coils starting from a simple initial guess. Results demonstrate significant advantages.

Simultaneous quantitation of hydroxychloroquine and its metabolites in mouse blood and tissues using LC-ESI-MS/MS: An application for pharmacokinetic studies.

PubMed

Chhonker, Yashpal S; Sleightholm, Richard L; Li, Jing; Oupický, David; Murry, Daryl J

2018-01-01

Hydroxychloroquine (HCQ) has been shown to disrupt autophagy and sensitize cancer cells to radiation and chemotherapeutic agents. However, the optimal delivery method, dose, and tumor concentrations required for these effects are not known. This is in part due to a lack of sensitive and reproducible analytical methods for HCQ quantitation in small animals. As such, we developed and validated a selective and sensitive liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) method for simultaneous quantitation of hydroxychloroquine and its metabolites in mouse blood and tissues. The chromatographic separation and detection of analytes were achieved on a reversed phase Thermo Aquasil C 18 (50×4.6mm, 3μ) column, with gradient elution using 0.2% formic acid and 0.1% formic acid in methanol as mobile phase at a flow rate of 0.5mL/min. Simple protein precipitation was utilized for extraction of analytes from the desired matrix. Analytes were separated and quantitated using MS/MS with an electrospray ionization source in positive multiple reaction monitoring (MRM) mode. The MS/MS response was linear over the concentration range from 1 to 2000ng/mL for all analytes with a correlation coefficient (R 2 ) of 0.998 or better. The within- and between-day precision (relative standard deviation, % RSD) and accuracy were within the acceptable limits per FDA guidelines. The validated method was successfully applied to a preclinical pharmacokinetic mouse study involving low volume blood and tissue samples for hydroxychloroquine and metabolites. Copyright © 2017 Elsevier B.V. All rights reserved.

Compensating for Effects of Humidity on Electronic Noses

NASA Technical Reports Server (NTRS)

Homer, Margie; Ryan, Margaret A.; Manatt, Kenneth; Zhou, Hanying; Manfreda, Allison

2004-01-01

A method of compensating for the effects of humidity on the readouts of electronic noses has been devised and tested. The method is especially appropriate for use in environments in which humidity is not or cannot be controlled for example, in the vicinity of a chemical spill, which can be accompanied by large local changes in humidity. Heretofore, it has been common practice to treat water vapor as merely another analyte, the concentration of which is determined, along with that of the other analytes, in a computational process based on deconvolution. This practice works well, but leaves room for improvement: changes in humidity can give rise to large changes in electronic-nose responses. If corrections for humidity are not made, the large humidity-induced responses may swamp smaller responses associated with low concentrations of analytes. The present method offers an improvement. The underlying concept is simple: One augments an electronic nose with a separate humidity and a separate temperature sensor. The outputs of the humidity and temperature sensors are used to generate values that are subtracted from the readings of the other sensors in an electronic nose to correct for the temperature-dependent contributions of humidity to those readings. Hence, in principle, what remains after corrections are the contributions of the analytes only. Laboratory experiments on a first-generation electronic nose have shown that this method is effective and improves the success rate of identification of analyte/ water mixtures. Work on a second-generation device was in progress at the time of reporting the information for this article.

Current antiviral drugs and their analysis in biological materials - Part II: Antivirals against hepatitis and HIV viruses.

PubMed

Nováková, Lucie; Pavlík, Jakub; Chrenková, Lucia; Martinec, Ondřej; Červený, Lukáš

2018-01-05

This review is a Part II of the series aiming to provide comprehensive overview of currently used antiviral drugs and to show modern approaches to their analysis. While in the Part I antivirals against herpes viruses and antivirals against respiratory viruses were addressed, this part concerns antivirals against hepatitis viruses (B and C) and human immunodeficiency virus (HIV). Many novel antivirals against hepatitis C virus (HCV) and HIV have been introduced into the clinical practice over the last decade. The recent broadening portfolio of these groups of antivirals is reflected in increasing number of developed analytical methods required to meet the needs of clinical terrain. Part II summarizes the mechanisms of action of antivirals against hepatitis B virus (HBV), HCV, and HIV, their use in clinical practice, and analytical methods for individual classes. It also provides expert opinion on state of art in the field of bioanalysis of these drugs. Analytical methods reflect novelty of these chemical structures and use by far the most current approaches, such as simple and high-throughput sample preparation and fast separation, often by means of UHPLC-MS/MS. Proper method validation based on requirements of bioanalytical guidelines is an inherent part of the developed methods. Copyright © 2017 Elsevier B.V. All rights reserved.

On Establishing Big Data Wave Breakwaters with Analytics (Invited)

NASA Astrophysics Data System (ADS)

Riedel, M.

2013-12-01

The Research Data Alliance Big Data Analytics (RDA-BDA) Interest Group seeks to develop community based recommendations on feasible data analytics approaches to address scientific community needs of utilizing large quantities of data. RDA-BDA seeks to analyze different scientific domain applications and their potential use of various big data analytics techniques. A systematic classification of feasible combinations of analysis algorithms, analytical tools, data and resource characteristics and scientific queries will be covered in these recommendations. These combinations are complex since a wide variety of different data analysis algorithms exist (e.g. specific algorithms using GPUs of analyzing brain images) that need to work together with multiple analytical tools reaching from simple (iterative) map-reduce methods (e.g. with Apache Hadoop or Twister) to sophisticated higher level frameworks that leverage machine learning algorithms (e.g. Apache Mahout). These computational analysis techniques are often augmented with visual analytics techniques (e.g. computational steering on large-scale high performance computing platforms) to put the human judgement into the analysis loop or new approaches with databases that are designed to support new forms of unstructured or semi-structured data as opposed to the rather tradtional structural databases (e.g. relational databases). More recently, data analysis and underpinned analytics frameworks also have to consider energy footprints of underlying resources. To sum up, the aim of this talk is to provide pieces of information to understand big data analytics in the context of science and engineering using the aforementioned classification as the lighthouse and as the frame of reference for a systematic approach. This talk will provide insights about big data analytics methods in context of science within varios communities and offers different views of how approaches of correlation and causality offer complementary methods to advance in science and engineering today. The RDA Big Data Analytics Group seeks to understand what approaches are not only technically feasible, but also scientifically feasible. The lighthouse Goal of the RDA Big Data Analytics Group is a classification of clever combinations of various Technologies and scientific applications in order to provide clear recommendations to the scientific community what approaches are technicalla and scientifically feasible.

On-line focusing of flavin derivatives using Dynamic pH junction-sweeping capillary electrophoresis with laser-induced fluorescence detection.

PubMed

Britz-McKibbin, Philip; Otsuka, Koji; Terabe, Shigeru

2002-08-01

Simple yet effective methods to enhance concentration sensitivity is needed for capillary electrophoresis (CE) to become a practical method to analyze trace levels of analytes in real samples. In this report, the development of a novel on-line preconcentration technique combining dynamic pH junction and sweeping modes of focusing is applied to the sensitive and selective analysis of three flavin derivatives: riboflavin, flavin mononucleotide (FMN) and flavin adenine dinucleotide (FAD). Picomolar (pM) detectability of flavins by CE with laser-induced fluorescence (LIF) detection is demonstrated through effective focusing of large sample volumes (up to 22% capillary length) using a dual pH junction-sweeping focusing mode. This results in greater than a 1,200-fold improvement in sensitivity relative to conventional injection methods, giving a limit of detection (S/N = 3) of approximately 4.0 pM for FAD and FMN. Flavin focusing is examined in terms of analyte mobility dependence on buffer pH, borate complexation and SDS interaction. Dynamic pH junction-sweeping extends on-line focusing to both neutral (hydrophobic) and weakly acidic (hydrophilic) species and is considered useful in cases when either conventional sweeping or dynamic pH junction techniques used alone are less effective for certain classes of analytes. Enhanced focusing performance by this hyphenated method was demonstrated by greater than a 4-fold reduction in flavin bandwidth, as compared to either sweeping or dynamic pH junction, reflected by analyte detector bandwidths <0.20 cm. Novel on-line focusing strategies are required to improve sensitivity in CE, which may be applied toward more effective biochemical analysis methods for diverse types of analytes.

A Simple and Direct LC-MS Method for Determination of Genotoxic Impurity Hydroxylamine in Pharmaceutical compounds.

PubMed

Kumar, Thangarathinam; Ramya, Mohandass; Srinivasan, Viswanathan; Xavier, N

2017-08-01

Hydroxylamine is a known genotoxic impurity compound that needs to be controlled down to ppm level in pharmaceutical processes. It is difficult to detect using conventional analytical techniques due to its physio-chemical properties like lack of chromophore, low molecular weight, absence of carbon atom and high polarity. In addition to that, analysis of the pharmaceutical samples encounters considerable obstruction from matrix components that greatly overshadow the response of hydroxylamine. This study describes a simple, sensitive and direct Liquid Chromatographic-Mass Spectrometric method (LC-MS) for detection of hydroxylamine in pharmaceutical compounds. The LC-MS method was detected up to 0.008 ppm of hydroxylamine with S/N > 3.0 and quantified up to 0.025 ppm of hydroxylamine with S/N ratio >10.0. This validated method can be applied as a generic method to detect the hydroxylamine for pharmaceutical process control and drug substance release. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Rapid Equipping Force (REF) Analytical Support

DTIC Science & Technology

2007-06-01

document contains color images. 14. ABSTRACT 15. SUBJECT TERMS 16. SECURITY CLASSIFICATION OF: 17. LIMITATION OF ABSTRACT UU 18. NUMBER OF PAGES 44...interface and performs actions via Excel formulae, ActiveX controls, and VBA code. – Plan to provide both simple and complex weighting and scoring methods...Requirements Quad Chart. –Solution Set Information Worksheet: A spreadsheet containing detailed information concerning every potential solution considered

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...

Explicit Low-Thrust Guidance for Reference Orbit Targeting

NASA Technical Reports Server (NTRS)

Lam, Try; Udwadia, Firdaus E.

2013-01-01

The problem of a low-thrust spacecraft controlled to a reference orbit is addressed in this paper. A simple and explicit low-thrust guidance scheme with constrained thrust magnitude is developed by combining the fundamental equations of motion for constrained systems from analytical dynamics with a Lyapunov-based method. Examples are given for a spacecraft controlled to a reference trajectory in the circular restricted three body problem.

Median of patient results as a tool for assessment of analytical stability.

PubMed

Jørgensen, Lars Mønster; Hansen, Steen Ingemann; Petersen, Per Hyltoft; Sölétormos, György

2015-06-15

In spite of the well-established external quality assessment and proficiency testing surveys of analytical quality performance in laboratory medicine, a simple tool to monitor the long-term analytical stability as a supplement to the internal control procedures is often needed. Patient data from daily internal control schemes was used for monthly appraisal of the analytical stability. This was accomplished by using the monthly medians of patient results to disclose deviations from analytical stability, and by comparing divergences with the quality specifications for allowable analytical bias based on biological variation. Seventy five percent of the twenty analytes achieved on two COBASs INTEGRA 800 instruments performed in accordance with the optimum and with the desirable specifications for bias. Patient results applied in analytical quality performance control procedures are the most reliable sources of material as they represent the genuine substance of the measurements and therefore circumvent the problems associated with non-commutable materials in external assessment. Patient medians in the monthly monitoring of analytical stability in laboratory medicine are an inexpensive, simple and reliable tool to monitor the steadiness of the analytical practice. Copyright © 2015 Elsevier B.V. All rights reserved.

General method of solving the Schroedinger equation of atoms and molecules

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

Nakatsuji, Hiroshi

2005-12-15

We propose a general method of solving the Schroedinger equation of atoms and molecules. We first construct the wave function having the exact structure, using the ICI (iterative configuration or complement interaction) method and then optimize the variables involved by the variational principle. Based on the scaled Schroedinger equation and related principles, we can avoid the singularity problem of atoms and molecules and formulate a general method of calculating the exact wave functions in an analytical expansion form. We choose initial function {psi}{sub 0} and scaling g function, and then the ICI method automatically generates the wave function that hasmore » the exact structure by using the Hamiltonian of the system. The Hamiltonian contains all the information of the system. The free ICI method provides a flexible and variationally favorable procedure of constructing the exact wave function. We explain the computational procedure of the analytical ICI method routinely performed in our laboratory. Simple examples are given using hydrogen atom for the nuclear singularity case, the Hooke's atom for the electron singularity case, and the helium atom for both cases.« less

Development and validation of a reversed-phase fluorescence HPLC method for determination of bucillamine in human plasma using pre-column derivatization with monobromobimane.

PubMed

Lee, Kang Choon; Chun, Young Goo; Kim, Insoo; Shin, Beom Soo; Park, Eun-Seok; Yoo, Sun Dong; Youn, Yu Seok

2009-07-15

A simple, specific and sensitive derivatization with monobromobimane (mBrB) and the corresponding HPLC-fluorescence quantitation method for the analysis of bucillamine in human plasma was developed and validated. The analytical procedure involves a simple protein precipitation, pre-column fluorescence derivatization, and separation by reversed-phase high performance liquid chromatography (RP-HPLC). The calibration curve showed good linearity over a wide concentration range (50 ng/mL to 10 microg/mL) in human plasma (r(2)=0.9998). The lower limit of quantitation (LLOQ) was 50 ng/mL. The average precision and accuracy at LLOQ were within 6.3% and 107.6%, respectively. This method was successfully applied to a pharmacokinetic study after oral administration of a dose (300 mg) of bucillamine to 20 healthy Korean volunteers.

Effects of Simple Leaching of Crushed and Powdered Materials on High-precision Pb Isotope Analyses

NASA Astrophysics Data System (ADS)

Todd, E.; Stracke, A.

2013-12-01

We present new results of simple leaching experiments on the Pb isotope composition of USGS standard reference material powders and on ocean island basalt whole rock splits and powders. Rock samples were leached with 6N HCl in two steps, first hot and then in an ultrasonic bath, and washed with ultrapure H2O before conventional sample digestion and chromatographic purification of Pb. Pb isotope analyses were determined with Tl-doped MC-ICP-MS. Intra- and inter-session analytical reproducibility of repeated analyses of both synthetic Pb solutions and Pb from single digests of chemically processed natural samples were generally < 100 ppm (2 S.D.). The comparison of leached and unleached samples shows that leaching reliably removes variable amounts of different contaminants for different starting materials. For repeated digests of a single sample, the leached samples reproduce better than the unleached ones, showing that leaching effectively removes heterogeneously distributed extraneous Pb. However, the reproducibility of repeated digests of variably contaminated natural samples is up to an order of magnitude worse than the analytical reproducibility of ca. 100 ppm. More complex leaching methods (e.g., Nobre Silva et al., 2009) yield Pb isotope ratios within error of and with similar reproducibility to our method, showing that the simple leaching method is reliable. The remaining Pb isotope heterogeneity of natural samples, which typically exceeds 100 ppm, is thus attributed to inherent isotopic sample heterogeneity. Tl-doped MC-ICP-MS Pb ratio determination is therefore a sufficiently precise method for Pb isotope analyses in natural rocks. More precise Pb double- or triple-spike methods (e.g., Galer, 1999; Thirlwall, 2000), may exploit their full potential only in cases where natural isotopic sample heterogeneity is demonstrably negligible. References: Galer, S., 1999, Chem. Geol. 157, 255-274. Nobre Silva, et al. 2009, Geochemistry Geophysics Geosystems 10, Q08012. Thirlwall, M.F., 2000, Chem. Geol. 163, 299-322.

An evolutionary view of chromatography data systems used in bioanalysis.

PubMed

McDowall, R D

2010-02-01

This is a personal view of how chromatographic peak measurement and analyte quantification for bioanalysis have evolved from the manual methods of 1970 to the electronic working possible in 2010. In four decades there have been major changes from a simple chart recorder output (that was interpreted and quantified manually) through simple automation of peak measurement, calculation of standard curves and quality control values and instrument control to the networked chromatography data systems of today that are capable of interfacing with Laboratory Information Management Systems and other IT applications. The incorporation of electronic signatures to meet regulatory requirements offers a great opportunity for business improvement and electronic working.

Dressed tunneling approximation for electronic transport through molecular transistors

NASA Astrophysics Data System (ADS)

Seoane Souto, R.; Yeyati, A. Levy; Martín-Rodero, A.; Monreal, R. C.

2014-02-01

A theoretical approach for the nonequilibrium transport properties of nanoscale systems coupled to metallic electrodes with strong electron-phonon interactions is presented. It consists of a resummation of the dominant Feynman diagrams from the perturbative expansion in the coupling to the leads. We show that this scheme eliminates the main pathologies found in previous simple analytical approaches for the polaronic regime. The results for the spectral and transport properties are compared with those from several other approaches for a wide range of parameters. The method can be formulated in a simple way to obtain the full counting statistics. Results for the shot and thermal noise are presented.

Accounting for Uncertainty in Decision Analytic Models Using Rank Preserving Structural Failure Time Modeling: Application to Parametric Survival Models.

PubMed

Bennett, Iain; Paracha, Noman; Abrams, Keith; Ray, Joshua

2018-01-01

Rank Preserving Structural Failure Time models are one of the most commonly used statistical methods to adjust for treatment switching in oncology clinical trials. The method is often applied in a decision analytic model without appropriately accounting for additional uncertainty when determining the allocation of health care resources. The aim of the study is to describe novel approaches to adequately account for uncertainty when using a Rank Preserving Structural Failure Time model in a decision analytic model. Using two examples, we tested and compared the performance of the novel Test-based method with the resampling bootstrap method and with the conventional approach of no adjustment. In the first example, we simulated life expectancy using a simple decision analytic model based on a hypothetical oncology trial with treatment switching. In the second example, we applied the adjustment method on published data when no individual patient data were available. Mean estimates of overall and incremental life expectancy were similar across methods. However, the bootstrapped and test-based estimates consistently produced greater estimates of uncertainty compared with the estimate without any adjustment applied. Similar results were observed when using the test based approach on a published data showing that failing to adjust for uncertainty led to smaller confidence intervals. Both the bootstrapping and test-based approaches provide a solution to appropriately incorporate uncertainty, with the benefit that the latter can implemented by researchers in the absence of individual patient data. Copyright © 2018 International Society for Pharmacoeconomics and Outcomes Research (ISPOR). Published by Elsevier Inc. All rights reserved.

Flow injection spectrophotometric method for chloride determination in natural waters using Hg(SCN)(2) immobilized in epoxy resin.

PubMed

Silva, Claudineia R; Vieira, Heberth J; Canaes, Larissa S; Nóbrega, Joaquim A; Fatibello-Filho, Orlando

2005-02-28

A flow injection (FI) spectrophotometric method was proposed for the determination of chloride ion in natural waters. The determination of chloride was carried out by reaction with Hg(SCN)(2) immobilized in an epoxy resin bead in a solid-phase reactor (SPR) and the thiocyanate ions released were determined spectrophotometrically at 480nm after complexing reaction with Fe(III). The analytical curve for chloride was linear in the concentration range from 5.6 x 10(-5) to 2.2 x 10(-4)moll(-1) with a detection limit of 1.4 x 10(-5)moll(-1). The relative standard deviation (R.S.D.) was 2.2% for a solution containing 2.2 x 10(-4)moll(-1) (n = 10). The simple manifold allows a routine analytical frequency of 100 determinations per hour. The main advantage of the developed method is the 400% reduction of the Hg waste solution generated when compared to conventional methods for chloride determination based on the same spectrophotometric reaction.

A novel multiple headspace extraction gas chromatographic method for measuring the diffusion coefficient of methanol in water and in olive oil.

PubMed

Zhang, Chun-Yun; Chai, Xin-Sheng

2015-03-13

A novel method for the determination of the diffusion coefficient (D) of methanol in water and olive oil has been developed. Based on multiple headspace extraction gas chromatography (MHE-GC), the methanol released from the liquid sample of interest in a closed sample vial was determined in a stepwise fashion. A theoretical model was derived to establish the relationship between the diffusion coefficient and the GC signals from MHE-GC measurements. The results showed that the present method has an excellent precision (RSD<1%) in the linear fitting procedure and good accuracy for the diffusion coefficients of methanol in both water and olive oil, when compared with data reported in the literature. The present method is simple and practical and can be a valuable tool for the determination of the diffusion coefficient of volatile analyte(s) into food simulants from food and beverage packaging material, both in research studies and in actual applications. Copyright © 2015 Elsevier B.V. All rights reserved.

Methods to assess bioavailability of hydrophobic organic contaminants: Principles, operations, and limitations.

PubMed

Cui, Xinyi; Mayer, Philipp; Gan, Jay

2013-01-01

Many important environmental contaminants are hydrophobic organic contaminants (HOCs), which include PCBs, PAHs, PBDEs, DDT and other chlorinated insecticides, among others. Owing to their strong hydrophobicity, HOCs have their final destination in soil or sediment, where their ecotoxicological effects are closely regulated by sorption and thus bioavailability. The last two decades have seen a dramatic increase in research efforts in developing and applying partitioning based methods and biomimetic extractions for measuring HOC bioavailability. However, the many variations of both analytical methods and associated measurement endpoints are often a source of confusion for users. In this review, we distinguish the most commonly used analytical approaches based on their measurement objectives, and illustrate their practical operational steps, strengths and limitations using simple flowcharts. This review may serve as guidance for new users on the selection and use of established methods, and a reference for experienced investigators to identify potential topics for further research. Copyright © 2012 Elsevier Ltd. All rights reserved.

Improved Analytical Sensitivity of Lateral Flow Assay using Sponge for HBV Nucleic Acid Detection.

PubMed

Tang, Ruihua; Yang, Hui; Gong, Yan; Liu, Zhi; Li, XiuJun; Wen, Ting; Qu, ZhiGuo; Zhang, Sufeng; Mei, Qibing; Xu, Feng

2017-05-02

Hepatitis B virus (HBV) infection is a serious public health problem, which can be transmitted through various routes (e.g., blood donation) and cause hepatitis, liver cirrhosis and liver cancer. Hence, it is necessary to do diagnostic screening for high-risk HBV patients in these transmission routes. Nowadays, protein-based technologies have been used for HBV testing, which however involve the issues of large sample volume, antibody instability and poor specificity. Nucleic acid hybridization-based lateral flow assay (LFA) holds great potential to address these limitations due to its low-cost, rapid, and simple features, but the poor analytical sensitivity of LFA restricts its application. In this study, we developed a low-cost, simple and easy-to-use method to improve analytical sensitivity by integrating sponge shunt into LFA to decrease the fluid flow rate. The thickness, length and hydrophobicity of the sponge shunt were sequentially optimized, and achieved 10-fold signal enhancement in nucleic acid testing of HBV as compared to the unmodified LFA. The enhancement was further confirmed by using HBV clinical samples, where we achieved the detection limit of 10 3 copies/ml as compared to 10 4 copies/ml in unmodified LFA. The improved LFA holds great potential for diseases diagnostics, food safety control and environment monitoring at point-of-care.

Dislocation-induced stress in polycrystalline materials: mesoscopic simulations in the dislocation density formalism

NASA Astrophysics Data System (ADS)

Berkov, D. V.; Gorn, N. L.

2018-06-01

In this paper we present a simple and effective numerical method which allows a fast Fourier transformation-based evaluation of stress generated by dislocations with arbitrary directions and Burgers vectors if the (site-dependent) dislocation density is known. Our method allows the evaluation of the dislocation stress using a rectangular grid with shape-anisotropic discretization cells without employing higher multipole moments of the dislocation interaction coefficients. Using the proposed method, we first simulate the stress created by relatively simple non-homogeneous distributions of vertical edge and so-called ‘mixed’ dislocations in a disk-shaped sample, which is necessary to understand the dislocation behavior in more complicated systems. The main part of our research is devoted to the stress distribution in polycrystalline layers with the dislocation density rapidly varying with the distance to the layer bottom. Considering GaN as a typical example of such systems, we investigate dislocation-induced stress for edge and mixed dislocations, having random orientations of Burgers vectors among crystal grains. We show that the rapid decay of the dislocation density leads to many highly non-trivial features of the stress distributions in such layers and study in detail the dependence of these features on the average grain size. Finally we develop an analytical approach which allows us to predict the evolution of the stress variance with the grain size and compare analytical predictions with numerical results.

A simple, analytical, axisymmetric microburst model for downdraft estimation

NASA Technical Reports Server (NTRS)

Vicroy, Dan D.

1991-01-01

A simple analytical microburst model was developed for use in estimating vertical winds from horizontal wind measurements. It is an axisymmetric, steady state model that uses shaping functions to satisfy the mass continuity equation and simulate boundary layer effects. The model is defined through four model variables: the radius and altitude of the maximum horizontal wind, a shaping function variable, and a scale factor. The model closely agrees with a high fidelity analytical model and measured data, particularily in the radial direction and at lower altitudes. At higher altitudes, the model tends to overestimate the wind magnitude relative to the measured data.

Simple analytical model of a thermal diode

NASA Astrophysics Data System (ADS)

Kaushik, Saurabh; Kaushik, Sachin; Marathe, Rahul

2018-05-01

Recently there is a lot of attention given to manipulation of heat by constructing thermal devices such as thermal diodes, transistors and logic gates. Many of the models proposed have an asymmetry which leads to the desired effect. Presence of non-linear interactions among the particles is also essential. But, such models lack analytical understanding. Here we propose a simple, analytically solvable model of a thermal diode. Our model consists of classical spins in contact with multiple heat baths and constant external magnetic fields. Interestingly the magnetic field is the only parameter required to get the effect of heat rectification.

Exact results in the large system size limit for the dynamics of the chemical master equation, a one dimensional chain of equations.

PubMed

Martirosyan, A; Saakian, David B

2011-08-01

We apply the Hamilton-Jacobi equation (HJE) formalism to solve the dynamics of the chemical master equation (CME). We found exact analytical expressions (in large system-size limit) for the probability distribution, including explicit expression for the dynamics of variance of distribution. We also give the solution for some simple cases of the model with time-dependent rates. We derived the results of the Van Kampen method from the HJE approach using a special ansatz. Using the Van Kampen method, we give a system of ordinary differential equations (ODEs) to define the variance in a two-dimensional case. We performed numerics for the CME with stationary noise. We give analytical criteria for the disappearance of bistability in the case of stationary noise in one-dimensional CMEs.

One-step patterning of hollow microstructures in paper by laser cutting to create microfluidic analytical devices.

PubMed

Nie, Jinfang; Liang, Yuanzhi; Zhang, Yun; Le, Shangwang; Li, Dunnan; Zhang, Songbai

2013-01-21

In this paper, we report a simple, low-cost method for rapid, highly reproductive fabrication of paper-based microfluidics by using a commercially available, minitype CO(2) laser cutting/engraving machine. This method involves only one operation of cutting a piece of paper by laser according to a predesigned pattern. The hollow microstructures formed in the paper are used as the 'hydrophobic barriers' to define the hydrophilic flowing paths. A typical paper device on a 4 cm × 4 cm piece of paper can be fabricated within ∼7-20 s; it is ready for use once the cutting process is finished. The main fabrication parameters such as the applied current and cutting rate of the laser were optimized. The fabrication resolution and multiplexed analytical capability of the hollow microstructure-patterned paper were also characterized.

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

PubMed

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

2005-03-09

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

Analysis of glyoxal and related substances by means of high-performance liquid chromatography with refractive index detection.

PubMed

Zhang, Zhiyong; Zhao, Dishun; Xu, Baoyun

2013-01-01

A simple and rapid method is described for the analysis of glyoxal and related substances by high-performance liquid chromatography with a refractive index detector. The following chromatographic conditions were adopted: Aminex HPX-87H column, mobile phase consisting of 0.01N H2SO4, flow rate of 0.8 mL/min and temperature of 65°C. The application of the analytical technique developed in this study demonstrated that the aqueous reaction mixture produced by the oxidation of acetaldehyde with HNO3 was composed of glyoxal, acetaldehyde, acetic acid, formic acid, glyoxylic acid, oxalic acid, butanedione and glycolic acid. The method was validated by evaluating analytical parameters such as linearity, limits of detection and quantification, precision, recovery and robustness. The proposed methodology was successfully applied to the production of glyoxal.

Foam separation of Rhodamine-G and Evans Blue using a simple separatory bottle system.

PubMed

Dasarathy, Dhweeja; Ito, Yoichiro

2017-09-29

A simple separatory glass bottle was used to improve separation effectiveness and cost efficiency while simultaneously creating a simpler system for separating biological compounds. Additionally, it was important to develop a scalable separation method so this would be applicable to both analytical and preparative separations. Compared to conventional foam separation methods, this method easily forms stable dry foam which ensures high purity of yielded fractions. A negatively charged surfactant, sodium dodecyl sulfate (SDS), was used as the ligand to carry a positively charged Rhodamine-G, leaving a negatively charged Evans Blue in the bottle. The performance of the separatory bottle was tested for separating Rhodamine-G from Evans Blue with sample sizes ranged from 1 to 12mg in preparative separations and 1-20μg in analytical separations under optimum conditions. These conditions including N 2 gas pressure, spinning speed of contents with a magnetic stirrer, concentration of the ligand, volume of the solvent, and concentration of the sample, were all modified and optimized. Based on the calculations at their peak absorbances, Rhodamine-G and Evans Blue were efficiently separated in times ranging from 1h to 3h, depending on sample volume. Optimal conditions were found to be 60psi N 2 pressure and 2mM SDS for the affinity ligand. This novel separation method will allow for rapid separation of biological compounds while simultaneously being scalable and cost effective. Published by Elsevier B.V.

Development and validation of a highly sensitive LC-MS/MS method for the determination of dexamethasone in nude mice plasma and its application to a pharmacokinetic study.

PubMed

Yuan, Yin; Zhou, Xuan; Li, Jian; Ye, Suofu; Ji, Xiwei; Li, Liang; Zhou, Tianyan; Lu, Wei

2015-04-01

In the current study, a simple, sensitive and rapid analytical method for the determination of dexamethasone was developed and applied to a pharmacokinetic study in nude mice. Using testosterone as an internal standard, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) approach after one-step precipitation with acetonitrile was validated and used to determine the concentrations of dexamethasone in nude mice plasma. The method utilized a simple isocratic reverse phase separation over a Dionex C18 column with a mobile phase composed of acetonitrile-water (40:60, v/v). The analyte was detected by a triple quadrupole tandem mass spectrometer via electrospray and multiple reaction monitoring was employed to select both dexamethasone at m/z 393.0/147.1 and testosterone at m/z 289.5/97.3 in the positive ion mode. The calibration curves were linear (r >0.99) ranging from 2.5 to 500 ng/mL with a lower limit of quantitation of 2.5 ng/mL. The relative standard deviation ranged from 1.69 to 9.22% while the relative error ranged from -1.92 to -8.46%. This method was successfully applied to a preclinical pharmacokinetic study of dexamethasone and its pharmacokinetics was characterized by a two-compartment model with first-order absorption in female nude mice. Copyright © 2014 John Wiley & Sons, Ltd.

