Computer language for identifying chemicals with comprehensive two-dimensional gas chromatography and mass spectrometry.

PubMed

Reichenbach, Stephen E; Kottapalli, Visweswara; Ni, Mingtian; Visvanathan, Arvind

2005-04-15

This paper describes a language for expressing criteria for chemical identification with comprehensive two-dimensional gas chromatography paired with mass spectrometry (GC x GC-MS) and presents computer-based tools implementing the language. The Computer Language for Indentifying Chemicals (CLIC) allows expressions that describe rules (or constraints) for selecting chemical peaks or data points based on multi-dimensional chromatographic properties and mass spectral characteristics. CLIC offers chromatographic functions of retention times, functions of mass spectra, numbers for quantitative and relational evaluation, and logical and arithmetic operators. The language is demonstrated with the compound-class selection rules described by Welthagen et al. [W. Welthagen, J. Schnelle-Kreis, R. Zimmermann, J. Chromatogr. A 1019 (2003) 233-249]. A software implementation of CLIC provides a calculator-like graphical user-interface (GUI) for building and applying selection expressions. From the selection calculator, expressions can be used to select chromatographic peaks that meet the criteria or create selection chromatograms that mask data points inconsistent with the criteria. Selection expressions can be combined with graphical, geometric constraints in the retention-time plane as a powerful component for chemical identification with template matching or used to speed and improve mass spectrum library searches.

Evaluation of comprehensive multidimensional separations using reversed-phase, reversed-phase liquid chromatography/mass spectrometry for shotgun proteomics.

PubMed

Nakamura, Tatsuji; Kuromitsu, Junro; Oda, Yoshiya

2008-03-01

Two-dimensional liquid-chromatographic (LC) separation followed by mass spectrometric (MS) analysis was examined for the identification of peptides in complex mixtures as an alternative to widely used two-dimensional gel electrophoresis followed by MS analysis for use in proteomics. The present method involves the off-line coupling of a narrow-bore, polymer-based, reversed-phase column using an acetonitrile gradient in an alkaline mobile phase in the first dimension with octadecylsilanized silica (ODS)-based nano-LC/MS in the second dimension. After the first separation, successive fractions were acidified and dried off-line, then loaded on the second dimension column. Both columns separate peptides according to hydrophobicity under different pH conditions, but more peptides were identified than with the conventional technique for shotgun proteomics, that is, the combination of a strong cation exchange column with an ODS column, and the system was robust because no salts were included in the mobile phases. The suitability of the method for proteomics measurements was evaluated.

Characterization of Atypical Off-Flavor Compounds in Natural Cork Stoppers by Multidimensional Gas Chromatographic Techniques.

PubMed

Slabizki, Petra; Fischer, Claus; Legrum, Charlotte; Schmarr, Hans-Georg

2015-09-09

Natural cork stoppers with sensory deviations other than the typical cork taint were subgrouped according to their sensory descriptions and compared with unaffected control cork stoppers. The assessment of purge and trap extracts obtained from corresponding cork soaks was performed by heart-cut multidimensional gas chromatography-olfactometry (MDGC-O). The identification of compounds responsible for atypical cork taint detected in MDGC-O was further supported with additional multidimensional GC analysis in combination with mass spectrometric detection. Geosmin and 2-methylisoborneol were mainly found in cork stoppers described as moldy and cellarlike; 3-isopropyl-2-methoxypyrazine and 3-isobutyl-2-methoxypyrazine were found in cork stoppers described with green attributes. Across all cork subgroups, the impact compound for typical cork taint, 2,4,6-trichloroanisole (TCA), was present and is therefore a good marker for cork taint in general. Another potent aroma compound, 3,5-dimethyl-2-methoxypyrazine (MDMP), was also detected in each subgroup, obviously playing an important role with regard to the atypical cork taint. Sensory deviations possibly affecting the wine could be generated by MDMP and its presence should thus be monitored in routine quality control.

Method to fabricate silicon chromatographic column comprising fluid ports

DOEpatents

Manginell, Ronald P.; Frye-Mason, Gregory C.; Heller, Edwin J.; Adkins, Douglas R.

2004-03-02

A new method for fabricating a silicon chromatographic column comprising through-substrate fluid ports has been developed. This new method enables the fabrication of multi-layer interconnected stacks of silicon chromatographic columns.

Chemometric strategy for automatic chromatographic peak detection and background drift correction in chromatographic data.

PubMed

Yu, Yong-Jie; Xia, Qiao-Ling; Wang, Sheng; Wang, Bing; Xie, Fu-Wei; Zhang, Xiao-Bing; Ma, Yun-Ming; Wu, Hai-Long

2014-09-12

Peak detection and background drift correction (BDC) are the key stages in using chemometric methods to analyze chromatographic fingerprints of complex samples. This study developed a novel chemometric strategy for simultaneous automatic chromatographic peak detection and BDC. A robust statistical method was used for intelligent estimation of instrumental noise level coupled with first-order derivative of chromatographic signal to automatically extract chromatographic peaks in the data. A local curve-fitting strategy was then employed for BDC. Simulated and real liquid chromatographic data were designed with various kinds of background drift and degree of overlapped chromatographic peaks to verify the performance of the proposed strategy. The underlying chromatographic peaks can be automatically detected and reasonably integrated by this strategy. Meanwhile, chromatograms with BDC can be precisely obtained. The proposed method was used to analyze a complex gas chromatography dataset that monitored quality changes in plant extracts during storage procedure. Copyright © 2014 Elsevier B.V. All rights reserved.

Chromatographic and computational assessment of lipophilicity using sum of ranking differences and generalized pair-correlation.

PubMed

Andrić, Filip; Héberger, Károly

2015-02-06

Lipophilicity (logP) represents one of the most studied and most frequently used fundamental physicochemical properties. At present there are several possibilities for its quantitative expression and many of them stems from chromatographic experiments. Numerous attempts have been made to compare different computational methods, chromatographic methods vs. computational approaches, as well as chromatographic methods and direct shake-flask procedure without definite results or these findings are not accepted generally. In the present work numerous chromatographically derived lipophilicity measures in combination with diverse computational methods were ranked and clustered using the novel variable discrimination and ranking approaches based on the sum of ranking differences and the generalized pair correlation method. Available literature logP data measured on HILIC, and classical reversed-phase combining different classes of compounds have been compared with most frequently used multivariate data analysis techniques (principal component and hierarchical cluster analysis) as well as with the conclusions in the original sources. Chromatographic lipophilicity measures obtained under typical reversed-phase conditions outperform the majority of computationally estimated logPs. Oppositely, in the case of HILIC none of the many proposed chromatographic indices overcomes any of the computationally assessed logPs. Only two of them (logkmin and kmin) may be selected as recommended chromatographic lipophilicity measures. Both ranking approaches, sum of ranking differences and generalized pair correlation method, although based on different backgrounds, provides highly similar variable ordering and grouping leading to the same conclusions. Copyright © 2015. Published by Elsevier B.V.

A Comparative Study of Online Item Calibration Methods in Multidimensional Computerized Adaptive Testing

ERIC Educational Resources Information Center

Chen, Ping

2017-01-01

Calibration of new items online has been an important topic in item replenishment for multidimensional computerized adaptive testing (MCAT). Several online calibration methods have been proposed for MCAT, such as multidimensional "one expectation-maximization (EM) cycle" (M-OEM) and multidimensional "multiple EM cycles"…

[Identification of impurity peaks in the HPLC chromatogram by LC-MS and two-dimensional chromatographic correlation spectroscopy].

PubMed

Chen, Zhen-Zhen; Zhang, Dou-Sheng; Wang, Nan; Feng, Fang; Hu, Chang-Qin

2012-04-01

A novel qualitative analytical method by using two-dimensional chromatographic correlation spectroscopy techniques for recognizing impurity peaks of HPLC methods of quality control and LC-MS chromatographic system was established. The structures of major degradation products of ceftizoxime and cefdinir were identified by LC-MS and MassWorks application; the standard chromatographic and spectral data of the degradation impurities were obtained by high-performance liquid chromatography with diode array detection. The impurity peaks of two-dimensional chromatography were matched by comparison of spectra and calculating correlation coefficients. Peaks in chromatography can be identified accurately and rapidly in different chromatographic systems such as column and mobile phase changed. The method provides a new way and thought to identify the peaks in quality control of impurities without reference impurity substances.

Method for the chromatographic separation of cations from aqueous samples

DOEpatents

Horwitz, E.P.; Chiarizia, R.; Dietz, M.L.

1997-07-29

An extraction chromatographic material is described for extracting metal cations from a liquid stream. The extraction chromatographic material is prepared by adsorbing a diesterified methanediphosphonic acid on an inert particulate support. 7 figs.

Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection

PubMed Central

Heshka, Nicole E.; Hager, Darcy B.

2015-01-01

A method for the analysis of dissolved hydrogen sulfide in crude oil samples is demonstrated using gas chromatography. In order to effectively eliminate interferences, a two dimensional column configuration is used, with a Deans switch employed to transfer hydrogen sulfide from the first to the second column (heart-cutting). Liquid crude samples are first separated on a dimethylpolysiloxane column, and light gases are heart-cut and further separated on a bonded porous layer open tubular (PLOT) column that is able to separate hydrogen sulfide from other light sulfur species. Hydrogen sulfide is then detected with a sulfur chemiluminescence detector, adding an additional layer of selectivity. Following separation and detection of hydrogen sulfide, the system is backflushed to remove the high-boiling hydrocarbons present in the crude samples and to preserve chromatographic integrity. Dissolved hydrogen sulfide has been quantified in liquid samples from 1.1 to 500 ppm, demonstrating wide applicability to a range of samples. The method has also been successfully applied for the analysis of gas samples from crude oil headspace and process gas bags, with measurement from 0.7 to 9,700 ppm hydrogen sulfide. PMID:26709594

Method for the chromatographic separation of cations from aqueous samples

DOEpatents

Horwitz, E.P.; Chiarizia, R.; Dietz, M.L.

1998-12-22

An extraction chromatographic material is described for extracting metal cations from a liquid stream. The extraction chromatographic material is prepared by adsorbing a diesterified methane-diphosphonic acid on an inert particulate support. 7 figs.

The Tunneling Method for Global Optimization in Multidimensional Scaling.

ERIC Educational Resources Information Center

Groenen, Patrick J. F.; Heiser, Willem J.

1996-01-01

A tunneling method for global minimization in multidimensional scaling is introduced and adjusted for multidimensional scaling with general Minkowski distances. The method alternates a local search step with a tunneling step in which a different configuration is sought with the same STRESS implementation. (SLD)

The gas-chromatographic and gas-chromatographic-mass-spectrometric identification of halogen-containing organic compounds

NASA Astrophysics Data System (ADS)

Gidaspov, B. V.; Zenkevich, I. G.; Rodin, A. A.

1989-09-01

The problem of identifying halogen-containing organic compounds in their gas-chromatographic and gas-chromatographic-mass-spectrometric (GC-MS) determination in different materials has been examined. Particular attention has been paid not to the complete characterisation of methods for carrying out this analysis but to the most important problem of increasing the selectivity at the stages of sampling, separation, and interpretation of the gas-chromatographic and GC-MS information. The bibliography contains 292 references.

21 CFR 172.860 - Fatty acids.

Code of Federal Regulations, 2013 CFR

2013-04-01

... the gas chromatographic-electron capture method prescribed in paragraph (c)(3) of this section. If..._locations.html. (3) The gas chromatographic-electron capture method for testing fatty acids for chick-edema...

21 CFR 172.860 - Fatty acids.

Code of Federal Regulations, 2012 CFR

2012-04-01

... the gas chromatographic-electron capture method prescribed in paragraph (c)(3) of this section. If..._locations.html. (3) The gas chromatographic-electron capture method for testing fatty acids for chick-edema...

[A method for the analysis of overlapped peaks in the high performance liquid chromatogram based on spectrum analysis].

PubMed

Liu, Bao; Fan, Xiaoming; Huo, Shengnan; Zhou, Lili; Wang, Jun; Zhang, Hui; Hu, Mei; Zhu, Jianhua

2011-12-01

A method was established to analyse the overlapped chromatographic peaks based on the chromatographic-spectra data detected by the diode-array ultraviolet detector. In the method, the three-dimensional data were de-noised and normalized firstly; secondly the differences and clustering analysis of the spectra at different time points were calculated; then the purity of the whole chromatographic peak were analysed and the region were sought out in which the spectra of different time points were stable. The feature spectra were extracted from the spectrum-stable region as the basic foundation. The nonnegative least-square method was chosen to separate the overlapped peaks and get the flow curve which was based on the feature spectrum. The three-dimensional divided chromatographic-spectrum peak could be gained by the matrix operations of the feature spectra with the flow curve. The results displayed that this method could separate the overlapped peaks.

MS-Electronic Nose Performance Improvement Using GC Retention Times And 2-Way And 3-Way Data Processing Methods

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

Burian, Cosmin; Llobet, Eduard; Vilanova, Xavier

We have designed a challenging experimental sample set in the form of 20 solutions with a high degree of similarity in order to study whether the addition of chromatographic separation information improves the performance of regular MS based electronic noses. In order to make an initial study of the approach, two different chromatographic methods were used. By processing the data of these experiments with 2 and 3-way algorithms, we have shown that the addition of chromatographic separation information improves the results compared to the 2-way analysis of mass spectra or total ion chromatogram treated separately. Our findings show that whenmore » the chromatographic peaks are resolved (longer measurement times), 2-way methods work better than 3-way methods, whereas in the case of a more challenging measurement (more coeluted chromatograms, much faster GC-MS measurements) 3-way methods work better.« less

A Novel High Performance Liquid Chromatographic Method for Simultaneous Determination of Ceftriaxone and Sulbactam in Sulbactomax

PubMed Central

Shrivastava, Sanjay Mohan; Singh, Rajkumar; Tariq, Abu; Siddiqui, Masoom Raza; Yadav, Jitendar; Negi, P. S.; Chaudhary, Manu

2009-01-01

An isocratic liquid chromatographic method with UV detection at 220 nm is described for simultaneous determination of ceftriaxone sodium and sulbactam sodium in Sulbactomax. Chromatographic separation of two drugs was achieved on a Hypersil ODS C-18 column using a mobile phase consisting of a binary mixture of acetonitrile and tetrabutyl ammonium hydroxide adjusted to pH7.0 with orthophosphoric acid in ratio 70:30. The developed Liquid Chromatographic method offers symmetric peak shape, good resolution and reasonable retention time for both drugs. Linearity, accuracy and precision were found to be acceptable over the concentration range of 125-750 ppm for ceftriaxone sodium and 62.5-375 ppm for sulbactam sodium. The LC method can be used for the quality control of formulated products containing ceftriaxone and sulbactam. PMID:23675112

Probabilistic peak detection for first-order chromatographic data.

PubMed

Lopatka, M; Vivó-Truyols, G; Sjerps, M J

2014-03-19

We present a novel algorithm for probabilistic peak detection in first-order chromatographic data. Unlike conventional methods that deliver a binary answer pertaining to the expected presence or absence of a chromatographic peak, our method calculates the probability of a point being affected by such a peak. The algorithm makes use of chromatographic information (i.e. the expected width of a single peak and the standard deviation of baseline noise). As prior information of the existence of a peak in a chromatographic run, we make use of the statistical overlap theory. We formulate an exhaustive set of mutually exclusive hypotheses concerning presence or absence of different peak configurations. These models are evaluated by fitting a segment of chromatographic data by least-squares. The evaluation of these competing hypotheses can be performed as a Bayesian inferential task. We outline the potential advantages of adopting this approach for peak detection and provide several examples of both improved performance and increased flexibility afforded by our approach. Copyright © 2014 Elsevier B.V. All rights reserved.