Advances in aptamer screening and small molecule aptasensors.

PubMed

Kim, Yeon Seok; Gu, Man Bock

2014-01-01

It has been 20 years since aptamer and SELEX (systematic evolution of ligands by exponential enrichment) were described independently by Andrew Ellington and Larry Gold. Based on the great advantages of aptamers, there have been numerous isolated aptamers for various targets that have actively been applied as therapeutic and analytical tools. Over 2,000 papers related to aptamers or SELEX have been published, attesting to their wide usefulness and the applicability of aptamers. SELEX methods have been modified or re-created over the years to enable aptamer isolation with higher affinity and selectivity in more labor- and time-efficient manners, including automation. Initially, most of the studies about aptamers have focused on the protein targets, which have physiological functions in the body, and their applications as therapeutic agents or receptors for diagnostics. However, aptamers for small molecules such as organic or inorganic compounds, drugs, antibiotics, or metabolites have not been studied sufficiently, despite the ever-increasing need for rapid and simple analytical methods for various chemical targets in the fields of medical diagnostics, environmental monitoring, food safety, and national defense against targets including chemical warfare. This review focuses on not only recent advances in aptamer screening methods but also its analytical application for small molecules.

Green analytical determination of emerging pollutants in environmental waters using excitation-emission photoinduced fluorescence data and multivariate calibration.

PubMed

Hurtado-Sánchez, María Del Carmen; Lozano, Valeria A; Rodríguez-Cáceres, María Isabel; Durán-Merás, Isabel; Escandar, Graciela M

2015-03-01

An eco-friendly strategy for the simultaneous quantification of three emerging pharmaceutical contaminants is presented. The proposed analytical method, which involves photochemically induced fluorescence matrix data combined with second-order chemometric analysis, was used for the determination of carbamazepine, ofloxacin and piroxicam in water samples of different complexity without the need of chromatographic separation. Excitation-emission photoinduced fluorescence matrices were obtained after UV irradiation, and processed with second-order algorithms. Only one of the tested algorithms was able to overcome the strong spectral overlapping among the studied pollutants and allowed their successful quantitation in very interferent media. The method sensitivity in superficial and underground water samples was enhanced by a simple solid-phase extraction with C18 membranes, which was successful for the extraction/preconcentration of the pollutants at trace levels. Detection limits in preconcentrated (1:125) real water samples ranged from 0.04 to 0.3 ng mL(-1). Relative prediction errors around 10% were achieved. The proposed strategy is significantly simpler and greener than liquid chromatography-mass spectrometry methods, without compromising the analytical quality of the results. Copyright © 2014 Elsevier B.V. All rights reserved.

[Scientific Evaluation of Crude Drugs and Kampo Medicines Using the Eastern Blotting Method and Its Application to Biological Metabolic Studies].

PubMed

Morinaga, Osamu

2018-01-01

　The scientific evaluation of crude drugs and kampo medicines (KMs) was demonstrated using the eastern blotting method with monoclonal antibodies (MAbs) against bioactive natural compounds. Scutellariae radix is one of the most important crude drugs used in KMs. Part of its pharmaceutical properties is due to the flavone glycoside baicalin (BI). A quantitative analysis method based on eastern blotting was developed for BI using an anti-BI MAb. A rapid, simple, sensitive, specific analytical system was subsequently established for BI with the eastern blotting technique using dot-blot and chemiluminescent methods. This system was useful as a high-throughput analytical method for the determination of BI in KMs as well as HPLC and enzyme-linked immunosorbent assay systems. Furthermore, an eastern blotting method was applied to the biological metabolic study of glycyrrhizic acid (GL), the major active constituent of licorice, for investigation of metabolites of GL such as 3-monoglucuronyl-glycyrrhetinic acid (3MGA) because licorice causes pseudoaldosteronism as a side effect. This approach may make it possible to determine the pathogenic agents of licorice-induced pseudoaldosteronism.

Simultaneous determination of fumonisins B1 and B2 in different types of maize by matrix solid phase dispersion and HPLC-MS/MS.

PubMed

de Oliveira, Gabriel Barros; de Castro Gomes Vieira, Carolyne Menezes; Orlando, Ricardo Mathias; Faria, Adriana Ferreira

2017-10-15

This work involved the optimization and validation of a method, according to Directive 2002/657/EC and the Analytical Quality Assurance Manual of Ministério da Agricultura, Pecuária e Abastecimento, Brazil, for simultaneous extraction and determination of fumonisins B1 and B2 in maize. The extraction procedure was based on a matrix solid phase dispersion approach, the optimization of which employed a sequence of different factorial designs. A liquid chromatography-tandem mass spectrometry method was developed for determining these analytes using the selected reaction monitoring mode. The optimized method employed only 1g of silica gel for dispersion and elution with 70% ammonium formate aqueous buffer (50mmolL -1 , pH 9), representing a simple, cheap and chemically friendly sample preparation method. Trueness (recoveries: 86-106%), precision (RSD ≤19%), decision limits, detection capabilities and measurement uncertainties were calculated for the validated method. The method scope was expanded to popcorn kernels, white maize kernels and yellow maize grits. Copyright © 2017 Elsevier Ltd. All rights reserved.

A green analytical method using ultrasound in sample preparation for the flow injection determination of iron, manganese, and zinc in soluble solid samples by flame atomic absorption spectrometry.

PubMed

Yebra, M Carmen

2012-01-01

A simple and rapid analytical method was developed for the determination of iron, manganese, and zinc in soluble solid samples. The method is based on continuous ultrasonic water dissolution of the sample (5-30 mg) at room temperature followed by flow injection flame atomic absorption spectrometric determination. A good precision of the whole procedure (1.2-4.6%) and a sample throughput of ca. 25 samples h(-1) were obtained. The proposed green analytical method has been successfully applied for the determination of iron, manganese, and zinc in soluble solid food samples (soluble cocoa and soluble coffee) and pharmaceutical preparations (multivitamin tablets). The ranges of concentrations found were 21.4-25.61 μg g(-1) for iron, 5.74-18.30 μg g(-1) for manganese, and 33.27-57.90 μg g(-1) for zinc in soluble solid food samples and 3.75-9.90 μg g(-1) for iron, 0.47-5.05 μg g(-1) for manganese, and 1.55-15.12 μg g(-1) for zinc in multivitamin tablets. The accuracy of the proposed method was established by a comparison with the conventional wet acid digestion method using a paired t-test, indicating the absence of systematic errors.

Fast and Simple Discriminative Analysis of Anthocyanins-Containing Berries Using LC/MS Spectral Data.

PubMed

Yang, Heejung; Kim, Hyun Woo; Kwon, Yong Soo; Kim, Ho Kyong; Sung, Sang Hyun

2017-09-01

Anthocyanins are potent antioxidant agents that protect against many degenerative diseases; however, they are unstable because they are vulnerable to external stimuli including temperature, pH and light. This vulnerability hinders the quality control of anthocyanin-containing berries using classical high-performance liquid chromatography (HPLC) analytical methodologies based on UV or MS chromatograms. To develop an alternative approach for the quality assessment and discrimination of anthocyanin-containing berries, we used MS spectral data acquired in a short analytical time rather than UV or MS chromatograms. Mixtures of anthocyanins were separated from other components in a short gradient time (5 min) due to their higher polarity, and the representative MS spectrum was acquired from the MS chromatogram corresponding to the mixture of anthocyanins. The chemometric data from the representative MS spectra contained reliable information for the identification and relative quantification of anthocyanins in berries with good precision and accuracy. This fast and simple methodology, which consists of a simple sample preparation method and short gradient analysis, could be applied to reliably discriminate the species and geographical origins of different anthocyanin-containing berries. These features make the technique useful for the food industry. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Analytical estimation on divergence and flutter vibrations of symmetrical three-phase induction stator via field-synchronous coordinates

NASA Astrophysics Data System (ADS)

Xia, Ying; Wang, Shiyu; Sun, Wenjia; Xiu, Jie

2017-01-01

The electromagnetically induced parametric vibration of the symmetrical three-phase induction stator is examined. While it can be analyzed by an approximate analytical or numerical method, more accurate and simple analytical method is desirable. This work proposes a new method based on the field-synchronous coordinates. A mechanical-electromagnetic coupling model is developed under this frame such that a time-invariant governing equation with gyroscopic term can be developed. With the general vibration theory, the eigenvalue is formulated; the transition curves between the stable and unstable regions, and response are all determined as closed-form expressions of basic mechanical-electromagnetic parameters. The dependence of these parameters on the instability behaviors is demonstrated. The results imply that the divergence and flutter instabilities can occur even for symmetrical motors with balanced, constant amplitude and sinusoidal voltage. To verify the analytical predictions, this work also builds up a time-variant model of the same system under the conventional inertial frame. The Floquét theory is employed to predict the parametric instability and the numerical integration is used to obtain the parametric response. The parametric instability and response are both well compared against those under the field-synchronous coordinates. The proposed field-synchronous coordinates allows a quick estimation on the electromagnetically induced vibration. The convenience offered by the body-fixed coordinates is discussed across various fields.

Dual-domain mass-transfer parameters from electrical hysteresis: theory and analytical approach applied to laboratory, synthetic streambed, and groundwater experiments

USGS Publications Warehouse

Briggs, Martin A.; Day-Lewis, Frederick D.; Ong, John B.; Harvey, Judson W.; Lane, John W.

2014-01-01

Models of dual-domain mass transfer (DDMT) are used to explain anomalous aquifer transport behavior such as the slow release of contamination and solute tracer tailing. Traditional tracer experiments to characterize DDMT are performed at the flow path scale (meters), which inherently incorporates heterogeneous exchange processes; hence, estimated “effective” parameters are sensitive to experimental design (i.e., duration and injection velocity). Recently, electrical geophysical methods have been used to aid in the inference of DDMT parameters because, unlike traditional fluid sampling, electrical methods can directly sense less-mobile solute dynamics and can target specific points along subsurface flow paths. Here we propose an analytical framework for graphical parameter inference based on a simple petrophysical model explaining the hysteretic relation between measurements of bulk and fluid conductivity arising in the presence of DDMT at the local scale. Analysis is graphical and involves visual inspection of hysteresis patterns to (1) determine the size of paired mobile and less-mobile porosities and (2) identify the exchange rate coefficient through simple curve fitting. We demonstrate the approach using laboratory column experimental data, synthetic streambed experimental data, and field tracer-test data. Results from the analytical approach compare favorably with results from calibration of numerical models and also independent measurements of mobile and less-mobile porosity. We show that localized electrical hysteresis patterns resulting from diffusive exchange are independent of injection velocity, indicating that repeatable parameters can be extracted under varied experimental designs, and these parameters represent the true intrinsic properties of specific volumes of porous media of aquifers and hyporheic zones.

Dual-domain mass-transfer parameters from electrical hysteresis: Theory and analytical approach applied to laboratory, synthetic streambed, and groundwater experiments

NASA Astrophysics Data System (ADS)

Briggs, Martin A.; Day-Lewis, Frederick D.; Ong, John B.; Harvey, Judson W.; Lane, John W.

2014-10-01

Models of dual-domain mass transfer (DDMT) are used to explain anomalous aquifer transport behavior such as the slow release of contamination and solute tracer tailing. Traditional tracer experiments to characterize DDMT are performed at the flow path scale (meters), which inherently incorporates heterogeneous exchange processes; hence, estimated "effective" parameters are sensitive to experimental design (i.e., duration and injection velocity). Recently, electrical geophysical methods have been used to aid in the inference of DDMT parameters because, unlike traditional fluid sampling, electrical methods can directly sense less-mobile solute dynamics and can target specific points along subsurface flow paths. Here we propose an analytical framework for graphical parameter inference based on a simple petrophysical model explaining the hysteretic relation between measurements of bulk and fluid conductivity arising in the presence of DDMT at the local scale. Analysis is graphical and involves visual inspection of hysteresis patterns to (1) determine the size of paired mobile and less-mobile porosities and (2) identify the exchange rate coefficient through simple curve fitting. We demonstrate the approach using laboratory column experimental data, synthetic streambed experimental data, and field tracer-test data. Results from the analytical approach compare favorably with results from calibration of numerical models and also independent measurements of mobile and less-mobile porosity. We show that localized electrical hysteresis patterns resulting from diffusive exchange are independent of injection velocity, indicating that repeatable parameters can be extracted under varied experimental designs, and these parameters represent the true intrinsic properties of specific volumes of porous media of aquifers and hyporheic zones.

Simple design of slanted grating with simplified modal method.

PubMed

Li, Shubin; Zhou, Changhe; Cao, Hongchao; Wu, Jun

2014-02-15

A simplified modal method (SMM) is presented that offers a clear physical image for subwavelength slanted grating. The diffraction characteristic of the slanted grating under Littrow configuration is revealed by the SMM as an equivalent rectangular grating, which is in good agreement with rigorous coupled-wave analysis. Based on the equivalence, we obtained an effective analytic solution for simplifying the design and optimization of a slanted grating. It offers a new approach for design of the slanted grating, e.g., a 1×2 beam splitter can be easily designed. This method should be helpful for designing various new slanted grating devices.

Optimization of magnet end-winding geometry

NASA Astrophysics Data System (ADS)

Reusch, Michael F.; Weissenburger, Donald W.; Nearing, James C.

1994-03-01

A simple, almost entirely analytic, method for the optimization of stress-reduced magnet-end winding paths for ribbon-like superconducting cable is presented. This technique is based on characterization of these paths as developable surfaces, i.e., surfaces whose intrinsic geometry is flat. The method is applicable to winding mandrels of arbitrary geometry. Computational searches for optimal winding paths are easily implemented via the technique. Its application to the end configuration of cylindrical Superconducting Super Collider (SSC)-type magnets is discussed. The method may be useful for other engineering problems involving the placement of thin sheets of material.

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.

Liquid chromatography-tandem mass spectrometry analysis of perfluorooctane sulfonate and perfluorooctanoic Acid in fish fillet samples.

PubMed

Paiano, Viviana; Fattore, Elena; Carrà, Andrea; Generoso, Caterina; Fanelli, Roberto; Bagnati, Renzo

2012-01-01

Perfluorooctane sulfonate (PFOS) and perfluorooctanoic (PFOA) acid are persistent contaminants which can be found in environmental and biological samples. A new and fast analytical method is described here for the analysis of these compounds in the edible part of fish samples. The method uses a simple liquid extraction by sonication, followed by a direct determination using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The linearity of the instrumental response was good, with average regression coefficients of 0.9971 and 0.9979 for PFOS and PFOA, respectively, and the coefficients of variation (CV) of the method ranged from 8% to 20%. Limits of detection (LOD) were 0.04 ng/g for both the analytes and recoveries were 90% for PFOS and 76% for PFOA. The method was applied to samples of homogenized fillets of wild and farmed fish from the Mediterranean Sea. Most of the samples showed little or no contamination by perfluorooctane sulfonate and perfluorooctanoic acid, and the highest concentrations detected among the fish species analyzed were, respectively, 5.96 ng/g and 1.89 ng/g. The developed analytical methodology can be used as a tool to monitor and to assess human exposure to perfluorinated compounds through sea food consumption.

Validated UHPLC-MS/MS assay for quantitative determination of etoposide, gemcitabine, vinorelbine and their metabolites in patients with lung cancer.

PubMed

Gong, Xiaobin; Yang, Le; Zhang, Feng; Liang, Youtian; Gao, Shouhong; Liu, Ke; Chen, Wansheng

2017-11-01

A fully valid UHPLC-MS/MS method was developed for the determination of etoposide, gemcitabine, vinorelbine and their metabolites (etoposide catechol, 2',2'-difluorodeoxyuridine and 4-O-deacetylvinorelbine) in human plasma. The multiple reaction monitoring mode was performed with an electrospray ionization interface operating in both the positive and negative ion modes per compound. The method required only 100 μL plasma with a one-step simple de-proteinization procedure, and a short run time of 7.5 min per sample. A Waters ACQUITY UPLC HSS T3 column (2.1 × 100 mm, 1.8 μm) provided chromatographic separation of analytes using a binary mobile phase gradient (A, 0.1% formic acid in acetonitrile, v/v; B, 0.1% formic acid in water, v/v). Linear coefficients of correlation were >0.995 for all analytes. The relative deviation of this method was <10% for intra- and inter-day assays and the accuracy ranged between 86.35% and 113.44%. The mean extraction recovery and matrix effect of all the analytes were 62.07-105.46% and 93.67-105.87%, respectively. This method was successfully applied to clinical samples from patients with lung cancer. Copyright © 2017 John Wiley & Sons, Ltd.

HPLC-ESI-MS/MS validated method for simultaneous quantification of zopiclone and its metabolites, N-desmethyl zopiclone and zopiclone-N-oxide in human plasma.

PubMed

Mistri, Hiren N; Jangid, Arvind G; Pudage, Ashutosh; Shrivastav, Pranav

2008-03-15

A simple, selective and sensitive isocratic HPLC method with triple quadrupole mass spectrometry detection has been developed and validated for simultaneous quantification of zopiclone and its metabolites in human plasma. The analytes were extracted using solid phase extraction, separated on Symmetry shield RP8 column (150 mm x 4.6 mm i.d., 3.5 microm particle size) and detected by tandem mass spectrometry with a turbo ion spray interface. Metaxalone was used as an internal standard. The method had a chromatographic run time of 4.5 min and linear calibration curves over the concentration range of 0.5-150 ng/mL for both zopiclone and N-desmethyl zopiclone and 1-150 ng/mL for zopiclone-N-oxide. The intra-batch and inter-batch accuracy and precision evaluated at lower limit of quantification and quality control levels were within 89.5-109.1% and 3.0-14.7%, respectively, for all the analytes. The recoveries calculated for the analytes and internal standard were > or = 90% from spiked plasma samples. The validated method was successfully employed for a comparative bioavailability study after oral administration of 7.5 mg zopiclone (test and reference) to 16 healthy volunteers under fasted condition.

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.

Backscattering and absorption coefficients for electrons: Solutions of invariant embedding transport equations using a method of convergence

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

Figueroa, C.; Brizuela, H.; Heluani, S. P.

2014-05-21

The backscattering coefficient is a magnitude whose measurement is fundamental for the characterization of materials with techniques that make use of particle beams and particularly when performing microanalysis. In this work, we report the results of an analytic method to calculate the backscattering and absorption coefficients of electrons in similar conditions to those of electron probe microanalysis. Starting on a five level states ladder model in 3D, we deduced a set of integro-differential coupled equations of the coefficients with a method know as invariant embedding. By means of a procedure proposed by authors, called method of convergence, two types ofmore » approximate solutions for the set of equations, namely complete and simple solutions, can be obtained. Although the simple solutions were initially proposed as auxiliary forms to solve higher rank equations, they turned out to be also useful for the estimation of the aforementioned coefficients. In previous reports, we have presented results obtained with the complete solutions. In this paper, we present results obtained with the simple solutions of the coefficients, which exhibit a good degree of fit with the experimental data. Both the model and the calculation method presented here can be generalized to other techniques that make use of different sorts of particle beams.« less

Determination of microbial phenolic acids in human faeces by UPLC-ESI-TQ MS.

PubMed

Sánchez-Patán, Fernando; Monagas, María; Moreno-Arribas, M Victoria; Bartolomé, Begoña

2011-03-23

The aim of the present work was to develop a reproducible, sensitive, and rapid UPLC-ESI-TQ MS analytical method for determination of microbial phenolic acids and other related compounds in faeces. A total of 47 phenolic compounds including hydroxyphenylpropionic, hydroxyphenylacetic, hydroxycinnamic, hydroxybenzoic, and hydroxymandelic acids and simple phenols were considered. To prepare an optimum pool standard solution, analytes were classified in 5 different groups with different starting concentrations according to their MS response. The developed UPLC method allowed a high resolution of the pool standard solution within an 18 min injection run time. The LOD of phenolic compounds ranged from 0.001 to 0.107 μg/mL and LOQ from 0.003 to 0.233 μg/mL. The method precision met acceptance criteria (<15% RSD) for all analytes, and accuracy was >80%. The method was applied to faecal samples collected before and after the intake of a flavan-3-ol supplement by a healthy volunteer. Both external and internal calibration methods were considered for quantification purposes, using 4-hydroxybenzoic-2,3,4,5-d4 acid as internal standard. For most analytes and samples, the level of microbial phenolic acids did not differ by using one or another calibration method. The results revealed an increase in protocatechuic, syringic, benzoic, p-coumaric, phenylpropionic, 3-hydroxyphenylacetic, and 3-hydroxyphenylpropionic acids, although differences due to the intake were only significant for the latter compound. In conclusion, the UPLC-DAD-ESI-TQ MS method developed is suitable for targeted analysis of microbial-derived phenolic metabolites in faecal samples from human intervention or in vitro fermentation studies, which requires high sensitivity and throughput.

Centrifugal ultrafiltration of human serum for improving immunoglobulin A quantification using attenuated total reflectance infrared spectroscopy.

PubMed

Elsohaby, Ibrahim; McClure, J Trenton; Riley, Christopher B; Bryanton, Janet; Bigsby, Kathryn; Shaw, R Anthony

2018-02-20

Attenuated total reflectance infrared (ATR-IR) spectroscopy is a simple, rapid and cost-effective method for the analysis of serum. However, the complex nature of serum remains a limiting factor to the reliability of this method. We investigated the benefits of coupling the centrifugal ultrafiltration with ATR-IR spectroscopy for quantification of human serum IgA concentration. Human serum samples (n = 196) were analyzed for IgA using an immunoturbidimetric assay. ATR-IR spectra were acquired for whole serum samples and for the retentate (residue) reconstituted with saline following 300 kDa centrifugal ultrafiltration. IR-based analytical methods were developed for each of the two spectroscopic datasets, and the accuracy of each of the two methods compared. Analytical methods were based upon partial least squares regression (PLSR) calibration models - one with 5-PLS factors (for whole serum) and the second with 9-PLS factors (for the reconstituted retentate). Comparison of the two sets of IR-based analytical results to reference IgA values revealed improvements in the Pearson correlation coefficient (from 0.66 to 0.76), and the root mean squared error of prediction in IR-based IgA concentrations (from 102 to 79 mg/dL) for the ultrafiltration retentate-based method as compared to the method built upon whole serum spectra. Depleting human serum low molecular weight proteins using a 300 kDa centrifugal filter thus enhances the accuracy IgA quantification by ATR-IR spectroscopy. Further evaluation and optimization of this general approach may ultimately lead to routine analysis of a range of high molecular-weight analytical targets that are otherwise unsuitable for IR-based analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Application Of A Potentiometric Electronic Tongue For The Determination Of Free SO2 And Other Analytical Parameters In White Wines From New Zealand

NASA Astrophysics Data System (ADS)

Mednova, Olga; Kirsanov, Dmitry; Rudnitskaya, Alisa; Kilmartin, Paul; Legin, Andrey

2009-05-01

The present study deals with a potentiometric electronic tongue (ET) multisensor system applied for the simultaneous determination of several chemical parameters for white wines produced in New Zealand. Methods in use for wine quality control are often expensive and require considerable time and skilled operation. The ET approach usually offers a simple and fast measurement protocol and allows automation for on-line analysis under industrial conditions. The ET device developed in this research is capable of quantifying the free and total SO2 content, total acids and some polyphenolic compounds in white wines with acceptable analytical errors.

Estimation of the curvature of the solid liquid interface during Bridgman crystal growth

NASA Astrophysics Data System (ADS)

Barat, Catherine; Duffar, Thierry; Garandet, Jean-Paul

1998-11-01

An approximate solution for the solid/liquid interface curvature due to the crucible effect in crystal growth is derived from simple heat flux considerations. The numerical modelling of the problem carried out with the help of the finite element code FIDAP supports the predictions of our analytical expression and allows to identify its range of validity. Experimental interface curvatures, measured in gallium antimonide samples grown by the vertical Bridgman method, are seen to compare satisfactorily to analytical and numerical results. Other literature data are also in fair agreement with the predictions of our models in the case where the amount of heat carried by the crucible is small compared to the overall heat flux.

Determination of transport wind speed in the gaussian plume diffusion equation for low-lying point sources

NASA Astrophysics Data System (ADS)

Wang, I. T.

A general method for determining the effective transport wind speed, overlineu, in the Gaussian plume equation is discussed. Physical arguments are given for using the generalized overlineu instead of the often adopted release-level wind speed with the plume diffusion equation. Simple analytical expressions for overlineu applicable to low-level point releases and a wide range of atmospheric conditions are developed. A non-linear plume kinematic equation is derived using these expressions. Crosswind-integrated SF 6 concentration data from the 1983 PNL tracer experiment are used to evaluate the proposed analytical procedures along with the usual approach of using the release-level wind speed. Results of the evaluation are briefly discussed.

Analytical solution for a class of network dynamics with mechanical and financial applications

NASA Astrophysics Data System (ADS)

Krejčí, P.; Lamba, H.; Melnik, S.; Rachinskii, D.

2014-09-01

We show that for a certain class of dynamics at the nodes the response of a network of any topology to arbitrary inputs is defined in a simple way by its response to a monotone input. The nodes may have either a discrete or continuous set of states and there is no limit on the complexity of the network. The results provide both an efficient numerical method and the potential for accurate analytic approximation of the dynamics on such networks. As illustrative applications, we introduce a quasistatic mechanical model with objects interacting via frictional forces and a financial market model with avalanches and critical behavior that are generated by momentum trading strategies.

Simultaneous Chloramphenicol and Florfenicol Determination by A Validated DLLME-HPLC-UV Method in Pasteurized Milk.

PubMed

Karami-Osboo, Rouhollah; Miri, Ramin; Javidnia, Katayoun; Kobarfard, Farzad

2016-01-01

The antibiotic residues in milk are a well-known serious problem and pose several health hazards to consumers. We have described a simple, rapid, and inexpensive DLLME-HPLC/UV technique for the extraction of chloramphenicol and florfenicol residues in milk samples. Under the optimum conditions, linearity of the method was observed over the range 0.02-0.85 µg/L with correlation coefficients > 0.999. The proposed method has been found to have a good limit of detection (signal to noise ratio = 3) for chloramphenicol (12.5 µg/Kg) and florfenicol (12.2 µg/Kg), and precision with relative standard deviation values under 15% (RSD, n = 3). Good recoveries (69.1-79.4%) were obtained for the extraction of the target analytes in milk samples. This simple and economic method has been applied for analyses of 15 real milk samples. Among all samples only one of them was contaminated to florfenicol; 62.4 µg/Kg and contamination to chloramphenicol was not detected.

Simultaneous Chloramphenicol and Florfenicol Determination by A Validated DLLME-HPLC-UV Method in Pasteurized Milk

PubMed Central

Karami-Osboo, Rouhollah; Miri, Ramin; Javidnia, Katayoun; Kobarfard, Farzad

2016-01-01

The antibiotic residues in milk are a well-known serious problem and pose several health hazards to consumers. We have described a simple, rapid, and inexpensive DLLME-HPLC/UV technique for the extraction of chloramphenicol and florfenicol residues in milk samples. Under the optimum conditions, linearity of the method was observed over the range 0.02-0.85 µg/L with correlation coefficients > 0.999. The proposed method has been found to have a good limit of detection (signal to noise ratio = 3) for chloramphenicol (12.5 µg/Kg) and florfenicol (12.2 µg/Kg), and precision with relative standard deviation values under 15% (RSD, n = 3). Good recoveries (69.1–79.4%) were obtained for the extraction of the target analytes in milk samples. This simple and economic method has been applied for analyses of 15 real milk samples. Among all samples only one of them was contaminated to florfenicol; 62.4 µg/Kg and contamination to chloramphenicol was not detected. PMID:27980571

Quantitative determination of the enantiomers of methadone in human plasma and saliva by chiral column chromatography coupled with mass spectrometric detection.

PubMed

George, Rani; Lobb, Michael; Haywood, Alison; Khan, Sohil; Hardy, Janet; Good, Phillip; Hennig, Stefanie; Norris, Ross

2016-01-01

Methadone is a potent lipophilic synthetic opioid that is effective in the treatment of cancer pain and perceived benefit in difficult pain control scenarios (especially in cases of neuropathic pain). The use of methadone in clinical practice is challenging however, due to the narrow therapeutic window and large inter- and intra-individual variability in therapeutic response. Quantitation of the enantiomers d- and l-methadone (d- and l-MTD) in plasma and saliva provides a basis for studying its pharmacokinetics in patients with cancer and for monitoring efficacy, toxicity and side-effects. This assay involves quantitation of the enantiomers of methadone using their respective deuterated internal standards, in plasma and saliva matrices with no impact of ion suppression in either matrix. The analytical recoveries of d- and l-MTD from the saliva collection devices (Salivette®) are optimised in this novel method with an accurate and simple extraction method employing dichloromethane. Optimal enantioselective separations were achieved using an α1-acid glycoprotein chiral stationary phase and triple quadrupole tandem mass spectrometer. Linearity was demonstrated over 0.05-1000µg/L for both enantiomers in plasma and in saliva with correlation coefficients greater than 0.998. The lower limit of quantitation (LLOQ) was determined to be 0.1µg/L in plasma and saliva for d- and l-MTD. Accuracy of the method ranges from 100% to 106% even at the LLOQ and total precision, expressed as the coefficient of variation, was between 0.2% and 4.4% for both analytes in both matrices. A simple one step extraction procedure resulted in recoveries greater than 95% for both analytes, at concentrations as low as 0.5µg/L, from the Salivette®. The validated method was applied successfully in 14 paired plasma and saliva samples obtained from adult patients with cancer pain receiving methadone. Copyright © 2015 Elsevier B.V. All rights reserved.

Correlation of finite element free vibration predictions using random vibration test data. M.S. Thesis - Cleveland State Univ.

NASA Technical Reports Server (NTRS)

Chambers, Jeffrey A.

1994-01-01

Finite element analysis is regularly used during the engineering cycle of mechanical systems to predict the response to static, thermal, and dynamic loads. The finite element model (FEM) used to represent the system is often correlated with physical test results to determine the validity of analytical results provided. Results from dynamic testing provide one means for performing this correlation. One of the most common methods of measuring accuracy is by classical modal testing, whereby vibratory mode shapes are compared to mode shapes provided by finite element analysis. The degree of correlation between the test and analytical mode shapes can be shown mathematically using the cross orthogonality check. A great deal of time and effort can be exhausted in generating the set of test acquired mode shapes needed for the cross orthogonality check. In most situations response data from vibration tests are digitally processed to generate the mode shapes from a combination of modal parameters, forcing functions, and recorded response data. An alternate method is proposed in which the same correlation of analytical and test acquired mode shapes can be achieved without conducting the modal survey. Instead a procedure is detailed in which a minimum of test information, specifically the acceleration response data from a random vibration test, is used to generate a set of equivalent local accelerations to be applied to the reduced analytical model at discrete points corresponding to the test measurement locations. The static solution of the analytical model then produces a set of deformations that once normalized can be used to represent the test acquired mode shapes in the cross orthogonality relation. The method proposed has been shown to provide accurate results for both a simple analytical model as well as a complex space flight structure.

Analysis of anabolic androgenic steroids in urine by full-capillary sample injection combined with a sweeping CE stacking method.

PubMed

Wang, Chun-Chi; Cheng, Shu-Fang; Cheng, Hui-Ling; Chen, Yen-Ling

2013-02-01

This study describes an on-line stacking CE approach by sweeping with whole capillary sample filling for analyzing five anabolic androgenic steroids in urine samples. The five anabolic steroids for detection were androstenedione, testosterone, epitestosterone, boldenone, and clostebol. Anabolic androgenic steroids are abused in sport doping because they can promote muscle growth. Therefore, a sensitive detection method is imperatively required for monitoring the urine samples of athletes. In this research, an interesting and reliable stacking capillary electrophoresis method was established for analysis of anabolic steroids in urine. After liquid-liquid extraction by n-hexane, the supernatant was dried and reconstituted with 30 mM phosphate buffer (pH 5.00) and loaded into the capillary by hydrodynamic injection (10 psi, 99.9 s). The stacking and separation were simultaneously accomplished at -20 kV in phosphate buffer (30 mM, pH 5.0) containing 100 mM sodium dodecyl sulfate and 40 % methanol. During the method validation, calibration curves were linear (r≥0.990) over a range of 50-1,000 ng/mL for the five analytes. In the evaluation of precision and accuracy for this method, the absolute values of the RSD and the RE in the intra-day (n=3) and inter-day (n=5) analyses were all less than 6.6 %. The limit of detection for the five analytes was 30 ng/mL (S/N=5, sampling 99.9 s at 10 psi). Compared with simple MECK, this stacking method possessed a 108- to 175-fold increase in sensitivity. This simple and sensitive stacking method could be used as a powerful tool for monitoring the illegal use of doping.

Simple and ultra-fast recognition and quantitation of compounded monoclonal antibodies: Application to flow injection analysis combined to UV spectroscopy and matching method.

PubMed

Jaccoulet, E; Schweitzer-Chaput, A; Toussaint, B; Prognon, P; Caudron, E

2018-09-01

Compounding of monoclonal antibody (mAbs) constantly increases in hospital. Quality control (QC) of the compounded mAbs based on quantification and identification is required to prevent potential errors and fast method is needed to manage outpatient chemotherapy administration. A simple and ultra-fast (less than 30 s) method using flow injection analysis associated to least square matching method issued from the analyzer software was performed and evaluated for the routine hospital QC of three compounded mAbs: bevacizumab, infliximab and rituximab. The method was evaluated through qualitative and quantitative parameters. Preliminary analysis of the UV absorption and second derivative spectra of the mAbs allowed us to adapt analytical conditions according to the therapeutic range of the mAbs. In terms of quantitative QC, linearity, accuracy and precision were assessed as specified in ICH guidelines. Very satisfactory recovery was achieved and the RSD (%) of the intermediate precision were less than 1.1%. Qualitative analytical parameters were also evaluated in terms of specificity, sensitivity and global precision through a matrix of confusion. Results showed to be concentration and mAbs dependant and excellent (100%) specificity and sensitivity were reached within specific concentration range. Finally, routine application on "real life" samples (n = 209) from different batch of the three mAbs complied with the specifications of the quality control i.e. excellent identification (100%) and ± 15% of targeting concentration belonging to the calibration range. The successful use of the combination of second derivative spectroscopy and partial least square matching method demonstrated the interest of FIA for the ultra-fast QC of mAbs after compounding using matching method. Copyright © 2018 Elsevier B.V. All rights reserved.

Development of new analytical methods for the determination of caffeine content in aqueous solution of green coffee beans.

PubMed

Weldegebreal, Blen; Redi-Abshiro, Mesfin; Chandravanshi, Bhagwan Singh

2017-12-05

This study was conducted to develop fast and cost effective methods for the determination of caffeine in green coffee beans. In the present work direct determination of caffeine in aqueous solution of green coffee bean was performed using FT-IR-ATR and fluorescence spectrophotometry. Caffeine was also directly determined in dimethylformamide solution using NIR spectroscopy with univariate calibration technique. The percentage of caffeine for the same sample of green coffee beans was determined using the three newly developed methods. The caffeine content of the green coffee beans was found to be 1.52 ± 0.09 (% w/w) using FT-IR-ATR, 1.50 ± 0.14 (% w/w) using NIR and 1.50 ± 0.05 (% w/w) using fluorescence spectroscopy. The means of the three methods were compared by applying one way analysis of variance and at p = 0.05 significance level the means were not significantly different. The percentage of caffeine in the same sample of green coffee bean was also determined by using the literature reported UV/Vis spectrophotometric method for comparison and found to be 1.40 ± 0.02 (% w/w). New simple, rapid and inexpensive methods were developed for direct determination of caffeine content in aqueous solution of green coffee beans using FT-IR-ATR and fluorescence spectrophotometries. NIR spectrophotometry can also be used as alternative choice of caffeine determination using reduced amount of organic solvent (dimethylformamide) and univariate calibration technique. These analytical methods may therefore, be recommended for the rapid, simple, safe and cost effective determination of caffeine in green coffee beans.

Monte Carlo solution of Boltzmann equation for a simple model of highly nonequilibrium diatomic gases: Translational rotational energy relaxation

NASA Technical Reports Server (NTRS)

Yoshikawa, K. K.

1978-01-01

The semiclassical transition probability was incorporated in the simulation for energy exchange between rotational and translational energy. The results provide details on the fundamental mechanisms of gas kinetics where analytical methods were impractical. The validity of the local Maxwellian assumption and relaxation time, rotational-translational energy transition, and a velocity analysis of the inelastic collision were discussed in detail.

Chirality sensing with stereodynamic copper(I) complexes.

PubMed

De Los Santos, Zeus A; Legaux, Nicholas M; Wolf, Christian

2017-11-01

Three Cu(I) complexes derived from stereodynamic diphosphine ligands were synthesized and used for chirality sensing. The coordination of diamines and amino acids to these complexes generates distinct circular dichroism signals. The chiroptical sensor response allows determination of the absolute configuration and the enantiomeric excess of the analyte at low concentrations. This method is operationally simple, fast, and attractive for high-throughput sensing applications. © 2017 Wiley Periodicals, Inc.

Resolution of plasma sample mix-ups through comparison of patient antibody patterns to E. coli.

PubMed

Vetter, Beatrice N; Orlowski, Vanessa; Schüpbach, Jörg; Böni, Jürg; Rühe, Bettina; Huder, Jon B

2015-12-01

Accidental sample mix-ups and the need for their swift resolution is a challenge faced by every analytical laboratory. To this end, we developed a simple immunoblot-based method, making use of a patient's characteristic plasma antibody profile to Escherichia coli (E. coli) proteins. Nitrocellulose strips of size-separated proteins from E. coli whole-cell lysates were incubated with patient plasma and visualised with an enzyme-coupled secondary antibody and substrate. Plasma samples of 20 random patients as well as five longitudinal samples of three patients were analysed for antibody band patterns, to evaluate uniqueness and consistency over time, respectively. For sample mix-ups, antibody band patterns of questionable samples were compared with samples of known identity. Comparison of anti-E. coli antibody patterns of 20 random patients showed a unique antibody profile for each patient. Antibody profiles remained consistent over time, as shown for three patients over several years. Three example cases demonstrate the use of this methodology in mis-labelling or -pipetting incidences. Our simple method for resolving plasma sample mix-ups between non-related individuals can be performed with basic laboratory equipment and thus can easily be adopted by analytical laboratories. Copyright © 2015 Elsevier B.V. All rights reserved.

Water equivalent thickness values of materials used in beams of protons, helium, carbon and iron ions.

PubMed

Zhang, Rui; Taddei, Phillip J; Fitzek, Markus M; Newhauser, Wayne D

2010-05-07

Heavy charged particle beam radiotherapy for cancer is of increasing interest because it delivers a highly conformal radiation dose to the target volume. Accurate knowledge of the range of a heavy charged particle beam after it penetrates a patient's body or other materials in the beam line is very important and is usually stated in terms of the water equivalent thickness (WET). However, methods of calculating WET for heavy charged particle beams are lacking. Our objective was to test several simple analytical formulas previously developed for proton beams for their ability to calculate WET values for materials exposed to beams of protons, helium, carbon and iron ions. Experimentally measured heavy charged particle beam ranges and WET values from an iterative numerical method were compared with the WET values calculated by the analytical formulas. In most cases, the deviations were within 1 mm. We conclude that the analytical formulas originally developed for proton beams can also be used to calculate WET values for helium, carbon and iron ion beams with good accuracy.

Water equivalent thickness values of materials used in beams of protons, helium, carbon and iron ions

PubMed Central

Zhang, Rui; Taddei, Phillip J; Fitzek, Markus M; Newhauser, Wayne D

2010-01-01

Heavy charged particle beam radiotherapy for cancer is of increasing interest because it delivers a highly conformal radiation dose to the target volume. Accurate knowledge of the range of a heavy charged particle beam after it penetrates a patient’s body or other materials in the beam line is very important and is usually stated in terms of the water equivalent thickness (WET). However, methods of calculating WET for heavy charged particle beams are lacking. Our objective was to test several simple analytical formulas previously developed for proton beams for their ability to calculate WET values for materials exposed to beams of protons, helium, carbon and iron ions. Experimentally measured heavy charged particle beam ranges and WET values from an iterative numerical method were compared with the WET values calculated by the analytical formulas. Inmost cases, the deviations were within 1 mm. We conclude that the analytical formulas originally developed for proton beams can also be used to calculate WET values for helium, carbon and iron ion beams with good accuracy. PMID:20371908

Quantitation of cocaine and cocaethylene in small volumes of rat whole blood using gas chromatography-mass spectrometry.

PubMed

Burdick, J D; Boni, R L; Fochtman, F W

1997-05-01

A simple solid phase extraction (SPE) technique combined with gas chromatography-mass spectrometry (GC/MS) operated in selected ion monitoring (SIM) mode is described for quantitation of cocaine and cocaethylene in small samples (250 microliters) of rat whole blood. Use of (N-[2H3C])-cocaine and (N-[2H3C])-cocaethylene internal standards resulted in high sensitivity and selectivity for this analytical method. Analysis was performed using a Hewlett-Packard 5890 GC equipped with a 7673A Automatic Liquid Sampler linked to a Hewlett-Packard 5972 Mass Selective Detector. Separation of analytes was accomplished on a cross-linked methyl silicone gum capillary column (Ultra 1: 12m x 0.2mm (i.d.) x 0.33 microns). Linearity was established over a wide range of concentrations (5.0-2000.0 ng ml-1) with good precision. Limits of detection (LOD) were 1.0 and 2.0 ng ml-1 for cocaine and cocaethylene, respectively. This analytical method was designed for use in pharmacokinetic experiments studying the formation of cocaethylene following ethanol pretreatment in rats administered cocaine.

Nuclear magnetic resonance signal dynamics of liquids in the presence of distant dipolar fields, revisited

PubMed Central

Barros, Wilson; Gochberg, Daniel F.; Gore, John C.

2009-01-01

The description of the nuclear magnetic resonance magnetization dynamics in the presence of long-range dipolar interactions, which is based upon approximate solutions of Bloch–Torrey equations including the effect of a distant dipolar field, has been revisited. New experiments show that approximate analytic solutions have a broader regime of validity as well as dependencies on pulse-sequence parameters that seem to have been overlooked. In order to explain these experimental results, we developed a new method consisting of calculating the magnetization via an iterative formalism where both diffusion and distant dipolar field contributions are treated as integral operators incorporated into the Bloch–Torrey equations. The solution can be organized as a perturbative series, whereby access to higher order terms allows one to set better boundaries on validity regimes for analytic first-order approximations. Finally, the method legitimizes the use of simple analytic first-order approximations under less demanding experimental conditions, it predicts new pulse-sequence parameter dependencies for the range of validity, and clarifies weak points in previous calculations. PMID:19425789

Feasibility and application of an HPLC/UVD to determine dinotefuran and its shorter wavelength metabolites residues in melon with tandem mass confirmation.

PubMed

Rahman, Md Musfiqur; Park, Jong-Hyouk; Abd El-Aty, A M; Choi, Jeong-Heui; Yang, Angel; Park, Ki Hun; Nashir Uddin Al Mahmud, Md; Im, Geon-Jae; Shim, Jae-Han

2013-01-15

A new analytical method was developed for dinotefuran and its metabolites, MNG, UF, and DN, in melon using high-performance liquid chromatography (HPLC) coupled with an ultraviolet detector (UVD). Due to shorter wavelength, lower sensitivity to UV detection, and high water miscibility of some metabolites, QuEChERs acetate-buffered version was modified for extraction and purification. Mobile phases with different ion pairing or ionisation agents were tested in different reverse phase columns, and ammonium bicarbonate buffer was found as the best choice to increase the sensitivity of target analytes to the UV detector. After failure of dispersive SPE clean-up with primary secondary amine, different solid phase extraction cartridges (SPE) were used to check the protecting capability of analytes against matrix interference. Finally, samples were extracted with a simple and rapid method using acetonitrile and salts, and purified through C(18)SPE. The method was validated at two spiking levels (three replicates for each) in the matrix. Good recoveries were observed for all of the analytes and ranged between 70.6% and 93.5%, with relative standard deviations of less than 10%. Calibration curves were linear over the calibration ranges for all the analytes with r(2)≥ 0.998. Limits of detection ranged from 0.02 to 0.05 mg kg(-1), whereas limits of quantitation ranged from 0.06 to 0.16 mg kg(-1) for dinotefuran and its metabolites. The method was successfully applied to real samples, where dinotefuran and UF residues were found in the field-incurred melon samples. Residues were confirmed via LC-tandem mass spectrometry (LC-MS/MS) in positive-ion electrospray ionisation (ESI(+)) mode. Copyright © 2012 Elsevier Ltd. All rights reserved.

A simple method to calculate first-passage time densities with arbitrary initial conditions

NASA Astrophysics Data System (ADS)

Nyberg, Markus; Ambjörnsson, Tobias; Lizana, Ludvig

2016-06-01

Numerous applications all the way from biology and physics to economics depend on the density of first crossings over a boundary. Motivated by the lack of general purpose analytical tools for computing first-passage time densities (FPTDs) for complex problems, we propose a new simple method based on the independent interval approximation (IIA). We generalise previous formulations of the IIA to include arbitrary initial conditions as well as to deal with discrete time and non-smooth continuous time processes. We derive a closed form expression for the FPTD in z and Laplace-transform space to a boundary in one dimension. Two classes of problems are analysed in detail: discrete time symmetric random walks (Markovian) and continuous time Gaussian stationary processes (Markovian and non-Markovian). Our results are in good agreement with Langevin dynamics simulations.

A method to design blended rolled edges for compact range reflectors

NASA Technical Reports Server (NTRS)

Gupta, Inder J.; Burnside, Walter D.

1989-01-01

A method to design blended rolled edges for arbitrary rim shape compact range reflectors is presented. The reflectors may be center-fed or offset-fed. The method leads to rolled edges with minimal surface discontinuities. It is shown that the reflectors designed using the prescribed method can be defined analytically using simple expressions. A procedure to obtain optimum rolled edges parameter is also presented. The procedure leads to blended rolled edges that minimize the diffracted fields emanating from the junction between the paraboloid and the rolled edge surface while satisfying certain constraints regarding the reflector size and the minimum operating frequency of the system.

A method to design blended rolled edges for compact range reflectors

NASA Technical Reports Server (NTRS)

Gupta, Inder J.; Ericksen, Kurt P.; Burnside, Walter D.

1990-01-01

A method to design blended rolled edges for arbitrary rim shape compact range reflectors is presented. The reflectors may be center-fed or offset-fed. The method leads to rolled edges with minimal surface discontinuities. It is shown that the reflectors designed using the prescribed method can be defined analytically using simple expressions. A procedure to obtain optimum rolled edges parameters is also presented. The procedure leads to blended rolled edges that minimize the diffracted fields emanating from the junction between the paraboloid and the rolled edge surface while satisfying certain constraints regarding the reflector size and the minimum operating frequency of the system.

Analysis of titanium content in titanium tetrachloride solution

NASA Astrophysics Data System (ADS)

Bi, Xiaoguo; Dong, Yingnan; Li, Shanshan; Guan, Duojiao; Wang, Jianyu; Tang, Meiling

2018-03-01

Strontium titanate, barium titan and lead titanate are new type of functional ceramic materials with good prospect, and titanium tetrachloride is a commonly in the production such products. Which excellent electrochemical performance of ferroelectric tempreature coefficient effect.In this article, three methods are used to calibrate the samples of titanium tetrachloride solution by back titration method, replacement titration method and gravimetric analysis method. The results show that the back titration method has many good points, for example, relatively simple operation, easy to judgment the titration end point, better accuracy and precision of analytical results, the relative standard deviation not less than 0.2%. So, it is the ideal of conventional analysis methods in the mass production.

A simple model for strong ground motions and response spectra

USGS Publications Warehouse

Safak, Erdal; Mueller, Charles; Boatwright, John

1988-01-01

A simple model for the description of strong ground motions is introduced. The model shows that response spectra can be estimated by using only four parameters of the ground motion, the RMS acceleration, effective duration and two corner frequencies that characterize the effective frequency band of the motion. The model is windowed band-limited white noise, and is developed by studying the properties of two functions, cumulative squared acceleration in the time domain, and cumulative squared amplitude spectrum in the frequency domain. Applying the methods of random vibration theory, the model leads to a simple analytical expression for the response spectra. The accuracy of the model is checked by using the ground motion recordings from the aftershock sequences of two different earthquakes and simulated accelerograms. The results show that the model gives a satisfactory estimate of the response spectra.

Modulational estimate for the maximal Lyapunov exponent in Fermi-Pasta-Ulam chains

NASA Astrophysics Data System (ADS)

Dauxois, Thierry; Ruffo, Stefano; Torcini, Alessandro

1997-12-01

In the framework of the Fermi-Pasta-Ulam (FPU) model, we show a simple method to give an accurate analytical estimation of the maximal Lyapunov exponent at high energy density. The method is based on the computation of the mean value of the modulational instability growth rates associated to unstable modes. Moreover, we show that the strong stochasticity threshold found in the β-FPU system is closely related to a transition in tangent space, the Lyapunov eigenvector being more localized in space at high energy.

HPLC-DAD-MS identification of bioactive secondary metabolites from Ferula communis roots.

PubMed

Arnoldi, Lolita; Ballero, Mauro; Fuzzati, Nicola; Maxia, Andrea; Mercalli, Enrico; Pagni, Luca

2004-06-01

A simple HPLC method was developed to distinguish between 'poisonous' and 'non-poisonous' chemotypes of Ferula communis. The method was performed on a C8 reverse phase analytical column using a binary eluent (aqueous TFA 0.01%-TFA 0.01% in acetonitrile) under gradient condition. The two chemotypes showed different fingerprints. The identification of five coumarins and eleven daucane derivatives by HPLC-diode array detection (HPLC-DAD) and HPLC-MS is described. A coumarin, not yet described, was detected. Copyright 2004 Elsevier B.V.

Analytical determination of space station response to crew motion and design of suspension system for microgravity experiments

NASA Technical Reports Server (NTRS)

Liu, F. C.

1986-01-01

The objective of this investigation is to make analytical determination of the acceleration produced by crew motion in an orbiting space station and define design parameters for the suspension system of microgravity experiments. A simple structural model for simulation of the IOC space station is proposed. Mathematical formulation of this model provides the engineers a simple and direct tool for designing an effective suspension system.

An Analytical State Transition Matrix for Orbits Perturbed by an Oblate Spheroid

NASA Technical Reports Server (NTRS)

Mueller, A. C.

1977-01-01

An analytical state transition matrix and its inverse, which include the short period and secular effects of the second zonal harmonic, were developed from the nonsingular PS satellite theory. The fact that the independent variable in the PS theory is not time is in no respect disadvantageous, since any explicit analytical solution must be expressed in the true or eccentric anomaly. This is shown to be the case for the simple conic matrix. The PS theory allows for a concise, accurate, and algorithmically simple state transition matrix. The improvement over the conic matrix ranges from 2 to 4 digits accuracy.

Exact short-time height distribution for the flat Kardar-Parisi-Zhang interface

NASA Astrophysics Data System (ADS)

Smith, Naftali R.; Meerson, Baruch

2018-05-01

We determine the exact short-time distribution -lnPf(" close=")H ,t )">H ,t =Sf(H )/√{t } of the one-point height H =h (x =0 ,t ) of an evolving 1 +1 Kardar-Parisi-Zhang (KPZ) interface for flat initial condition. This is achieved by combining (i) the optimal fluctuation method, (ii) a time-reversal symmetry of the KPZ equation in 1 +1 dimension, and (iii) the recently determined exact short-time height distribution -lnPst(H ) of the latter, one encounters two branches: an analytic and a nonanalytic. The analytic branch is nonphysical beyond a critical value of H where a second-order dynamical phase transition occurs. Here we show that, remarkably, it is the analytic branch of Sst(H ) which determines the large-deviation function Sf(H ) of the flat interface via a simple mapping Sf(H )=2-3 /2SstAnalysis of Mathematical Modelling on Potentiometric Biosensors

PubMed Central

Mehala, N.; Rajendran, L.

2014-01-01

A mathematical model of potentiometric enzyme electrodes for a nonsteady condition has been developed. The model is based on the system of two coupled nonlinear time-dependent reaction diffusion equations for Michaelis-Menten formalism that describes the concentrations of substrate and product within the enzymatic layer. Analytical expressions for the concentration of substrate and product and the corresponding flux response have been derived for all values of parameters using the new homotopy perturbation method. Furthermore, the complex inversion formula is employed in this work to solve the boundary value problem. The analytical solutions obtained allow a full description of the response curves for only two kinetic parameters (unsaturation/saturation parameter and reaction/diffusion parameter). Theoretical descriptions are given for the two limiting cases (zero and first order kinetics) and relatively simple approaches for general cases are presented. All the analytical results are compared with simulation results using Scilab/Matlab program. The numerical results agree with the appropriate theories. PMID:25969765

Analysis of mathematical modelling on potentiometric biosensors.

PubMed

Mehala, N; Rajendran, L

2014-01-01

A mathematical model of potentiometric enzyme electrodes for a nonsteady condition has been developed. The model is based on the system of two coupled nonlinear time-dependent reaction diffusion equations for Michaelis-Menten formalism that describes the concentrations of substrate and product within the enzymatic layer. Analytical expressions for the concentration of substrate and product and the corresponding flux response have been derived for all values of parameters using the new homotopy perturbation method. Furthermore, the complex inversion formula is employed in this work to solve the boundary value problem. The analytical solutions obtained allow a full description of the response curves for only two kinetic parameters (unsaturation/saturation parameter and reaction/diffusion parameter). Theoretical descriptions are given for the two limiting cases (zero and first order kinetics) and relatively simple approaches for general cases are presented. All the analytical results are compared with simulation results using Scilab/Matlab program. The numerical results agree with the appropriate theories.

A Short Research Note on Calculating Exact Distribution Functions and Random Sampling for the 3D NFW Profile

NASA Astrophysics Data System (ADS)

Robotham, A. S. G.; Howlett, Cullan

2018-06-01

In this short note we publish the analytic quantile function for the Navarro, Frenk & White (NFW) profile. All known published and coded methods for sampling from the 3D NFW PDF use either accept-reject, or numeric interpolation (sometimes via a lookup table) for projecting random Uniform samples through the quantile distribution function to produce samples of the radius. This is a common requirement in N-body initial condition (IC), halo occupation distribution (HOD), and semi-analytic modelling (SAM) work for correctly assigning particles or galaxies to positions given an assumed concentration for the NFW profile. Using this analytic description allows for much faster and cleaner code to solve a common numeric problem in modern astronomy. We release R and Python versions of simple code that achieves this sampling, which we note is trivial to reproduce in any modern programming language.

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.

On the analytical modeling of the nonlinear vibrations of pretensioned space structures

NASA Technical Reports Server (NTRS)

Housner, J. M.; Belvin, W. K.

1983-01-01

Pretensioned structures are receiving considerable attention as candidate large space structures. A typical example is a hoop-column antenna. The large number of preloaded members requires efficient analytical methods for concept validation and design. Validation through analyses is especially important since ground testing may be limited due to gravity effects and structural size. The present investigation has the objective to present an examination of the analytical modeling of pretensioned members undergoing nonlinear vibrations. Two approximate nonlinear analysis are developed to model general structural arrangements which include beam-columns and pretensioned cables attached to a common nucleus, such as may occur at a joint of a pretensioned structure. Attention is given to structures undergoing nonlinear steady-state oscillations due to sinusoidal excitation forces. Three analyses, linear, quasi-linear, and nonlinear are conducted and applied to study the response of a relatively simple cable stiffened structure.

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.

Analytical Method Development and Validation for the Quantification of Acetone and Isopropyl Alcohol in the Tartaric Acid Base Pellets of Dipyridamole Modified Release Capsules by Using Headspace Gas Chromatographic Technique

PubMed Central

2018-01-01

A simple, sensitive, accurate, robust headspace gas chromatographic method was developed for the quantitative determination of acetone and isopropyl alcohol in tartaric acid-based pellets of dipyridamole modified release capsules. The residual solvents acetone and isopropyl alcohol were used in the manufacturing process of the tartaric acid-based pellets of dipyridamole modified release capsules by considering the solubility of the dipyridamole and excipients in the different manufacturing stages. The method was developed and optimized by using fused silica DB-624 (30 m × 0.32 mm × 1.8 µm) column with the flame ionization detector. The method validation was carried out with regard to the guidelines for validation of analytical procedures Q2 demanded by the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH). All the validation characteristics were meeting the acceptance criteria. Hence, the developed and validated method can be applied for the intended routine analysis. PMID:29686931

Analytical Method Development and Validation for the Quantification of Acetone and Isopropyl Alcohol in the Tartaric Acid Base Pellets of Dipyridamole Modified Release Capsules by Using Headspace Gas Chromatographic Technique.

PubMed

Valavala, Sriram; Seelam, Nareshvarma; Tondepu, Subbaiah; Jagarlapudi, V Shanmukha Kumar; Sundarmurthy, Vivekanandan

2018-01-01

A simple, sensitive, accurate, robust headspace gas chromatographic method was developed for the quantitative determination of acetone and isopropyl alcohol in tartaric acid-based pellets of dipyridamole modified release capsules. The residual solvents acetone and isopropyl alcohol were used in the manufacturing process of the tartaric acid-based pellets of dipyridamole modified release capsules by considering the solubility of the dipyridamole and excipients in the different manufacturing stages. The method was developed and optimized by using fused silica DB-624 (30 m × 0.32 mm × 1.8  µ m) column with the flame ionization detector. The method validation was carried out with regard to the guidelines for validation of analytical procedures Q2 demanded by the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH). All the validation characteristics were meeting the acceptance criteria. Hence, the developed and validated method can be applied for the intended routine analysis.

Method for the analysis of triadimefon and ethofumesate from dislodgeable foliar residues on turfgrass by solid-phase extraction and in-vial elution.

PubMed

Runes, H B; Jenkins, J J; Field, J A

1999-08-01

Triadimefon, a fungicide, and ethofumesate, an herbicide, are commonly applied to turfgrass in the Pacific Northwest, resulting in foliar residues. A simple and rapid method was developed to determine triadimefon and ethofumesate concentrations from dislodgeable foliar residues on turfgrass. Turfgrass samples were washed, and wash water containing surfactant (a 0.126% solution) was collected for residue analysis. This analytical method utilizes a 25 mm C(8) Empore disk and in-vial elution to quantitatively determine triadimefon and ethofumesate in 170 mL aqueous samples. The analytes were eluted by placing the disk in a 2 mL autosampler vial with 980 microL of ethyl acetate and 20 microL of 2-chlorolepidine, the internal standard, for analysis by GC/MS. The method quantitation limits are 0.29 microg/L for ethofumesate and 0.59 microg/L for triadimefon. The method detection limits are 0.047 microg/L and 0.29 microg/L for ethofumesate and triadimefon, respectively. Concentrations of triadimefon and ethofumesate from dislodgeable foliar residues from a field study are reported.

Green and simple analytical method to determine benzimidazoles in milk samples by using salting-out assisted liquid-liquid extraction and capillary liquid chromatography.

PubMed

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

2018-08-01

A green and simple multiresidue method using capillary liquid chromatography (CLC) with UV-diode array detection (DAD) has been developed for the determination of sixteen benzimidazoles (BZs) and its metabolites in milk samples. The separation was achieved in <32 min, using a Zorbax XDB-C18 column (150 mm × 0.5 mm I.D, 5 μm), with a mobile phase consisting of 50 mM ammonium acetate (solvent A) and a mixture of acetonitrile/methanol (1:1 v/v) (solvent B), at a flow rate of 9 μL min -1 . The temperature of the column was 20 °C and 6 μL of sample were injected. In spite of the complexity of milk samples, an effective, simple and fast sample preparation method called salting out-assisted liquid-liquid extraction (SALLE) was developed for the analysis of these compounds in cow milk samples. To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized including the amount of sample, type and volume of the extraction solvent, and the nature and amount of the salt. Good linearity was obtained (R 2  > 0.9985 for all BZs) with limits of detection (LOD) between 1.0 and 2.8 μg kg -1 . Relative standard deviations of repeatability and intermediate precision were below 1.6 and 14.2%, respectively. Satisfactory recoveries between 79.1 and 99.6% were also obtained for three types of milk samples (cow, sheep and goat). The advantages of a miniaturized technique such as CLC in terms of better efficiencies and reduced solvent consumption, combined with the simplicity of the SALLE procedure, make this method a useful alternative for the monitoring of these residues at trace level. Copyright © 2018 Elsevier B.V. All rights reserved.