Rapid isolation, reliable characterization, and water solubility improvement of polymethoxyflavones from cold-pressed mandarin essential oil.

PubMed

Russo, Marina; Rigano, Francesca; Arigò, Adriana; Sciarrone, Danilo; Calabrò, Maria Luisa; Farnetti, Sara; Dugo, Paola; Mondello, Luigi

2016-06-01

Polymethoxyflavones possess many biological properties, as lipid-lowering, hypoglycaemic, anti-inflammatory, antioxidant, and anticancer activities, therefore, they may be employed as nutraceuticals or therapeutic agents. The scarcity of pure polymethoxyflavones on the market as well as their low water solubility limited in vivo studies and the use of polymethoxyflavones as food or pharmaceutical supplements. Since mandarin peels are a rich source of polymethoxyflavones, tangeretin, nobiletin, sinensetin, tetra-O-methyl scutellarein, and heptamethoxyflavone were purified from a nonvolatile residue of a cold-pressed mandarin essential oil using a multidimensional preparative liquid chromatographic system coupled with a photodiode array detector and a single quadrupole mass spectrometer. A new prototype, consisting of a nano-liquid chromatography system coupled with an electron ionization mass spectrometer, was used for the characterization of the pure isolated molecules. Finally, due to the collection of highly pure nobiletin and tangeretin, the ability of 2-hydroxypropyl-β-cyclodextrin to enhance the water solubility of both polymethoxyflavones was evaluated by phase solubility studies and Job's plot method. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Chromatographic immunoassays: strategies and recent developments in the analysis of drugs and biological agents

PubMed Central

Matsuda, Ryan; Rodriguez, Elliott; Suresh, Doddavenkatanna; Hage, David S

2015-01-01

A chromatographic immunoassay is a technique in which an antibody or antibody-related agent is used as part of a chromatographic system for the isolation or measurement of a specific target. Various binding agents, detection methods, supports and assay formats have been developed for this group of methods, and applications have been reported that range from drugs, hormones and herbicides to peptides, proteins and bacteria. This review discusses the general principles and applications of chromatographic immunoassays, with an emphasis being given to methods and formats that have been developed for the analysis of drugs and biological agents. The relative advantages or limitations of each format are discussed. Recent developments and research in this field, as well as possible future directions, are also considered. PMID:26571109

Multidimensional spectrometer

DOEpatents

Zanni, Martin Thomas; Damrauer, Niels H.

2010-07-20

A multidimensional spectrometer for the infrared, visible, and ultraviolet regions of the electromagnetic spectrum, and a method for making multidimensional spectroscopic measurements in the infrared, visible, and ultraviolet regions of the electromagnetic spectrum. The multidimensional spectrometer facilitates measurements of inter- and intra-molecular interactions.

Multidimensional upwind hydrodynamics on unstructured meshes using graphics processing units - I. Two-dimensional uniform meshes

NASA Astrophysics Data System (ADS)

Paardekooper, S.-J.

2017-08-01

We present a new method for numerical hydrodynamics which uses a multidimensional generalization of the Roe solver and operates on an unstructured triangular mesh. The main advantage over traditional methods based on Riemann solvers, which commonly use one-dimensional flux estimates as building blocks for a multidimensional integration, is its inherently multidimensional nature, and as a consequence its ability to recognize multidimensional stationary states that are not hydrostatic. A second novelty is the focus on graphics processing units (GPUs). By tailoring the algorithms specifically to GPUs, we are able to get speedups of 100-250 compared to a desktop machine. We compare the multidimensional upwind scheme to a traditional, dimensionally split implementation of the Roe solver on several test problems, and we find that the new method significantly outperforms the Roe solver in almost all cases. This comes with increased computational costs per time-step, which makes the new method approximately a factor of 2 slower than a dimensionally split scheme acting on a structured grid.

Method for liquid chromatographic extraction of strontium from acid solutions

DOEpatents

Horwitz, E. Philip; Dietz, Mark L.

1992-01-01

A method and apparatus for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column is described. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water.

DEVELOPMENT AND VALIDATION OF AN ION CHROMATOGRAPHIC METHOD FOR DETERMINING PERCHLORATE IN FERTILIZERS

EPA Science Inventory

A method has been developed for the determination of perchlorate in fertilizers. Materials are leached with deionized water to dissolve any soluble perchlorate compounds. Ion chromatographic separation is followed by suppressed conductivity for detection. Perchlorate is retained ...

Mixed-bed ion exchange chromatography employing a salt-free pH gradient for improved sensitivity and compatibility in MudPIT.

PubMed

Mommen, Geert P M; Meiring, Hugo D; Heck, Albert J R; de Jong, Ad P J M

2013-07-16

In proteomics, comprehensive analysis of peptides mixtures necessitates multiple dimensions of separation prior to mass spectrometry analysis to reduce sample complexity and increase the dynamic range of analysis. The main goal of this work was to improve the performance of (online) multidimensional protein identification technology (MudPIT) in terms of sensitivity, compatibility and recovery. The method employs weak anion and strong cation mixed-bed ion exchange chromatography (ACE) in the first separation dimension and reversed phase chromatography (RP) in the second separation dimension (Motoyama et.al. Anal. Chem 2007, 79, 3623-34.). We demonstrated that the chromatographic behavior of peptides in ACE chromatography depends on both the WAX/SCX mixing ratio as the ionic strength of the mobile phase system. This property allowed us to replace the conventional salt gradient by a (discontinuous) salt-free, pH gradient. First dimensional separation of peptides was accomplished with mixtures of aqueous formic acid and dimethylsulfoxide with increasing concentrations. The overall performance of this mobile phase system was found comparable to ammonium acetate buffers in application to ACE chromatography, but clearly outperformed strong cation exchange for use in first dimensional peptide separation. The dramatically improved compatibility between (salt-free) ion exchange chromatography and reversed phase chromatography-mass spectrometry allowed us to downscale the dimensions of the RP analytical column down to 25 μm i.d. for an additional 2- to 3-fold improvement in performance compared to current technology. The achieved levels of sensitivity, orthogonality, and compatibility demonstrates the potential of salt-free ACE MudPIT for the ultrasensitive, multidimensional analysis of very modest amounts of sample material.

The Efficacy of Multidimensional Constraint Keys in Database Query Performance

ERIC Educational Resources Information Center

Cardwell, Leslie K.

2012-01-01

This work is intended to introduce a database design method to resolve the two-dimensional complexities inherent in the relational data model and its resulting performance challenges through abstract multidimensional constructs. A multidimensional constraint is derived and utilized to implement an indexed Multidimensional Key (MK) to abstract a…

Multidimensional Programming Methods for Energy Facility Siting: Alternative Approaches

NASA Technical Reports Server (NTRS)

Solomon, B. D.; Haynes, K. E.

1982-01-01

The use of multidimensional optimization methods in solving power plant siting problems, which are characterized by several conflicting, noncommensurable objectives is addressed. After a discussion of data requirements and exclusionary site screening methods for bounding the decision space, classes of multiobjective and goal programming models are discussed in the context of finite site selection. Advantages and limitations of these approaches are highlighted and the linkage of multidimensional methods with the subjective, behavioral components of the power plant siting process is emphasized.

GENERAL: Scattering Phase Correction for Semiclassical Quantization Rules in Multi-Dimensional Quantum Systems

NASA Astrophysics Data System (ADS)

Huang, Wen-Min; Mou, Chung-Yu; Chang, Cheng-Hung

2010-02-01

While the scattering phase for several one-dimensional potentials can be exactly derived, less is known in multi-dimensional quantum systems. This work provides a method to extend the one-dimensional phase knowledge to multi-dimensional quantization rules. The extension is illustrated in the example of Bogomolny's transfer operator method applied in two quantum wells bounded by step potentials of different heights. This generalized semiclassical method accurately determines the energy spectrum of the systems, which indicates the substantial role of the proposed phase correction. Theoretically, the result can be extended to other semiclassical methods, such as Gutzwiller trace formula, dynamical zeta functions, and semiclassical Landauer-Büttiker formula. In practice, this recipe enhances the applicability of semiclassical methods to multi-dimensional quantum systems bounded by general soft potentials.

The Protein/Peptide Direct Virus Inactivation During Chromatographic Process: Developing Approaches.

PubMed

Volkov, Georgii L; Havryliuk, Sergiy P; Krasnobryzha, Ievgenia M; Havryliuk, Olena S

2017-01-01

Virus clearance is required for pharmaceutical preparations derived from animal or human sources such as blood products, vaccines, recombinant proteins produced in mammalian cell lines, etc. High cost and substantial protein losses during virus inactivation are significant problems for protein/peptide manufacturing. The goal of this project was to develop a method to perform virus inactivation in a course of protein chromatographic purification. Another goal was to show that the chromatographic adsorbent can serve as reliable "sieva" for mechanical washing away of infecting viruses. Using chromatographic, photometric, IFA, and RT-PCR approaches, it was discovered that high temperature-depending dynamic capacity of adsorbent allowed to perform a virus inactivation directly in a chromatographic column by solvent/detergent treatment. The peptide/protein biological activity was completely preserved. Using this new approach enveloped and nonenveloped viruses were effectively removed protein preparation. In addition, it was shown that RT-PCR method demonstrates more precise and reproducible results and robust properties for assessment of virus reduction than virus titer followed by infectivity studies. Presented method allowed to obtain the factor of virus concentration decrease (FVD) values that were higher than those provided by known technologies and was sufficient for a full inactivation of viruses. The method is recommended to use in pharmaceutical industry.

Determination of pore size distributions of porous chromatographic adsorbents by inverse size-exclusion chromatography.

PubMed

Yao, Yan; Lenhoff, Abraham M

2004-05-28

The macroscopic properties of porous chromatographic adsorbents are directly influenced by the pore structure, with the pore size distribution (PSD) playing a major role beyond simply the mean pore size. Inverse size-exclusion chromatography (ISEC), a widely used chromatographic method for determining the PSD of porous media, provides more relevant information on liquid chromatographic materials in situ than traditional methods, such as gas sorption and mercury intrusion. The fundamentals and applications of ISEC in the characterization of the pore structure are reviewed. The description of the probe solutes and the pore space, as well as theoretical models for deriving the PSD from solute partitioning behavior, are discussed. Precautions to ensure integrity of the experiments are also outlined, including accounting for probe polydispersity and minimization of solute-adsorbent interactions. The results that emerge are necessarily model-dependent, but ISEC nonetheless represents a powerful and non-destructive source of quantitative pore structure information that can help to elucidate chromatographic performance observations covering both retention and rate aspects.

Method of data mining including determining multidimensional coordinates of each item using a predetermined scalar similarity value for each item pair

DOEpatents

Meyers, Charles E.; Davidson, George S.; Johnson, David K.; Hendrickson, Bruce A.; Wylie, Brian N.

1999-01-01

A method of data mining represents related items in a multidimensional space. Distance between items in the multidimensional space corresponds to the extent of relationship between the items. The user can select portions of the space to perceive. The user also can interact with and control the communication of the space, focusing attention on aspects of the space of most interest. The multidimensional spatial representation allows more ready comprehension of the structure of the relationships among the items.

Gas chromatograph-mass spectrometer (GC/MS) system for quantitative analysis of reactive chemical compounds

DOEpatents

Grindstaff, Quirinus G.

1992-01-01

Described is a new gas chromatograph-mass spectrometer (GC/MS) system and method for quantitative analysis of reactive chemical compounds. All components of such a GC/MS system external to the oven of the gas chromatograph are programmably temperature controlled to operate at a volatilization temperature specific to the compound(s) sought to be separated and measured.

[UPLC characteristic chromatographic profile of Poria].

PubMed

Zhang, Qi; Wang, Zhenzhong; Xiao, Wei; Zhang, Liangqi; Bi, Kaishun; Jia, Ying

2012-04-01

To establish a UPLC characteristic chromatographic profile analysis method to quickly assess Poria quality and provide basis fro controlling Poria quality. The UPLC characteristic chromatographic profiles of fifteen batches of Poria were determined by ACQUITY UPLC, with HSS T3 Column (2.1 mm x 100 mm, 1.8 microm) eluted with the mobile phases of water containing 0.05% phosphoric acid and acetonitrile in gradient mode. The detection wavelength was set at 243 nm. The common mode of the UPLC characteristic chromatographic profile was set up. There were 20 common peaks, seven of which were identified, and the similar degrees of the fifteen samples to the common mode were between 0.787 and 0.974. The method was so time-saving that it can be used for the quality control of Poria.

Simple automatic strategy for background drift correction in chromatographic data analysis.

PubMed

Fu, Hai-Yan; Li, He-Dong; Yu, Yong-Jie; Wang, Bing; Lu, Peng; Cui, Hua-Peng; Liu, Ping-Ping; She, Yuan-Bin

2016-06-03

Chromatographic background drift correction, which influences peak detection and time shift alignment results, is a critical stage in chromatographic data analysis. In this study, an automatic background drift correction methodology was developed. Local minimum values in a chromatogram were initially detected and organized as a new baseline vector. Iterative optimization was then employed to recognize outliers, which belong to the chromatographic peaks, in this vector, and update the outliers in the baseline until convergence. The optimized baseline vector was finally expanded into the original chromatogram, and linear interpolation was employed to estimate background drift in the chromatogram. The principle underlying the proposed method was confirmed using a complex gas chromatographic dataset. Finally, the proposed approach was applied to eliminate background drift in liquid chromatography quadrupole time-of-flight samples used in the metabolic study of Escherichia coli samples. The proposed method was comparable with three classical techniques: morphological weighted penalized least squares, moving window minimum value strategy and background drift correction by orthogonal subspace projection. The proposed method allows almost automatic implementation of background drift correction, which is convenient for practical use. Copyright © 2016 Elsevier B.V. All rights reserved.

Nonlinear Conservation Laws and Finite Volume Methods

NASA Astrophysics Data System (ADS)

Leveque, Randall J.

Introduction Software Notation Classification of Differential Equations Derivation of Conservation Laws The Euler Equations of Gas Dynamics Dissipative Fluxes Source Terms Radiative Transfer and Isothermal Equations Multi-dimensional Conservation Laws The Shock Tube Problem Mathematical Theory of Hyperbolic Systems Scalar Equations Linear Hyperbolic Systems Nonlinear Systems The Riemann Problem for the Euler Equations Numerical Methods in One Dimension Finite Difference Theory Finite Volume Methods Importance of Conservation Form - Incorrect Shock Speeds Numerical Flux Functions Godunov's Method Approximate Riemann Solvers High-Resolution Methods Other Approaches Boundary Conditions Source Terms and Fractional Steps Unsplit Methods Fractional Step Methods General Formulation of Fractional Step Methods Stiff Source Terms Quasi-stationary Flow and Gravity Multi-dimensional Problems Dimensional Splitting Multi-dimensional Finite Volume Methods Grids and Adaptive Refinement Computational Difficulties Low-Density Flows Discrete Shocks and Viscous Profiles Start-Up Errors Wall Heating Slow-Moving Shocks Grid Orientation Effects Grid-Aligned Shocks Magnetohydrodynamics The MHD Equations One-Dimensional MHD Solving the Riemann Problem Nonstrict Hyperbolicity Stiffness The Divergence of B Riemann Problems in Multi-dimensional MHD Staggered Grids The 8-Wave Riemann Solver Relativistic Hydrodynamics Conservation Laws in Spacetime The Continuity Equation The 4-Momentum of a Particle The Stress-Energy Tensor Finite Volume Methods Multi-dimensional Relativistic Flow Gravitation and General Relativity References

Best Design for Multidimensional Computerized Adaptive Testing With the Bifactor Model

PubMed Central

Seo, Dong Gi; Weiss, David J.