Rapid B-rep model preprocessing for immersogeometric analysis using analytic surfaces

PubMed Central

Wang, Chenglong; Xu, Fei; Hsu, Ming-Chen; Krishnamurthy, Adarsh

2017-01-01

Computational fluid dynamics (CFD) simulations of flow over complex objects have been performed traditionally using fluid-domain meshes that conform to the shape of the object. However, creating shape conforming meshes for complicated geometries like automobiles require extensive geometry preprocessing. This process is usually tedious and requires modifying the geometry, including specialized operations such as defeaturing and filling of small gaps. Hsu et al. (2016) developed a novel immersogeometric fluid-flow method that does not require the generation of a boundary-fitted mesh for the fluid domain. However, their method used the NURBS parameterization of the surfaces for generating the surface quadrature points to enforce the boundary conditions, which required the B-rep model to be converted completely to NURBS before analysis can be performed. This conversion usually leads to poorly parameterized NURBS surfaces and can lead to poorly trimmed or missing surface features. In addition, converting simple geometries such as cylinders to NURBS imposes a performance penalty since these geometries have to be dealt with as rational splines. As a result, the geometry has to be inspected again after conversion to ensure analysis compatibility and can increase the computational cost. In this work, we have extended the immersogeometric method to generate surface quadrature points directly using analytic surfaces. We have developed quadrature rules for all four kinds of analytic surfaces: planes, cones, spheres, and toroids. We have also developed methods for performing adaptive quadrature on trimmed analytic surfaces. Since analytic surfaces have frequently been used for constructing solid models, this method is also faster to generate quadrature points on real-world geometries than using only NURBS surfaces. To assess the accuracy of the proposed method, we perform simulations of a benchmark problem of flow over a torpedo shape made of analytic surfaces and compare those to immersogeometric simulations of the same model with NURBS surfaces. We also compare the results of our immersogeometric method with those obtained using boundary-fitted CFD of a tessellated torpedo shape, and quantities of interest such as drag coefficient are in good agreement. Finally, we demonstrate the effectiveness of our immersogeometric method for high-fidelity industrial scale simulations by performing an aerodynamic analysis of a truck that has a large percentage of analytic surfaces. Using analytic surfaces over NURBS avoids unnecessary surface type conversion and significantly reduces model-preprocessing time, while providing the same accuracy for the aerodynamic quantities of interest. PMID:29051678

Rapid determination of anti-estrogens by gas chromatography/mass spectrometry in urine: Method validation and application to real samples.

PubMed

Gerace, E; Salomone, A; Abbadessa, G; Racca, S; Vincenti, M

2012-02-01

A fast screening protocol was developed for the simultaneous determination of nine anti-estrogenic agents (aminoglutethimide, anastrozole, clomiphene, drostanolone, formestane, letrozole, mesterolone, tamoxifen, testolactone) plus five of their metabolites in human urine. After an enzymatic hydrolysis, these compounds can be extracted simultaneously from urine with a simple liquid-liquid extraction at alkaline conditions. The analytes were subsequently analyzed by fast-gas chromatography/mass spectrometry (fast-GC/MS) after derivatization. The use of a short column, high-flow carrier gas velocity and fast temperature ramping produced an efficient separation of all analytes in about 4 min, allowing a processing rate of 10 samples/h. The present analytical method was validated according to UNI EN ISO/IEC 17025 guidelines for qualitative methods. The range of investigated parameters included the limit of detection, selectivity, linearity, repeatability, robustness and extraction efficiency. High MS-sampling rate, using a benchtop quadrupole mass analyzer, resulted in accurate peak shape definition under both scan and selected ion monitoring modes, and high sensitivity in the latter mode. Therefore, the performances of the method are comparable to the ones obtainable from traditional GC/MS analysis. The method was successfully tested on real samples arising from clinical treatments of hospitalized patients and could profitably be used for clinical studies on anti-estrogenic drug administration.

Rapid determination of anti-estrogens by gas chromatography/mass spectrometry in urine: Method validation and application to real samples

PubMed Central

Gerace, E.; Salomone, A.; Abbadessa, G.; Racca, S.; Vincenti, M.

2011-01-01

A fast screening protocol was developed for the simultaneous determination of nine anti-estrogenic agents (aminoglutethimide, anastrozole, clomiphene, drostanolone, formestane, letrozole, mesterolone, tamoxifen, testolactone) plus five of their metabolites in human urine. After an enzymatic hydrolysis, these compounds can be extracted simultaneously from urine with a simple liquid–liquid extraction at alkaline conditions. The analytes were subsequently analyzed by fast-gas chromatography/mass spectrometry (fast-GC/MS) after derivatization. The use of a short column, high-flow carrier gas velocity and fast temperature ramping produced an efficient separation of all analytes in about 4 min, allowing a processing rate of 10 samples/h. The present analytical method was validated according to UNI EN ISO/IEC 17025 guidelines for qualitative methods. The range of investigated parameters included the limit of detection, selectivity, linearity, repeatability, robustness and extraction efficiency. High MS-sampling rate, using a benchtop quadrupole mass analyzer, resulted in accurate peak shape definition under both scan and selected ion monitoring modes, and high sensitivity in the latter mode. Therefore, the performances of the method are comparable to the ones obtainable from traditional GC/MS analysis. The method was successfully tested on real samples arising from clinical treatments of hospitalized patients and could profitably be used for clinical studies on anti-estrogenic drug administration. PMID:29403714

A rapid and sensitive analytical method for the determination of 14 pyrethroids in water samples.

PubMed

Feo, M L; Eljarrat, E; Barceló, D

2010-04-09

A simple, efficient and environmentally friendly analytical methodology is proposed for extracting and preconcentrating pyrethroids from water samples prior to gas chromatography-negative ion chemical ionization mass spectrometry (GC-NCI-MS) analysis. Fourteen pyrethroids were selected for this work: bifenthrin, cyfluthrin, lambda-cyhalothrin, cypermethrin, deltamethrin, esfenvalerate, fenvalerate, fenpropathrin, tau-fluvalinate, permethrin, phenothrin, resmethrin, tetramethrin and tralomethrin. The method is based on ultrasound-assisted emulsification-extraction (UAEE) of a water-immiscible solvent in an aqueous medium. Chloroform was used as extraction solvent in the UAEE technique. Target analytes were quantitatively extracted achieving an enrichment factor of 200 when 20 mL aliquot of pure water spiked with pyrethroid standards was extracted. The method was also evaluated with tap water and river water samples. Method detection limits (MDLs) ranged from 0.03 to 35.8 ng L(-1) with RSDs values < or =3-25% (n=5). The coefficients of estimation of the calibration curves obtained following the proposed methodology were > or =0.998. Recovery values were in the range of 45-106%, showing satisfactory robustness of the method for analyzing pyrethroids in water samples. The proposed methodology was applied for the analysis of river water samples. Cypermethrin was detected at concentration levels ranging from 4.94 to 30.5 ng L(-1). Copyright 2010 Elsevier B.V. All rights reserved.

Sensitive determination of estrogens in environmental waters treated with polymeric ionic liquid-based stir cake sorptive extraction and liquid chromatographic analysis.

PubMed

Chen, Lei; Mei, Meng; Huang, Xiaojia; Yuan, Dongxing

2016-05-15

A simple, sensitive and environmentally friendly method using polymeric ionic liquid-based stir cake sorptive extraction followed by high performance liquid chromatography with diode array detection (HPLC/DAD) has been developed for efficient quantification of six selected estrogens in environmental waters. To extract trace estrogens effectively, a poly (1-ally-3-vinylimidazolium chloride-co-ethylene dimethacrylate) monolithic cake was prepared and used as the sorbent of stir cake sorptive extraction (SCSE). The effects of preparation conditions of sorbent and extraction parameters of SCSE for estrogens were investigated and optimized. Under optimal conditions, the developed method showed satisfactory analytical performance for targeted analytes. Low limits of detection (S/N=3) and quantification limits (S/N=10) were achieved within the range of 0.024-0.057 µg/L and 0.08-0.19 µg/L, respectively. Good linearity of method was obtained for analytes with the correlation coefficients (R(2)) above 0.99. At the same time, satisfactory method repeatability and reproducibility was achieved in terms of intra- and inter-day precisions, respectively. Finally, the established SCSE-HPLC/DAD method was successfully applied for the determination of estrogens in different environmental water samples. Recoveries obtained for the determination of estrogens in spiked samples ranged from 71.2% to 108%, with RSDs below 10% in all cases. Copyright © 2016 Elsevier B.V. All rights reserved.

Rapid and sensitive analysis of polychlorinated biphenyls and acrylamide in food samples using ionic liquid-based in situ dispersive liquid-liquid microextraction coupled to headspace gas chromatography.

PubMed

Zhang, Cheng; Cagliero, Cecilia; Pierson, Stephen A; Anderson, Jared L

2017-01-20

A simple and rapid ionic liquid (IL)-based in situ dispersive liquid-liquid microextraction (DLLME) method was developed and coupled to headspace gas chromatography (HS-GC) employing electron capture (ECD) and mass spectrometry (MS) detection for the analysis of polychlorinated biphenyls (PCBs) and acrylamide at trace levels from milk and coffee samples. The chemical structures of the halide-based ILs were tailored by introducing various functional groups to the cations to evaluate the effect of different structural features on the extraction efficiency of the target analytes. Extraction parameters including the molar ratio of IL to metathesis reagent and IL mass were optimized. The effects of HS oven temperature and the HS sample vial volume on the analyte response were also evaluated. The optimized in situ DLLME method exhibited good analytical precision, good linearity, and provided detection limits down to the low ppt level for PCBs and the low ppb level for acrylamide in aqueous samples. The matrix-compatibility of the developed method was also established by quantifying acrylamide in brewed coffee samples. This method is much simpler and faster compared to previously reported GC-MS methods using solid-phase microextraction (SPME) for the extraction/preconcentration of PCBs and acrylamide from complex food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Application of analytical quality by design principles for the determination of alkyl p-toluenesulfonates impurities in Aprepitant by HPLC. Validation using total-error concept.

PubMed

Zacharis, Constantinos K; Vastardi, Elli

2018-02-20

In the research presented we report the development of a simple and robust liquid chromatographic method for the quantification of two genotoxic alkyl sulphonate impurities (namely methyl p-toluenesulfonate and isopropyl p-toluenesulfonate) in Aprepitant API substances using the Analytical Quality by Design (AQbD) approach. Following the steps of AQbD protocol, the selected critical method attributes (CMAs) were the separation criterions between the critical peak pairs, the analysis time and the peak efficiencies of the analytes. The critical method parameters (CMPs) included the flow rate, the gradient slope and the acetonitrile content at the first step of the gradient elution program. Multivariate experimental designs namely Plackett-Burman and Box-Behnken designs were conducted sequentially for factor screening and optimization of the method parameters. The optimal separation conditions were estimated using the desirability function. The method was fully validated in the range of 10-200% of the target concentration limit of the analytes using the "total error" approach. Accuracy profiles - a graphical decision making tool - were constructed using the results of the validation procedures. The β-expectation tolerance intervals did not exceed the acceptance criteria of±10%, meaning that 95% of future results will be included in the defined bias limits. The relative bias ranged between - 1.3-3.8% for both analytes, while the RSD values for repeatability and intermediate precision were less than 1.9% in all cases. The achieved limit of detection (LOD) and the limit of quantification (LOQ) were adequate for the specific purpose and found to be 0.02% (corresponding to 48μgg -1 in sample) for both methyl and isopropyl p-toluenesulfonate. As proof-of-concept, the validated method was successfully applied in the analysis of several Aprepitant batches indicating that this methodology could be used for routine quality control analyses. Copyright © 2017 Elsevier B.V. All rights reserved.

Prevalidation in pharmaceutical analysis. Part I. Fundamentals and critical discussion.

PubMed

Grdinić, Vladimir; Vuković, Jadranka

2004-05-28

A complete prevalidation, as a basic prevalidation strategy for quality control and standardization of analytical procedure was inaugurated. Fast and simple, the prevalidation methodology based on mathematical/statistical evaluation of a reduced number of experiments (N < or = 24) was elaborated and guidelines as well as algorithms were given in detail. This strategy has been produced for the pharmaceutical applications and dedicated to the preliminary evaluation of analytical methods where linear calibration model, which is very often occurred in practice, could be the most appropriate to fit experimental data. The requirements presented in this paper should therefore help the analyst to design and perform the minimum number of prevalidation experiments needed to obtain all the required information to evaluate and demonstrate the reliability of its analytical procedure. In complete prevalidation process, characterization of analytical groups, checking of two limiting groups, testing of data homogeneity, establishment of analytical functions, recognition of outliers, evaluation of limiting values and extraction of prevalidation parameters were included. Moreover, system of diagnosis for particular prevalidation step was suggested. As an illustrative example for demonstration of feasibility of prevalidation methodology, among great number of analytical procedures, Vis-spectrophotometric procedure for determination of tannins with Folin-Ciocalteu's phenol reagent was selected. Favourable metrological characteristics of this analytical procedure, as prevalidation figures of merit, recognized the metrological procedure as a valuable concept in preliminary evaluation of quality of analytical procedures.

Characterization, thermal stability studies, and analytical method development of Paromomycin for formulation development.

PubMed

Khan, Wahid; Kumar, Neeraj

2011-06-01

Paromomycin (PM) is an aminoglycoside antibiotic, first isolated in the 1950s, and approved in 2006 for treatment of visceral leishmaniasis. Although isolated six decades back, sufficient information essential for development of pharmaceutical formulation is not available for PM. The purpose of this paper was to determine thermal stability and development of new analytical method for formulation development of PM. PM was characterized by thermoanalytical (DSC, TGA, and HSM) and by spectroscopic (FTIR) techniques and these techniques were used to establish thermal stability of PM after heating PM at 100, 110, 120, and 130 °C for 24 h. Biological activity of these heated samples was also determined by microbiological assay. Subsequently, a simple, rapid and sensitive RP-HPLC method for quantitative determination of PM was developed using pre-column derivatization with 9-fluorenylmethyl chloroformate. The developed method was applied to estimate PM quantitatively in two parenteral dosage forms. PM was successfully characterized by various stated techniques. These techniques indicated stability of PM for heating up to 120 °C for 24 h, but when heated at 130 °C, PM is liable to degradation. This degradation is also observed in microbiological assay where PM lost ∼30% of its biological activity when heated at 130 °C for 24 h. New analytical method was developed for PM in the concentration range of 25-200 ng/ml with intra-day and inter-day variability of < 2%RSD. Characterization techniques were established and stability of PM was determined successfully. Developed analytical method was found sensitive, accurate, and precise for quantification of PM. Copyright © 2010 John Wiley & Sons, Ltd. Copyright © 2010 John Wiley & Sons, Ltd.

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

Advantages of using tetrahydrofuran-water as mobile phases in the quantitation of cyclosporin A in monkey and rat plasma by liquid chromatography-tandem mass spectrometry.

PubMed

Li, Austin C; Li, Yinghe; Guirguis, Micheal S; Caldwell, Robert G; Shou, Wilson Z

2007-01-04

A new analytical method is described here for the quantitation of anti-inflammatory drug cyclosporin A (CyA) in monkey and rat plasma. The method used tetrahydrofuran (THF)-water mobile phases to elute the analyte and internal standard, cyclosporin C (CyC). The gradient mobile phase program successfully eluted CyA into a sharp peak and therefore improved resolution between the analyte and possible interfering materials compared with previously reported analytical approaches, where CyA was eluted as a broad peak due to the rapid conversion between different conformers. The sharp peak resulted from this method facilitated the quantitative calculation as multiple smoothing and large number of bunching factors were not necessary. The chromatography in the new method was performed at 30 degrees C instead of 65-70 degrees C as reported previously. Other advantages of the method included simple and fast sample extraction-protein precipitation, direct injection of the extraction supernatant to column for analysis, and elimination of evaporation and reconstitution steps, which were needed in solid phase extraction or liquid-liquid extraction reported before. This method is amenable to high-throughput analysis with a total chromatographic run time of 3 min. This approach has been verified as sensitive, linear (0.977-4000 ng/mL), accurate and precise for the quantitation of CyA in monkey and rat plasma. However, compared with the usage of conventional mobile phases, the only drawback of this approach was the reduced detection response from the mass spectrometer that was possibly caused by poor desolvation in the ionization source. This is the first report to demonstrate the advantages of using THF-water mobile phases to elute CyA in liquid chromatography.

An improved algorithm for balanced POD through an analytic treatment of impulse response tails

NASA Astrophysics Data System (ADS)

Tu, Jonathan H.; Rowley, Clarence W.

2012-06-01

We present a modification of the balanced proper orthogonal decomposition (balanced POD) algorithm for systems with simple impulse response tails. In this new method, we use dynamic mode decomposition (DMD) to estimate the slowly decaying eigenvectors that dominate the long-time behavior of the direct and adjoint impulse responses. This is done using a new, low-memory variant of the DMD algorithm, appropriate for large datasets. We then formulate analytic expressions for the contribution of these eigenvectors to the controllability and observability Gramians. These contributions can be accounted for in the balanced POD algorithm by simply appending the impulse response snapshot matrices (direct and adjoint, respectively) with particular linear combinations of the slow eigenvectors. Aside from these additions to the snapshot matrices, the algorithm remains unchanged. By treating the tails analytically, we eliminate the need to run long impulse response simulations, lowering storage requirements and speeding up ensuing computations. To demonstrate its effectiveness, we apply this method to two examples: the linearized, complex Ginzburg-Landau equation, and the two-dimensional fluid flow past a cylinder. As expected, reduced-order models computed using an analytic tail match or exceed the accuracy of those computed using the standard balanced POD procedure, at a fraction of the cost.

A simple mass-conserved level set method for simulation of multiphase flows

NASA Astrophysics Data System (ADS)

Yuan, H.-Z.; Shu, C.; Wang, Y.; Shu, S.

2018-04-01

In this paper, a modified level set method is proposed for simulation of multiphase flows with large density ratio and high Reynolds number. The present method simply introduces a source or sink term into the level set equation to compensate the mass loss or offset the mass increase. The source or sink term is derived analytically by applying the mass conservation principle with the level set equation and the continuity equation of flow field. Since only a source term is introduced, the application of the present method is as simple as the original level set method, but it can guarantee the overall mass conservation. To validate the present method, the vortex flow problem is first considered. The simulation results are compared with those from the original level set method, which demonstrates that the modified level set method has the capability of accurately capturing the interface and keeping the mass conservation. Then, the proposed method is further validated by simulating the Laplace law, the merging of two bubbles, a bubble rising with high density ratio, and Rayleigh-Taylor instability with high Reynolds number. Numerical results show that the mass is a well-conserved by the present method.

Simplified, inverse, ejector design tool

NASA Technical Reports Server (NTRS)

Dechant, Lawrence J.

1993-01-01

A simple lumped parameter based inverse design tool has been developed which provides flow path geometry and entrainment estimates subject to operational, acoustic, and design constraints. These constraints are manifested through specification of primary mass flow rate or ejector thrust, fully-mixed exit velocity, and static pressure matching. Fundamentally, integral forms of the conservation equations coupled with the specified design constraints are combined to yield an easily invertible linear system in terms of the flow path cross-sectional areas. Entrainment is computed by back substitution. Initial comparison with experimental and analogous one-dimensional methods show good agreement. Thus, this simple inverse design code provides an analytically based, preliminary design tool with direct application to High Speed Civil Transport (HSCT) design studies.

WHAEM: PROGRAM DOCUMENTATION FOR THE WELLHEAD ANALYTIC ELEMENT MODEL (EPA/600/SR-94/210)

EPA Science Inventory

A new computer program has been developed to determine time-of-travel capture zones in relatively simple geohydrological settings. The WhAEM package contains an analytic element model that uses superposition of (many) closed form analytical solutions to generate a groundwater flo...

Application of modified hollow fiber liquid phase microextraction in conjunction with chromatography-electron capture detection for quantification of acrylamide in waste water samples at ultra-trace levels.

PubMed

Sobhi, Hamid Reza; Ghambarian, Mahnaz; Behbahani, Mohammad; Esrafili, Ali

2017-03-03

Herein, a simple and sensitive method was successfully developed for the extraction and quantification of acrylamide in water samples. Initially, acrylamide was derivatized through a bromination process. Subsequently, a modified hollow-fiber liquid-phase microextraction was applied for the extraction of the brominated acrylamide from a 10-ml portion of an aqueous sample. Briefly, in this method, the derivatized acrylamide (2,3-dibromopropionamide) was extracted from the aqueous sample into a thin layer of an organic solvent sustained in pores of a porous hollow fiber. Then, it was back-extracted using a small volume of organic acceptor solution (acetonitril, 25μl) located inside the lumen of the hollow fiber followed by gas chromatography-electron capture detection (GC-ECD). The optimal conditions were examined for the extraction of the analyte such as: the organic solvent: dihexyl ether+10% tri-n-octyl phosphine oxide; stirring rate: 750rpm; no salt addition and 30min extraction time. These optimal extraction conditions allowed excellent enrichment factor values for the method. Enrichment factor, detection limit (S/N=3) and dynamic linear range of 60, 2ngL -1 and 50-1000ngL -1 to be determined for the analyte. The relative standard deviations (RSD%) representing precision of the method were in the range of 2.2-5.8 based on the average of three measurements. Accuracy of the method was tested by the relative recovery experiments on spiked samples, with results ranging from 93 to 108%. Finally, the method proved to be simple, rapid, and cost-effective for routine screen of acrylamide-contaminated highly-complicated untreated waste water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

A simple method for identifying parameter correlations in partially observed linear dynamic models.

PubMed

Li, Pu; Vu, Quoc Dong

2015-12-14

Parameter estimation represents one of the most significant challenges in systems biology. This is because biological models commonly contain a large number of parameters among which there may be functional interrelationships, thus leading to the problem of non-identifiability. Although identifiability analysis has been extensively studied by analytical as well as numerical approaches, systematic methods for remedying practically non-identifiable models have rarely been investigated. We propose a simple method for identifying pairwise correlations and higher order interrelationships of parameters in partially observed linear dynamic models. This is made by derivation of the output sensitivity matrix and analysis of the linear dependencies of its columns. Consequently, analytical relations between the identifiability of the model parameters and the initial conditions as well as the input functions can be achieved. In the case of structural non-identifiability, identifiable combinations can be obtained by solving the resulting homogenous linear equations. In the case of practical non-identifiability, experiment conditions (i.e. initial condition and constant control signals) can be provided which are necessary for remedying the non-identifiability and unique parameter estimation. It is noted that the approach does not consider noisy data. In this way, the practical non-identifiability issue, which is popular for linear biological models, can be remedied. Several linear compartment models including an insulin receptor dynamics model are taken to illustrate the application of the proposed approach. Both structural and practical identifiability of partially observed linear dynamic models can be clarified by the proposed method. The result of this method provides important information for experimental design to remedy the practical non-identifiability if applicable. The derivation of the method is straightforward and thus the algorithm can be easily implemented into a software packet.

Analysis of short-chain fatty acids in human feces: A scoping review.

PubMed

Primec, Maša; Mičetić-Turk, Dušanka; Langerholc, Tomaž

2017-06-01

Short-chain fatty acids (SCFAs) play a crucial role in maintaining homeostasis in humans, therefore the importance of a good and reliable SCFAs analytical detection has raised a lot in the past few years. The aim of this scoping review is to show the trends in the development of different methods of SCFAs analysis in feces, based on the literature published in the last eleven years in all major indexing databases. The search criteria included analytical quantification techniques of SCFAs in different human clinical and in vivo studies. SCFAs analysis is still predominantly performed using gas chromatography (GC), followed by high performance liquid chromatography (HPLC), nuclear magnetic resonance (NMR) and capillary electrophoresis (CE). Performances, drawbacks and advantages of these methods are discussed, especially in the light of choosing a proper pretreatment, as feces is a complex biological material. Further optimization to develop a simple, cost effective and robust method for routine use is needed. Copyright © 2017 Elsevier Inc. All rights reserved.

Simple and clean determination of tetracyclines by flow injection analysis

NASA Astrophysics Data System (ADS)

Rodríguez, Michael Pérez; Pezza, Helena Redigolo; Pezza, Leonardo

2016-01-01

An environmentally reliable analytical methodology was developed for direct quantification of tetracycline (TC) and oxytetracycline (OTC) using continuous flow injection analysis with spectrophotometric detection. The method is based on the diazo coupling reaction between the tetracyclines and diazotized sulfanilic acid in a basic medium, resulting in the formation of an intense orange azo compound that presents maximum absorption at 434 nm. Experimental design was used to optimize the analytical conditions. The proposed technique was validated over the concentration range of 1 to 40 μg mL- 1, and was successfully applied to samples of commercial veterinary pharmaceuticals. The detection (LOD) and quantification (LOQ) limits were 0.40 and 1.35 μg mL- 1, respectively. The samples were also analyzed by an HPLC method, and the results showed agreement with the proposed technique. The new flow injection method can be immediately used for quality control purposes in the pharmaceutical industry, facilitating monitoring in real time during the production processes of tetracycline formulations for veterinary use.

Platform construction and extraction mechanism study of magnetic mixed hemimicelles solid-phase extraction

NASA Astrophysics Data System (ADS)

Xiao, Deli; Zhang, Chan; He, Jia; Zeng, Rong; Chen, Rong; He, Hua

2016-12-01

Simple, accurate and high-throughput pretreatment method would facilitate large-scale studies of trace analysis in complex samples. Magnetic mixed hemimicelles solid-phase extraction has the power to become a key pretreatment method in biological, environmental and clinical research. However, lacking of experimental predictability and unsharpness of extraction mechanism limit the development of this promising method. Herein, this work tries to establish theoretical-based experimental designs for extraction of trace analytes from complex samples using magnetic mixed hemimicelles solid-phase extraction. We selected three categories and six sub-types of compounds for systematic comparative study of extraction mechanism, and comprehensively illustrated the roles of different force (hydrophobic interaction, π-π stacking interactions, hydrogen-bonding interaction, electrostatic interaction) for the first time. What’s more, the application guidelines for supporting materials, surfactants and sample matrix were also summarized. The extraction mechanism and platform established in the study render its future promising for foreseeable and efficient pretreatment under theoretical based experimental design for trace analytes from environmental, biological and clinical samples.

Determination of oxyfluorfen herbicide and oxyfluorfen amine residues in garbanzo beans by liquid chromatography.

PubMed

Zhou, M; Miles, C J

1991-01-01

Oxyfluorfen and oxyfluorfen amine were determined by liquid chromatography (LC) with ultraviolet (UV) and photoconductivity detection (PCD). A simple extraction procedure acceptably recovered both analytes from garbanzo beans over a wide range of fortifications (0.05 to 20 ppm) (83 +/- 4 for oxyfluorfen; 85 +/- 4 for oxyfluorfen amine). Percent recoveries decreased slightly as the fortification level decreased. Both analytes could be determined simultaneously at a concentration greater than 0.2 ppm in garbanzo beans. Detection limits were 3 ng for oxyfluorfen and 100 ng for oxyfluorfen amine using LC/UV, and 12 ng for both oxyfluorfen and oxyfluorfen amine with LC/PCD. Different knitted reaction coils and photoreactors were evaluated. Photoproduct yields and identification were determined by ion chromatography. The LC/PCD method measures oxyfluorfen and oxyfluorfen amine separately and has a shorter analysis time, while the standard method using gas chromatography measures total residues and is more sensitive.

Design a New Strategy Based on Nanoparticle-Enhanced Chemiluminescence Sensor Array for Biothiols Discrimination

NASA Astrophysics Data System (ADS)

Shahrajabian, Maryam; Hormozi-Nezhad, M. Reza

2016-08-01

Array-based sensor is an interesting approach that suggests an alternative to expensive analytical methods. In this work, we introduce a novel, simple, and sensitive nanoparticle-based chemiluminescence (CL) sensor array for discrimination of biothiols (e.g., cysteine, glutathione and glutathione disulfide). The proposed CL sensor array is based on the CL efficiencies of four types of enhanced nanoparticle-based CL systems. The intensity of CL was altered to varying degrees upon interaction with biothiols, producing unique CL response patterns. These distinct CL response patterns were collected as “fingerprints” and were then identified through chemometric methods, including linear discriminant analysis (LDA) and hierarchical cluster analysis (HCA). The developed array was able to successfully differentiate between cysteine, glutathione and glutathione disulfide in a wide concentration range. Moreover, it was applied to distinguish among the above analytes in human plasma.

From pixel to voxel: a deeper view of biological tissue by 3D mass spectral imaging

PubMed Central

Ye, Hui; Greer, Tyler; Li, Lingjun

2011-01-01

Three dimensional mass spectral imaging (3D MSI) is an exciting field that grants the ability to study a broad mass range of molecular species ranging from small molecules to large proteins by creating lateral and vertical distribution maps of select compounds. Although the general premise behind 3D MSI is simple, factors such as choice of ionization method, sample handling, software considerations and many others must be taken into account for the successful design of a 3D MSI experiment. This review provides a brief overview of ionization methods, sample preparation, software types and technological advancements driving 3D MSI research of a wide range of low- to high-mass analytes. Future perspectives in this field are also provided to conclude that the positive and promises ever-growing applications in the biomedical field with continuous developments of this powerful analytical tool. PMID:21320052

Numerics made easy: solving the Navier-Stokes equation for arbitrary channel cross-sections using Microsoft Excel.

PubMed

Richter, Christiane; Kotz, Frederik; Giselbrecht, Stefan; Helmer, Dorothea; Rapp, Bastian E

2016-06-01

The fluid mechanics of microfluidics is distinctively simpler than the fluid mechanics of macroscopic systems. In macroscopic systems effects such as non-laminar flow, convection, gravity etc. need to be accounted for all of which can usually be neglected in microfluidic systems. Still, there exists only a very limited selection of channel cross-sections for which the Navier-Stokes equation for pressure-driven Poiseuille flow can be solved analytically. From these equations, velocity profiles as well as flow rates can be calculated. However, whenever a cross-section is not highly symmetric (rectangular, elliptical or circular) the Navier-Stokes equation can usually not be solved analytically. In all of these cases, numerical methods are required. However, in many instances it is not necessary to turn to complex numerical solver packages for deriving, e.g., the velocity profile of a more complex microfluidic channel cross-section. In this paper, a simple spreadsheet analysis tool (here: Microsoft Excel) will be used to implement a simple numerical scheme which allows solving the Navier-Stokes equation for arbitrary channel cross-sections.

Steady-state groundwater recharge in trapezoidal-shaped aquifers: A semi-analytical approach based on variational calculus

NASA Astrophysics Data System (ADS)

Mahdavi, Ali; Seyyedian, Hamid

2014-05-01

This study presents a semi-analytical solution for steady groundwater flow in trapezoidal-shaped aquifers in response to an areal diffusive recharge. The aquifer is homogeneous, anisotropic and interacts with four surrounding streams of constant-head. Flow field in this laterally bounded aquifer-system is efficiently constructed by means of variational calculus. This is accomplished by minimizing a properly defined penalty function for the associated boundary value problem. Simple yet demonstrative scenarios are defined to investigate anisotropy effects on the water table variation. Qualitative examination of the resulting equipotential contour maps and velocity vector field illustrates the validity of the method, especially in the vicinity of boundary lines. Extension to the case of triangular-shaped aquifer with or without an impervious boundary line is also demonstrated through a hypothetical example problem. The present solution benefits from an extremely simple mathematical expression and exhibits strictly close agreement with the numerical results obtained from Modflow. Overall, the solution may be used to conduct sensitivity analysis on various hydrogeological parameters that affect water table variation in aquifers defined in trapezoidal or triangular-shaped domains.

PLS and first derivative of ratio spectra methods for determination of hydrochlorothiazide and propranolol hydrochloride in tablets.

PubMed

Vignaduzzo, Silvana E; Maggio, Rubén M; Castellano, Patricia M; Kaufman, Teodoro S

2006-12-01

Two new analytical methods have been developed as convenient and useful alternatives for simultaneous determination of hydrochlorothiazide (HCT) and propranolol hydrochloride (PRO) in pharmaceutical formulations. The methods are based on the first derivative of ratio spectra (DRS) and on partial least squares (PLS) analysis of the ultraviolet absorption spectra of the samples in the 250-350-nm region. The methods were calibrated between 8.7 and 16.0 mg L(-1) for HCT and between 14.0 and 51.5 mg L(-1) for PRO. An asymmetric full-factorial design and wavelength selection (277-294 nm for HCT and 297-319 for PRO) were used for the PLS method and signal intensities at 276 and 322 nm were used in the DRS method for HCT and PRO, respectively. Performance characteristics of the analytical methods were evaluated by use of validation samples and both methods showed to be accurate and precise, furnishing near quantitative analyte recoveries (100.4 and 99.3% for HCT and PRO by use of PLS) and relative standard deviations below 2%. For PLS the lower limits of quantification were 0.37 and 0.66 mg L(-1) for HCT and PRO, respectively, whereas for DRS they were 1.15 and 3.05 mg L(-1) for HCT and PRO, respectively. The methods were used for quantification of HCT and PRO in synthetic mixtures and in two commercial tablet preparations containing different proportions of the analytes. The results of the drug content assay and the tablet dissolution test were in statistical agreement (p < 0.05) with those furnished by the official procedures of the USP 29. Preparation of dissolution profiles of the combined tablet formulations was also performed with the aid of the proposed methods. The methods are easy to apply, use relatively simple equipment, require minimum sample pre-treatment, enable high sample throughput, and generate less solvent waste than other procedures.

Consistent Yokoya-Chen Approximation to Beamstrahlung(LCC-0010)

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

Peskin, M

2004-04-22

I reconsider the Yokoya-Chen approximate evolution equation for beamstrahlung and modify it slightly to generate simple, consistent analytical approximations for the electron and photon energy spectra. I compare these approximations to previous ones, and to simulation data.I reconsider the Yokoya-Chen approximate evolution equation for beamstrahlung and modify it slightly to generate simple, consistent analytical approximations for the electron and photon energy spectra. I compare these approximations to previous ones, and to simulation data.

Advanced Signal Processing Analysis of Laser-Induced Breakdown Spectroscopy Data for the Discrimination of Obsidian Sources

DTIC Science & Technology

2012-02-09

different sources [12,13], but the analytical techniques needed for such analysis (XRD, INAA , & ICP-MS) are time consuming and require expensive...partial least-squares discriminant analysis (PLSDA) that used the SIMPLS solving method [33]. In the experi- ment design, a leave-one-sample-out (LOSO) para...REPORT Advanced signal processing analysis of laser-induced breakdown spectroscopy data for the discrimination of obsidian sources 14. ABSTRACT 16

Autocatalytic polymerization generates persistent random walk of crawling cells.

PubMed

Sambeth, R; Baumgaertner, A

2001-05-28

The autocatalytic polymerization kinetics of the cytoskeletal actin network provides the basic mechanism for a persistent random walk of a crawling cell. It is shown that network remodeling by branching processes near the cell membrane is essential for the bimodal spatial stability of the network which induces a spontaneous breaking of isotropic cell motion. Details of the phenomena are analyzed using a simple polymerization model studied by analytical and simulation methods.

Selective detection of Co2+ by fluorescent nano probe: Diagnostic approach for analysis of environmental samples and biological activities

NASA Astrophysics Data System (ADS)

Mahajan, Prasad G.; Dige, Nilam C.; Desai, Netaji K.; Patil, Shivajirao R.; Kondalkar, Vijay V.; Hong, Seong-Karp; Lee, Ki Hwan

2018-06-01

Nowadays scientist over the world are engaging to put forth improved methods to detect metal ion in an aqueous medium based on fluorescence studies. A simple, selective and sensitive method was proposed for detection of Co2+ ion using fluorescent organic nanoparticles. We synthesized a fluorescent small molecule viz. 4,4‧-{benzene-1,4-diylbis-[(Z)methylylidenenitrilo]}dibenzoic acid (BMBA) to explore its suitability as sensor for Co2+ ion and biocompatibility in form of nanoparticles. Fluorescence nanoparticles (BMBANPs) prepared by simple reprecipitation method. Aggregation induced enhanced emission of BMBANPs exhibits the narrower particle size of 68 nm and sphere shape morphology. The selective fluorescence quenching was observed by addition of Co2+ and does not affected by presence of other coexisting ion solutions. The photo-physical properties, viz. UV-absorption, fluorescence emission, and lifetime measurements are in support of ligand-metal interaction followed by static fluorescence quenching phenomenon in emission of BMBANPs. Finally, we develop a simple analytical method for selective and sensitive determination of Co2+ ion in environmental samples. The cell culture E. coli, Bacillus sps., and M. tuberculosis H37RV strain in the vicinity of BMBANPs indicates virtuous anti-bacterial and anti-tuberculosis activity which is of additional novel application shown by prepared nanoparticles.

SUPRAMOLECULAR COMPOSITE MATERIALS FROM CELLULOSE, CHITOSAN AND CYCLODEXTRIN: FACILE PREPARATION AND THEIR SELECTIVE INCLUSION COMPLEX FORMATION WITH ENDOCRINE DISRUPTORS

PubMed Central

Duri, Simon; Tran, Chieu D.

2013-01-01

We have successfully developed a simple and one step method to prepare high performance supramolecular polysaccharide composites from cellulose (CEL), chitosan (CS) and (2,3,6-tri-O-acetyl)-α-, β- and γ-cyclodextrin (α-, β- and γ-TCD). In this method, [BMIm+Cl−], an ionic liquid (IL), was used as a solvent to dissolve and prepare the composites. Since majority (>88%) of the IL used was recovered for reuse, the method is recyclable. XRD, FT-IR, NIR and SEM were used to monitor the dissolution process and to confirm that the polysaccharides were regenerated without any chemical modifications. It was found that unique properties of each component including superior mechanical properties (from CEL), excellent adsorbent for pollutants and toxins (from CS) and size/structure selectivity through inclusion complex formation (from TCDs) remain intact in the composites. Specifically, results from kinetics and adsorption isotherms show that while CS-based composites can effectively adsorb the endocrine disruptors (polychlrophenols, bisphenol-A), its adsorption is independent on the size and structure of the analytes. Conversely, the adsorption by γ-TCD-based composites exhibits strong dependency on size and structure of the analytes. For example, while all three TCD-based composites (i.e., α-, β- and γ-TCD) can effectively adsorb 2-, 3- and 4-chlorophenol, only γ-TCD-based composite can adsorb analytes with bulky groups including 3,4-dichloro- and 2,4,5-trichlorophenol. Furthermore, equilibrium sorption capacities for the analytes with bulky groups by γ-TCD-based composite are much higher than those by CS-based composites. Together, these results indicate that γ-TCD-based composite with its relatively larger cavity size can readily form inclusion complexes with analytes with bulky groups, and through inclusion complex formation, it can strongly adsorb much more analytes and with size/structure selectivity compared to CS-based composites which can adsorb the analyte only by surface adsorption. PMID:23517477

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

PubMed Central

Lin, Chen-Yen; Halabi, Susan

2017-01-01

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

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

PubMed

Lin, Chen-Yen; Halabi, Susan

2017-01-01

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

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.

Simultaneous determination of nine β-lactam antibiotics in human plasma by an ultrafast hydrophilic-interaction chromatography-tandem mass spectrometry.

PubMed

Abdulla, Alan; Bahmany, Soma; Wijma, Rixt A; van der Nagel, Bart C H; Koch, Birgit C P

2017-08-15

Contemporary β-lactam antibiotic dosing is debatable in severely ill patients, since the occurrence of pathophysiological changes in critical illness can result in great inter-individual variability. Therapeutic drug monitoring (TDM) is a commonly used dosing strategy to optimize exposure and thereby minimize toxicity and maximize the efficacy. Currently, TDM of β-lactam antibiotics is rarely performed, due to poor availability in clinical practice. We describe an ultrafast Hydrophilic-Interaction Chromatography (HILIC) based UPLC-MS/MS method for the determination of amoxicillin, benzylpenicillin, cefotaxime, cefuroxime, ceftazidime, flucloxacillin, imipenem, meropenem and piperacillin in human plasma. This method involves simple sample preparation steps and was comprehensively validated according to standard FDA guidelines. For all analytes, mean accuracy and precision values were within the acceptance value. The lower and upper limits of quantification were found to be sufficient to cover the therapeutic range for all antibiotics. Finally, the method was successfully applied in a large pharmacokinetic study performed in the intensive care setting, and the feasibility of the analytical procedure was demonstrated in routine clinical practice. To the best of our knowledge, we report here the first HILIC-based UPLC-MS/MS assay for the determination of β-lactam antibiotics in human plasma. This simple, sensitive and ultrafast assay requires small-volume samples and can easily be implemented in clinical laboratories to promote the TDM of β-lactam antibiotics. Copyright © 2017 Elsevier B.V. All rights reserved.

Pharmaceutical supply chain risk assessment in Iran using analytic hierarchy process (AHP) and simple additive weighting (SAW) methods.

PubMed

Jaberidoost, Mona; Olfat, Laya; Hosseini, Alireza; Kebriaeezadeh, Abbas; Abdollahi, Mohammad; Alaeddini, Mahdi; Dinarvand, Rassoul

2015-01-01

Pharmaceutical supply chain is a significant component of the health system in supplying medicines, particularly in countries where main drugs are provided by local pharmaceutical companies. No previous studies exist assessing risks and disruptions in pharmaceutical companies while assessing the pharmaceutical supply chain. Any risks affecting the pharmaceutical companies could disrupt supply medicines and health system efficiency. The goal of this study was the risk assessment in pharmaceutical industry in Iran considering process's priority, hazard and probability of risks. The study was carried out in 4 phases; risk identification through literature review, risk identification in Iranian pharmaceutical companies through interview with experts, risk analysis through a questionnaire and consultation with experts using group analytic hierarchy process (AHP) method and rating scale (RS) and risk evaluation of simple additive weighting (SAW) method. In total, 86 main risks were identified in the pharmaceutical supply chain with perspective of pharmaceutical companies classified in 11 classes. The majority of risks described in this study were related to the financial and economic category. Also financial management was found to be the most important factor for consideration. Although pharmaceutical industry and supply chain were affected by current political conditions in Iran during the study time, but half of total risks in the pharmaceutical supply chain were found to be internal risks which could be fixed by companies, internally. Likewise, political status and related risks forced companies to focus more on financial and supply management resulting in less attention to quality management.

Development of a validated liquid chromatographic method for quantification of sorafenib tosylate in the presence of stress-induced degradation products and in biological matrix employing analytical quality by design approach.

PubMed

Sharma, Teenu; Khurana, Rajneet Kaur; Jain, Atul; Katare, O P; Singh, Bhupinder

2018-05-01

The current research work envisages an analytical quality by design-enabled development of a simple, rapid, sensitive, specific, robust and cost-effective stability-indicating reversed-phase high-performance liquid chromatographic method for determining stress-induced forced-degradation products of sorafenib tosylate (SFN). An Ishikawa fishbone diagram was constructed to embark upon analytical target profile and critical analytical attributes, i.e. peak area, theoretical plates, retention time and peak tailing. Factor screening using Taguchi orthogonal arrays and quality risk assessment studies carried out using failure mode effect analysis aided the selection of critical method parameters, i.e. mobile phase ratio and flow rate potentially affecting the chosen critical analytical attributes. Systematic optimization using response surface methodology of the chosen critical method parameters was carried out employing a two-factor-three-level-13-run, face-centered cubic design. A method operable design region was earmarked providing optimum method performance using numerical and graphical optimization. The optimum method employed a mobile phase composition consisting of acetonitrile and water (containing orthophosphoric acid, pH 4.1) at 65:35 v/v at a flow rate of 0.8 mL/min with UV detection at 265 nm using a C 18 column. Response surface methodology validation studies confirmed good efficiency and sensitivity of the developed method for analysis of SFN in mobile phase as well as in human plasma matrix. The forced degradation studies were conducted under different recommended stress conditions as per ICH Q1A (R2). Mass spectroscopy studies showed that SFN degrades in strongly acidic, alkaline and oxidative hydrolytic conditions at elevated temperature, while the drug was per se found to be photostable. Oxidative hydrolysis using 30% H 2 O 2 showed maximum degradation with products at retention times of 3.35, 3.65, 4.20 and 5.67 min. The absence of any significant change in the retention time of SFN and degradation products, formed under different stress conditions, ratified selectivity and specificity of the systematically developed method. Copyright © 2017 John Wiley & Sons, Ltd.

Development and validation of a rapid LC-MS/MS method for simultaneous determination of netupitant and palonosetron in human plasma and its application to a pharmacokinetic study.

PubMed

Xu, Mingzhen; Ni, Yang; Li, Shihong; Du, Juan; Li, Huqun; Zhou, Ying; Li, Weiyong; Chen, Hui

2016-08-01

A simple liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was firstly developed and validated for simultaneous determination of netupitant and palonosetron in human plasma using ibrutinib as the internal standard (IS). Following liquid-liquid extraction, the compounds were eluted isocratically on a Phenomenex C18 column (50mm×2.0mm, 3μm) with the mobile phase consisting of acetonitrile and 10mM ammonium acetate buffer (pH 9.0) (89:11, v/v) at the flow rate of 0.3mL/min. The monitored ion transitions were m/z 579.5→522.4 for netupitant, m/z 297.3→110.2 for palonosetron and m/z 441.2→138.1 for IS. Chromatographic run time was 2.5min per injection, which made it possible to analyze more than 300 of samples per day. The assay exhibited a linear dynamic range of 5-1000ng/mL for netupitant and 0.02-10ng/mL for palonosetron in plasma. The values for both within- and between-day precision and accuracy were well within the generally accepted criteria for analytical methods (<15%). Selectivity, linearity, lower limit of quantification (LLOQ), accuracy, precision, stability, matrix effect, recovery and carry-over effect were evaluated for all analytes. The method is simple, rapid, and has been applied successfully to a pharmacokinetic study of netupitant and palonosetron in healthy volunteers. Copyright © 2016 Elsevier B.V. All rights reserved.

Entanglement transitions induced by large deviations

NASA Astrophysics Data System (ADS)

Bhosale, Udaysinh T.

2017-12-01

The probability of large deviations of the smallest Schmidt eigenvalue for random pure states of bipartite systems, denoted as A and B , is computed analytically using a Coulomb gas method. It is shown that this probability, for large N , goes as exp[-β N2Φ (ζ ) ] , where the parameter β is the Dyson index of the ensemble, ζ is the large deviation parameter, while the rate function Φ (ζ ) is calculated exactly. Corresponding equilibrium Coulomb charge density is derived for its large deviations. Effects of the large deviations of the extreme (largest and smallest) Schmidt eigenvalues on the bipartite entanglement are studied using the von Neumann entropy. Effect of these deviations is also studied on the entanglement between subsystems 1 and 2, obtained by further partitioning the subsystem A , using the properties of the density matrix's partial transpose ρ12Γ. The density of states of ρ12Γ is found to be close to the Wigner's semicircle law with these large deviations. The entanglement properties are captured very well by a simple random matrix model for the partial transpose. The model predicts the entanglement transition across a critical large deviation parameter ζ . Log negativity is used to quantify the entanglement between subsystems 1 and 2. Analytical formulas for it are derived using the simple model. Numerical simulations are in excellent agreement with the analytical results.

Entanglement transitions induced by large deviations.

PubMed

Bhosale, Udaysinh T

2017-12-01

The probability of large deviations of the smallest Schmidt eigenvalue for random pure states of bipartite systems, denoted as A and B, is computed analytically using a Coulomb gas method. It is shown that this probability, for large N, goes as exp[-βN^{2}Φ(ζ)], where the parameter β is the Dyson index of the ensemble, ζ is the large deviation parameter, while the rate function Φ(ζ) is calculated exactly. Corresponding equilibrium Coulomb charge density is derived for its large deviations. Effects of the large deviations of the extreme (largest and smallest) Schmidt eigenvalues on the bipartite entanglement are studied using the von Neumann entropy. Effect of these deviations is also studied on the entanglement between subsystems 1 and 2, obtained by further partitioning the subsystem A, using the properties of the density matrix's partial transpose ρ_{12}^{Γ}. The density of states of ρ_{12}^{Γ} is found to be close to the Wigner's semicircle law with these large deviations. The entanglement properties are captured very well by a simple random matrix model for the partial transpose. The model predicts the entanglement transition across a critical large deviation parameter ζ. Log negativity is used to quantify the entanglement between subsystems 1 and 2. Analytical formulas for it are derived using the simple model. Numerical simulations are in excellent agreement with the analytical results.

Fracture mechanics life analytical methods verification testing

NASA Technical Reports Server (NTRS)

Favenesi, J. A.; Clemmons, T. G.; Lambert, T. J.

1994-01-01

Verification and validation of the basic information capabilities in NASCRAC has been completed. The basic information includes computation of K versus a, J versus a, and crack opening area versus a. These quantities represent building blocks which NASCRAC uses in its other computations such as fatigue crack life and tearing instability. Several methods were used to verify and validate the basic information capabilities. The simple configurations such as the compact tension specimen and a crack in a finite plate were verified and validated versus handbook solutions for simple loads. For general loads using weight functions, offline integration using standard FORTRAN routines was performed. For more complicated configurations such as corner cracks and semielliptical cracks, NASCRAC solutions were verified and validated versus published results and finite element analyses. A few minor problems were identified in the basic information capabilities of the simple configurations. In the more complicated configurations, significant differences between NASCRAC and reference solutions were observed because NASCRAC calculates its solutions as averaged values across the entire crack front whereas the reference solutions were computed for a single point.

The transfer of analytical procedures.

PubMed

Ermer, J; Limberger, M; Lis, K; Wätzig, H

2013-11-01

Analytical method transfers are certainly among the most discussed topics in the GMP regulated sector. However, they are surprisingly little regulated in detail. General information is provided by USP, WHO, and ISPE in particular. Most recently, the EU emphasized the importance of analytical transfer by including it in their draft of the revised GMP Guideline. In this article, an overview and comparison of these guidelines is provided. The key to success for method transfers is the excellent communication between sending and receiving unit. In order to facilitate this communication, procedures, flow charts and checklists for responsibilities, success factors, transfer categories, the transfer plan and report, strategies in case of failed transfers, tables with acceptance limits are provided here, together with a comprehensive glossary. Potential pitfalls are described such that they can be avoided. In order to assure an efficient and sustainable transfer of analytical procedures, a practically relevant and scientifically sound evaluation with corresponding acceptance criteria is crucial. Various strategies and statistical tools such as significance tests, absolute acceptance criteria, and equivalence tests are thoroughly descibed and compared in detail giving examples. Significance tests should be avoided. The success criterion is not statistical significance, but rather analytical relevance. Depending on a risk assessment of the analytical procedure in question, statistical equivalence tests are recommended, because they include both, a practically relevant acceptance limit and a direct control of the statistical risks. However, for lower risk procedures, a simple comparison of the transfer performance parameters to absolute limits is also regarded as sufficient. Copyright © 2013 Elsevier B.V. All rights reserved.

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.

Streamflow variability and optimal capacity of run-of-river hydropower plants

NASA Astrophysics Data System (ADS)

Basso, S.; Botter, G.

2012-10-01

The identification of the capacity of a run-of-river plant which allows for the optimal utilization of the available water resources is a challenging task, mainly because of the inherent temporal variability of river flows. This paper proposes an analytical framework to describe the energy production and the economic profitability of small run-of-river power plants on the basis of the underlying streamflow regime. We provide analytical expressions for the capacity which maximize the produced energy as a function of the underlying flow duration curve and minimum environmental flow requirements downstream of the plant intake. Similar analytical expressions are derived for the capacity which maximize the economic return deriving from construction and operation of a new plant. The analytical approach is applied to a minihydro plant recently proposed in a small Alpine catchment in northeastern Italy, evidencing the potential of the method as a flexible and simple design tool for practical application. The analytical model provides useful insight on the major hydrologic and economic controls (e.g., streamflow variability, energy price, costs) on the optimal plant capacity and helps in identifying policy strategies to reduce the current gap between the economic and energy optimizations of run-of-river plants.

Numerical solutions to the time-dependent Bloch equations revisited.

PubMed

Murase, Kenya; Tanki, Nobuyoshi

2011-01-01

The purpose of this study was to demonstrate a simple and fast method for solving the time-dependent Bloch equations. First, the time-dependent Bloch equations were reduced to a homogeneous linear differential equation, and then a simple equation was derived to solve it using a matrix operation. The validity of this method was investigated by comparing with the analytical solutions in the case of constant radiofrequency irradiation. There was a good agreement between them, indicating the validity of this method. As a further example, this method was applied to the time-dependent Bloch equations in the two-pool exchange model for chemical exchange saturation transfer (CEST) or amide proton transfer (APT) magnetic resonance imaging (MRI), and the Z-spectra and asymmetry spectra were calculated from their solutions. They were also calculated using the fourth/fifth-order Runge-Kutta-Fehlberg (RKF) method for comparison. There was also a good agreement between them, and this method was much faster than the RKF method. In conclusion, this method will be useful for analyzing the complex CEST or APT contrast mechanism and/or investigating the optimal conditions for CEST or APT MRI. Copyright © 2011 Elsevier Inc. All rights reserved.

A Green Analytical Method Using Ultrasound in Sample Preparation for the Flow Injection Determination of Iron, Manganese, and Zinc in Soluble Solid Samples by Flame Atomic Absorption Spectrometry

PubMed Central

Yebra, M. Carmen

2012-01-01

A simple and rapid analytical method was developed for the determination of iron, manganese, and zinc in soluble solid samples. The method is based on continuous ultrasonic water dissolution of the sample (5–30 mg) at room temperature followed by flow injection flame atomic absorption spectrometric determination. A good precision of the whole procedure (1.2–4.6%) and a sample throughput of ca. 25 samples h–1 were obtained. The proposed green analytical method has been successfully applied for the determination of iron, manganese, and zinc in soluble solid food samples (soluble cocoa and soluble coffee) and pharmaceutical preparations (multivitamin tablets). The ranges of concentrations found were 21.4–25.61 μg g−1 for iron, 5.74–18.30 μg g−1 for manganese, and 33.27–57.90 μg g−1 for zinc in soluble solid food samples and 3.75–9.90 μg g−1 for iron, 0.47–5.05 μg g−1 for manganese, and 1.55–15.12 μg g−1 for zinc in multivitamin tablets. The accuracy of the proposed method was established by a comparison with the conventional wet acid digestion method using a paired t-test, indicating the absence of systematic errors. PMID:22567553

Selective and rapid determination of tadalafil and finasteride using solid phase extraction by high performance liquid chromatography and tandem mass spectrometry.

PubMed

Pappula, Nagaraju; Kodali, Balaji; Datla, Peda Varma

2018-04-15

Highly selective and fast liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed and validated for simultaneous determination of tadalafil (TDL) and finasteride (FNS) in human plasma. The method was successfully applied for analysis of TDL and FNS samples in clinical study. The method was validated as per USFDA (United States Food and Drug Administration), EMA (European Medicines Agency), and ANVISA (Agência Nacional de Vigilância Sanitária-Brazil) bio analytical method validation guidelines. Glyburide (GLB) was used as common internal standard (ISTD) for both analytes. The selected multiple reaction monitoring (MRM) transitions for mass spectrometric analysis were m/z 390.2/268.2, m/z 373.3/305.4 and m/z 494.2/369.1 for TDL, FNS and ISTD respectively. The extraction of analytes and ISTD was accomplished by a simple solid phase extraction (SPE) procedure. Rapid analysis time was achieved on Zorbax Eclipse C18 column (50 × 4.6 mm, 5 μm). The calibration ranges for TDL and FNS were 5-800 ng/ml and 0.2-30 ng/ml respectively. The results of precision and accuracy, linearity, recovery and matrix effect of the method are acceptable. The accuracy was in the range of 92.9%-106.4% and method precision was also good; %CV was less than 8.1%. Copyright © 2018 Elsevier B.V. All rights reserved.

Test of a potential link between analytic and nonanalytic category learning and automatic, effortful processing.

PubMed

Tracy, J I; Pinsk, M; Helverson, J; Urban, G; Dietz, T; Smith, D J

2001-08-01

The link between automatic and effortful processing and nonanalytic and analytic category learning was evaluated in a sample of 29 college undergraduates using declarative memory, semantic category search, and pseudoword categorization tasks. Automatic and effortful processing measures were hypothesized to be associated with nonanalytic and analytic categorization, respectively. Results suggested that contrary to prediction strong criterion-attribute (analytic) responding on the pseudoword categorization task was associated with strong automatic, implicit memory encoding of frequency-of-occurrence information. Data are discussed in terms of the possibility that criterion-attribute category knowledge, once established, may be expressed with few attentional resources. The data indicate that attention resource requirements, even for the same stimuli and task, vary depending on the category rule system utilized. Also, the automaticity emerging from familiarity with analytic category exemplars is very different from the automaticity arising from extensive practice on a semantic category search task. The data do not support any simple mapping of analytic and nonanalytic forms of category learning onto the automatic and effortful processing dichotomy and challenge simple models of brain asymmetries for such procedures. Copyright 2001 Academic Press.

Characterization and modeling of an advanced flexible thermal protection material for space applications

NASA Technical Reports Server (NTRS)

Clayton, Joseph P.; Tinker, Michael L.

1991-01-01

This paper describes experimental and analytical characterization of a new flexible thermal protection material known as Tailorable Advanced Blanket Insulation (TABI). This material utilizes a three-dimensional ceramic fabric core structure and an insulation filler. TABI is the leading candidate for use in deployable aeroassisted vehicle designs. Such designs require extensive structural modeling, and the most significant in-plane material properties necessary for model development are measured and analytically verified in this study. Unique test methods are developed for damping measurements. Mathematical models are developed for verification of the experimental modulus and damping data, and finally, transverse properties are described in terms of the inplane properties through use of a 12-dof finite difference model of a simple TABI configuration.

Quantitative Detection of Nucleoside Analogues by Multi-enzyme Biosensors using Time-Resolved Kinetic Measurements.

PubMed

Muthu, Pravin; Lutz, Stefan

2016-04-05

Fast, simple and cost-effective methods for detecting and quantifying pharmaceutical agents in patients are highly sought after to replace equipment and labor-intensive analytical procedures. The development of new diagnostic technology including portable detection devices also enables point-of-care by non-specialists in resource-limited environments. We have focused on the detection and dose monitoring of nucleoside analogues used in viral and cancer therapies. Using deoxyribonucleoside kinases (dNKs) as biosensors, our chemometric model compares observed time-resolved kinetics of unknown analytes to known substrate interactions across multiple enzymes. The resulting dataset can simultaneously identify and quantify multiple nucleosides and nucleoside analogues in complex sample mixtures. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Stability analysis of magnetized neutron stars - a semi-analytic approach

NASA Astrophysics Data System (ADS)

Herbrik, Marlene; Kokkotas, Kostas D.

2017-04-01

We implement a semi-analytic approach for stability analysis, addressing the ongoing uncertainty about stability and structure of neutron star magnetic fields. Applying the energy variational principle, a model system is displaced from its equilibrium state. The related energy density variation is set up analytically, whereas its volume integration is carried out numerically. This facilitates the consideration of more realistic neutron star characteristics within the model compared to analytical treatments. At the same time, our method retains the possibility to yield general information about neutron star magnetic field and composition structures that are likely to be stable. In contrast to numerical studies, classes of parametrized systems can be studied at once, finally constraining realistic configurations for interior neutron star magnetic fields. We apply the stability analysis scheme on polytropic and non-barotropic neutron stars with toroidal, poloidal and mixed fields testing their stability in a Newtonian framework. Furthermore, we provide the analytical scheme for dropping the Cowling approximation in an axisymmetric system and investigate its impact. Our results confirm the instability of simple magnetized neutron star models as well as a stabilization tendency in the case of mixed fields and stratification. These findings agree with analytical studies whose spectrum of model systems we extend by lifting former simplifications.