2015-01-01

Most computerized adaptive tests (CATs) have been studied using the framework of unidimensional item response theory. However, many psychological variables are multidimensional and might benefit from using a multidimensional approach to CATs. This study investigated the accuracy, fidelity, and efficiency of a fully multidimensional CAT algorithm (MCAT) with a bifactor model using simulated data. Four item selection methods in MCAT were examined for three bifactor pattern designs using two multidimensional item response theory models. To compare MCAT item selection and estimation methods, a fixed test length was used. The Ds-optimality item selection improved θ estimates with respect to a general factor, and either D- or A-optimality improved estimates of the group factors in three bifactor pattern designs under two multidimensional item response theory models. The MCAT model without a guessing parameter functioned better than the MCAT model with a guessing parameter. The MAP (maximum a posteriori) estimation method provided more accurate θ estimates than the EAP (expected a posteriori) method under most conditions, and MAP showed lower observed standard errors than EAP under most conditions, except for a general factor condition using Ds-optimality item selection. PMID:29795848

High-performance liquid chromatographic method for potency determination of amoxicillin in commercial preparations and for stability studies.

PubMed Central

Hsu, M C; Hsu, P W

1992-01-01

A reversed-phase column liquid chromatographic method was developed for the assay of amoxicillin and its preparations. The linear calibration range was 0.2 to 2.0 mg/ml (r = 0.9998), and recoveries were generally greater than 99%. The high-performance liquid chromatographic assay results were compared with those obtained from a microbiological assay of bulk drug substance and capsule, injection, and granule formulations containing amoxicillin and degraded amoxicillin. At the 99% confidence level, no significant intermethod differences were noted for the paired results. Commercial formulations were also analyzed, and the results obtained by the proposed method closely agreed with those found by the microbiological method. The results indicated that the proposed method is a suitable substitute for the microbiological method for assays and stability studies of amoxicillin preparations. PMID:1416827

Application of a multidimensional gas chromatography system with simultaneous mass spectrometric and flame ionization detection to the analysis of sandalwood oil.

PubMed

Sciarrone, Danilo; Costa, Rosaria; Ragonese, Carla; Tranchida, Peter Quinto; Tedone, Laura; Santi, Luca; Dugo, Paola; Dugo, Giovanni; Joulain, Daniel; Mondello, Luigi

2011-01-07

The production and trade of Indian sandalwood oil is strictly regulated, due to the impoverishment of the plantations; for such a reason, Australian sandalwood oil has been evaluated as a possible substitute of the Indian type. International directives report, for both the genuine essential oils, specific ranges for the sesquiterpene alcohols (santalols). In the present investigation, a multidimensional gas chromatographic system (MDGC), equipped with simultaneous flame ionization and mass spectrometric detection (FID/MS), has been successfully applied to the analysis of a series of sandalwood oils of different origin. A detailed description of the system utilized is reported. Three santalol isomers, (Z)-α-trans-bergamotol, (E,E)-farnesol, (Z)-nuciferol, epi-α-bisabolol and (Z)-lanceol have been quantified. LoD (MS) and LoQ (FID) values were determined for (E,E)-farnesol, used as representative of the oxygenated sesquiterpenic group, showing levels equal to 0.002% and 0.003%, respectively. A great advantage of the instrumental configuration herein discussed, is represented by the fact that identification and quantitation of target analytes are carried out in one step, without the need to perform two separate analyses. Copyright © 2010 Elsevier B.V. All rights reserved.

Gas Chromatographic Determination of Enrivonmentally Significant Pesticides.

ERIC Educational Resources Information Center

Rudzinski, Walter E.; Beu, Steve

1982-01-01

A chromatographic procedure for analyzing organophosphorus pesticides (such as PCB's, nitrosamines, and phthalate esters) in orange juice is described, including a summary of the method, instrumentation, methodology, results/discussion, and calculations. (JN)

Chromatographic determination of the diffusion coefficients of light hydrocarbons in polymers

NASA Astrophysics Data System (ADS)

Yakubenko, E. E.; Korolev, A. A.; Chapala, P. P.; Bermeshev, M. V.; Kanat'eva, A. Yu.; Kurganov, A. A.

2017-01-01

Gas-chromatographic determination of the diffusion coefficients that allows for the compressibility of the mobile phase has been suggested. The diffusion coefficients were determined for light hydrocarbons C1-C4 in four polymers with a high free volume, which are candidates for use as gas-separating membranes. The diffusion coefficients calculated from chromatographic data were shown to be one or two orders of magnitude smaller than the values obtained by the membrane method. This may be due to the presence of an additional flow through the membrane caused by the pressure gradient across the membrane in membrane methods.

INTERLABORATORY STUDY OF A THERMOSPRAY-LIQUID CHROMATOGRAPHIC/MASS SPECTROMETRIC METHOD FOR SELECTED N-METHYL CARBAMATES, N-METHYL CARBAMOYLOXIMES, AND SUBSTITUTED UREA PESTICIDES

EPA Science Inventory

A thermospray-liquid chromatographic/mass spectrometric (TS-LC/MS) method was evaluated in an interlaboratory study for determining 3 N-methyl carbamates (bendiocarb, carbaryl, and carbofuran), 3-N-methyl carbamoyloximes (aldicarb, methomyl, and oxamyl), 2 substituted urea pestic...

LIQUID CHROMATOGRAPHIC DETERMINATION OF 5-(METHYLAMINO)-2-PHENYL-4-[3-(TRIFLUROMETHYL) PHENYL]-3-(2H)-FURANONE IN SOIL

EPA Science Inventory

A rapid, sensitive method is described for the determination of 5-(methylamino)-2-phenyl-4-[3-(trifluromethyl)phenyl]-3-(2H)-furanone RE-40885) concentrations in three soil types. he method consists of extraction of soil samples with methanol, filtration, liquid chromatographic s...

High Performance Liquid Chromatographic Analysis of Phytoplankton Pigments Using a C16-Amide Column

EPA Science Inventory

A reverse-phase high performance liquid chromatographic (RP-HPLC) method was developed to analyze in a single run, most polar and non-polar chlorophylls and carotenoids from marine phytoplankton. The method is based on a RP-C16-Amide column and a ternary gradient system consistin...

Chromatographic and mass spectral methods of identification for the side-chain and ring regioisomers of methylenedioxymethamphetamine.

PubMed

Aalberg, L; DeRuiter, J; Noggle, F T; Sippola, E; Clark, C R

2000-08-01

The popular drug of abuse 3,4-methylenedioxymethamphetamine (MDMA) is one of a total of 10 regioisomeric 2,3- and 3,4-methylenedioxyphenethylamines of MW 193 that yields regioisomeric fragment ions with equivalent mass (m/z 58 and 135/136) in the electron-impact (EI) mass spectrum. Thus, these 10 methylenedioxyphenethylamines are uniquely isomeric; they have the same molecular weight and equivalent major fragments in their mass spectra. The specific identification of one of these compounds (i.e., Ecstasy or 3,4-MDMA) in a forensic drug sample depends upon the analyst's ability to eliminate the other regioisomers as possible interfering or coeluting substances. This study reports the synthesis, chemical properties, spectral characterization, and chromatographic analysis of these 10 unique regioisomers. The ten 2,3- and 3,4-regioisomers of MDMA are synthesized from commercially available precursor chemicals. In the EI mass spectra, the side-chain regioisomers show some variation in the relative intensity of the major ions, with the exception of only one or two minor ions that might be considered side-chain specific fragments. The position of substitution for the methylenedioxy ring is not easily determined by mass spectral techniques, and the ultimate identification of any one of these amines with the elimination of the other nine must depend heavily upon chromatographic methods. The chromatographic separation of these 10 uniquely regioisomeric amines are studied using reversed-phase liquid chromatographic methods with gradient elution and gas chromatographic techniques with temperature program optimization.

Simultaneous enantioselective separation of polychlorinated biphenyls and their methyl sulfone metabolites by heart-cut MDGC: determination of enantiomeric fractions in fish oils and cow liver samples.

PubMed

Pérez-Fernández, Virginia; Castro-Puyana, María; González, María José; Marina, María Luisa; García, María Ángeles; Gómara, Belén

2012-07-01

The potential of three capillary columns based on β-cyclodextrin (i.e., Chirasil-Dex, BGB-172, and BGB-176SE) has been studied for the simultaneous enantiomeric separation of polychlorinated biphenyls (PCBs) and methylsulfonyl metabolites of PCBs (MeSO(2)-PCBs) employing a heart-cut multidimensional gas chromatographic system (heart-cut MDGC). Among the columns studied, the BGB-176SE capillary column provided the best results, allowing the simultaneous enantioselective resolution of six MeSO(2)-PCBs and six chiral PCBs; the Chirasil-Dex column did not resolve any of the studied MeSO(2)-PCBs; and a poor resolution was obtained for three MeSO(2)-PCBs when the BGB-172 column was employed. The developed method was successfully applied to two fish oil and one cow liver samples commercially available, which showed different enantioselective pattern. PCBs 91 and 176 presented a clear enrichment of the second eluted atropisomer in codfish oil, whereas in fish oil sample, slight enrichment of the first eluted atropisomer of CB45 and the second eluted atropisomer of CB136 were observed. © 2012 Wiley Periodicals, Inc.

Non-triglyceride components modulate the fat crystal network of palm kernel oil and coconut oil.

PubMed

Chai, Xiuhang; Meng, Zong; Jiang, Jiang; Cao, Peirang; Liang, Xinyu; Piatko, Michael; Campbell, Shawn; Lo, Seong Koon; Liu, Yuanfa

2018-03-01

PKO and CNO are composed of 97-98% triacylglycerols and 2-3% minor non-triglyceride components (FFA, DAG and MAG). Triglycerides were separated from minor components by chromatographic method. The lipid composition, thermal properties, polymorphism, isothermal crystallization behavior, nanostructure and microstructure of PKO, PKO-TAG, CNO and CNO-TAG were evaluated. Removal of minor components had no effect on lipid composition and equilibrium solid fat contents. However, presence of minor components did increase the slip melting point and promoted the onset of crystallization from DSC crystallization profiles. The thickness of the nanoscale crystals increased with no polymorphic transformation after removing the minor components. Crystallization kinetics revealed that minor components decreased crystal growth rate with higher t 1/2 . Sharp changes in the values of the Avrami constant k and exponent n were observed for all fats around 10°C. Increases in n around 10°C indicated a change from one-dimensional to multi-dimensional growth . From the results of polarized light micrographs, the transformation from the coarser crystal structure to tiny crystal structure occurred in microstructure networks at the action of minor components. Copyright © 2017 Elsevier Ltd. All rights reserved.

Multiple, simultaneous, independent gradients for a versatile multidimensional liquid chromatography. Part II: Application 1 - Large increases in isoform resolution of human transferrin by use of dual simultaneous independent gradients of pH & acetonitrile on a mixed bed (anion exchange plus reversed phase) stationary phase.

PubMed

Tsonev, Latchezar I; Hirsh, Allen G

2016-10-14

We have previously described a liquid chromatographic (LC) method for uncoupling controlled, wide range pH gradients and simultaneous controlled gradients of a non-buffering solute on ion exchange resins (Hirsh and Tsonev, 2012) [1]. Here we report the application of this two dimensional LC technique to the problem of resolving Human Transferrin (HT) isoforms. This important iron transporting protein should theoretically occur in several thousand glycoforms, but only about a dozen have been reported. Using dual simultaneous independent gradients (DSIGs) of acetonitrile (ACN) and pH on a mixed bed stationary phase (SP) consisting of a mixture of an anion exchange resin and a reversed phase (RP) resin we partially resolve about 60 isoforms. These are likely to be partially refolded glycoforms generated by interaction of HT with the highly hydrophobic RP SP, as well as distinct folded glycoforms. Thus this study should have interesting implications for both glycoform separation and the study of protein folding. Copyright © 2016 Elsevier B.V. All rights reserved.

QbD-oriented development and validation of a bioanalytical method for nevirapine with enhanced liquid-liquid extraction and chromatographic separation.

PubMed

Beg, Sarwar; Chaudhary, Vandna; Sharma, Gajanand; Garg, Babita; Panda, Sagar Suman; Singh, Bhupinder

2016-06-01

The present studies describe the systematic quality by design (QbD)-oriented development and validation of a simple, rapid, sensitive and cost-effective reversed-phase HPLC bioanalytical method for nevirapine in rat plasma. Chromatographic separation was carried out on a C18 column using isocratic 68:9:23% v/v elution of methanol, acetonitrile and water (pH 3, adjusted by orthophosphoric acid) at a flow rate of 1.0 mL/min using UV detection at 230 nm. A Box-Behnken design was applied for chromatographic method optimization taking mobile phase ratio, pH and flow rate as the critical method parameters (CMPs) from screening studies. Peak area, retention time, theoretical plates and peak tailing were measured as the critical analytical attributes (CAAs). Further, the bioanalytical liquid-liquid extraction process was optimized using an optimal design by selecting extraction time, centrifugation speed and temperature as the CMPs for percentage recovery of nevirapine as the CAA. The search for an optimum chromatographic solution was conducted through numerical desirability function. Validation studies performed as per the US Food and Drug Administration requirements revealed results within the acceptance limit. In a nutshell, the studies successfully demonstrate the utility of analytical QbD approach for the rational development of a bioanalytical method with enhanced chromatographic separation and recovery of nevirapine in rat plasma. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

New method for evaluating irreversible adsorption and stationary phase bleed in gas chromatographic capillary columns.

PubMed

Wright, Bob W; Wright, Cherylyn W

2012-10-26

A novel method is described for the evaluation of irreversible adsorption and column bleed in gas chromatographic (GC) columns using a tandem GC approach. This work specifically determined the degree of irreversible adsorption behavior of specific sulfur and phosphorous containing test probe compounds at levels ranging from approximately 50 picograms (pg) to 1 nanogram (ng) on selected gas chromatographic columns. This method does not replace existing evaluation methods that characterize reversible adsorption but provides an additional tool. The test compounds were selected due to their ease of adsorption and their importance in the specific trace analytical detection methodology being developed. Replicate chromatographic columns with 5% phenylmethylpolysiloxane (PMS), polyethylene glycol (wax), trifluoropropylpolysiloxane (TFP), or 78% cyanopropylpolysiloxane stationary phases from a variety of vendors were evaluated. As expected, the results demonstrate that the different chromatographic phases exhibit differing degrees of irreversible adsorption behavior. The results also indicate that all manufacturers do not produce equally inert columns nor are columns from a given manufacturer identical. The wax-coated columns for the test probes used were more inert as a group than 5% PMS coated columns, and they were more reproducibly manufactured. Both TFP and 78% cyanopropylpolysiloxane columns displayed superior inertness to the test compounds compared to either 5% PMS- or wax-coated columns. Irreversible adsorption behavior was characterized for a limited range of stationary phase film thicknesses. In addition, the method was shown effective for characterizing column bleed and methods to remove bleed components. This method is useful in screening columns for demanding applications and to obtain diagnostic information related to improved preparation methods. Copyright © 2012 Elsevier B.V. All rights reserved.

Liquid chromatographic extraction medium

DOEpatents

Horwitz, E. Philip; Dietz, Mark L.

1994-01-01

A method and apparatus for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column is described. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water.

Comparison of core-shell and totally porous ultra high performance liquid chromatographic stationary phases based on their selectivity towards alfuzosin compounds.