Compensation for matrix effects in the gas chromatography-mass spectrometry analysis of 186 pesticides in tea matrices using analyte protectants.

PubMed

Li, Yan; Chen, Xi; Fan, Chunlin; Pang, Guofang

2012-11-30

A gas chromatography-mass spectrometry (GC-MS) analytical method was developed for simultaneously determining 186 pesticides in tea matrices using analyte protectants to counteract the matrix-induced effect. The matrix effects were evaluated for green, oolong and black tea, representing unfermented, partially fermented and completely fermented teas respectively and depending on the type of tea, 72%, 94% and 94% of the pesticides presented strong response enhancement effect. Several analyte protectants as well as certain combinations of these protectants were evaluated to check their compensation effects. A mixture of triglycerol and d-ribonic acid-γ-lactone (both at 2mg/mL in the injected samples) was found to be the most effective in improving the chromatographic behavior of the 186 pesticides. More than 96% of the 186 pesticides achieved recoveries within the range of 70-120% when using the selected mixture of analyte protectants. The simple addition of analyte protectants offers a more convenient solution to overcome matrix effects, results in less active sites compared to matrix-matched standardization and can be an effective approach to compensate for matrix effects in the GC-MS analysis of pesticide residues. Copyright © 2012 Elsevier B.V. All rights reserved.

Testing and Validation of the Dynamic Inertia Measurement Method

NASA Technical Reports Server (NTRS)

Chin, Alexander W.; Herrera, Claudia Y.; Spivey, Natalie D.; Fladung, William A.; Cloutier, David

2015-01-01

The Dynamic Inertia Measurement (DIM) method uses a ground vibration test setup to determine the mass properties of an object using information from frequency response functions. Most conventional mass properties testing involves using spin tables or pendulum-based swing tests, which for large aerospace vehicles becomes increasingly difficult and time-consuming, and therefore expensive, to perform. The DIM method has been validated on small test articles but has not been successfully proven on large aerospace vehicles. In response, the National Aeronautics and Space Administration Armstrong Flight Research Center (Edwards, California) conducted mass properties testing on an "iron bird" test article that is comparable in mass and scale to a fighter-type aircraft. The simple two-I-beam design of the "iron bird" was selected to ensure accurate analytical mass properties. Traditional swing testing was also performed to compare the level of effort, amount of resources, and quality of data with the DIM method. The DIM test showed favorable results for the center of gravity and moments of inertia; however, the products of inertia showed disagreement with analytical predictions.

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

PubMed

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

2014-09-15

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

Enantioresolution of (RS)-baclofen by liquid chromatography: A review.

PubMed

Batra, Sonika; Bhushan, Ravi

2017-01-01

Baclofen is a commonly used racemic drug and has a simple chemical structure in terms of the presence of only one stereogenic center. Since the desirable pharmacological effect is in only one enantiomer, several possibilities exist for the other enantiomer for evaluation of the disposition of the racemic mixture of the drug. This calls for the development of enantioselective analytical methodology. This review summarizes and evaluates different methods of enantioseparation of (RS)-baclofen using both direct and indirect approaches, application of certain chiral reagents and chiral stationary phases (though very expensive). Methods of separation of diastereomers of (RS)-baclofen prepared with different chiral derivatizing reagents (under microwave irradiation at ease and in less time) on reversed-phase achiral columns or via a ligand exchange approach providing high-sensitivity detection by the relatively less expensive methods of TLC and HPLC are discussed. The methods may be helpful for determination of enantiomers in biological samples and in pharmaceutical formulations for control of enantiomeric purity and can be practiced both in analytical laboratories and industry for routine analysis and R&D activities. Copyright © 2016 John Wiley & Sons, Ltd.

A microanalytical method for ammonium and short-chain primary aliphatic amines using precolumn derivatization and capillary liquid chromatography.

PubMed

Moliner-Martínez, Y; Herráez-Hernández, R; Campíns-Falcó, P

2007-09-14

A new microscale method is presented for the determination of ammonium and primary short-chain aliphatic amines (methylamine, ethylamine, propylamine, n-butylamine and n-pentylamine) in water. The assay uses precolumn derivatization with the reagent o-phthaldialdehyde (OPA) in combination with the thiol N-acetyl-L-cysteine (NAC), and capillary liquid chromatography with UV detection at 330 nm. The described method is very simple and rapid as no preconcentration of the analytes is necessary, and the volume of sample required is only 0.1 mL. Under the proposed conditions good linearity has been obtained up to a concentration of the analytes of 10.0 mgL(-1), the limits of detection being of 8-50 microgL(-1). No matrix effect was found, and recoveries between 97 and 110% were obtained. The precision of the method was good, and the achieved variation coefficients were below 12%. The reliability of the proposed approach has been tested by analyzing a microsample of fogwater collected from leaf surfaces.

Solvent signal suppression for high-resolution MAS-DNP

NASA Astrophysics Data System (ADS)

Lee, Daniel; Chaudhari, Sachin R.; De Paëpe, Gaël

2017-05-01

Dynamic nuclear polarization (DNP) has become a powerful tool to substantially increase the sensitivity of high-field magic angle spinning (MAS) solid-state NMR experiments. The addition of dissolved hyperpolarizing agents usually results in the presence of solvent signals that can overlap and obscure those of interest from the analyte. Here, two methods are proposed to suppress DNP solvent signals: a Forced Echo Dephasing experiment (FEDex) and TRAnsfer of Populations in DOuble Resonance Echo Dephasing (TRAPDORED) NMR. These methods reintroduce a heteronuclear dipolar interaction that is specific to the solvent, thereby forcing a dephasing of recoupled solvent spins and leaving acquired NMR spectra free of associated resonance overlap with the analyte. The potency of these methods is demonstrated on sample types common to MAS-DNP experiments, namely a frozen solution (of L-proline) and a powdered solid (progesterone), both containing deuterated glycerol as a DNP solvent. The proposed methods are efficient, simple to implement, compatible with other NMR experiments, and extendable past spectral editing for just DNP solvents. The sensitivity gains from MAS-DNP in conjunction with FEDex or TRAPDORED then permits rapid and uninterrupted sample analysis.

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

NASA Astrophysics Data System (ADS)

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

2014-09-01

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

Properties of vapor detector arrays formed through plasticization of carbon black-organic polymer composites.

PubMed

Koscho, Michael E; Grubbs, Robert H; Lewis, Nathan S

2002-03-15

Arrays of vapor detectors have been formed through addition of varying mass fractions of the plasticizer diethylene glycol dibenzoate to carbon black-polymer composites of poly(vinyl acetate) (PVAc) or of poly(N-vinylpyrrolidone). Addition of plasticizer in 5% mass fraction increments produced 20 compositionally different detectors from each polymer composite. Differences in vapor sorption and permeability that effected changes in the dc electrical resistance response of these compositionally different detectors allowed identification and classification of various test analytes using standard chemometric methods. Glass transition temperatures, Tg, were measured using differential scanning calorimetry for plasticized polymers having a mass fraction of 0, 0.10, 0.20, 0.30, 0.40, or 0.50 of plasticizer in the composite. The plasticized PVAc composites with Tg < 25 degrees C showed rapid responses at room temperature to all of the test analyte vapors studied in this work, whereas composites with Tg > 25 degrees C showed response times that were highly dependent on the polymer/analyte combination. These composites showed a discontinuity in the temperature dependence of their resistance, and this discontinuity provided a simple method for determining the Tg of the composite and for determining the temperature or plasticizer mass fraction above which rapid resistance responses could be obtained for all members of the test set of analyte vapors. The plasticization approach provides a method for achieving rapid detector response times as well as for producing a large number of chemically different vapor detectors from a limited number of initial chemical feedstocks.

Direct ultrasonic agitation for rapid extraction of organic matter from airborne particulate.

PubMed

Lee, S C; Zou, S C; Ho, K F; Chan, L Y

2001-01-02

Direct ultrasonic extraction (DUE) is proposed as simple and rapid sample pretreatment method. This new approach is applied to the extraction of particulate organic matter (POM) from airborne particulate by using dichloromethane (DCM) or DCM/methanol (90/10, v/v) as extractant. The analytical determination was carried out by weighing the extractable POM on an electrobalance. Total recovery for POM could be obtained when the sample was extracted three times with 25-50 mL extractant each for about 5 min at 50 W ultrasonic power. In comparison with conventional Soxhlet extraction, less extraction time (total 15 min only) and solvent consumption (100 mL) were required by DUE. The efficiency of the DUE was similar or even higher than the routine Soxhlet method. Additionally, the new extractor is very simple and easy to use and can accelerate the extraction procedures of organic components from various solid samples.

A simple LC/MRM-MS-based method to quantify free linker-payload in antibody-drug conjugate preparations.

PubMed

Zmolek, Wesley; Bañas, Stefanie; Barfield, Robyn M; Rabuka, David; Drake, Penelope M

2016-10-01

Antibody-drug conjugates represent a growing class of biologic drugs that use the targeted specificity of an antibody to direct the localization of a small molecule drug, often a cytotoxic payload. After conjugation, antibody-drug conjugate preparations typically retain a residual amount of free (unconjugated) linker-payload. Monitoring this free small molecule drug component is important due to the potential for free payload to mediate unintended (off-target) toxicity. We developed a simple RP-HPLC/MRM-MS-based assay that can be rapidly employed to quantify free linker-payload. The method uses low sample volumes and offers an LLOQ of 10nM with 370pg on column. This analytical approach was used to monitor free linker-payload removal during optimization of the tangential flow filtration manufacturing step. Copyright © 2016 Elsevier B.V. All rights reserved.

Crack Path Selection in Thermally Loaded Borosilicate/Steel Bibeam Specimen

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

Grutzik, Scott Joseph; Reedy, Jr., E. D.

Here, we have developed a novel specimen for studying crack paths in glass. Under certain conditions, the specimen reaches a state where the crack must select between multiple paths satisfying the K II = 0 condition. This path selection is a simple but challenging benchmark case for both analytical and numerical methods of predicting crack propagation. We document the development of the specimen, using an uncracked and instrumented test case to study the effect of adhesive choice and validate the accuracy of both a simple beam theory model and a finite element model. In addition, we present preliminary fracture testmore » results and provide a comparison to the path predicted by two numerical methods (mesh restructuring and XFEM). The directional stability of the crack path and differences in kink angle predicted by various crack kinking criteria is analyzed with a finite element model.« less

Capacitive touch sensing : signal and image processing algorithms

NASA Astrophysics Data System (ADS)

Baharav, Zachi; Kakarala, Ramakrishna

2011-03-01

Capacitive touch sensors have been in use for many years, and recently gained center stage with the ubiquitous use in smart-phones. In this work we will analyze the most common method of projected capacitive sensing, that of absolute capacitive sensing, together with the most common sensing pattern, that of diamond-shaped sensors. After a brief introduction to the problem, and the reasons behind its popularity, we will formulate the problem as a reconstruction from projections. We derive analytic solutions for two simple cases: circular finger on a wire grid, and square finger on a square grid. The solutions give insight into the ambiguities of finding finger location from sensor readings. The main contribution of our paper is the discussion of interpolation algorithms including simple linear interpolation , curve fitting (parabolic and Gaussian), filtering, general look-up-table, and combinations thereof. We conclude with observations on the limits of the present algorithmic methods, and point to possible future research.

Crack Path Selection in Thermally Loaded Borosilicate/Steel Bibeam Specimen

DOE PAGES

Grutzik, Scott Joseph; Reedy, Jr., E. D.

2017-08-04

Here, we have developed a novel specimen for studying crack paths in glass. Under certain conditions, the specimen reaches a state where the crack must select between multiple paths satisfying the K II = 0 condition. This path selection is a simple but challenging benchmark case for both analytical and numerical methods of predicting crack propagation. We document the development of the specimen, using an uncracked and instrumented test case to study the effect of adhesive choice and validate the accuracy of both a simple beam theory model and a finite element model. In addition, we present preliminary fracture testmore » results and provide a comparison to the path predicted by two numerical methods (mesh restructuring and XFEM). The directional stability of the crack path and differences in kink angle predicted by various crack kinking criteria is analyzed with a finite element model.« less

Development of a rapid, simple and sensitive HPLC-FLD method for determination of rhodamine B in chili-containing products.

PubMed

Qi, Ping; Lin, Zhihao; Li, Jiaxu; Wang, ChengLong; Meng, WeiWei; Hong, Hong; Zhang, Xuewu

2014-12-01

In this work, a simple, rapid and sensitive analytical method for the determination of rhodamine B in chili-containing foodstuffs is described. The dye is extracted from samples with methanol and analysed without further cleanup procedure by high-performance liquid chromatography (HPLC) coupled to fluorescence detection (FLD). The influence of matrix fluorescent compounds (capsaicin and dihydrocapsaicin) on the analysis was overcome by the optimisation of mobile-phase composition. The limit of determination (LOD) and limit of quantification (LOQ) were 3.7 and 10 μg/kg, respectively. Validation data show a good repeatability and within-lab reproducibility with relative standard deviations <10%. The overall recoveries are in the range of 98-103% in chili powder and in the range of 87-100% in chili oil depending on the concentration of rhodamine B in foodstuffs. This method is suitable for the routine analysis of rhodamine B due to its sensitivity, simplicity, reasonable time and cost. Copyright © 2014 Elsevier Ltd. All rights reserved.

Simultaneous determination of dextromethorphan HBr and bromhexine HCl in tablets by first-derivative spectrophotometry.

PubMed

Tantishaiyakul, V; Poeaknapo, C; Sribun, P; Sirisuppanon, K

1998-06-01

A rapid, simple and direct assay procedure based on first-derivative spectrophotometry, using a zero-crossing and peak-to-base measurement at 234 and 324 nm, respectively, has been developed for the specific determination of dextromethorphan HBr and bromhexine HCl in tablets. Calibration graphs were linear with the correlation coefficients of 0.9999 for both analytes. The limit of detections were 0.033 and 0.103 microgram ml-1 for dextromethorphan HBr and bromhexine HCl, respectively. A HPLC method has been developed as the reference method. The results obtained by the first-derivative spectrophotometry were in good agreement with those found by the HPLC method.

Manipulators with flexible links: A simple model and experiments

NASA Technical Reports Server (NTRS)

Shimoyama, Isao; Oppenheim, Irving J.

1989-01-01

A simple dynamic model proposed for flexible links is briefly reviewed and experimental control results are presented for different flexible systems. A simple dynamic model is useful for rapid prototyping of manipulators and their control systems, for possible application to manipulator design decisions, and for real time computation as might be applied in model based or feedforward control. Such a model is proposed, with the further advantage that clear physical arguments and explanations can be associated with its simplifying features and with its resulting analytical properties. The model is mathematically equivalent to Rayleigh's method. Taking the example of planar bending, the approach originates in its choice of two amplitude variables, typically chosen as the link end rotations referenced to the chord (or the tangent) motion of the link. This particular choice is key in establishing the advantageous features of the model, and it was used to support the series of experiments reported.

SERS-based pesticide detection by using nanofinger sensors

NASA Astrophysics Data System (ADS)

Kim, Ansoon; Barcelo, Steven J.; Li, Zhiyong

2015-01-01

Simple, sensitive, and rapid detection of trace levels of extensively used and highly toxic pesticides are in urgent demand for public health. Surface-enhanced Raman scattering (SERS)-based sensor was designed to achieve ultrasensitive and simple pesticide sensing. We developed a portable sensor system composed of high performance and reliable gold nanofinger sensor strips and a custom-built portable Raman spectrometer. Compared to the general procedure and previously reported studies that are limited to laboratory settings, our analytical method is simple, sensitive, rapid, and cost-effective. Based on the SERS results, the chemical interaction of two pesticides, chlorpyrifos (CPF) and thiabendazole (TBZ), with gold nanofingers was studied to determine a fingerprint for each pesticide. The portable SERS-sensor system was successfully demonstrated to detect CPF and TBZ pesticides within 15 min with a detection limit of 35 ppt in drinking water and 7 ppb on apple skin, respectively.

The Role of Nanoparticle Design in Determining Analytical Performance of Lateral Flow Immunoassays.

PubMed

Zhan, Li; Guo, Shuang-Zhuang; Song, Fayi; Gong, Yan; Xu, Feng; Boulware, David R; McAlpine, Michael C; Chan, Warren C W; Bischof, John C

2017-12-13

Rapid, simple, and cost-effective diagnostics are needed to improve healthcare at the point of care (POC). However, the most widely used POC diagnostic, the lateral flow immunoassay (LFA), is ∼1000-times less sensitive and has a smaller analytical range than laboratory tests, requiring a confirmatory test to establish truly negative results. Here, a rational and systematic strategy is used to design the LFA contrast label (i.e., gold nanoparticles) to improve the analytical sensitivity, analytical detection range, and antigen quantification of LFAs. Specifically, we discovered that the size (30, 60, or 100 nm) of the gold nanoparticles is a main contributor to the LFA analytical performance through both the degree of receptor interaction and the ultimate visual or thermal contrast signals. Using the optimal LFA design, we demonstrated the ability to improve the analytical sensitivity by 256-fold and expand the analytical detection range from 3 log 10 to 6 log 10 for diagnosing patients with inflammatory conditions by measuring C-reactive protein. This work demonstrates that, with appropriate design of the contrast label, a simple and commonly used diagnostic technology can compete with more expensive state-of-the-art laboratory tests.

Tungsten devices in analytical atomic spectrometry

NASA Astrophysics Data System (ADS)

Hou, Xiandeng; Jones, Bradley T.

2002-04-01

Tungsten devices have been employed in analytical atomic spectrometry for approximately 30 years. Most of these atomizers can be electrically heated up to 3000 °C at very high heating rates, with a simple power supply. Usually, a tungsten device is employed in one of two modes: as an electrothermal atomizer with which the sample vapor is probed directly, or as an electrothermal vaporizer, which produces a sample aerosol that is then carried to a separate atomizer for analysis. Tungsten devices may take various physical shapes: tubes, cups, boats, ribbons, wires, filaments, coils and loops. Most of these orientations have been applied to many analytical techniques, such as atomic absorption spectrometry, atomic emission spectrometry, atomic fluorescence spectrometry, laser excited atomic fluorescence spectrometry, metastable transfer emission spectroscopy, inductively coupled plasma optical emission spectrometry, inductively coupled plasma mass spectrometry and microwave plasma atomic spectrometry. The analytical figures of merit and the practical applications reported for these techniques are reviewed. Atomization mechanisms reported for tungsten atomizers are also briefly summarized. In addition, less common applications of tungsten devices are discussed, including analyte preconcentration by adsorption or electrodeposition and electrothermal separation of analytes prior to analysis. Tungsten atomization devices continue to provide simple, versatile alternatives for analytical atomic spectrometry.

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.

Full Flight Envelope Direct Thrust Measurement on a Supersonic Aircraft

NASA Technical Reports Server (NTRS)

Conners, Timothy R.; Sims, Robert L.

1998-01-01

Direct thrust measurement using strain gages offers advantages over analytically-based thrust calculation methods. For flight test applications, the direct measurement method typically uses a simpler sensor arrangement and minimal data processing compared to analytical techniques, which normally require costly engine modeling and multisensor arrangements throughout the engine. Conversely, direct thrust measurement has historically produced less than desirable accuracy because of difficulty in mounting and calibrating the strain gages and the inability to account for secondary forces that influence the thrust reading at the engine mounts. Consequently, the strain-gage technique has normally been used for simple engine arrangements and primarily in the subsonic speed range. This paper presents the results of a strain gage-based direct thrust-measurement technique developed by the NASA Dryden Flight Research Center and successfully applied to the full flight envelope of an F-15 aircraft powered by two F100-PW-229 turbofan engines. Measurements have been obtained at quasi-steady-state operating conditions at maximum non-augmented and maximum augmented power throughout the altitude range of the vehicle and to a maximum speed of Mach 2.0 and are compared against results from two analytically-based thrust calculation methods. The strain-gage installation and calibration processes are also described.

Multiresidue analytical method using dispersive solid-phase extraction and gas chromatography/ion trap mass spectrometry to determine pharmaceuticals in whole blood.

PubMed

Plössl, Florian; Giera, Martin; Bracher, Franz

2006-11-24

A convenient analytical method for the simultaneous determination of more than 40 pharmaceuticals belonging to various therapeutic categories in whole blood has been developed. Exemplarily, the method was fully validated for eight different pharmaceuticals. The procedure entails addition of acetonitrile, magnesium sulfate and sodium chloride to a small amount of blood, then the mixture is shaken intensively and centrifuged for phase separation. An aliquot of the organic layer is cleaned up by dispersive solid-phase extraction employing bulk sorbents as well as magnesium sulfate for the removal of residual water. This method was based on the QuEChERS approach developed for pesticide residue analysis in food. Gas chromatography/ion trap mass spectrometry (GC/MS) with electron (EI) and chemical (CI) ionisation was then used for qualitative and quantitative determination of the pharmaceuticals. The dispersive SPE with PSA (sorbent functionalized with primary and secondary amines) was found more suitable than aminopropyl and a styrene-divinylbenzene sorbent for sample clean-up before drug level determination in whole blood and plasma, as it was found that most of endogenous matrix components were removed and the analytes were isolated from spiked samples with recoveries above 80%. Variation coefficients of the repeatability typically smaller than 10% have been achieved for a wide range of the investigated substances. The used analytical conditions allowed to separate successively a variety of drugs and poisons with the typical limit of detection at <20 ng mL(-1) levels using 1 microL injection of equivalent blood sample in whole blood. The method is simple, rapid, cheap and very effective for therapeutic drug monitoring and forensic chemistry.

Analysis of variation matrix array by bilinear least squares-residual bilinearization (BLLS-RBL) for resolving and quantifying of foodstuff dyes in a candy sample.

PubMed

Asadpour-Zeynali, Karim; Maryam Sajjadi, S; Taherzadeh, Fatemeh; Rahmanian, Reza

2014-04-05

Bilinear least square (BLLS) method is one of the most suitable algorithms for second-order calibration. Original BLLS method is not applicable to the second order pH-spectral data when an analyte has more than one spectroscopically active species. Bilinear least square-residual bilinearization (BLLS-RBL) was developed to achieve the second order advantage for analysis of complex mixtures. Although the modified method is useful, the pure profiles cannot be obtained and only the linear combination will be obtained. Moreover, for prediction of analyte in an unknown sample, the original algorithm of RBL may diverge; instead of converging to the desired analyte concentrations. Therefore, Gauss Newton-RLB algorithm should be used, which is not as simple as original protocol. Also, the analyte concentration can be predicted on the basis of each of the equilibrating species of the component of interest that are not exactly the same. The aim of the present work is to tackle the non-uniqueness problem in the second order calibration of monoprotic acid mixtures and divergence of RBL. Each pH-absorbance matrix was pretreated by subtraction of the first spectrum from other spectra in the data set to produce full rank array that is called variation matrix. Then variation matrices were analyzed uniquely by original BLLS-RBL that is more parsimonious than its modified counterpart. The proposed method was performed on the simulated as well as the analysis of real data. Sunset yellow and Carmosine as monoprotic acids were determined in candy sample in the presence of unknown interference by this method. Copyright © 2013 Elsevier B.V. All rights reserved.

Computationally efficient finite-difference modal method for the solution of Maxwell's equations.

PubMed

Semenikhin, Igor; Zanuccoli, Mauro

2013-12-01

In this work, a new implementation of the finite-difference (FD) modal method (FDMM) based on an iterative approach to calculate the eigenvalues and corresponding eigenfunctions of the Helmholtz equation is presented. Two relevant enhancements that significantly increase the speed and accuracy of the method are introduced. First of all, the solution of the complete eigenvalue problem is avoided in favor of finding only the meaningful part of eigenmodes by using iterative methods. Second, a multigrid algorithm and Richardson extrapolation are implemented. Simultaneous use of these techniques leads to an enhancement in terms of accuracy, which allows a simple method such as the FDMM with a typical three-point difference scheme to be significantly competitive with an analytical modal method.

Forgetfulness can help you win games.

PubMed

Burridge, James; Gao, Yu; Mao, Yong

2015-09-01

We present a simple game model where agents with different memory lengths compete for finite resources. We show by simulation and analytically that an instability exists at a critical memory length, and as a result, different memory lengths can compete and coexist in a dynamical equilibrium. Our analytical formulation makes a connection to statistical urn models, and we show that temperature is mirrored by the agent's memory. Our simple model of memory may be incorporated into other game models with implications that we briefly discuss.

Method development and optimization for the determination of benzene, toluene, ethylbenzene and xylenes in water at trace levels by static headspace extraction coupled to gas chromatography-barrier ionization discharge detection.

PubMed

Pascale, Raffaella; Bianco, Giuliana; Calace, Stefania; Masi, Salvatore; Mancini, Ignazio M; Mazzone, Giuseppina; Caniani, Donatella

2018-05-04

Benzene, toluene, ethylbenzene, and xylenes, more commonly named BTEX, represent one of the most ubiquitous and hazardous groups of atmospheric pollutants. The goal of our research was the trace quantification of BTEX in water by using a new simple, low-cost, and accurate method, based on headspace (HS) extraction and gas chromatography (GC) coupled to barrier ionization discharge detector (BID). This water application dealt with simple matrices without protein, fat, or humic material that adsorb target analytes, thus the external standard calibration was suitable to quantify each compound. The validation steps included the study of linearity, detection and quantification limits, and accuracy. LODs and LOQs varied from 0.159 to 1.845 μg/L and from 0.202 to 2.452 μg/L, respectively. The recovery was between 0.74 ± 0.13 and 1.15 ± 0.09; relative standard deviations (% RDSs) were less than 12.81% (n = 5) and 14.84% (n = 10). Also, GC performance was evaluated in term of efficiency, peak tailing and resolution. Preliminary results from practical applications to analyses of real samples are presented. The results indicate that static HS coupled to GC-BID is a successful method for BTEX analysis in water samples at the μg/L levels, provided that hydrocarbons interference occur at similar concentration levels. GC-BID may become a routine reference method alongside the official analytical techniques for quality control purposes of contaminated waters. Moreover, the new method is amenable to automation by using commercial HS units. Copyright © 2018. Published by Elsevier B.V.

Limited analytical capacity for cyanotoxins in developing countries may hide serious environmental health problems: simple and affordable methods may be the answer.

PubMed

Pírez, Macarena; Gonzalez-Sapienza, Gualberto; Sienra, Daniel; Ferrari, Graciela; Last, Michael; Last, Jerold A; Brena, Beatriz M

2013-01-15

In recent years, the international demand for commodities has prompted enormous growth in agriculture in most South American countries. Due to intensive use of fertilizers, cyanobacterial blooms have become a recurrent phenomenon throughout the continent, but their potential health risk remains largely unknown due to the lack of analytical capacity. In this paper we report the main results and conclusions of more than five years of systematic monitoring of cyanobacterial blooms in 20 beaches of Montevideo, Uruguay, on the Rio de la Plata, the fifth largest basin in the world. A locally developed microcystin ELISA was used to establish a sustainable monitoring program that revealed seasonal peaks of extremely high toxicity, more than one-thousand-fold greater than the WHO limit for recreational water. Comparison with cyanobacterial cell counts and chlorophyll-a determination, two commonly used parameters for indirect estimation of toxicity, showed that such indicators can be highly misleading. On the other hand, the accumulated experience led to the definition of a simple criterion for visual classification of blooms, that can be used by trained lifeguards and technicians to take rapid on-site decisions on beach management. The simple and low cost approach is broadly applicable to risk assessment and risk management in developing countries. Copyright © 2012 Elsevier Ltd. All rights reserved.

Validation of a Stability-Indicating Method for Methylseleno-l-Cysteine (l-SeMC)

PubMed Central

Canady, Kristin; Cobb, Johnathan; Deardorff, Peter; Larson, Jami; White, Jonathan M.; Boring, Dan

2016-01-01

Methylseleno-l-cysteine (l-SeMC) is a naturally occurring amino acid analogue used as a general dietary supplement and is being explored as a chemopreventive agent. As a known dietary supplement, l-SeMC is not regulated as a pharmaceutical and there is a paucity of analytical methods available. To address the lack of methodology, a stability-indicating method was developed and validated to evaluate l-SeMC as both the bulk drug and formulated drug product (400 µg Se/capsule). The analytical approach presented is a simple, nonderivatization method that utilizes HPLC with ultraviolet detection at 220 nm. A C18 column with a volatile ion-pair agent and methanol mobile phase was used for the separation. The method accuracy was 99–100% from 0.05 to 0.15 mg/mL l-SeMC for the bulk drug, and 98–99% from 0.075 to 0.15 mg/mL l-SeMC for the drug product. Method precision was <1% for the bulk drug and was 3% for the drug product. The LOQ was 0.1 µg/mL l-SeMC or 0.002 µg l-SeMC on column. PMID:26199341

pH-Triggered Molecular Alignment for Reproducible SERS Detection via an AuNP/Nanocellulose Platform

PubMed Central

Wei, Haoran; Vikesland, Peter J.

2015-01-01

The low affinity of neutral and hydrophobic molecules towards noble metal surfaces hinders their detection by surface-enhanced Raman spectroscopy (SERS). Herein, we present a method to enhance gold nanoparticle (AuNP) surface affinity by lowering the suspension pH below the analyte pKa. We developed an AuNP/bacterial cellulose (BC) nanocomposite platform and applied it to two common pollutants, carbamazepine (CBZ) and atrazine (ATZ) with pKa values of 2.3 and 1.7, respectively. Simple mixing of the analytes with AuNP/BC at pH < pKa resulted in consistent electrostatic alignment of the CBZ and ATZ molecules across the nanocomposite and highly reproducible SERS spectra. Limits of detection of 3 nM and 11 nM for CBZ and ATZ, respectively, were attained. Tests with additional analytes (melamine, 2,4-dichloroaniline, 4-chloroaniline, 3-bromoaniline, and 3-nitroaniline) further illustrate that the AuNP/BC platform provides reproducible analyte detection and quantification while avoiding the uncontrolled aggregation and flocculation of AuNPs that often hinder low pH detection. PMID:26658696

pH-Triggered Molecular Alignment for Reproducible SERS Detection via an AuNP/Nanocellulose Platform

NASA Astrophysics Data System (ADS)

Wei, Haoran; Vikesland, Peter J.