PubMed

Szulfer, Jarosław; Plenis, Alina; Bączek, Tomasz

2014-06-13

This paper focuses on the application of a column classification system based on the Katholieke Universiteit Leuven for the characterization of physicochemical properties of core-shell and ultra-high performance liquid chromatographic stationary phases, followed by the verification of the reliability of the obtained column classification in pharmaceutical practice. In the study, 7 stationary phases produced in core-shell technology and 18 ultra-high performance liquid chromatographic columns were chromatographically tested, and ranking lists were built on the FKUL-values calculated against two selected reference columns. In the column performance test, an analysis of alfuzosin in the presence of related substances was carried out using the brands of the stationary phases with the highest ranking positions. Next, a system suitability test as described by the European Pharmacopoeia monograph was performed. Moreover, a study was also performed to achieve a purposeful shortening of the analysis time of the compounds of interest using the selected stationary phases. Finally, it was checked whether methods using core-shell and ultra-high performance liquid chromatographic columns can be an interesting alternative to the high-performance liquid chromatographic method for the analysis of alfuzosin in pharmaceutical practice. Copyright © 2014 Elsevier B.V. All rights reserved.

A New Time-varying Concept of Risk in a Changing Climate.

PubMed

Sarhadi, Ali; Ausín, María Concepción; Wiper, Michael P

2016-10-20

In a changing climate arising from anthropogenic global warming, the nature of extreme climatic events is changing over time. Existing analytical stationary-based risk methods, however, assume multi-dimensional extreme climate phenomena will not significantly vary over time. To strengthen the reliability of infrastructure designs and the management of water systems in the changing environment, multidimensional stationary risk studies should be replaced with a new adaptive perspective. The results of a comparison indicate that current multi-dimensional stationary risk frameworks are no longer applicable to projecting the changing behaviour of multi-dimensional extreme climate processes. Using static stationary-based multivariate risk methods may lead to undesirable consequences in designing water system infrastructures. The static stationary concept should be replaced with a flexible multi-dimensional time-varying risk framework. The present study introduces a new multi-dimensional time-varying risk concept to be incorporated in updating infrastructure design strategies under changing environments arising from human-induced climate change. The proposed generalized time-varying risk concept can be applied for all stochastic multi-dimensional systems that are under the influence of changing environments.

Gas chromatographic analysis of simmondsins and simmondsin ferulates in jojoba meal.

PubMed

Van Boven, M; Holser, R; Cokelaere, M; Flo, G; Decuypere, E

2000-09-01

A capillary gas chromatographic method was developed for the simultaneous determination of simmondsins and simmondsin ferulates in jojoba meal, in detoxified jojoba meal, in jojoba meal extracts, and in animal food mixtures.

Identification and phylogeny of Arabian snakes: Comparison of venom chromatographic profiles versus 16S rRNA gene sequences.

PubMed

Al Asmari, Abdulrahman; Manthiri, Rajamohammed Abbas; Khan, Haseeb Ahmad

2014-11-01

Identification of snake species is important for various reasons including the emergency treatment of snake bite victims. We present a simple method for identification of six snake species using the gel filtration chromatographic profiles of their venoms. The venoms of Echis coloratus, Echis pyramidum, Cerastes gasperettii, Bitis arietans, Naja arabica, and Walterinnesia aegyptia were milked, lyophilized, diluted and centrifuged to separate the mucus from the venom. The clear supernatants were filtered and chromatographed on fast protein liquid chromatography (FPLC). We obtained the 16S rRNA gene sequences of the above species and performed phylogenetic analysis using the neighbor-joining method. The chromatograms of venoms from different snake species showed peculiar patterns based on the number and location of peaks. The dendrograms generated from similarity matrix based on the presence/absence of particular chromatographic peaks clearly differentiated Elapids from Viperids. Molecular cladistics using 16S rRNA gene sequences resulted in jumping clades while separating the members of these two families. These findings suggest that chromatographic profiles of snake venoms may provide a simple and reproducible chemical fingerprinting method for quick identification of snake species. However, the validation of this methodology requires further studies on large number of specimens from within and across species.

[A peak recognition algorithm designed for chromatographic peaks of transformer oil].

PubMed

Ou, Linjun; Cao, Jian

2014-09-01

In the field of the chromatographic peak identification of the transformer oil, the traditional first-order derivative requires slope threshold to achieve peak identification. In terms of its shortcomings of low automation and easy distortion, the first-order derivative method was improved by applying the moving average iterative method and the normalized analysis techniques to identify the peaks. Accurate identification of the chromatographic peaks was realized through using multiple iterations of the moving average of signal curves and square wave curves to determine the optimal value of the normalized peak identification parameters, combined with the absolute peak retention times and peak window. The experimental results show that this algorithm can accurately identify the peaks and is not sensitive to the noise, the chromatographic peak width or the peak shape changes. It has strong adaptability to meet the on-site requirements of online monitoring devices of dissolved gases in transformer oil.

On-line gas chromatographic analysis of airborne particles

DOEpatents

Hering, Susanne V [Berkeley, CA; Goldstein, Allen H [Orinda, CA

2012-01-03

A method and apparatus for the in-situ, chemical analysis of an aerosol. The method may include the steps of: collecting an aerosol; thermally desorbing the aerosol into a carrier gas to provide desorbed aerosol material; transporting the desorbed aerosol material onto the head of a gas chromatography column; analyzing the aerosol material using a gas chromatograph, and quantizing the aerosol material as it evolves from the gas chromatography column. The apparatus includes a collection and thermal desorption cell, a gas chromatograph including a gas chromatography column, heated transport lines coupling the cell and the column; and a quantization detector for aerosol material evolving from the gas chromatography column.

Chromatographic extraction with di(2-ethylhexyl)orthophosphoric acid for production and purification of promethium-147

DOEpatents

Boll, Rose A [Knoxville, TN; Mirzadeh, Saed [Knoxville, TN

2008-10-14

A method of producing and purifying promethium-147 including the steps of: irradiating a target material including neodymium-146 with neutrons to produce promethium-147 within the irradiated target material; dissolving the irradiated target material to form an acidic solution; loading the acidic solution onto a chromatographic separation apparatus containing HDEHP; and eluting the apparatus to chromatographically separate the promethium-147 from the neodymium-146.

Liquid chromatographic extraction medium

DOEpatents

Horwitz, E.P.; Dietz, M.L.

1994-09-13

A method and apparatus are disclosed for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water. 1 fig.

Authentication of Piper betle L. folium and quantification of their antifungal-activity.

PubMed

Wirasuta, I Made Agus Gelgel; Srinadi, I Gusti Ayu Made; Dwidasmara, Ida Bagus Gede; Ardiyanti, Ni Luh Putu Putri; Trisnadewi, I Gusti Ayu Arya; Paramita, Ni Luh Putu Vidya

2017-07-01

The TLC profiles of intra- and inter-day precision for Piper betle L . (PBL) folium methanol extract was studied for their peak marker recognition and identification. The Numerical chromatographic parameters (NCPs) of the peak markers, the hierarchical clustering analysis (HCA) and the principal component analysis (PCA) were applied to authenticate the PBL. folium extract from other Piper species folium extract and to ensure the antifungal activity quality of the PBL essential oil. The spotted extract was developed with the mobile phase of toluene: ethyl acetate; 93:7, (v/v). The eluted plate was viewed with the TLC-Visualizer, scanned under absorption and fluorescent mode detection, and on each sample the in-situ UV spectra were recorded between 190 to 400 nm. The NCPs profiles of intra- and inter-day precision results offered multi-dimensional chromatogram fingerprints for better marker peak pattern recognition and identification. Using the r -value fingerprints data series generated with this method allowed more precise discrimination the PBL. from other Piper species compared to the marker peak area fingerprint method. The cosine pair comparison was a simple method for authentication of two different fingerprints. The ward linkage clustering and the pair cross-correlation comparison were better chemometric methods to determine the consistency peak area ratio between fingerprints. The first component PCA-loading values of peak marker area fingerprints were correlated linearly to both the bio-marker concentration as well as the antifungal activity. This relationship could be used to control the quality and pharmacological potency. This simple method was developed for the authentication and quantification of herbal medicine.

Quantitative determination and classification of energy drinks using near-infrared spectroscopy.

PubMed

Rácz, Anita; Héberger, Károly; Fodor, Marietta

2016-09-01

Almost a hundred commercially available energy drink samples from Hungary, Slovakia, and Greece were collected for the quantitative determination of their caffeine and sugar content with FT-NIR spectroscopy and high-performance liquid chromatography (HPLC). Calibration models were built with partial least-squares regression (PLSR). An HPLC-UV method was used to measure the reference values for caffeine content, while sugar contents were measured with the Schoorl method. Both the nominal sugar content (as indicated on the cans) and the measured sugar concentration were used as references. Although the Schoorl method has larger error and bias, appropriate models could be developed using both references. The validation of the models was based on sevenfold cross-validation and external validation. FT-NIR analysis is a good candidate to replace the HPLC-UV method, because it is much cheaper than any chromatographic method, while it is also more time-efficient. The combination of FT-NIR with multidimensional chemometric techniques like PLSR can be a good option for the detection of low caffeine concentrations in energy drinks. Moreover, three types of energy drinks that contain (i) taurine, (ii) arginine, and (iii) none of these two components were classified correctly using principal component analysis and linear discriminant analysis. Such classifications are important for the detection of adulterated samples and for quality control, as well. In this case, more than a hundred samples were used for the evaluation. The classification was validated with cross-validation and several randomization tests (X-scrambling). Graphical Abstract The way of energy drinks from cans to appropriate chemometric models.

Bioanalytical method transfer considerations of chromatographic-based assays.

PubMed

Williard, Clark V

2016-07-01

Bioanalysis is an important part of the modern drug development process. The business practice of outsourcing and transferring bioanalytical methods from laboratory to laboratory has increasingly become a crucial strategy for successful and efficient delivery of therapies to the market. This chapter discusses important considerations when transferring various types of chromatographic-based assays in today's pharmaceutical research and development environment.

A gas chromatographic method for the determination of bicarbonate and dissolved gases

USDA-ARS?s Scientific Manuscript database

A gas chromatographic method for the rapid determination of aqueous carbon dioxide and its speciation into solvated carbon dioxide and bicarbonate is presented. One-half mL samples are injected through a rubber septum into 20-mL vials that are filled with 9.5 mL of 0.1 N HCl. A one mL portion of the...

Design of a portable gas chromatography with a conducting polymer nanocomposite detector device and a method to analyze a gas mixture.

PubMed

Pirsa, Sajad

2017-04-01

A portable chromatography device and a method were developed to analyze a gas mixture. The device comprises a chromatographic column for separating components of a sample of the gas mixture. It has an air pump coupled to the inlet of a chromatographic column for pumping air and an injector coupled to the inlet of chromatographic column for feeding the sample using the air as a carrier gas. A detector is arranged downstream from and coupled to the outlet of the chromatographic column. The detector is a nanostructure semiconductive microfiber. The device further comprises an evaluation unit arranged and configured to evaluate each detected component to determine the concentration. The designed portable system was used for simultaneous detection of amines. The possibility of applying dispersive liquid-liquid microextraction for the determination of analytes in trace levels is demonstrated. The reproducibility of this method is acceptable, and good standard deviations were obtained. The relative standard deviation value is less than 6% for all analytes. Finally, the method was successfully applied to the extraction and determination of analytes in water samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The Use of the Visualisation of Multidimensional Data Using PCA to Evaluate Possibilities of the Division of Coal Samples Space Due to their Suitability for Fluidised Gasification

NASA Astrophysics Data System (ADS)

Jamróz, Dariusz; Niedoba, Tomasz; Surowiak, Agnieszka; Tumidajski, Tadeusz

2016-09-01

Methods serving to visualise multidimensional data through the transformation of multidimensional space into two-dimensional space, enable to present the multidimensional data on the computer screen. Thanks to this, qualitative analysis of this data can be performed in the most natural way for humans, through the sense of sight. An example of such a method of multidimensional data visualisation is PCA (principal component analysis) method. This method was used in this work to present and analyse a set of seven-dimensional data (selected seven properties) describing coal samples obtained from Janina and Wieczorek coal mines. Coal from these mines was previously subjected to separation by means of a laboratory ring jig, consisting of ten rings. With 5 layers of both types of coal (with 2 rings each) were obtained in this way. It was decided to check if the method of multidimensional data visualisation enables to divide the space of such divided samples into areas with different suitability for the fluidised gasification process. To that end, the card of technological suitability of coal was used (Sobolewski et al., 2012; 2013), in which key, relevant and additional parameters, having effect on the gasification process, were described. As a result of analyses, it was stated that effective determination of coal samples suitability for the on-surface gasification process in a fluidised reactor is possible. The PCA method enables the visualisation of the optimal subspace containing the set requirements concerning the properties of coals intended for this process.

Comparison of the ion exclusion chromatographic method with the Monier-Williams method for determination of total sulfite in foods.

PubMed

Kim, H J

1989-01-01

Experimental data comparing the alkali extraction/ion exclusion chromatographic method with the Monier-Williams method for determination of total sulfite are presented in (a) enzymatic and nonenzymatic browning systems, (b) vegetables containing naturally occurring sulfite, and (c) a carbohydrate-type food additive, erythorbic acid. Excellent agreement, with a linear correlation coefficient of 0.99, was observed in fresh potato samples homogenized with sulfite and allowed to react for different time intervals (enzymatic browning system). A good overall correlation was observed in dehydrated, sulfited apple samples heated for different times (nonenzymatic browning system); however, as heating time increased, higher results were obtained by the Monier-Williams method than by the alkali extraction/ion exclusion chromatographic method. The results of determining sulfite in the alkali trapping solution following acid distillation or acid treatment without heat suggested that this deviation was due to a fraction of sulfite bound to the browning reaction products in such a way that it was released by acid distillation but not by alkali extraction or acid treatment without heat. Similar behavior was demonstrated in cabbage with naturally occurring sulfite, which was released by acid distillation but not by alkali extraction or acid treatment without heat. The ion exclusion chromatographic method could overcome interference by the volatile caramelization reaction products in the Monier-Williams determination of erythorbic acid.

A multiresidue method by high performance liquid chromatography-based fractionation and gas chromatographic determination of trace levels of pesticides in air and water.

PubMed

Seiber, J N; Glotfelty, D E; Lucas, A D; McChesney, M M; Sagebiel, J C; Wehner, T A

1990-01-01

A multiresidue analytical method is described for pesticides, transformation products, and related toxicants based upon high performance liquid chromatographic (HPLC) fractionation of extracted residue on a Partisil silica gel normal phase column followed by selective-detector gas chromatographic (GC) determination of components in each fraction. The HPLC mobile phase gradient (hexane to methyl t-butyl ether) gave good chromatographic efficiency, resolution, reproducibility and recovery for 61 test compounds, and allowed for collection in four fractions spanning polarities from low polarity organochlorine compounds (fraction 1) to polar N-methylcarbamates and organophosphorus oxons (fraction 4). The multiresidue method was developed for use with air samples collected on XAD-4 and related trapping agents, and water samples extracted with methylene chloride. Detection limits estimated from spiking experiments were generally 0.3-1 ng/m3 for high-volume air samples, and 0.01-0.1 microgram/L for one-liter water samples. Applications were made to determination of pesticides in fogwater and air samples.

Freeze drying for gas chromatography stationary phase deposition

DOEpatents

Sylwester, Alan P [Livermore, CA

2007-01-02

The present disclosure relates to methods for deposition of gas chromatography (GC) stationary phases into chromatography columns, for example gas chromatography columns. A chromatographic medium is dissolved or suspended in a solvent to form a composition. The composition may be inserted into a chromatographic column. Alternatively, portions of the chromatographic column may be exposed or filled with the composition. The composition is permitted to solidify, and at least a portion of the solvent is removed by vacuum sublimation.

Measurement of water absorption capacity in wheat flour by a headspace gas chromatographic technique.

PubMed

Xie, Wei-Qi; Yu, Kong-Xian; Gong, Yi-Xian

2018-04-17

The purpose of this work is to introduce a new method for quantitatively analyzing water absorption capacity in wheat flour by a headspace gas chromatographic technique. This headspace gas chromatographic technique was based on measuring the water vapor released from a series of wheat flour samples with different contents of water addition. According to the different trends between the vapor and wheat flour phase before and after the water absorption capacity in wheat flour, a turning point (corresponding to water absorption capacity in wheat flour) can be obtained by fitting the data of the water gas chromatography peak area from different wheat flour samples. The data showed that the phase equilibrium in the vial can be achieved in 25 min at desired temperature (35°C). The relative standard deviation of the reaction headspace gas chromatographic technique in water absorption capacity determination was within 3.48%, the relative differences has been determined by comparing the water absorption capacity obtained from this new analytical technique with the data from the reference technique (i.e., the filtration method), which are less than 8.92%. The new headspace gas chromatographic method is automated, accurate and be a reliable tool for quantifying water absorption capacity in wheat flour in both laboratory research and mill applications. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Improving Multidimensional Wireless Sensor Network Lifetime Using Pearson Correlation and Fractal Clustering

PubMed Central

Almeida, Fernando R.; Brayner, Angelo; Rodrigues, Joel J. P. C.; Maia, Jose E. Bessa

2017-01-01

An efficient strategy for reducing message transmission in a wireless sensor network (WSN) is to group sensors by means of an abstraction denoted cluster. The key idea behind the cluster formation process is to identify a set of sensors whose sensed values present some data correlation. Nowadays, sensors are able to simultaneously sense multiple different physical phenomena, yielding in this way multidimensional data. This paper presents three methods for clustering sensors in WSNs whose sensors collect multidimensional data. The proposed approaches implement the concept of multidimensional behavioral clustering. To show the benefits introduced by the proposed methods, a prototype has been implemented and experiments have been carried out on real data. The results prove that the proposed methods decrease the amount of data flowing in the network and present low root-mean-square error (RMSE). PMID:28590450

Improving Multidimensional Wireless Sensor Network Lifetime Using Pearson Correlation and Fractal Clustering.

PubMed

Almeida, Fernando R; Brayner, Angelo; Rodrigues, Joel J P C; Maia, Jose E Bessa

2017-06-07

An efficient strategy for reducing message transmission in a wireless sensor network (WSN) is to group sensors by means of an abstraction denoted cluster. The key idea behind the cluster formation process is to identify a set of sensors whose sensed values present some data correlation. Nowadays, sensors are able to simultaneously sense multiple different physical phenomena, yielding in this way multidimensional data. This paper presents three methods for clustering sensors in WSNs whose sensors collect multidimensional data. The proposed approaches implement the concept of multidimensional behavioral clustering . To show the benefits introduced by the proposed methods, a prototype has been implemented and experiments have been carried out on real data. The results prove that the proposed methods decrease the amount of data flowing in the network and present low root-mean-square error (RMSE).

The Multidimensional Assessment of Interoceptive Awareness (MAIA)

PubMed Central

Mehling, Wolf E.; Price, Cynthia; Daubenmier, Jennifer J.; Acree, Mike; Bartmess, Elizabeth; Stewart, Anita

2012-01-01

This paper describes the development of a multidimensional self-report measure of interoceptive body awareness. The systematic mixed-methods process involved reviewing the current literature, specifying a multidimensional conceptual framework, evaluating prior instruments, developing items, and analyzing focus group responses to scale items by instructors and patients of body awareness-enhancing therapies. Following refinement by cognitive testing, items were field-tested in students and instructors of mind-body approaches. Final item selection was achieved by submitting the field test data to an iterative process using multiple validation methods, including exploratory cluster and confirmatory factor analyses, comparison between known groups, and correlations with established measures of related constructs. The resulting 32-item multidimensional instrument assesses eight concepts. The psychometric properties of these final scales suggest that the Multidimensional Assessment of Interoceptive Awareness (MAIA) may serve as a starting point for research and further collaborative refinement. PMID:23133619

HPLC-PFD determination of priority pollutant PAHs in water, sediment, and semipermeable membrane devices

USGS Publications Warehouse

Williamson, K.S.; Petty, J.D.; Huckins, J.N.; Lebo, J.A.; Kaiser, E.M.

2002-01-01

High performance liquid chromatography coupled with programmable fluorescence detection was employed for the determination of 15 priority pollutant polycyclic aromatic hydrocarbons (PPPAHs) in water, sediment, and semipermeable membrane devices (SPMDs). Chromatographic separation using this analytical method facilitates selectivity, sensitivity (ppt levels), and can serve as a non-destructive technique for subsequent analysis by other chromatographic and spectroscopic techniques. Extraction and sample cleanup procedures were also developed for water, sediment, and SPMDs using various chromatographic and wet chemical methods. The focus of this publication is to examine the enrichment techniques and the analytical methodologies used in the isolation, characterization, and quantitation of 15 PPPAHs in different sample matrices.

Method for preparing high specific activity 177Lu

DOEpatents

Mirzadeh, Saed; Du, Miting; Beets, Arnold L.; Knapp, Jr., Furn F.

2004-04-06

A method of separating lutetium from a solution containing Lu and Yb, particularly reactor-produced .sup.177 Lu and .sup.177 Yb, includes the steps of: providing a chromatographic separation apparatus containing LN resin; loading the apparatus with a solution containing Lu and Yb; and eluting the apparatus to chromatographically separate the Lu and the Yb in order to produce high-specific-activity .sup.177 Yb.

Rapid and improved gas-liquid chromatography technique for detection of hippurate hydrolysis by Campylobacter jejuni and Campylobacter coli.

PubMed Central

Bär, W; Fricke, G

1987-01-01

A gas-liquid chromatographic method which requires no chloroform extraction of the split products has been investigated for the detection of hippurate hydrolysis by Campylobacter spp. This technique gave better reproducibility than other tests also used in this study and allows the routine use of the gas-liquid chromatographic method for identification of Campylobacter isolates. PMID:3654950

Investigation of Soman Adducts of Human Hemoglobin by Liquid Chromatography

DTIC Science & Technology

2004-04-01

acid standard, with fifteen primary amino acids , was used to evaluate and refine the chromatographic methods . An LC/MS/MS was used to analyze the non...several chromatographic conditions and stationary phases were used to create an LC/MS/MS method to directly analyze the amino acids , these studies...terminated because of a lack of resolution of the amino acid peaks. Also, initial attempts to develop an HPLC method to separate individual amino acids

Determination of the molecular weight of low-molecular-weight heparins by using high-pressure size exclusion chromatography on line with a triple detector array and conventional methods.

PubMed

Bisio, Antonella; Mantegazza, Alessandra; Vecchietti, Davide; Bensi, Donata; Coppa, Alessia; Torri, Giangiacomo; Bertini, Sabrina

2015-03-19

The evaluation of weight average molecular weight (Mw) and molecular weight distribution represents one of the most controversial aspects concerning the characterization of low molecular weight heparins (LMWHs). As the most commonly used method for the measurement of such parameters is high performance size exclusion chromatography (HP-SEC), the soundness of results mainly depends on the appropriate calibration of the chromatographic columns used. With the aim of meeting the requirement of proper Mw standards for LMWHs, in the present work the determination of molecular weight parameters (Mw and Mn) by HP-SEC combined with a triple detector array (TDA) was performed. The HP-SEC/TDA technique permits the evaluation of polymeric samples by exploiting the combined and simultaneous action of three on-line detectors: light scattering detectors (LALLS/RALLS); refractometer and viscometer. Three commercial LMWH samples, enoxaparin, tinzaparin and dalteparin, a γ-ray depolymerized heparin (γ-Hep) and its chromatographic fractions, and a synthetic pentasaccharide were analysed by HP-SEC/TDA. The same samples were analysed also with a conventional HP-SEC method employing refractive index (RI) and UV detectors and two different chromatographic column set, silica gel and polymeric gel columns. In both chromatographic systems, two different calibration curves were built up by using (i) γ-Hep chromatographic fractions and the corresponding Mw parameters obtained via HP-SEC/TDA; (ii) the whole γ-Hep preparation with broad Mw dispersion and the corresponding cumulative distribution function calculated via HP-SEC/TDA. In addition, also a chromatographic column calibration according to European Pharmacopoeia indication was built up. By comparing all the obtained results, some important differences among Mw and size distribution values of the three LMWHs were found with the five different calibration methods and with HP-SEC/TDA method. In particular, the detection of the lower molecular weight components turned out to be the most critical aspect. Whereas HP-SEC/TDA may underestimate species under 2 KDa when present in low concentration, other methods appeared to emphasize their content.

A Heterogeneous Network Based Method for Identifying GBM-Related Genes by Integrating Multi-Dimensional Data.

PubMed

Chen Peng; Ao Li

2017-01-01

The emergence of multi-dimensional data offers opportunities for more comprehensive analysis of the molecular characteristics of human diseases and therefore improving diagnosis, treatment, and prevention. In this study, we proposed a heterogeneous network based method by integrating multi-dimensional data (HNMD) to identify GBM-related genes. The novelty of the method lies in that the multi-dimensional data of GBM from TCGA dataset that provide comprehensive information of genes, are combined with protein-protein interactions to construct a weighted heterogeneous network, which reflects both the general and disease-specific relationships between genes. In addition, a propagation algorithm with resistance is introduced to precisely score and rank GBM-related genes. The results of comprehensive performance evaluation show that the proposed method significantly outperforms the network based methods with single-dimensional data and other existing approaches. Subsequent analysis of the top ranked genes suggests they may be functionally implicated in GBM, which further corroborates the superiority of the proposed method. The source code and the results of HNMD can be downloaded from the following URL: http://bioinformatics.ustc.edu.cn/hnmd/ .

The Extraction of One-Dimensional Flow Properties from Multi-Dimensional Data Sets

NASA Technical Reports Server (NTRS)

Baurle, Robert A.; Gaffney, Richard L., Jr.

2007-01-01

The engineering design and analysis of air-breathing propulsion systems relies heavily on zero- or one-dimensional properties (e.g. thrust, total pressure recovery, mixing and combustion efficiency, etc.) for figures of merit. The extraction of these parameters from experimental data sets and/or multi-dimensional computational data sets is therefore an important aspect of the design process. A variety of methods exist for extracting performance measures from multi-dimensional data sets. Some of the information contained in the multi-dimensional flow is inevitably lost when any one-dimensionalization technique is applied. Hence, the unique assumptions associated with a given approach may result in one-dimensional properties that are significantly different than those extracted using alternative approaches. The purpose of this effort is to examine some of the more popular methods used for the extraction of performance measures from multi-dimensional data sets, reveal the strengths and weaknesses of each approach, and highlight various numerical issues that result when mapping data from a multi-dimensional space to a space of one dimension.

The Art of Extracting One-Dimensional Flow Properties from Multi-Dimensional Data Sets

NASA Technical Reports Server (NTRS)

Baurle, R. A.; Gaffney, R. L.

2007-01-01

The engineering design and analysis of air-breathing propulsion systems relies heavily on zero- or one-dimensional properties (e:g: thrust, total pressure recovery, mixing and combustion efficiency, etc.) for figures of merit. The extraction of these parameters from experimental data sets and/or multi-dimensional computational data sets is therefore an important aspect of the design process. A variety of methods exist for extracting performance measures from multi-dimensional data sets. Some of the information contained in the multi-dimensional flow is inevitably lost when any one-dimensionalization technique is applied. Hence, the unique assumptions associated with a given approach may result in one-dimensional properties that are significantly different than those extracted using alternative approaches. The purpose of this effort is to examine some of the more popular methods used for the extraction of performance measures from multi-dimensional data sets, reveal the strengths and weaknesses of each approach, and highlight various numerical issues that result when mapping data from a multi-dimensional space to a space of one dimension.

Multidimensional scaling analysis of financial time series based on modified cross-sample entropy methods

NASA Astrophysics Data System (ADS)

He, Jiayi; Shang, Pengjian; Xiong, Hui

2018-06-01

Stocks, as the concrete manifestation of financial time series with plenty of potential information, are often used in the study of financial time series. In this paper, we utilize the stock data to recognize their patterns through out the dissimilarity matrix based on modified cross-sample entropy, then three-dimensional perceptual maps of the results are provided through multidimensional scaling method. Two modified multidimensional scaling methods are proposed in this paper, that is, multidimensional scaling based on Kronecker-delta cross-sample entropy (MDS-KCSE) and multidimensional scaling based on permutation cross-sample entropy (MDS-PCSE). These two methods use Kronecker-delta based cross-sample entropy and permutation based cross-sample entropy to replace the distance or dissimilarity measurement in classical multidimensional scaling (MDS). Multidimensional scaling based on Chebyshev distance (MDSC) is employed to provide a reference for comparisons. Our analysis reveals a clear clustering both in synthetic data and 18 indices from diverse stock markets. It implies that time series generated by the same model are easier to have similar irregularity than others, and the difference in the stock index, which is caused by the country or region and the different financial policies, can reflect the irregularity in the data. In the synthetic data experiments, not only the time series generated by different models can be distinguished, the one generated under different parameters of the same model can also be detected. In the financial data experiment, the stock indices are clearly divided into five groups. Through analysis, we find that they correspond to five regions, respectively, that is, Europe, North America, South America, Asian-Pacific (with the exception of mainland China), mainland China and Russia. The results also demonstrate that MDS-KCSE and MDS-PCSE provide more effective divisions in experiments than MDSC.

Performance evaluation of a versatile multidimensional chromatographic preparative system based on three-dimensional gas chromatography and liquid chromatography-two-dimensional gas chromatography for the collection of volatile constituents.

PubMed

Pantò, Sebastiano; Sciarrone, Danilo; Maimone, Mariarosa; Ragonese, Carla; Giofrè, Salvatore; Donato, Paola; Farnetti, Sara; Mondello, Luigi

2015-10-23

The present research deals with the multi-collection of the most important sesquiterpene alcohols belonging to sandalwood essential oil, as reported by the international regulations: (Z)-α-santalol, (Z)-α-trans bergamotol, (Z)-β-santalol, epi-(Z)-β-santalol, α-bisabolol, (Z)-lanceol, and (Z)-nuciferol. A versatile multidimensional preparative system, based on the hyphenation of liquid and gas chromatography techniques, was operated in the LC-GC-GC-prep or GC-GC-GC-prep configuration, depending on the concentration to be collected from the sample, without any hardware or software modification. The system was equipped with a silica LC column in combination with polyethylene glycol-poly(5% diphenyl/95% dimethylsiloxane)-medium polarity ionic liquid or β-cyclodextrin based GC stationary phases. The GC-GC-GC-prep configuration was exploited for the collection of four components, by using a conventional split/splitless injector, while the LC-GC-GC-prep approach was applied for three low abundant components (<5%), in order to increase the quantity collected within a single run, by the LC injection of a high sample amount. All target compounds, whose determination is hampered by the unavailability of commercial standards, were collected at milligram levels and with a high degree of purity (>87%). Copyright © 2015 Elsevier B.V. All rights reserved.

High Order Finite Difference Methods, Multidimensional Linear Problems and Curvilinear Coordinates

NASA Technical Reports Server (NTRS)

Nordstrom, Jan; Carpenter, Mark H.

1999-01-01

Boundary and interface conditions are derived for high order finite difference methods applied to multidimensional linear problems in curvilinear coordinates. The boundary and interface conditions lead to conservative schemes and strict and strong stability provided that certain metric conditions are met.

Simple and rapid high-performance liquid chromatographic method for the determination of aspartame and its metabolites in foods.