2015-12-01

The low affinity of neutral and hydrophobic molecules towards noble metal surfaces hinders their detection by surface-enhanced Raman spectroscopy (SERS). Herein, we present a method to enhance gold nanoparticle (AuNP) surface affinity by lowering the suspension pH below the analyte pKa. We developed an AuNP/bacterial cellulose (BC) nanocomposite platform and applied it to two common pollutants, carbamazepine (CBZ) and atrazine (ATZ) with pKa values of 2.3 and 1.7, respectively. Simple mixing of the analytes with AuNP/BC at pH < pKa resulted in consistent electrostatic alignment of the CBZ and ATZ molecules across the nanocomposite and highly reproducible SERS spectra. Limits of detection of 3 nM and 11 nM for CBZ and ATZ, respectively, were attained. Tests with additional analytes (melamine, 2,4-dichloroaniline, 4-chloroaniline, 3-bromoaniline, and 3-nitroaniline) further illustrate that the AuNP/BC platform provides reproducible analyte detection and quantification while avoiding the uncontrolled aggregation and flocculation of AuNPs that often hinder low pH detection.

Analytic Formulation and Numerical Implementation of an Acoustic Pressure Gradient Prediction

NASA Technical Reports Server (NTRS)

Lee, Seongkyu; Brentner, Kenneth S.; Farassat, Fereidoun

2007-01-01

The scattering of rotor noise is an area that has received little attention over the years, yet the limited work that has been done has shown that both the directivity and intensity of the acoustic field may be significantly modified by the presence of scattering bodies. One of the inputs needed to compute the scattered acoustic field is the acoustic pressure gradient on a scattering surface. Two new analytical formulations of the acoustic pressure gradient have been developed and implemented in the PSU-WOPWOP rotor noise prediction code. These formulations are presented in this paper. The first formulation is derived by taking the gradient of Farassat's retarded-time Formulation 1A. Although this formulation is relatively simple, it requires numerical time differentiation of the acoustic integrals. In the second formulation, the time differentiation is taken inside the integrals analytically. The acoustic pressure gradient predicted by these new formulations is validated through comparison with the acoustic pressure gradient determined by a purely numerical approach for two model rotors. The agreement between analytic formulations and numerical method is excellent for both stationary and moving observers case.

Design considerations of a hollow microneedle-optofluidic biosensing platform incorporating enzyme-linked assays

NASA Astrophysics Data System (ADS)

Ranamukhaarachchi, Sahan A.; Padeste, Celestino; Häfeli, Urs O.; Stoeber, Boris; Cadarso, Victor J.

2018-02-01

A hollow metallic microneedle is integrated with microfluidics and photonic components to form a microneedle-optofluidic biosensor suitable for therapeutic drug monitoring (TDM) in biological fluids, like interstitial fluid, that can be collected in a painless and minimally-invasive manner. The microneedle inner lumen surface is bio-functionalized to trap and bind target analytes on-site in a sample volume as small as 0.6 nl, and houses an enzyme-linked assay on its 0.06 mm2 wall. The optofluidic components are designed to rapidly quantify target analytes present in the sample and collected in the microneedle using a simple and sensitive absorbance scheme. This contribution describes how the biosensor components were optimized to detect in vitro streptavidin-horseradish peroxidase (Sav-HRP) as a model analyte over a large detection range (0-7.21 µM) and a very low limit of detection (60.2 nM). This biosensor utilizes the lowest analyte volume reported for TDM with microneedle technology, and presents significant avenues to improve current TDM methods for patients, by potentially eliminating blood draws for several drug candidates.

Development and validation of a sensitive and fast UPLC-MS/MS method for simultaneous determination of seven bioactive compounds in rat plasma after oral administration of Guizhi-gancao decoction.

PubMed

Ji, Bin; Zhuo, Limeng; Yang, Bin; Wang, Yang; Li, Lin; Yu, Miao; Zhao, Yunli; Yu, Zhiguo

2017-04-15

Rapid, sensitive, selective and accurate UPLC-MS/MS method was developed and fully validated for simultaneous determination of cinnamaldehyde, cinnamic acid, 2-methoxy cinnamic acid, glycyrrhizic acid, glycyrrhetinic acid, liquiritigenin and isoliquiritin in rat plasma after oral administration of Guizhi-gancao decoction. Plasma samples were processed with a simple protein precipitation technique using acetonitrile, followed by chromatographic separation using a Thermo Hypersil GOLD C 18 column. A 11.0min linear gradient elution was used at a flow rate of 0.2mL/min with a mobile phase of 0.1% acetic acid containing 0.2mM ammonium acetate in water and acetonitrile. The analytes and internal standard, schisandrin, were detected using both positive and negative ion electrospray ionization in multiple reaction monitoring mode. The developed method was validated for intra-day and inter-day accuracy and precision whose values fell in the acceptable limits. Matrix effect was found to be minimal. Recovery efficiency of all the analytes was found to be >60%. Stability results showed that the analytes were stable at all the conditions. This validated method was successfully used to study the pharmacokinetics of multiple compounds in rat plasma after oral administration of Guizhi-gancao decoction. Copyright © 2017 Elsevier B.V. All rights reserved.

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

PubMed

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

2016-10-01

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

Application of surface analytical methods for hazardous situation in the Adriatic Sea: monitoring of organic matter dynamics and oil pollution

NASA Astrophysics Data System (ADS)

Pletikapić, Galja; Ivošević DeNardis, Nadica

2017-01-01

Surface analytical methods are applied to examine the environmental status of seawaters. The present overview emphasizes advantages of combining surface analytical methods, applied to a hazardous situation in the Adriatic Sea, such as monitoring of the first aggregation phases of dissolved organic matter in order to potentially predict the massive mucilage formation and testing of oil spill cleanup. Such an approach, based on fast and direct characterization of organic matter and its high-resolution visualization, sets a continuous-scale description of organic matter from micro- to nanometre scales. Electrochemical method of chronoamperometry at the dropping mercury electrode meets the requirements for monitoring purposes due to the simple and fast analysis of a large number of natural seawater samples enabling simultaneous differentiation of organic constituents. In contrast, atomic force microscopy allows direct visualization of biotic and abiotic particles and provides an insight into structural organization of marine organic matter at micro- and nanometre scales. In the future, merging data at different spatial scales, taking into account experimental input on micrometre scale, observations on metre scale and modelling on kilometre scale, will be important for developing sophisticated technological platforms for knowledge transfer, reports and maps applicable for the marine environmental protection and management of the coastal area, especially for tourism, fishery and cruiser trafficking.

Analytical method for fast screening and confirmation of multi-class veterinary drug residues in fish and shrimp by LC-MS/MS.

PubMed

Kim, Junghyun; Suh, Joon Hyuk; Cho, Hyun-Deok; Kang, Wonjae; Choi, Yong Seok; Han, Sang Beom

2016-01-01

A multi-class, multi-residue analytical method based on LC-MS/MS detection was developed for the screening and confirmation of 28 veterinary drug and metabolite residues in flatfish, shrimp and eel. The chosen veterinary drugs are prohibited or unauthorised compounds in Korea, which were categorised into various chemical classes including nitroimidazoles, benzimidazoles, sulfones, quinolones, macrolides, phenothiazines, pyrethroids and others. To achieve fast and simultaneous extraction of various analytes, a simple and generic liquid extraction procedure using EDTA-ammonium acetate buffer and acetonitrile, without further clean-up steps, was applied to sample preparation. The final extracts were analysed by ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). The method was validated for each compound in each matrix at three different concentrations (5, 10 and 20 ng g(-1)) in accordance with Codex guidelines (CAC/GL 71-2009). For most compounds, the recoveries were in the range of 60-110%, and precision, expressed as the relative standard deviation (RSD), was in the range of 5-15%. The detection capabilities (CCβs) were below or equal to 5 ng g(-1), which indicates that the developed method is sufficient to detect illegal fishery products containing the target compounds above the residue limit (10 ng g(-1)) of the new regulatory system (Positive List System - PLS).

Multiclass screening method based on solvent extraction and liquid chromatography-tandem mass spectrometry for the determination of antimicrobials and mycotoxins in egg.

PubMed

Capriotti, Anna Laura; Cavaliere, Chiara; Piovesana, Susy; Samperi, Roberto; Laganà, Aldo

2012-12-14

A QuEChERS (Quick Easy Cheap Effective Rugged Safe)-like extraction method was developed for the simultaneous analysis of veterinary drugs and mycotoxins in hen eggs by liquid chromatography-tandem mass spectrometry (LC-MS/MS) with electrospray (ESI) source. Various classes of antimicrobials (tetracyclines, ionophores, coccidiostats, penicillins, cephalosporins, fluoroquinolones, sulfonamides) and mycotoxins (enniatins, beauvericin, ochratoxins, aflatoxins) were considered for the development of this method. Particular attention was devoted to extraction optimization: different solvents (acetone, acetonitrile and methanol), different pH values and different sample to extracting volume ratios were tested and evaluated in terms of recovery, relative standard deviation (RSD) and ESI signal suppression due to matrix effect. Chromatographic and mass spectrometric conditions were optimized to obtain the best instrumental performances for most of the analytes. Quantitative analysis was performed by means of matrix-matched calibration, in a range that varied depending on the analyte and its established maximum limit, when there was one. Recoveries at 100 μg kg(-1) spiking level were >62% (3

Validated spectroscopic methods for determination of anti-histaminic drug azelastine in pure form: Analytical application for quality control of its pharmaceutical preparations.

PubMed

El-Masry, Amal A; Hammouda, Mohammed E A; El-Wasseef, Dalia R; El-Ashry, Saadia M

2018-02-15

Two simple, sensitive, rapid, validated and cost effective spectroscopic methods were established for quantification of antihistaminic drug azelastine (AZL) in bulk powder as well as in pharmaceutical dosage forms. In the first method (A) the absorbance difference between acidic and basic solutions was measured at 228nm, whereas in the second investigated method (B) the binary complex formed between AZL and Eosin Y in acetate buffer solution (pH3) was measured at 550nm. Different criteria that have critical influence on the intensity of absorption were deeply studied and optimized so as to achieve the highest absorption. The proposed methods obeyed Beer ' s low in the concentration range of (2.0-20.0μg·mL -1 ) and (0.5-15.0μg·mL -1 ) with % recovery±S.D. of (99.84±0.87), (100.02±0.78) for methods (A) and (B), respectively. Furthermore, the proposed methods were easily applied for quality control of pharmaceutical preparations without any conflict with its co-formulated additives, and the analytical results were compatible with those obtained by the comparison one with no significant difference as insured by student's t-test and the variance ratio F-test. Validation of the proposed methods was performed according the ICH guidelines in terms of linearity, limit of quantification, limit of detection, accuracy, precision and specificity, where the analytical results were persuasive. Copyright © 2017 Elsevier B.V. All rights reserved.

Experimental Validation of Lightning-Induced Electromagnetic (Indirect) Coupling to Short Monopole Antennas

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

Crull, E W; Brown Jr., C G; Perkins, M P

2008-07-30

For short monopoles in this low-power case, it has been shown that a simple circuit model is capable of accurate predictions for the shape and magnitude of the antenna response to lightning-generated electric field coupling effects, provided that the elements of the circuit model have accurate values. Numerical EM simulation can be used to provide more accurate values for the circuit elements than the simple analytical formulas, since the analytical formulas are used outside of their region of validity. However, even with the approximate analytical formulas the simple circuit model produces reasonable results, which would improve if more accurate analyticalmore » models were used. This report discusses the coupling analysis approaches taken to understand the interaction between a time-varying EM field and a short monopole antenna, within the context of lightning safety for nuclear weapons at DOE facilities. It describes the validation of a simple circuit model using laboratory study in order to understand the indirect coupling of energy into a part, and the resulting voltage. Results show that in this low-power case, the circuit model predicts peak voltages within approximately 32% using circuit component values obtained from analytical formulas and about 13% using circuit component values obtained from numerical EM simulation. We note that the analytical formulas are used outside of their region of validity. First, the antenna is insulated and not a bare wire and there are perhaps fringing field effects near the termination of the outer conductor that the formula does not take into account. Also, the effective height formula is for a monopole directly over a ground plane, while in the time-domain measurement setup the monopole is elevated above the ground plane by about 1.5-inch (refer to Figure 5).« less

Simultaneous determination of domperidone and Itopride in pharmaceuticals and human plasma using RP-HPLC/UV detection: Method development, validation and application of the method in in-vivo evaluation of fast dispersible tablets.

PubMed

Khan, Amjad; Iqbal, Zafar; Khadra, Ibrahim; Ahmad, Lateef; Khan, Abad; Khan, Muhammad Imran; Ullah, Zia; Ismail

2016-03-20

Domperidone and Itopride are pro-kinetic agents, regulating the gastric motility and are commonly prescribed as anti emetic drugs. In the present study a simple, rapid and sensitive RP-HPLC/UV method was developed for simultaneous determination of Domperidone and Itopride in pharmaceutical samples and human plasma, using Tenofavir as internal standard. Experimental conditions were optimized and method was validated according to the standard guidelines. Combination of water (pH 3.0) and acetonitrile (65:35 v/v) was used as mobile phase, pumped at the flow rate of 1.5 ml/min. Detector wavelength was set at 210 nm and column oven temperature was 40oC. Unlike conventional liquid-liquid extraction, simple precipitation technique was applied for drug extraction from human plasma using acetonitrile for deprotienation. The method showed adequate separation of both the analytes and best resolution was achieved using Hypersil BDS C8 column (150 mm × 4.6 mm, 5 μm). The method was quite linear in the range of 20-600 ng/ml. Recovery of the method was 92.31% and 89.82% for Domperidone and Itopride, respectively. Retention time of both the analytes and internal standard was below 15 min. The lower limit of detection (LLOD) and lower limit of quantification (LLOQ) for Domperidone were 5 and 10 ng/ml while for Itopride was 12 and 15 ng/ml, respectively. The developed method was successfully applied for in-vivo analysis of fast dispersible tablets of Domperidone in healthy human volunteer. The proposed method was a part of formulation development study and was efficiently applied for determination of the two drugs in various pharmaceutical products and human plasma. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

Multi-residue pesticide analysis (gas chromatography-tandem mass spectrometry detection)-Improvement of the quick, easy, cheap, effective, rugged, and safe method for dried fruits and fat-rich cereals-Benefit and limit of a standardized apple purée calibration (screening).

PubMed

Rasche, Claudia; Fournes, Britta; Dirks, Uwe; Speer, Karl

2015-07-17

Some steps of the QuEChERS method for the analysis of pesticides with GC-MS/MS in cereals and dried fruits were improved or simplified. For the latter, a mixing vessel with stator-rotor-system proved to be advantageous. The extraction procedure of dried fruits is much easier and safer than the Ultra Turrax and results in excellent validation data at a concentration level of 0.01mg/kg (116 of 118 analytes with recoveries in the range of 70-120%, 117 of 118 analytes with RSD <20%). After qualifying problematic lipophilic pesticides in fat-rich cereals (fat content >7%), predominantly organochlorines showed recoveries of <70% in quantification when the standard QuEChERS method with water was used. A second extraction was carried out analogous to the QuEChERS method, however, without the addition of water. With this simple modification, the problematic lipophilic pesticides, which had been strongly affected by the fat content of the commodities, could be determined with recoveries above 70% even at a concentration level of 0.01mg/kg. Moreover, a GC-MS/MS screening method for 120 pesticides at a concentration level of 0.01mg/kg was established by employing analyte protectants (ethylglycerol, gulonolactone, and sorbitol). The use of only one standardized calibration, made of an apple purée extract in combination with analyte protectants, allowed for a qualitative and quantitative analysis of 120 pesticides in different matrix extracts (tomato, red pepper, sour cherries, dried apples, black currant powder, raisins, wheat flour, rolled oats, wheat germ). The analyte protectants leveled the differences in the matrix-induced protection effect of the analyzed extracts over a wide range. The majority of the pesticides were analyzed with good analytical results (recoveries in the range of 70-120% and RSD <20%). Copyright © 2015 Elsevier B.V. All rights reserved.

Electromagnetic Launch Technology Assessment. Scientific Basis and Unified Treatment: Forces and Electromechanical Power Conversion (Analytical and Numerical Methods),

DTIC Science & Technology

1990-06-01

on simple railgun accelerators andI homopolar generators. Complex rotating flux compressors would drastically improve the performance of EM launchers...velocities. If this is the direction of improvement, then energies stored in the electric trains built with linear electric motors in Japan and Western I...laboratories which had power supplies 3 already built for other programs ( homopolar generators in conjunction with an inductor and an opening switch

Electrochemical hydrogen sulfide biosensors.

PubMed

Xu, Tailin; Scafa, Nikki; Xu, Li-Ping; Zhou, Shufeng; Abdullah Al-Ghanem, Khalid; Mahboob, Shahid; Fugetsu, Bunshi; Zhang, Xueji

2016-02-21

The measurement of sulfide, especially hydrogen sulfide, has held the attention of the analytical community due to its unique physiological and pathophysiological roles in biological systems. Electrochemical detection offers a rapid, highly sensitive, affordable, simple, and real-time technique to measure hydrogen sulfide concentration, which has been a well-documented and reliable method. This review details up-to-date research on the electrochemical detection of hydrogen sulfide (ion selective electrodes, polarographic hydrogen sulfide sensors, etc.) in biological samples for potential therapeutic use.

Fingerprinting of Non-resolved Three-axis Stabilized Space Objects Using a Two-Facet Analytical Model

DTIC Science & Technology

2011-09-01

Crawford, K., " Time - Resolved Infrared Spectrophotometric Observations of IRIDIUM satellites and related Resident Space Objects", IAC-09-A6.1.17...Figure 10 for a geosynchronous (GEO) satellite . The figure shows three sets of multi-spectral signatures were collected at different times of the...provides a simple method to determine suitable observation conditions for the cluster of satellites . For instance, on Day 0, the times of the

Experimental Method for Characterizing Electrical Steel Sheets in the Normal Direction

PubMed Central

Hihat, Nabil; Lecointe, Jean Philippe; Duchesne, Stephane; Napieralska, Ewa; Belgrand, Thierry

2010-01-01

This paper proposes an experimental method to characterise magnetic laminations in the direction normal to the sheet plane. The principle, which is based on a static excitation to avoid planar eddy currents, is explained and specific test benches are proposed. Measurements of the flux density are made with a sensor moving in and out of an air-gap. A simple analytical model is derived in order to determine the permeability in the normal direction. The experimental results for grain oriented steel sheets are presented and a comparison is provided with values obtained from literature. PMID:22163394

Quantum Mechanics, Path Integrals and Option Pricing:. Reducing the Complexity of Finance

NASA Astrophysics Data System (ADS)

Baaquie, Belal E.; Corianò, Claudio; Srikant, Marakani

2003-04-01

Quantum Finance represents the synthesis of the techniques of quantum theory (quantum mechanics and quantum field theory) to theoretical and applied finance. After a brief overview of the connection between these fields, we illustrate some of the methods of lattice simulations of path integrals for the pricing of options. The ideas are sketched out for simple models, such as the Black-Scholes model, where analytical and numerical results are compared. Application of the method to nonlinear systems is also briefly overviewed. More general models, for exotic or path-dependent options are discussed.

Electrochemical Determination of Trace Sudan I Contamination in Chili Powder at Carbon Nanotube Modified Electrodes

PubMed Central

Ming, Liang; Xi, Xia; Chen, Tingting; Liu, Jie

2008-01-01

We have developed a simple, convenient and inexpensive voltammetric method for determining trace Sudan I contamination in chili powder, based on the catalyzed electrochemical reduction of Sudan I at the carbon nanotube modified electrode. Under optimized conditions, the method exhibited acceptable analytical performance in terms of linearity (over the concentration range 6.0×10−7 to 7.5×10−5 M, r = 0.9967), detection limit (2.0×10−7 M) and reproducibility (RSD = 4.6%, n=10, for 2.0×10−5 M Sudan I). PMID:27879800

Three-dimensional wax patterning of paper fluidic devices.

PubMed

Renault, Christophe; Koehne, Jessica; Ricco, Antonio J; Crooks, Richard M

2014-06-17

In this paper we describe a method for three-dimensional wax patterning of microfluidic paper-based analytical devices (μPADs). The method is rooted in the fundamental details of wax transport in paper and provides a simple way to fabricate complex channel architectures such as hemichannels and fully enclosed channels. We show that three-dimensional μPADs can be fabricated with half as much paper by using hemichannels rather than ordinary open channels. We also provide evidence that fully enclosed channels are efficiently isolated from the exterior environment, decreasing contamination risks, simplifying the handling of the device, and slowing evaporation of solvents.

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

PubMed

Amelin, Vasiliy; Korotkov, Anton

2017-02-01

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

Versatile fabrication of paper-based microfluidic devices with high chemical resistance using scholar glue and magnetic masks.

PubMed

Cardoso, Thiago M G; de Souza, Fabrício R; Garcia, Paulo T; Rabelo, Denilson; Henry, Charles S; Coltro, Wendell K T

2017-06-29

Simple methods have been developed for fabricating microfluidic paper-based analytical devices (μPADs) but few of these devices can be used with organic solvents and/or aqueous solutions containing surfactants. This study describes a simple fabrication strategy for μPADs that uses readily available scholar glue to create the hydrophobic flow barriers that are resistant to surfactants and organic solvents. Microfluidic structures were defined by magnetic masks designed with either neodymium magnets or magnetic sheets to define the patter, and structures were created by spraying an aqueous solution of glue on the paper surface. The glue-coated paper was then exposed to UV/Vis light for cross-linking to maximize chemical resistance. Examples of microzone arrays and microfluidic devices are demonstrated. μPADs fabricated with scholar glue retained their barriers when used with surfactants, organic solvents, and strong/weak acids and bases unlike common wax-printed barriers. Paper microzones and microfluidic devices were successfully used for colorimetric assays of clinically relevant analytes commonly detected in urinalysis to demonstrate the low background of the barrier material and generally applicability to sensing. The proposed fabrication method is attractive for both its ability to be used with diverse chemistries and the low cost and simplicity of the materials and process. Copyright © 2017 Elsevier B.V. All rights reserved.

Comparative study between univariate spectrophotometry and multivariate calibration as analytical tools for quantitation of Benazepril alone and in combination with Amlodipine.

PubMed

Farouk, M; Elaziz, Omar Abd; Tawakkol, Shereen M; Hemdan, A; Shehata, Mostafa A

2014-04-05

Four simple, accurate, reproducible, and selective methods have been developed and subsequently validated for the determination of Benazepril (BENZ) alone and in combination with Amlodipine (AML) in pharmaceutical dosage form. The first method is pH induced difference spectrophotometry, where BENZ can be measured in presence of AML as it showed maximum absorption at 237nm and 241nm in 0.1N HCl and 0.1N NaOH, respectively, while AML has no wavelength shift in both solvents. The second method is the new Extended Ratio Subtraction Method (EXRSM) coupled to Ratio Subtraction Method (RSM) for determination of both drugs in commercial dosage form. The third and fourth methods are multivariate calibration which include Principal Component Regression (PCR) and Partial Least Squares (PLSs). A detailed validation of the methods was performed following the ICH guidelines and the standard curves were found to be linear in the range of 2-30μg/mL for BENZ in difference and extended ratio subtraction spectrophotometric method, and 5-30 for AML in EXRSM method, with well accepted mean correlation coefficient for each analyte. The intra-day and inter-day precision and accuracy results were well within the acceptable limits. Copyright © 2013 Elsevier B.V. All rights reserved.

A candidate reference method for serum potassium measurement by inductively coupled plasma mass spectrometry.

PubMed

Yan, Ying; Han, Bingqing; Zeng, Jie; Zhou, Weiyan; Zhang, Tianjiao; Zhang, Jiangtao; Chen, Wenxiang; Zhang, Chuanbao

2017-08-28

Potassium is an important serum ion that is frequently assayed in clinical laboratories. Quality assurance requires reference methods; thus, the establishment of a candidate reference method for serum potassium measurements is important. An inductively coupled plasma mass spectrometry (ICP-MS) method was developed. Serum samples were gravimetrically spiked with an aluminum internal standard, digested with 69% ultrapure nitric acid, and diluted to the required concentration. The 39K/27Al ratios were measured by ICP-MS in hydrogen mode. The method was calibrated using 5% nitric acid matrix calibrators, and the calibration function was established using the bracketing method. The correlation coefficients between the measured 39K/27Al ratios and the analyte concentration ratios were >0.9999. The coefficients of variation were 0.40%, 0.68%, and 0.22% for the three serum samples, and the analytical recovery was 99.8%. The accuracy of the measurement was also verified by measuring certified reference materials, SRM909b and SRM956b. Comparison with the ion selective electrode routine method and international inter-laboratory comparisons gave satisfied results. The new ICP-MS method is specific, precise, simple, and low-cost, and it may be used as a candidate reference method for standardizing serum potassium measurements.

Capillarity Guided Patterning of Microliquids.

PubMed

Kang, Myeongwoo; Park, Woohyun; Na, Sangcheol; Paik, Sang-Min; Lee, Hyunjae; Park, Jae Woo; Kim, Ho-Young; Jeon, Noo Li

2015-06-01

Soft lithography and other techniques have been developed to investigate biological and chemical phenomena as an alternative to photolithography-based patterning methods that have compatibility problems. Here, a simple approach for nonlithographic patterning of liquids and gels inside microchannels is described. Using a design that incorporates strategically placed microstructures inside the channel, microliquids or gels can be spontaneously trapped and patterned when the channel is drained. The ability to form microscale patterns inside microfluidic channels using simple fluid drain motion offers many advantages. This method is geometrically analyzed based on hydrodynamics and verified with simulation and experiments. Various materials (i.e., water, hydrogels, and other liquids) are successfully patterned with complex shapes that are isolated from each other. Multiple cell types are patterned within the gels. Capillarity guided patterning (CGP) is fast, simple, and robust. It is not limited by pattern shape, size, cell type, and material. In a simple three-step process, a 3D cancer model that mimics cell-cell and cell-extracellular matrix interactions is engineered. The simplicity and robustness of the CGP will be attractive for developing novel in vitro models of organ-on-a-chip and other biological experimental platforms amenable to long-term observation of dynamic events using advanced imaging and analytical techniques. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A simple spectrophotometric method for determination of zirconium or hafnium in selected molybdenum-base alloys

NASA Technical Reports Server (NTRS)

Dupraw, W. A.

1972-01-01

A simple analytical procedure is described for accurately and precisely determining the zirconium or hafnium content of molybdenum-base alloys. The procedure is based on the reaction of the reagent Arsenazo III with zirconium or hafnium in strong hydrochloric acid solution. The colored complexes of zirconium or hafnium are formed in the presence of molybdenum. Titanium or rhenium in the alloy have no adverse effect on the zirconium or hafnium complex at the following levels in the selected aliquot: Mo, 10 mg; Re, 10 mg; Ti, 1 mg. The spectrophotometric measurement of the zirconium or hafnium complex is accomplished without prior separation with a relative standard deviation of 1.3 to 2.7 percent.

Comprehensive quantification of signal-to-noise ratio and g-factor for image-based and k-space-based parallel imaging reconstructions.

PubMed

Robson, Philip M; Grant, Aaron K; Madhuranthakam, Ananth J; Lattanzi, Riccardo; Sodickson, Daniel K; McKenzie, Charles A

2008-10-01

Parallel imaging reconstructions result in spatially varying noise amplification characterized by the g-factor, precluding conventional measurements of noise from the final image. A simple Monte Carlo based method is proposed for all linear image reconstruction algorithms, which allows measurement of signal-to-noise ratio and g-factor and is demonstrated for SENSE and GRAPPA reconstructions for accelerated acquisitions that have not previously been amenable to such assessment. Only a simple "prescan" measurement of noise amplitude and correlation in the phased-array receiver, and a single accelerated image acquisition are required, allowing robust assessment of signal-to-noise ratio and g-factor. The "pseudo multiple replica" method has been rigorously validated in phantoms and in vivo, showing excellent agreement with true multiple replica and analytical methods. This method is universally applicable to the parallel imaging reconstruction techniques used in clinical applications and will allow pixel-by-pixel image noise measurements for all parallel imaging strategies, allowing quantitative comparison between arbitrary k-space trajectories, image reconstruction, or noise conditioning techniques. (c) 2008 Wiley-Liss, Inc.

Accurate mass measurement by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry. I. Measurement of positive radical ions using porphyrin standard reference materials.

PubMed

Griffiths, Nia W; Wyatt, Mark F; Kean, Suzanna D; Graham, Andrew E; Stein, Bridget K; Brenton, A Gareth

2010-06-15

A method for the accurate mass measurement of positive radical ions by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOFMS) is described. Initial use of a conjugated oligomeric calibration material was rejected in favour of a series of meso-tetraalkyl/tetraalkylaryl-functionalised porphyrins, from which the two calibrants required for a particular accurate mass measurement were chosen. While all measurements of monoisotopic species were within +/-5 ppm, and the method was rigorously validated using chemometrics, mean values of five measurements were used for extra confidence in the generation of potential elemental formulae. Potential difficulties encountered when measuring compounds containing multi-isotopic elements are discussed, where the monoisotopic peak is no longer the lowest mass peak, and a simple mass-correction solution can be applied. The method requires no significant expertise to implement, but care and attention is required to obtain valid measurements. The method is operationally simple and will prove useful to the analytical chemistry community. Copyright (c) 2010 John Wiley & Sons, Ltd.

Analytical detection and method development of anticancer drug Gemcitabine HCl using gold nanoparticles.

PubMed

Menon, Shobhana K; Mistry, Bhoomika R; Joshi, Kuldeep V; Sutariya, Pinkesh G; Patel, Ravindra V

2012-08-01

A simple, rapid, cost effective and extractive UV spectrophotometric method was developed for the determination of Gemcitabine HCl (GMCT) in bulk drug and pharmaceutical formulation. It was based on UV spectrophotometric measurements in which the drug reacts with gold nanoparticles (AuNP) and changes the original colour of AuNP and forms a dark blue coloured solution which exhibits absorption maximum at 688nm. The apparent molar absorptivity and Sandell's sensitivity coefficient were found to be 3.95×10(-5)lmol(-1)cm(-1) and 0.060μgcm(-2) respectively. Beer's law was obeyed in the concentration range of 2.0-40μgml(-1). This method was tested and validated for various parameters according to ICH guidelines. The proposed method was successfully applied for the determination of GMCT in pharmaceutical formulation (parental formulation). The results demonstrated that the procedure is accurate, precise and reproducible (relative standard deviation <2%). As it is simple, cheap and less time consuming, it can be suitably applied for the estimation of GMCT in dosage forms. Copyright © 2012 Elsevier B.V. All rights reserved.