PubMed

Gibbs, B F; Alli, I; Mulligan, C N

1996-02-23

A method for the determination of aspartame (N-L-alpha-aspartyl-L-phenylalanine methyl ester) and its metabolites, applicable on a routine quality assurance basis, is described. Liquid samples (diet Coke, 7-Up, Pepsi, etc.) were injected directly onto a mini-cartridge reversed-phase column on a high-performance liquid chromatographic system, whereas solid samples (Equal, hot chocolate powder, pudding, etc.) were extracted with water. Optimising chromatographic conditions resulted in resolved components of interest within 12 min. The by-products were confirmed by mass spectrometry. Although the method was developed on a two-pump HPLC system fitted with a diode-array detector, it is straightforward and can be transformed to the simplest HPLC configuration. Using a single-piston pump (with damper), a fixed-wavelength detector and a recorder/integrator, the degradation of products can be monitored as they decompose. The results obtained were in harmony with previously reported tedious methods. The method is simple, rapid, quantitative and does not involve complex, hazardous or toxic chemistry.

Gas chromatographic simulated distillation-mass spectrometry for the determination of the boiling point distributions of crude oils

PubMed

Roussis; Fitzgerald

2000-04-01

The coupling of gas chromatographic simulated distillation with mass spectrometry for the determination of the distillation profiles of crude oils is reported. The method provides the boiling point distributions of both weight and volume percent amounts. The weight percent distribution is obtained from the measured total ion current signal. The total ion current signal is converted to weight percent amount by calibration with a reference crude oil of a known distillation profile. Knowledge of the chemical composition of the crude oil across the boiling range permits the determination of the volume percent distribution. The long-term repeatability is equivalent to or better than the short-term repeatability of the currently available American Society for Testing and Materials (ASTM) gas chromatographic method for simulated distillation. Results obtained by the mass spectrometric method are in very good agreement with results obtained by conventional methods of physical distillation. The compositional information supplied by the method can be used to extensively characterize crude oils.

QbD-Based Development and Validation of a Stability-Indicating HPLC Method for Estimating Ketoprofen in Bulk Drug and Proniosomal Vesicular System.

PubMed

Yadav, Nand K; Raghuvanshi, Ashish; Sharma, Gajanand; Beg, Sarwar; Katare, Om P; Nanda, Sanju

2016-03-01

The current studies entail systematic quality by design (QbD)-based development of simple, precise, cost-effective and stability-indicating high-performance liquid chromatography method for estimation of ketoprofen. Analytical target profile was defined and critical analytical attributes (CAAs) were selected. Chromatographic separation was accomplished with an isocratic, reversed-phase chromatography using C-18 column, pH 6.8, phosphate buffer-methanol (50 : 50v/v) as a mobile phase at a flow rate of 1.0 mL/min and UV detection at 258 nm. Systematic optimization of chromatographic method was performed using central composite design by evaluating theoretical plates and peak tailing as the CAAs. The method was validated as per International Conference on Harmonization guidelines with parameters such as high sensitivity, specificity of the method with linearity ranging between 0.05 and 250 µg/mL, detection limit of 0.025 µg/mL and quantification limit of 0.05 µg/mL. Precision was demonstrated using relative standard deviation of 1.21%. Stress degradation studies performed using acid, base, peroxide, thermal and photolytic methods helped in identifying the degradation products in the proniosome delivery systems. The results successfully demonstrated the utility of QbD for optimizing the chromatographic conditions for developing highly sensitive liquid chromatographic method for ketoprofen. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Progress in multi-dimensional upwind differencing

NASA Technical Reports Server (NTRS)

Vanleer, Bram

1992-01-01

Multi-dimensional upwind-differencing schemes for the Euler equations are reviewed. On the basis of the first-order upwind scheme for a one-dimensional convection equation, the two approaches to upwind differencing are discussed: the fluctuation approach and the finite-volume approach. The usual extension of the finite-volume method to the multi-dimensional Euler equations is not entirely satisfactory, because the direction of wave propagation is always assumed to be normal to the cell faces. This leads to smearing of shock and shear waves when these are not grid-aligned. Multi-directional methods, in which upwind-biased fluxes are computed in a frame aligned with a dominant wave, overcome this problem, but at the expense of robustness. The same is true for the schemes incorporating a multi-dimensional wave model not based on multi-dimensional data but on an 'educated guess' of what they could be. The fluctuation approach offers the best possibilities for the development of genuinely multi-dimensional upwind schemes. Three building blocks are needed for such schemes: a wave model, a way to achieve conservation, and a compact convection scheme. Recent advances in each of these components are discussed; putting them all together is the present focus of a worldwide research effort. Some numerical results are presented, illustrating the potential of the new multi-dimensional schemes.

[Progresses in screening active compounds from herbal medicine by affinity chromatography].

PubMed

Feng, Ying-shu; Tong, Shan-shan; Xu, Xi-ming; Yu, Jiang-nan

2015-03-01

Affinity chromatography is a chromatographic method for separating molecules using the binding characteristics of the stationary phase with potential drug molecules. This method can be performed as a high throughput screening method and a chromatographic separation method to screen a variety of active drugs. This paper summarizes the history of affinity chromatography, screening technology of affinity chromatography, and application of affinity chromatography in screening bio-active compounds in herbal medicines, and then discusses its application prospects, in order to broaden applications of the affinity chromatography in drug screening.

High-performance liquid chromatographic determination of ambroxol in human plasma.

PubMed

Nobilis, M; Pastera, J; Svoboda, D; Kvêtina, J; Macek, K

1992-10-23

Ambroxol has been determined in biological fluids using a rapid and sensitive high-performance liquid chromatographic method. The samples prepared from plasma by liquid-liquid extraction were analysed on reversed-phase silica gel by competing-ion chromatography with ultraviolet detection. The method was applied to the determination of ambroxol levels in twelve healthy volunteers after oral administration of 90 mg of ambroxol in tablets of Mucosolvan and Ambrosan.

Quantitative interference by cysteine and N-acetylcysteine metabolites during the LC-MS/MS bioanalysis of a small molecule.

PubMed

Barricklow, Jason; Ryder, Tim F; Furlong, Michael T

2009-08-01

During LC-MS/MS quantification of a small molecule in human urine samples from a clinical study, an unexpected peak was observed to nearly co-elute with the analyte of interest in many study samples. Improved chromatographic resolution revealed the presence of at least 3 non-analyte peaks, which were identified as cysteine metabolites and N-acetyl (mercapturic acid) derivatives thereof. These metabolites produced artifact responses in the parent compound MRM channel due to decomposition in the ionization source of the mass spectrometer. Quantitative comparison of the analyte concentrations in study samples using the original chromatographic method and the improved chromatographic separation method demonstrated that the original method substantially over-estimated the analyte concentration in many cases. The substitution of electrospray ionization (ESI) for atmospheric pressure chemical ionization (APCI) nearly eliminated the source instability of these metabolites, which would have mitigated their interference in the quantification of the analyte, even without chromatographic separation. These results 1) demonstrate the potential for thiol metabolite interferences during the quantification of small molecules in pharmacokinetic samples, and 2) underscore the need to carefully evaluate LC-MS/MS methods for molecules that can undergo metabolism to thiol adducts to ensure that they are not susceptible to such interferences during quantification.

High-Throughput Analysis of Methylmalonic Acid in Serum, Plasma, and Urine by LC-MS/MS. Method for Analyzing Isomers Without Chromatographic Separation.

PubMed

Kushnir, Mark M; Nelson, Gordon J; Frank, Elizabeth L; Rockwood, Alan L

2016-01-01

Measurement of methylmalonic acid (MMA) plays an important role in the diagnosis of vitamin B12 deficiency. Vitamin B12 is an essential cofactor for the enzymatic carbon rearrangement of methylmalonyl-CoA (MMA-CoA) to succinyl-CoA (SA-CoA), and the lack of vitamin B12 leads to elevated concentrations of MMA. Presence of succinic acid (SA) complicates the analysis because mass spectra of MMA and SA are indistinguishable, when analyzed in negative ion mode and the peaks are difficult to resolve chromatographically. We developed a method for the selective analysis of MMA that exploits the significant difference in fragmentation patterns of di-butyl derivatives of the isomers MMA and SA in a tandem mass spectrometer when analyzed in positive ion mode. Tandem mass spectra of di-butyl derivatives of MMA and SA are very distinct; this allows selective analysis of MMA in the presence of SA. The instrumental analysis is performed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive ion mode, which is, in combination with selective extraction of acidic compounds, is highly selective for organic acids with multiple carboxyl groups (dicarboxylic, tricarboxylic, etc.). In this method organic acids with a single carboxyl group are virtually undetectable in the mass spectrometer; the only organic acid, other than MMA, that is detected by this method is its isomer, SA. Quantitative measurement of MMA in this method is performed using a deconvolution algorithm, which mathematically resolves the signal corresponding to MMA and does not require chromatographic resolution of the MMA and SA peaks. Because of its high selectivity, the method utilizes isocratic chromatographic separation; reconditioning and re-equilibration of the chromatographic column between injections is unnecessary. The above features of the method allow high-throughput analysis of MMA with analysis cycle time of 1 min.

Linear regression analysis and its application to multivariate chromatographic calibration for the quantitative analysis of two-component mixtures.

PubMed

Dinç, Erdal; Ozdemir, Abdil

2005-01-01

Multivariate chromatographic calibration technique was developed for the quantitative analysis of binary mixtures enalapril maleate (EA) and hydrochlorothiazide (HCT) in tablets in the presence of losartan potassium (LST). The mathematical algorithm of multivariate chromatographic calibration technique is based on the use of the linear regression equations constructed using relationship between concentration and peak area at the five-wavelength set. The algorithm of this mathematical calibration model having a simple mathematical content was briefly described. This approach is a powerful mathematical tool for an optimum chromatographic multivariate calibration and elimination of fluctuations coming from instrumental and experimental conditions. This multivariate chromatographic calibration contains reduction of multivariate linear regression functions to univariate data set. The validation of model was carried out by analyzing various synthetic binary mixtures and using the standard addition technique. Developed calibration technique was applied to the analysis of the real pharmaceutical tablets containing EA and HCT. The obtained results were compared with those obtained by classical HPLC method. It was observed that the proposed multivariate chromatographic calibration gives better results than classical HPLC.

Interfacing a robotic station with a gas chromatograph for the full automation of the determination of organochlorine pesticides in vegetables

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

Torres, P.; Luque de Castro, M.D.

1996-12-31

A fully automated method for the determination of organochlorine pesticides in vegetables is proposed. The overall system acts as an {open_quotes}analytical black box{close_quotes} because a robotic station performs the prelimninary operations, from weighing to capping the leached analytes and location in an autosampler of an automated gas chromatograph with electron capture detection. The method has been applied to the determination of lindane, heptachlor, captan, chlordane and metoxcychlor in tea, marjoram, cinnamon, pennyroyal, and mint with good results in most cases. A gas chromatograph has been interfaced to a robotic station for the determination of pesticides in vegetables. 15 refs., 4more » figs., 2 tabs.« less

Gas-liquid chromatographic determination of resmethrin in corn, cornmeal, flour, and wheat.

PubMed

Simonaitis, R A; Cail, R S

1975-09-01

A gas-liquid chromatographic (GLC) method was developed for the determination of residues of resmethrin ((5-benzyl-3-furyl)methyl cis-trans-(+/-)-2,2-dimethyl-3-(2-methylpropenyl)-cyclopropanecarboxylate) in corn, cornmeal, flour, and wheat. The commodity, fortified with resmethrin, was extracted by tumbling with pentane and transferred to acetonitrile, the fat was partitioned off, and the sample was chromatographed with 3% ethyl acetate in pentane on Florisil containing 0.5% water. The resmethrin residue was determined by GLC with a flame ionization detector. The results were compared with known standards that had undergone the same cleanup procedures. The method was sensitive to concentrations of resmethrin to 0.2 ppm, recoveries averaged 83%, and reproducibility was good.

An asymptotic preserving multidimensional ALE method for a system of two compressible flows coupled with friction

NASA Astrophysics Data System (ADS)

Del Pino, S.; Labourasse, E.; Morel, G.

2018-06-01

We present a multidimensional asymptotic preserving scheme for the approximation of a mixture of compressible flows. Fluids are modelled by two Euler systems of equations coupled with a friction term. The asymptotic preserving property is mandatory for this kind of model, to derive a scheme that behaves well in all regimes (i.e. whatever the friction parameter value is). The method we propose is defined in ALE coordinates, using a Lagrange plus remap approach. This imposes a multidimensional definition and analysis of the scheme.

Patent data mining method and apparatus

DOEpatents

Boyack, Kevin W.; Grafe, V. Gerald; Johnson, David K.; Wylie, Brian N.

2002-01-01

A method of data mining represents related patents in a multidimensional space. Distance between patents in the multidimensional space corresponds to the extent of relationship between the patents. The relationship between pairings of patents can be expressed based on weighted combinations of several predicates. The user can select portions of the space to perceive. The user also can interact with and control the communication of the space, focusing attention on aspects of the space of most interest. The multidimensional spatial representation allows more ready comprehension of the structure of the relationships among the patents.

Research on technology of online gas chromatograph for SF6 decomposition products

NASA Astrophysics Data System (ADS)

Li, L.; Fan, X. P.; Zhou, Y. Y.; Tang, N.; Zou, Z. L.; Liu, M. Z.; Huang, G. J.

2017-12-01

Sulfur hexafluoride (SF6) decomposition products were qualitatively and quantitatively analyzed by several gas chromatographs in the laboratory. Test conditions and methods were selected and optimized to minimize and eliminate the SF6’ influences on detection of other trace components. The effective separation and detection of selected characteristic gases were achieved. And by comparison among different types of gas chromatograph, it was found that GPTR-S101 can effectively separate and detect SF6 decomposition products and has best the best detection limit and sensitivity. On the basis of GPTR-S101, online gas chromatograph for SF6decomposition products (GPTR-S201) was developed. It lays the foundation for further online monitoring and diagnosis of SF6.

[Research on the application of grey system theory in the pattern recognition for chromatographic fingerprints of traditional Chinese medicine].

PubMed

Wei, Hang; Lin, Li; Zhang, Yuan; Wang, Lianjing; Chen, Qinqun

2013-02-01

A model based on grey system theory was proposed for pattern recognition in chromatographic fingerprints (CF) of traditional Chinese medicine (TCM). The grey relational grade among the data series of each testing CF and the ideal CF was obtained by entropy and norm respectively, then the principle of "maximal matching degree" was introduced to make judgments, so as to achieve the purpose of variety identification and quality evaluation. A satisfactory result in the high performance liquid chromatographic (HPLC) analysis of 56 batches of different varieties of Exocarpium Citrus Grandis was achieved with this model. The errors in the chromatographic fingerprint analysis caused by traditional similarity method or grey correlation method were overcome, as the samples of Citrus grandis 'Tomentosa' and Citrus grandis (L.) Osbeck were correctly distinguished in the experiment. Furthermore in the study on the variety identification of Citrus grandis 'Tomentosa', the recognition rates were up to 92.85%, although the types and the contents of the chemical compositions of the samples were very close. At the same time, the model had the merits of low computation complexity and easy operation by computer programming. The research indicated that the grey system theory has good applicability to pattern recognition in the chromatographic fingerprints of TCM.

Heuristic extraction of rules in pruned artificial neural networks models used for quantifying highly overlapping chromatographic peaks.

PubMed

Hervás, César; Silva, Manuel; Serrano, Juan Manuel; Orejuela, Eva

2004-01-01

The suitability of an approach for extracting heuristic rules from trained artificial neural networks (ANNs) pruned by a regularization method and with architectures designed by evolutionary computation for quantifying highly overlapping chromatographic peaks is demonstrated. The ANN input data are estimated by the Levenberg-Marquardt method in the form of a four-parameter Weibull curve associated with the profile of the chromatographic band. To test this approach, two N-methylcarbamate pesticides, carbofuran and propoxur, were quantified using a classic peroxyoxalate chemiluminescence reaction as a detection system for chromatographic analysis. Straightforward network topologies (one and two outputs models) allow the analytes to be quantified in concentration ratios ranging from 1:7 to 5:1 with an average standard error of prediction for the generalization test of 2.7 and 2.3% for carbofuran and propoxur, respectively. The reduced dimensions of the selected ANN architectures, especially those obtained after using heuristic rules, allowed simple quantification equations to be developed that transform the input variables into output variables. These equations can be easily interpreted from a chemical point of view to attain quantitative analytical information regarding the effect of both analytes on the characteristics of chromatographic bands, namely profile, dispersion, peak height, and residence time. Copyright 2004 American Chemical Society

ION-EXCLUSION CHROMATOGRAPHIC DETERMINATION OF CARBOXYLIC ACIDS USED TO SUPPORT THE MICROBIALLY MEDIATED REDUCTIVE DECHLORINATION OF TETRACHLOROETHENE

EPA Science Inventory

An analytical method was developed for the determination of lactic acid, formic acid, acetic acid, propionic acid, and butyric acid in environmental microcosm samples using ion-exclusion chromatography. The chromatographic behavior of various eluents was studied to determine the ...

GAS CHROMATOGRAPHIC METHOD FOR QUANTITATIVE DETERMINATION OF C2 TO C13 HYDROCARBONS IN ROADWAY VEHICLE EMISSIONS

EPA Science Inventory

A gas chromatographic system was used to quantitate more than 300 gas-phase hydrocarbons from background and roadside ambient air samples. Samples were simultaneously collected in Tedlar bags and on Tenax cartridges. Hydrocarbons from Tedlar bag-collected samples were quantitated...

GC-MS (GAS CHROMATOGRAPHIC-MASS SPECTROMETRIC) SUITABILITY TESTING OF RCRA APPENDIX VIII AND MICHIGAN LIST ANALYTES

EPA Science Inventory

As a first step in a hierarchical scheme to demonstrate the suitability of present U.S. Environmental Protection Agency (USEPA) analysis methods and/or develop new methodology, the gas chromatographic (GC) separation and mass spectrometric (MS) detection characteristics of 328 to...

Using the Pearson Distribution for Synthesis of the Suboptimal Algorithms for Filtering Multi-Dimensional Markov Processes

NASA Astrophysics Data System (ADS)

Mit'kin, A. S.; Pogorelov, V. A.; Chub, E. G.

2015-08-01

We consider the method of constructing the suboptimal filter on the basis of approximating the a posteriori probability density of the multidimensional Markov process by the Pearson distributions. The proposed method can efficiently be used for approximating asymmetric, excessive, and finite densities.

The Necessity-Concerns-Framework: A Multidimensional Theory Benefits from Multidimensional Analysis

PubMed Central

Phillips, L. Alison; Diefenbach, Michael; Kronish, Ian M.; Negron, Rennie M.; Horowitz, Carol R.

2014-01-01

Background Patients’ medication-related concerns and necessity-beliefs predict adherence. Evaluation of the potentially complex interplay of these two dimensions has been limited because of methods that reduce them to a single dimension (difference scores). Purpose We use polynomial regression to assess the multidimensional effect of stroke-event survivors’ medication-related concerns and necessity-beliefs on their adherence to stroke-prevention medication. Methods Survivors (n=600) rated their concerns, necessity-beliefs, and adherence to medication. Confirmatory and exploratory polynomial regression determined the best-fitting multidimensional model. Results As posited by the Necessity-Concerns Framework (NCF), the greatest and lowest adherence was reported by those with strong necessity-beliefs/weak concerns and strong concerns/weak necessity-beliefs, respectively. However, as could not be assessed using a difference-score model, patients with ambivalent beliefs were less adherent than those exhibiting indifference. Conclusions Polynomial regression allows for assessment of the multidimensional nature of the NCF. Clinicians/Researchers should be aware that concerns and necessity dimensions are not polar opposites. PMID:24500078

Deconvolution of gas chromatographic data

NASA Technical Reports Server (NTRS)

Howard, S.; Rayborn, G. H.

1980-01-01

The use of deconvolution methods on gas chromatographic data to obtain an accurate determination of the relative amounts of each material present by mathematically separating the merged peaks is discussed. Data were obtained on a gas chromatograph with a flame ionization detector. Chromatograms of five xylenes with differing degrees of separation were generated by varying the column temperature at selected rates. The merged peaks were then successfully separated by deconvolution. The concept of function continuation in the frequency domain was introduced in striving to reach the theoretical limit of accuracy, but proved to be only partially successful.

Multidimensional chromatographic techniques for hydrophilic copolymers II. Analysis of poly(ethylene glycol)-poly(vinyl acetate) graft copolymers.

PubMed

Knecht, Daniela; Rittig, Frank; Lange, Ronald F M; Pasch, Harald

2006-10-13

A large variety of hydrophilic copolymers is applied in different fields of chemical industry including bio, pharma and pharmaceutical applications. For example, poly(ethylene glycol)-poly(vinyl alcohol) graft copolymers that are used as tablet coatings are responsible for the controlled release of the active compounds. These copolymers are produced by grafting of vinyl acetate onto polyethylene glycol (PEG) and subsequent hydrolysis of the poly(ethylene glycol)-poly(vinyl acetate) graft copolymers. The poly(ethylene glycol)-poly(vinyl acetate) copolymers are distributed with regard to molar mass and chemical composition. In addition, they frequently contain the homopolymers polyethylene glycol and polyvinyl acetate. The comprehensive analysis of such complex systems requires hyphenated analytical techniques, including two-dimensional liquid chromatography and combined LC and nuclear magnetic resonance spectroscopy. The development and application of these techniques are discussed in the present paper.

Rapid comprehensive characterization of crude oils by thermogravimetry coupled to fast modulated gas chromatography-single photon ionization time-of-flight mass spectrometry.

PubMed

Wohlfahrt, S; Fischer, M; Saraji-Bozorgzad, M; Matuschek, G; Streibel, T; Post, E; Denner, T; Zimmermann, R

2013-09-01

Comprehensive multi-dimensional hyphenation of a thermogravimetry device (i.e. a thermobalance) to gas chromatography and single photon ionization-time-of-flight mass spectrometry (TG-GC×SPI-MS) has been used to investigate two crude oil samples of different geographical origin. The source of the applied vacuum ultraviolet radiation is an electron beam pumped rare gas excimer lamp (EBEL). The soft photoionization favors the formation of molecular ions. Introduction of a fast, rapidly modulated gas chromatographic separation step in comparison with solely TG-SPI-MS enables strongly enhanced detection especially with such highly complex organic matrices as crude oil. In contrast with former TG-SPI-MS measurements, separation and identification of overlying substances is possible because of different GC retention times. The specific contribution of isobaric compounds to one mass signal is determined for alkanes, naphthalenes, alkylated benzenes, and other compounds.

Coupled LC-GC techniques for the characterisation of polycyclic aromatic compounds in fuel materials

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

Askey, S.A.; Holden, K.M.L.; Bartle, K.D.

1995-12-31

Exposure to polycyclic aromatic compounds (PAC) has long been identified as of considerable environmental concern. Originating from both natural and anthropogenic sources, many PAC exhibit significant carcinogenic and mutagenic properties. Multi-dimensional chromatographic techniques which provide separation by virtue of chemical class (group-type) or by molecular mass greatly simplifies the analysis of inherently complex fuel materials. In this study, on-line LC-GC techniques in which high resolution gas chromatography (HPLC) have been investigated. Comprehensive characterisation of fuel feedstocks and post-pyrolysis and combustion products was achieved by coupling LC-GC to low resolution ion trap mass spectrometry (ITD-MS) and atomic emission detection (AED). Themore » identification of PAC in diesel and coal materials, as well as urban air and diesel exhaust particulate extracts has provided valuable insight into the source, formation and distribution of such compounds pre- and post processing.« less

Gas-chromatographic determination of camylofine dihydrochloride in tablets and suppositories.

PubMed

Crombez, E; van den Bossche, W; De Moerloose, P

1976-02-04

A gas-chromatographic method for the quantitative determination of camylofine dihydrochloride, a spasmolytic agent, is described. The analysis is made on a porous polymer packing material, by determining the 3-methyl-1-butanol formed on alkaline hydrolysis of the drug. The method has been applied to the quantitative determination of the drug in two galenical forms, namely tablets and suppositories, in the presence of papaverine hydrochloride, codeine phosphate, novalgin and aminopyrine.

High-performance liquid chromatographic determination of the beta2-selective adrenergic agonist fenoterol in human plasma after fluorescence derivatization.

PubMed

Kramer, S; Blaschke, G

2001-02-10

A sensitive high-performance liquid chromatographic method has been developed for the determination of the beta2-selective adrenergic agonist fenoterol in human plasma. To improve the sensitivity of the method, fenoterol was derivatized with N-(chloroformyl)-carbazole prior to HPLC analysis yielding highly fluorescent derivatives. The assay involves protein precipitation with acetonitrile, liquid-liquid-extraction of fenoterol from plasma with isobutanol under alkaline conditions followed by derivatization with N-(chloroformyl)-carbazole. Reversed-phase liquid chromatographic determination of the fenoterol derivative was performed using a column-switching system consisting of a LiChrospher 100 RP 18 and a LiChrospher RP-Select B column with acetonitrile, methanol and water as mobile phase. The limit of quantitation in human plasma was 376 pg fenoterol/ml. The method was successfully applied for the assay of fenoterol in patient plasma.

Gas chromatographic determination of carboxylic acid chlorides and residual carboxylic acid precursors used in the production of some penicillins.

PubMed

Lauback, R G; Balitz, D F; Mays, D L

1976-05-01

An improved gas chromatographic method is described for the simultaneous determination of carboxylic acid chlorides and related carboxylic acids used in the production of some commercial semisynthetic penicillins. The acid chloride reacts with diethylamine to form the corresponding diethylamide. Carboxylic acid impurities are converted to trimethylsilyl esters. The two derivatives are separated and quantitated in the same chromatographic run. This method, an extension of the earlier procedure of Hishta and Bomstein (1), has been applied to the acid chlorides used to make oxacillin, cloxacillin, dicloxacillin, and methicillin (Figure 1); it shows promise of application to other acid chlorides. The determination is more selective than the usual titration methods, which do not differentiate among acids with similar pK's. Relative standard deviations of the acid chloride determination are 1.0-2.5%. Residual carboxylic acid can be repetitively determined within a range of 0.6% absolute.

Chromatographic fingerprint analysis of yohimbe bark and related dietary supplements using UHPLC/UV/MS.

PubMed

Sun, Jianghao; Chen, Pei

2012-03-05

A practical ultra high-performance liquid chromatography (UHPLC) method was developed for fingerprint analysis of and determination of yohimbine in yohimbe barks and related dietary supplements. Good separation was achieved using a Waters Acquity BEH C(18) column with gradient elution using 0.1% (v/v) aqueous ammonium hydroxide and 0.1% ammonium hydroxide in methanol as the mobile phases. The study is the first reported chromatographic method that separates corynanthine from yohimbine in yohimbe bark extract. The chromatographic fingerprint analysis was applied to the analysis of 18 yohimbe commercial dietary supplement samples. Quantitation of yohimbine, the traditional method for analysis of yohimbe barks, were also performed to evaluate the results of the fingerprint analysis. Wide variability was observed in fingerprints and yohimbine content among yohimbe dietary supplement samples. For most of the dietary supplements, the yohimbine content was not consistent with the label claims. Copyright © 2011. Published by Elsevier B.V.

Label-free assay based on immobilized capillary enzyme reactor of Leishmania infantum nucleoside triphosphate diphosphohydrolase (LicNTPDase-2-ICER-LC/UV).

PubMed

Magalhães, Luana; de Oliveira, Arthur Henrique Cavalcante; de Souza Vasconcellos, Raphael; Mariotini-Moura, Christiane; de Cássia Firmino, Rafaela; Fietto, Juliana Lopes Rangel; Cardoso, Carmen Lúcia

2016-01-01

Nucleoside triphosphate diphosphohydrolase (NTPDase) is an enzyme belonging to the apyrase family that participates in the hydrolysis of the nucleosides di- and triphosphate to the corresponding nucleoside monophosphate. This enzyme underlies the virulence of parasites such as Leishmania. Recently, an NTPDase from Leishmania infantum (LicNTPDase-2) was cloned and expressed and has been considered as a new drug target for the treatment of leishmaniasis. With the intent of developing label-free online screening methodologies, LicNTPDase-2 was covalently immobilized onto a fused silica capillary tube in the present study to create an immobilized capillary enzyme reactor (ICER) based on LicNTPDase-2 (LicNTPDase-2-ICER). To perform the activity assays, a multidimensional chromatographic method was developed employing the LicNTPDase-2-ICER in the first dimension, and an analytical Ascentis C8 column was used in the second dimension to provide analytical separation of the substrates and products. The validated LicNTPDase-2-ICER method provided the following kinetic parameters of the immobilized enzyme: KM of 2.2 and 1.8mmolL(-1) for the ADP and ATP substrates, respectively. Suramin (1mmolL(-1)) was also shown to inhibit 32.9% of the enzymatic activity. The developed method is applicable to kinetic studies and enables the recognition of the ligands. Furthermore, a comparison of the values of LicNTPDase-2-ICER with those obtained with an LC method using free enzyme in solution showed that LicNTPDase-2-ICER-LC/UV was an accurate and reproducible method that enabled automated measurements for the rapid screening of ligands. Copyright © 2015 Elsevier B.V. All rights reserved.

Multidimensional CAT Item Selection Methods for Domain Scores and Composite Scores with Item Exposure Control and Content Constraints

ERIC Educational Resources Information Center

Yao, Lihua

2014-01-01

The intent of this research was to find an item selection procedure in the multidimensional computer adaptive testing (CAT) framework that yielded higher precision for both the domain and composite abilities, had a higher usage of the item pool, and controlled the exposure rate. Five multidimensional CAT item selection procedures (minimum angle;…

Development and evaluation of a gas chromatographic method for the determination of triazine herbicides in natural water samples

USGS Publications Warehouse

Steinheimer, T.R.; Brooks, M.G.

1984-01-01

A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0.1 ??g/L in a 1-litre sample. Three different natural water samples were used for error analysis via evaluation of recovery efficiencies and estimation of overall method precision. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0. 1 mu g/L in a 1-litre sample. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.

Partition/Ion-Exclusion Chromatographic Ion Stacking for the Analysis of Trace Anions in Water and Salt Samples by Ion Chromatography.

PubMed

Akter, Fouzia; Saito, Shingo; Tasaki-Handa, Yuiko; Shibukawa, Masami

2018-01-01

A new analytical methodology for a simple and efficient on-line preconcentration of trace inorganic anions in water and salt samples prior to ion chromatographic determination is proposed. The preconcentration method is based on partition/ion-exclusion chromatographic ion stacking (PIEC ion stacking) with a hydrophilic polymer gel column containing a small amount of fixed anionic charges. The developed on-line PIEC ion stacking-ion chromatography method was validated by recovery experiments for the determination of nitrate in tap water in terms of both accuracy and precision, and the results showed the reliability of the method. The method proposed was also successfully applied to the determination of trace impurity nitrite and nitrate in reagent-grade salts of sodium sulfate. A low background level can be achieved since pure water is used as the eluant for the PIEC ion stacking. It is possible to reach sensitive detection at sub-μg L -1 levels by on-line PIEC ion stacking-ion chromatography.

Gas-liquid chromatographic method for determining ethylenethiourea in potatoes, spinach, applesauce, and milk: collaborative study.