Separation and simultaneous determination of rutin, puerarin, daidzein, esculin and esculetin in medicinal preparations by non-aqueous capillary.

PubMed

Li, Cunhong; Chen, Anjia; Chen, Xiaofeng; Chen, Xingguo; Hu, Zhide

2005-09-01

A simple method for the simultaneous determination of five bioactive components (rutin, puerarin, daidzein esculin and esculetin) in traditional medicinal preparations by non-aqueous capillary electrophoresis with UV detection has been developed for the first time. A running buffer composed of 15% acetonitrile, 2.5% acetic acid and 90 mM sodium cholate in methanol was found to be the most suitable for this separation. The limits of detection for five analytes were over the range of 0.050-1.216 microg ml(-1). The relative standard deviations (R.S.Ds.) of the migration times and the peak areas of the analytes were in the range of 1.3-2.9% and 2.2-2.7% (intraday), 1.7-1.9% and 2.8-3.6% (interday), respectively. In the tested concentration range, linear relationships (correlation coefficients: 0.9974 for rutin, 0.9976 for puerarin, 0.9981 for daidzein, 0.9972 for esculin and 0.9929 for esculetin) between peak areas and concentrations of the analytes were obtained. This method has been successfully applied to simultaneous determination of the five bioactive components with recoveries over the range of 89.4-107.4%.

Analytical assessment of some characteristic ratios for s-wave superconductors

NASA Astrophysics Data System (ADS)

Gonczarek, Ryszard; Krzyzosiak, Mateusz; Gonczarek, Adam; Jacak, Lucjan

2018-04-01

We evaluate some thermodynamic quantities and characteristic ratios that describe low- and high-temperature s-wave superconducting systems. Based on a set of fundamental equations derived within the conformal transformation method, a simple model is proposed and studied analytically. After including a one-parameter class of fluctuations in the density of states, the mathematical structure of the s-wave superconducting gap, the free energy difference, and the specific heat difference is found and discussed in an analytic manner. Both the zero-temperature limit T = 0 and the subcritical temperature range T ≲ T c are discussed using the method of successive approximations. The equation for the ratio R 1, relating the zero-temperature energy gap and the critical temperature, is formulated and solved numerically for various values of the model parameter. Other thermodynamic quantities are analyzed, including a characteristic ratio R 2, quantifying the dynamics of the specific heat jump at the critical temperature. It is shown that the obtained model results coincide with experimental data for low- T c superconductors. The prospect of application of the presented model in studies of high- T c superconductors and other superconducting systems of the new generation is also discussed.

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.

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).

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

PubMed

Aydin, Funda Armagan; Soylak, Mustafa

2010-01-15

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

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

PubMed

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

2010-10-22

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

Detecting a wide range of environmental contaminants in human blood samples--combining QuEChERS with LC-MS and GC-MS methods.

PubMed

Plassmann, Merle M; Schmidt, Magdalena; Brack, Werner; Krauss, Martin

2015-09-01

Exposure to environmental pollution and consumer products may result in an uptake of chemicals into human tissues. Several studies have reported the presence of diverse environmental contaminants in human blood samples. However, previously developed multi-target methods for the analysis of human blood include a fairly limited amount of compounds stemming from one or two related compound groups. Thus, the sample preparation method QuEChERS (quick easy cheap effective rugged and safe) was tested for the extraction of 64 analytes covering a broad compound domain followed by detection using liquid and gas chromatography coupled to mass spectrometry (LC- and GC-MS). Forty-seven analytes showed absolute recoveries above 70% in the first QuEChERS step, being a simple liquid-liquid extraction (LLE) using acetonitrile and salt. The second QuEChERS step, being a dispersive solid phase extraction, did not result in an overall improvement of recoveries or removal of background signals. Using solely the LLE step, eight analytes could subsequently be detected in human blood samples from the German Environmental Specimen Bank. Using a LC-multiple reaction monitoring (MRM) method with a triple quadrupole instrument, better recoveries were achieved than with an older LC-high-resolution (HR) MS full scan orbitrap instrument, which required a higher concentration factor of the extracts. However, the application of HRMS full scan methods could be used for the detection of additional compounds retrospectively.

Development, validation and application of a sensitive analytical method for residue determination and dissipation of imidacloprid in sugarcane under tropical field condition.

PubMed

Ramasubramanian, T; Paramasivam, M; Nirmala, R

2016-06-01

A simple and sensitive analytical method has been developed and validated for the determination of trace amounts of imidacloprid in/on sugarcane sett, stalk and leaf. The method optimized in the present study requires less volume of organic solvent and time. Hence, this method is suitable for high-throughput analyses involving large number of samples. The limit of detection (LOD) and limit of quantification (LOQ) of the method were 0.003 and 0.01 mg/kg, respectively. The recovery and relative standard deviation were more than 93 % and less than 4 %, respectively. Thus, it is obvious that the analytical method standardized in this study is more precise and accurate enough to determine the residues of imidacloprid in sugarcane sett, stalk and leaf. The dissipation and translocation of imidacloprid residues from treated cane setts to leaf and stalk were studied by adopting this method. In sugarcane setts, the residues of imidacloprid persisted up to 120 days with half-life of 15.4 days at its recommended dose (70 g a.i./ha). The residues of imidacloprid were found to be translocated from setts to stalk and leaf. The imidacloprid residues were detected up to 105 days in both leaf and stalk. Dipping of sugarcane setts in imidacloprid at its recommended dose may result in better protection of cane setts and established crop because of higher initial deposit (>100 mg/kg) and longer persistence (>120 days).

Determination of acrylamide and methacrylamide by normal phase high performance liquid chromatography and UV detection.

PubMed

Paleologos, E K; Kontominas, M G

2005-06-10

A method using normal phase high performance liquid chromatography (NP-HPLC) with UV detection was developed for the analysis of acrylamide and methacrylamide. The method relies on the chromatographic separation of these analytes on a polar HPLC column designed for the separation of organic acids. Identification of acrylamide and methacrylamide is approached dually, that is directly in their protonated forms and as their hydrolysis products acrylic and methacrylic acid respectively, for confirmation. Detection and quantification is performed at 200 nm. The method is simple allowing for clear resolution of the target peaks from any interfering substances. Detection limits of 10 microg L(-1) were obtained for both analytes with the inter- and intra-day RSD for standard analysis lying below 1.0%. Use of acetonitrile in the elution solvent lowers detection limits and retention times, without impairing resolution of peaks. The method was applied for the determination of acrylamide and methacrylamide in spiked food samples without native acrylamide yielding recoveries between 95 and 103%. Finally, commercial samples of french and roasted fries, cookies, cocoa and coffee were analyzed to assess applicability of the method towards acrylamide, giving results similar with those reported in the literature.

Homogeneous Immunoassays: Historical Perspective and Future Promise

NASA Astrophysics Data System (ADS)

Ullman, Edwin F.

1999-06-01

The founding and growth of Syva Company is examined in the context of its leadership role in the development of homogeneous immunoassays. The simple mix and read protocols of these methods offer advantages in routine analytical and clinical applications. Early homogeneous methods were based on insensitive detection of immunoprecipitation during antigen/antibody binding. The advent of reporter groups in biology provided a means of quantitating immunochemical binding by labeling antibody or antigen and physically separating label incorporated into immune complexes from free label. Although high sensitivity was achieved, quantitative separations were experimentally demanding. Only when it became apparent that reporter groups could provide information, not only about the location of a molecule but also about its microscopic environment, was it possible to design practical non-separation methods. The evolution of early homogenous immunoassays was driven largely by the development of improved detection strategies. The first commercial spin immunoassays, developed by Syva for drug abuse testing during the Vietnam war, were followed by increasingly powerful methods such as immunochemical modulation of enzyme activity, fluorescence, and photo-induced chemiluminescence. Homogeneous methods that quantify analytes at femtomolar concentrations within a few minutes now offer important new opportunities in clinical diagnostics, nucleic acid detection and drug discovery.

A rapid quantitative determination of phenolic acids in Brassica oleracea by capillary zone electrophoresis.

PubMed

Lee, Iris S L; Boyce, Mary C; Breadmore, Michael C

2011-07-15

A simple and rapid capillary zone electrophoresis method to quantitatively determine the phenolic acid contents in brassica vegetables is described. Phenolic compounds were extracted from broccoli, broccolini, Brussels sprouts, cabbage and cauliflower and the main hydroxycinnamic acids (sinapic, ferulic, p-coumaric and caffeic acids) were isolated by solid phase extraction with C18 cartridges. Using an optimised method, the four analytes were separated in less than 7min in a 50μm×60cm capillary with a 15mM borate buffer (pH=9.13) and a separation voltage of 30kV at 30°C. A linear relationship was observed for the method (r=0.9997-0.9999) with detection limits ranging from 1.1 to 2.3mg/kg of vegetables for the analytes. This method demonstrated good reproducibility with coefficients of variation of less than 5% for peak area and less than 1% for migration time (n=7). The method was successfully applied to quantitatively determine the phenolic acid contents in a range of brassica vegetables and the results were in good agreement when compared to those from high performance liquid chromatography analysis. Crown Copyright © 2011. Published by Elsevier Ltd. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2017-09-01

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

Recent Advances in Paper-Based Sensors

PubMed Central

Liana, Devi D.; Raguse, Burkhard; Gooding, J. Justin; Chow, Edith

2012-01-01

Paper-based sensors are a new alternative technology for fabricating simple, low-cost, portable and disposable analytical devices for many application areas including clinical diagnosis, food quality control and environmental monitoring. The unique properties of paper which allow passive liquid transport and compatibility with chemicals/biochemicals are the main advantages of using paper as a sensing platform. Depending on the main goal to be achieved in paper-based sensors, the fabrication methods and the analysis techniques can be tuned to fulfill the needs of the end-user. Current paper-based sensors are focused on microfluidic delivery of solution to the detection site whereas more advanced designs involve complex 3-D geometries based on the same microfluidic principles. Although paper-based sensors are very promising, they still suffer from certain limitations such as accuracy and sensitivity. However, it is anticipated that in the future, with advances in fabrication and analytical techniques, that there will be more new and innovative developments in paper-based sensors. These sensors could better meet the current objectives of a viable low-cost and portable device in addition to offering high sensitivity and selectivity, and multiple analyte discrimination. This paper is a review of recent advances in paper-based sensors and covers the following topics: existing fabrication techniques, analytical methods and application areas. Finally, the present challenges and future outlooks are discussed. PMID:23112667

A simple high performance liquid chromatography method for analyzing paraquat in soil solution samples.

PubMed

Ouyang, Ying; Mansell, Robert S; Nkedi-Kizza, Peter

2004-01-01

A high performance liquid chromatography (HPLC) method with UV detection was developed to analyze paraquat (1,1'-dimethyl-4,4'-dipyridinium dichloride) herbicide content in soil solution samples. The analytical method was compared with the liquid scintillation counting (LSC) method using 14C-paraquat. Agreement obtained between the two methods was reasonable. However, the detection limit for paraquat analysis was 0.5 mg L(-1) by the HPLC method and 0.05 mg L(-1) by the LSC method. The LSC method was, therefore, 10 times more precise than the HPLC method for solution concentrations less than 1 mg L(-1). In spite of the high detection limit, the UC (nonradioactive) HPLC method provides an inexpensive and environmentally safe means for determining paraquat concentration in soil solution compared with the 14C-LSC method.

Integrated miniature fluorescent probe to leverage the sensing potential of ZnO quantum dots for the detection of copper (II) ions.

PubMed

Ng, Sing Muk; Wong, Derrick Sing Nguong; Phung, Jane Hui Chiun; Chin, Suk Fun; Chua, Hong Siang

2013-11-15

Quantum dots are fluorescent semiconductor nanoparticles that can be utilised for sensing applications. This paper evaluates the ability to leverage their analytical potential using an integrated fluorescent sensing probe that is portable, cost effective and simple to handle. ZnO quantum dots were prepared using the simple sol-gel hydrolysis method at ambient conditions and found to be significantly and specifically quenched by copper (II) ions. This ZnO quantum dots system has been incorporated into an in-house developed miniature fluorescent probe for the detection of copper (II) ions in aqueous medium. The probe was developed using a low power handheld black light as excitation source and three photo-detectors as sensor. The sensing chamber placed between the light source and detectors was made of 4-sided clear quartz windows. The chamber was housed within a dark compartment to avoid stray light interference. The probe was operated using a microcontroller (Arduino Uno Revision 3) that has been programmed with the analytical response and the working algorithm of the electronics. The probe was sourced with a 12 V rechargeable battery pack and the analytical readouts were given directly using a LCD display panel. Analytical optimisations of the ZnO quantum dots system and the probe have been performed and further described. The probe was found to have a linear response range up to 0.45 mM (R(2)=0.9930) towards copper (II) ion with a limit of detection of 7.68×10(-7) M. The probe has high repeatable and reliable performance. Copyright © 2013 Elsevier B.V. All rights reserved.

A Simple Transmission Electron Microscopy Method for Fast Thickness Characterization of Suspended Graphene and Graphite Flakes.

PubMed

Rubino, Stefano; Akhtar, Sultan; Leifer, Klaus

2016-02-01

We present a simple, fast method for thickness characterization of suspended graphene/graphite flakes that is based on transmission electron microscopy (TEM). We derive an analytical expression for the intensity of the transmitted electron beam I 0(t), as a function of the specimen thickness t (t<λ; where λ is the absorption constant for graphite). We show that in thin graphite crystals the transmitted intensity is a linear function of t. Furthermore, high-resolution (HR) TEM simulations are performed to obtain λ for a 001 zone axis orientation, in a two-beam case and in a low symmetry orientation. Subsequently, HR (used to determine t) and bright-field (to measure I 0(0) and I 0(t)) images were acquired to experimentally determine λ. The experimental value measured in low symmetry orientation matches the calculated value (i.e., λ=225±9 nm). The simulations also show that the linear approximation is valid up to a sample thickness of 3-4 nm regardless of the orientation and up to several ten nanometers for a low symmetry orientation. When compared with standard techniques for thickness determination of graphene/graphite, the method we propose has the advantage of being simple and fast, requiring only the acquisition of bright-field images.

Construction and electrochemical characterization of microelectrodes for improved sensitivity in paper-based analytical devices

PubMed Central

Santhiago, Murilo; Wydallis, John B.; Kubota, Lauro T.; Henry, Charles S.

2013-01-01

This work presents a simple, low cost method for creating microelectrodes for electrochemical paper-based analytical devices (ePADs). The microelectrodes were constructed by backfilling small holes made in polyester sheets using a CO2 laser etching system. To make electrical connections, the working electrodes were combined with silver screen-printed paper in a sandwich type two-electrode configuration. The devices were characterized using linear sweep voltammetry and the results are in good agreement with theoretical predictions for electrode size and shape. As a proof-of-concept, cysteine was measured using cobalt phthalocyanine as a redox mediator. The rate constant (kobs) for the chemical reaction between cysteine and the redox mediator was obtained by chronoamperometry and found to be on the order of 105 s−1 M−1. Using a microelectrode array, it was possible to reach a limit of detection of 4.8 μM for cysteine. The results show that carbon paste microelectrodes can be easily integrated with paper-based analytical devices. PMID:23581428

Construction and electrochemical characterization of microelectrodes for improved sensitivity in paper-based analytical devices.

PubMed

Santhiago, Murilo; Wydallis, John B; Kubota, Lauro T; Henry, Charles S

2013-05-21

This work presents a simple, low cost method for creating microelectrodes for electrochemical paper-based analytical devices (ePADs). The microelectrodes were constructed by backfilling small holes made in polyester sheets using a CO2 laser etching system. To make electrical connections, the working electrodes were combined with silver screen-printed paper in a sandwich type two-electrode configuration. The devices were characterized using linear sweep voltammetry, and the results are in good agreement with theoretical predictions for electrode size and shape. As a proof-of-concept, cysteine was measured using cobalt phthalocyanine as a redox mediator. The rate constant (k(obs)) for the chemical reaction between cysteine and the redox mediator was obtained by chronoamperometry and found to be on the order of 10(5) s(-1) M(-1). Using a microelectrode array, it was possible to reach a limit of detection of 4.8 μM for cysteine. The results show that carbon paste microelectrodes can be easily integrated with paper-based analytical devices.

Analytical balance-based Faraday magnetometer

NASA Astrophysics Data System (ADS)

Riminucci, Alberto; Uhlarz, Marc; De Santis, Roberto; Herrmannsdörfer, Thomas

2017-03-01

We introduce a Faraday magnetometer based on an analytical balance in which we were able to apply magnetic fields up to 0.14 T. We calibrated it with a 1 mm Ni sphere previously characterized in a superconducting quantum interference device (SQUID) magnetometer. The proposed magnetometer reached a theoretical sensitivity of 3 × 10-8 A m2. We demonstrated its operation on magnetic composite scaffolds made of poly(ɛ-caprolactone)/iron-doped hydroxyapatite. To confirm the validity of the method, we measured the same scaffold properties in a SQUID magnetometer. The agreement between the two measurements was within 5% at 0.127 T and 12% at 24 mT. With the addition, for a small cost, of a permanent magnet and computer controlled linear translators, we were thus able to assemble a Faraday magnetometer based on an analytical balance, which is a virtually ubiquitous instrument. This will make simple but effective magnetometry easily accessible to most laboratories, in particular, to life sciences ones, which are increasingly interested in magnetic materials.

Non-aqueous capillary electrophoretic separation of cholesterol and 25-hydroxycholesterol after derivatization with Girard P reagent.

PubMed

Gregus, Michal; Roberg-Larsen, Hanne; Lundanes, Elsa; Foret, Frantisek; Kuban, Petr; Wilson, Steven Ray

2017-10-01

Capillary electrophoresis (CE) can provide high separation efficiency with very simple instrumentation, but has yet to be explored regarding oxysterols/cholesterol. Cholesterol and 25-hydroxycholesterol (both are 4-ene-3-ketosteroids) were quantitatively transformed into hydrazones using Girard P reagent after enzymatic oxidation by cholesterol oxidase. Separation was achieved using non-aqueous capillary electrophoresis with UV detection at 280nm; the "charge-tagging" Girard P reagent ensured both charge and chromophore (which are requirements for CE-UV). Excess reagent was also separated from the two analytes, eliminating the need for removal prior to the analysis. The compounds were separated in less than 5min with excellent separation efficiency, using separation electrolytes fully compatible with mass spectrometry. The CE-UV method was used to optimize steps for charge-tagging, revealing that the procedure is affected by the analyte/reagent ratio and reaction time, but also the analyte structure. Copyright © 2017 Elsevier B.V. All rights reserved.

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

Understanding wax screen-printing: a novel patterning process for microfluidic cloth-based analytical devices.

PubMed

Liu, Min; Zhang, Chunsun; Liu, Feifei

2015-09-03

In this work, we first introduce the fabrication of microfluidic cloth-based analytical devices (μCADs) using a wax screen-printing approach that is suitable for simple, inexpensive, rapid, low-energy-consumption and high-throughput preparation of cloth-based analytical devices. We have carried out a detailed study on the wax screen-printing of μCADs and have obtained some interesting results. Firstly, an analytical model is established for the spreading of molten wax in cloth. Secondly, a new wax screen-printing process has been proposed for fabricating μCADs, where the melting of wax into the cloth is much faster (∼5 s) and the heating temperature is much lower (75 °C). Thirdly, the experimental results show that the patterning effects of the proposed wax screen-printing method depend to a certain extent on types of screens, wax melting temperatures and melting time. Under optimized conditions, the minimum printing width of hydrophobic wax barrier and hydrophilic channel is 100 μm and 1.9 mm, respectively. Importantly, the developed analytical model is also well validated by these experiments. Fourthly, the μCADs fabricated by the presented wax screen-printing method are used to perform a proof-of-concept assay of glucose or protein in artificial urine with rapid high-throughput detection taking place on a 48-chamber cloth-based device and being performed by a visual readout. Overall, the developed cloth-based wax screen-printing and arrayed μCADs should provide a new research direction in the development of advanced sensor arrays for detection of a series of analytes relevant to many diverse applications. Copyright © 2015 Elsevier B.V. All rights reserved.

Solid-phase microextraction with temperature-programmed desorption for the analysis of iodination disinfection byproducts.

PubMed

Frazey, P A; Barkley, R M; Sievers, R E

1998-02-01

An analytical approach for the determination of chlorination and iodination disinfection byproducts based on solid-phase microextraction (SPME) was developed. Solid-phase microextraction presents a simple, rapid, sensitive, and solvent-free approach to sample preparation in which analytes in either air or water matrixes are extracted into the polymeric coating of an optical fiber. Analytes are subsequently thermally desorbed in the injection port of a gas chromatograph for separation, detection, and quantitation. Thermal degradation of iodoform was observed during desorption from a polyacrylate fiber in initial GC/MS and GC/ECD experiments. Experiments were designed to determine SPME conditions that would allow quantification without significant degradation of analytes. Isothermal and temperature-programmed thermal desorptions were evaluated for efficacy in transferring analytes with wide-ranging volatilities and thermal stabilities into chromatographic analysis columns. A temperature-programmed desorption (TPD) (120-200 degrees C at 5 degrees C/min with an on-column injection port or 150-200 degrees C at 25 degrees C/min with a split/splitless injection port) was able to efficiently remove analytes with wide-ranging volatilities without causing thermal degradation. The SPME-TPD method was linear over 2-3 orders of magnitude with an electron capture detector and detection limits were in the submicrogram per liter range. Precision and detection limits for selected trihalomethanes were comparable to those of EPA method 551. Extraction efficiencies were not affected by the presence of 10 mg/L soap, 15 mg/L sodium iodide, and 6000 mg/L sodium thiosulfate. The SPME-TPD technique was applied to the determination of iodination disinfection byproducts from individual precursor compounds using GC/MS and to the quantitation of iodoform at trace levels in a water recycle system using GC/ECD.

Comparison of maximum runup through analytical and numerical approaches for different fault parameters estimates

NASA Astrophysics Data System (ADS)

Kanoglu, U.; Wronna, M.; Baptista, M. A.; Miranda, J. M. A.

2017-12-01

The one-dimensional analytical runup theory in combination with near shore synthetic waveforms is a promising tool for tsunami rapid early warning systems. Its application in realistic cases with complex bathymetry and initial wave condition from inverse modelling have shown that maximum runup values can be estimated reasonably well. In this study we generate a simplistic bathymetry domains which resemble realistic near-shore features. We investigate the accuracy of the analytical runup formulae to the variation of fault source parameters and near-shore bathymetric features. To do this we systematically vary the fault plane parameters to compute the initial tsunami wave condition. Subsequently, we use the initial conditions to run the numerical tsunami model using coupled system of four nested grids and compare the results to the analytical estimates. Variation of the dip angle of the fault plane showed that analytical estimates have less than 10% difference for angles 5-45 degrees in a simple bathymetric domain. These results shows that the use of analytical formulae for fast run up estimates constitutes a very promising approach in a simple bathymetric domain and might be implemented in Hazard Mapping and Early Warning.

A simple assay for the simultaneous determination of rosuvastatin acid, rosuvastatin-5S-lactone, and N-desmethyl rosuvastatin in human plasma using liquid chromatography-tandem mass spectrometry (LC-MS/MS).

PubMed

Macwan, Joyce S; Ionita, Ileana A; Akhlaghi, Fatemeh

2012-01-01

A simple and sensitive assay was developed and validated for the simultaneous quantification of rosuvastatin acid (RST), rosuvastatin-5S-lactone (RST-LAC), and N-desmethyl rosuvastatin (DM-RST), in buffered human plasma using liquid chromatography-tandem mass spectrometry (LC-MS/MS). All the three analytes and the corresponding deuterium-labeled (d6) internal standards were extracted from 50 μL of buffered human plasma by protein precipitation. The analytes were chromatographically separated using a Zorbax-SB Phenyl column (2.1 mm × 100 mm, 3.5 μm). The mobile phase comprised of a gradient mixture of 0.1% v/v glacial acetic acid in 10% v/v methanol in water (solvent A) and 40% v/v methanol in acetonitrile (solvent B). The analytes were separated at baseline within 6.0 min using a flow rate of 0.35 mL/min. Mass spectrometry detection was carried out in positive electrospray ionization mode. The calibration curves for all three analytes were linear (R ≥ 0.9964, n = 3) over the concentration range of 0.1-100 ng/mL for RST and RST-LAC, and 0.5-100 ng/mL for DM-RST. Mean extraction recoveries ranged within 88.0-106%. Intra- and inter-run mean percent accuracy were within 91.8-111% and percent imprecision was ≤15%. Stability studies revealed that all the analytes were stable in matrix during bench-top (6 h on ice-water slurry), at the end of three successive freeze and thaw cycles and at -80°C for 1 month. The method was successfully applied in a clinical study to determine the concentrations of RST and the lactone metabolite over 12-h post-dose in patients who received a single dose of rosuvastatin.

Nanomaterial-Based Sensing and Biosensing of Phenolic Compounds and Related Antioxidant Capacity in Food.

PubMed

Della Pelle, Flavio; Compagnone, Dario

2018-02-04

Polyphenolic compounds (PCs) have received exceptional attention at the end of the past millennium and as much at the beginning of the new one. Undoubtedly, these compounds in foodstuffs provide added value for their well-known health benefits, for their technological role and also marketing. Many efforts have been made to provide simple, effective and user friendly analytical methods for the determination and antioxidant capacity (AOC) evaluation of food polyphenols. In a parallel track, over the last twenty years, nanomaterials (NMs) have made their entry in the analytical chemistry domain; NMs have, in fact, opened new paths for the development of analytical methods with the common aim to improve analytical performance and sustainability, becoming new tools in quality assurance of food and beverages. The aim of this review is to provide information on the most recent developments of new NMs-based tools and strategies for total polyphenols (TP) determination and AOC evaluation in food. In this review optical, electrochemical and bioelectrochemical approaches have been reviewed. The use of nanoparticles, quantum dots, carbon nanomaterials and hybrid materials for the detection of polyphenols is the main subject of the works reported. However, particular attention has been paid to the success of the application in real samples, in addition to the NMs. In particular, the discussion has been focused on methods/devices presenting, in the opinion of the authors, clear advancement in the fields, in terms of simplicity, rapidity and usability. This review aims to demonstrate how the NM-based approaches represent valid alternatives to classical methods for polyphenols analysis, and are mature to be integrated for the rapid quality assessment of food quality in lab or directly in the field.

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

PubMed

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

2016-01-01

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

Nanomaterial-Based Sensing and Biosensing of Phenolic Compounds and Related Antioxidant Capacity in Food

PubMed Central

2018-01-01

Polyphenolic compounds (PCs) have received exceptional attention at the end of the past millennium and as much at the beginning of the new one. Undoubtedly, these compounds in foodstuffs provide added value for their well-known health benefits, for their technological role and also marketing. Many efforts have been made to provide simple, effective and user friendly analytical methods for the determination and antioxidant capacity (AOC) evaluation of food polyphenols. In a parallel track, over the last twenty years, nanomaterials (NMs) have made their entry in the analytical chemistry domain; NMs have, in fact, opened new paths for the development of analytical methods with the common aim to improve analytical performance and sustainability, becoming new tools in quality assurance of food and beverages. The aim of this review is to provide information on the most recent developments of new NMs-based tools and strategies for total polyphenols (TP) determination and AOC evaluation in food. In this review optical, electrochemical and bioelectrochemical approaches have been reviewed. The use of nanoparticles, quantum dots, carbon nanomaterials and hybrid materials for the detection of polyphenols is the main subject of the works reported. However, particular attention has been paid to the success of the application in real samples, in addition to the NMs. In particular, the discussion has been focused on methods/devices presenting, in the opinion of the authors, clear advancement in the fields, in terms of simplicity, rapidity and usability. This review aims to demonstrate how the NM-based approaches represent valid alternatives to classical methods for polyphenols analysis, and are mature to be integrated for the rapid quality assessment of food quality in lab or directly in the field. PMID:29401719

Analytic algorithms for determining radiative transfer optical properties of ocean waters.

PubMed

Kaskas, Ayse; Güleçyüz, Mustafa C; Tezcan, Cevdet; McCormick, Norman J

2006-10-10

A synthetic model for the scattering phase function is used to develop simple algebraic equations, valid for any water type, for evaluating the ratio of the backscattering to absorption coefficients of spatially uniform, very deep waters with data from upward and downward planar irradiances and the remotely sensed reflectance. The phase function is a variable combination of a forward-directed Dirac delta function plus isotropic scattering, which is an elementary model for strongly forward scattering such as that encountered in oceanic optics applications. The incident illumination at the surface is taken to be diffuse plus a collimated beam. The algorithms are compared with other analytic correlations that were previously derived from extensive numerical simulations, and they are also numerically tested with forward problem results computed with a modified FN method.

The Wide-Field Imaging Interferometry Testbed: Enabling Techniques for High Angular Resolution Astronomy

NASA Technical Reports Server (NTRS)

Rinehart, S. A.; Armstrong, T.; Frey, Bradley J.; Jung, J.; Kirk, J.; Leisawitz, David T.; Leviton, Douglas B.; Lyon, R.; Maher, Stephen; Martino, Anthony J.;

Copper(II)-rubeanic acid coprecipitation system for separation-preconcentration of trace metal ions in environmental samples for their flame atomic absorption spectrometric determinations.

PubMed

Soylak, Mustafa; Erdogan, Nilgun D

2006-09-21

A simple and facile preconcentration procedure based on the coprecipitation of trace heavy metal ions with copper(II)-rubeanic acid complex has been developed. The analytical parameters including pH, amounts of rubeanic acid, sample volume, etc. was investigated for the quantitative recoveries of Pb(II), Fe(III), Cd(II), Au(III), Pd(II) and Ni(II). No interferic effects were observed from the concomitant ions. The detection limits for analyte ions by 3 sigma were in the range of 0.14 microg/l for iron-3.4 microg/l for lead. The proposed coprecipitation method was successfully applied to water samples from Palas Lake-Kayseri, soil and sediment samples from Kayseri and Yozgat-Turkey.