PubMed

Onley, H H

1977-09-01

Eight laboratories collaboratively tested a gas-liquid chromatographic method for determining ethylenetiourea (ETU) in potatoes, spinach, applesauce, and milk. In the determinative step, ETU is converted to the S-butyl derivative (2-n-butylmercapto-2-imidazoline) which is detected by a flame photometric detector, sulfur mode. For unknown fortification levels of 0.06, 0.12, and 0.30 ppm, the collaborators reported an overall average recovery range of 85-97% in the various commodities. The method has been adopted as interim official first action.

High-performance liquid chromatographic determination of benzil in air as an indicator of emissions derived from polyester powder coatings.

PubMed

Pukkila, J; Kokotti, H; Peltonen, K

1989-10-06

A method to estimate occupational exposure to emissions from the curing of polyester powder paints was developed. The method is based on the monitoring only of a certain marker compound in workroom air in order to make the determinations easier. Benzil, reproducibly emitted from all the powders tested, was chosen as the indicator for curing (220 degrees C)-derived emissions. A method for the air sampling and high-performance liquid chromatographic benzil is described. Aspects of the use of marker compounds are discussed.

[HPLC specific chromatogram of Dendrobium officinale].

PubMed

Yan, Mei-Qiu; Chen, Su-Hong; Lv, Gui-Yuan; Zhou, Gui-Fen; Liu, Xia

2013-02-01

To establish the method of specific chromatogram analysis of ether extract of Dendrobium officinale for identification of D. officinale. Chromatographic separation was carried out at 30 degrees C on an Ultimate C18 column (4.6 mm x 250 mm, 5 microm) eluted with methanol and water containing 0.2% phosphoric acid in a gradient elution at a flow rate of 1.0 mL x min(-1). The detection wavelength was set at 280 nm. The similarity evaluation system for chromatographic fingerprint of NPC (National Pharmacopoeia Committee) was adopted to specific chromatogram construction. The HPLC specific chromatogram of D. officinale was constructed with 6 common specific chromatographic peaks including naringenin as a reference peak. The method shows good precision and repeatability of relative retention time. It can be used to identify D. officinale.

A nonlinear model for gas chromatograph systems

NASA Technical Reports Server (NTRS)

Feinberg, M. P.

1975-01-01

Fundamental engineering design techniques and concepts were studied for the optimization of a gas chromatograph-mass spectrometer chemical analysis system suitable for use on an unmanned, Martian roving vehicle. Previously developed mathematical models of the gas chromatograph are found to be inadequate for predicting peak heights and spreading for some experimental conditions and chemical systems. A modification to the existing equilibrium adsorption model is required; the Langmuir isotherm replaces the linear isotherm. The numerical technique of Crank-Nicolson was studied for use with the linear isotherm to determine the utility of the method. Modifications are made to the method eliminate unnecessary calculations which result in an overall reduction of the computation time of about 42 percent. The Langmuir isotherm is considered which takes into account the composition-dependent effects on the thermodynamic parameter, mRo.

An Examination of Alternative Multidimensional Scaling Techniques

ERIC Educational Resources Information Center

Papazoglou, Sofia; Mylonas, Kostas

2017-01-01

The purpose of this study is to compare alternative multidimensional scaling (MDS) methods for constraining the stimuli on the circumference of a circle and on the surface of a sphere. Specifically, the existing MDS-T method for plotting the stimuli on the circumference of a circle is applied, and its extension is proposed for constraining the…

Multivariate curve resolution based chromatographic peak alignment combined with parallel factor analysis to exploit second-order advantage in complex chromatographic measurements.

PubMed

Parastar, Hadi; Akvan, Nadia

2014-03-13

In the present contribution, a new combination of multivariate curve resolution-correlation optimized warping (MCR-COW) with trilinear parallel factor analysis (PARAFAC) is developed to exploit second-order advantage in complex chromatographic measurements. In MCR-COW, the complexity of the chromatographic data is reduced by arranging the data in a column-wise augmented matrix, analyzing using MCR bilinear model and aligning the resolved elution profiles using COW in a component-wise manner. The aligned chromatographic data is then decomposed using trilinear model of PARAFAC in order to exploit pure chromatographic and spectroscopic information. The performance of this strategy is evaluated using simulated and real high-performance liquid chromatography-diode array detection (HPLC-DAD) datasets. The obtained results showed that the MCR-COW can efficiently correct elution time shifts of target compounds that are completely overlapped by coeluted interferences in complex chromatographic data. In addition, the PARAFAC analysis of aligned chromatographic data has the advantage of unique decomposition of overlapped chromatographic peaks to identify and quantify the target compounds in the presence of interferences. Finally, to confirm the reliability of the proposed strategy, the performance of the MCR-COW-PARAFAC is compared with the frequently used methods of PARAFAC, COW-PARAFAC, multivariate curve resolution-alternating least squares (MCR-ALS), and MCR-COW-MCR. In general, in most of the cases the MCR-COW-PARAFAC showed an improvement in terms of lack of fit (LOF), relative error (RE) and spectral correlation coefficients in comparison to the PARAFAC, COW-PARAFAC, MCR-ALS and MCR-COW-MCR results. Copyright © 2014 Elsevier B.V. All rights reserved.

Differentiation of Panax quinquefolius grown in United States and China using LC/MS-based chromatographic fingerprinting and metabolomic approaches

USDA-ARS?s Scientific Manuscript database

American ginseng (Panax quinquefolius) is one of the most commonly used herbal medicines in the world. Discriminating between P. quinquefolius grown in different countries is difficult using the traditional quantitation methods. In this study, a liquid chromatographic mass spectrometry (LC-MS) fing...

40 CFR 59.505 - How do I demonstrate compliance with the reactivity limits?

Code of Federal Regulations, 2011 CFR

2011-07-01

... for both the liquid and propellant phases), California Air Resources Board Method 310—Determination of... Pollutant Compounds in Paints and Coatings by Direct Injection into a Gas Chromatograph (40 CFR part 63... Injection into a Gas Chromatograph (40 CFR part 63, appendix A) results, the California Air Resources Board...

Determination of total and polycyclic aromatic hydrocarbons in aviation jet fuel.

PubMed

Bernabei, M; Reda, R; Galiero, R; Bocchinfuso, G

2003-01-24

The aviation jet fuel widely used in turbine engine aircraft is manufactured from straight-run kerosene. The combustion quality of jet fuel is largely related to the hydrocarbon composition of the fuel itself; paraffins have better burning properties than aromatic compounds, especially naphthalenes and light polycyclic aromatic hydrocarbons (PAHs), which are characterised as soot and smoke producers. For this reason the burning quality of fuel is generally measured as smoke fermation. This evaluation is carried out with UV spectrophotometric determination of total naphthalene hydrocarbons and a chromatographic analysis to determine the total aromatic compounds. These methods can be considered insufficient to evaluate the human health impact of these compounds due to their inability to measure trace (ppm) amounts of each aromatic hyrcarbon and each PAH in accordance with limitations imposed because of their toxicological properties. In this paper two analytical methods are presented. Both are based on a gas chromatographic technique with a mass detector operating in be selected ion monitoring mode. The first method was able to determine more than 60 aromatic hydrocarbons in a fuel sample in a 35-min chromatographic run, while the second was able to carry out the analysis of more than 30 PAHs in a 40-min chromatographic run. The linearity and sensitivity of the methods in measuring these analytes at trace levels are described.

Probes for multidimensional nanospectroscopic imaging and methods of fabrication thereof

DOEpatents

Weber-Bargioni, Alexander; Cabrini, Stefano; Bao, Wei; Melli, Mauro; Yablonovitch, Eli; Schuck, Peter J

2015-03-17

This disclosure provides systems, methods, and apparatus related to probes for multidimensional nanospectroscopic imaging. In one aspect, a method includes providing a transparent tip comprising a dielectric material. A four-sided pyramidal-shaped structure is formed at an apex of the transparent tip using a focused ion beam. Metal layers are deposited over two opposing sides of the four-sided pyramidal-shaped structure.

Quality assessment of Herba Leonuri based on the analysis of multiple components using normal- and reversed-phase chromatographic methods.

PubMed

Dong, Shuya; He, Jiao; Hou, Huiping; Shuai, Yaping; Wang, Qi; Yang, Wenling; Sun, Zheng; Li, Qing; Bi, Kaishun; Liu, Ran

2017-12-01

A novel, improved, and comprehensive method for quality evaluation and discrimination of Herba Leonuri has been developed and validated based on normal- and reversed-phase chromatographic methods. To identify Herba Leonuri, normal- and reversed-phase high-performance thin-layer chromatography fingerprints were obtained by comparing the colors and R f values of the bands, and reversed-phase high-performance liquid chromatography fingerprints were obtained by using an Agilent Poroshell 120 SB-C18 within 28 min. By similarity analysis and hierarchical clustering analysis, we show that there are similar chromatographic patterns in Herba Leonuri samples, but significant differences in counterfeits and variants. To quantify the bio-active components of Herba Leonuri, reversed-phase high-performance liquid chromatography was performed to analyze syringate, leonurine, quercetin-3-O-robiniaglycoside, hyperoside, rutin, isoquercitrin, wogonin, and genkwanin simultaneously by single standard to determine multi-components method with rutin as internal standard. Meanwhile, normal-phase high-performance liquid chromatography was performed by using an Agilent ZORBAX HILIC Plus within 6 min to determine trigonelline and stachydrine using trigonelline as internal standard. Innovatively, among these compounds, bio-active components of quercetin-3-O-robiniaglycoside and trigonelline were first determined in Herba Leonuri. In general, the method integrating multi-chromatographic analyses offered an efficient way for the standardization and identification of Herba Leonuri. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A new analytical method for quantification of olive and palm oil in blends with other vegetable edible oils based on the chromatographic fingerprints from the methyl-transesterified fraction.

PubMed

Jiménez-Carvelo, Ana M; González-Casado, Antonio; Cuadros-Rodríguez, Luis

2017-03-01

A new analytical method for the quantification of olive oil and palm oil in blends with other vegetable edible oils (canola, safflower, corn, peanut, seeds, grapeseed, linseed, sesame and soybean) using normal phase liquid chromatography, and applying chemometric tools was developed. The procedure for obtaining of chromatographic fingerprint from the methyl-transesterified fraction from each blend is described. The multivariate quantification methods used were Partial Least Square-Regression (PLS-R) and Support Vector Regression (SVR). The quantification results were evaluated by several parameters as the Root Mean Square Error of Validation (RMSEV), Mean Absolute Error of Validation (MAEV) and Median Absolute Error of Validation (MdAEV). It has to be highlighted that the new proposed analytical method, the chromatographic analysis takes only eight minutes and the results obtained showed the potential of this method and allowed quantification of mixtures of olive oil and palm oil with other vegetable oils. Copyright © 2016 Elsevier B.V. All rights reserved.

Sensitive liquid chromatography-tandem mass spectrometry method for the simultaneous determination of paracetamol and guaifenesin in human plasma.

PubMed

Chen, Xiaoyan; Huang, Jia; Kong, Zhang; Zhong, Dafang

2005-03-25

A rapid and sensitive method for the simultaneous determination of paracetamol and guaifenesin in human plasma was developed and validated, using high-performance liquid chromatographic separation with tandem mass spectrometric detection. After extracted from plasma samples by diethyl ether-dichloromethane (3:2, v/v), the analytes and internal standard osalmide were chromatographed on a C18 column. Detection was performed on a triple quadrupole tandem mass spectrometer by selected reaction monitoring (SRM) mode via atmospheric pressure chemical ionization (APCI). The method was linear in the concentration range of 0.05-20.0 microg/ml for paracetamol and 5.0-2000.0 ng/ml for guaifenesin. The intra- and inter-day precision was within 14% for both paracetamol and guaifenesin. The assay accuracy was within +/-2.4% for the analytes. This is the first assay method described for the simultaneous determination of paracetamol and guaifenesin in plasma using one chromatographic run. The method was successfully employed in a pharmacokinetic study after an oral administration of a multicomponent formulation, containing 650 mg paracetamol, 200 mg guaifenesin, 60 mg pseudoephedrine and 20 mg dextrorphan.

A novel multidimensional protein identification technology approach combining protein size exclusion prefractionation, peptide zwitterion-ion hydrophilic interaction chromatography, and nano-ultraperformance RP chromatography/nESI-MS2 for the in-depth analysis of the serum proteome and phosphoproteome: application to clinical sera derived from humans with benign prostate hyperplasia.

PubMed

Garbis, Spiros D; Roumeliotis, Theodoros I; Tyritzis, Stavros I; Zorpas, Kostas M; Pavlakis, Kitty; Constantinides, Constantinos A

2011-02-01

The current proof-of-principle study was aimed toward development of a novel multidimensional protein identification technology (MudPIT) approach for the in-depth proteome analysis of human serum derived from patients with benign prostate hyperplasia (BPH) using rational chromatographic design principles. This study constituted an extension of our published work relating to the identification and relative quantification of potential clinical biomarkers in BPH and prostate cancer (PCa) tissue specimens. The proposed MudPIT approach encompassed the use of three distinct yet complementary liquid chromatographic chemistries. High-pressure size-exclusion chromatography (SEC) was used for the prefractionation of serum proteins followed by their dialysis exchange and solution phase trypsin proteolysis. The tryptic peptides were then subjected to offline zwitterion-ion hydrophilic interaction chromatography (ZIC-HILIC) fractionation followed by their online analysis with reversed-phase nano-ultraperformance chromatography (RP-nUPLC) hyphenated to nanoelectrospray ionization-tandem mass spectrometry using an ion trap mass analyzer. For the spectral processing, the sequential use of the SpectrumMill, Scaffold, and InsPecT software tools was applied for the tryptic peptide product ion MS(2) spectral processing, false discovery rate (FDR) assessment, validation, and protein identification. This milestone serum analysis study allowed the confident identification of over 1955 proteins (p ≤ 0.05; FDR ≤ 5%) with a broad spectrum of biological and physicochemical properties including secreted, tissue-specific proteins spanning approximately 12 orders of magnitude as they occur in their native abundance levels in the serum matrix. Also encompassed in this proteome was the confident identification of 375 phosphoproteins (p ≤ 0.05; FDR ≤ 5%) with potential importance to cancer biology. To demonstrate the performance characteristics of this novel MudPIT approach, a comparison was made with the proteomes resulting from the immunodepletion of the high abundant albumin and IgG proteins with offline first dimensional tryptic peptide separation with both ZIC-HILIC and strong cation exchange (SCX) chromatography and their subsequent online RP-nUPLC-nESI-MS(2) analysis.

Chromatographic methods for determination of S-substituted cysteine derivatives--a comparative study.

PubMed

Kubec, Roman; Dadáková, Eva

2009-10-09

A novel HPLC method for determination of a wide variety of S-substituted cysteine derivatives in Allium species has been developed and validated. This method allows simultaneous separation and quantification of S-alk(en)ylcysteine S-oxides, gamma-glutamyl-S-alk(en)ylcysteines and gamma-glutamyl-S-alk(en)ylcysteine S-oxides in a single run. The procedure is based on extraction of these amino acids and dipeptides by methanol, their derivatization by dansyl chloride and subsequent separation by reversed phase HPLC. The main advantages of the new method are simplicity, excellent stability of derivatives, high sensitivity, specificity and the ability to simultaneously analyze the whole range of S-substituted cysteine derivatives. This method was critically compared with other chromatographic procedures used for quantification of S-substituted cysteine derivatives, namely with two other HPLC methods (derivatization by o-phthaldialdehyde/tert-butylthiol and fluorenylmethyl chloroformate), and with determination by gas chromatography or capillary electrophoresis. Major advantages and drawbacks of these analytical procedures are discussed. Employing these various chromatographic methods, the content and relative proportions of individual S-substituted cysteine derivatives were determined in four most frequently consumed alliaceous vegetables (garlic, onion, shallot, and leek).

Validation of a fast and accurate chromatographic method for detailed quantification of vitamin E in green leafy vegetables.

PubMed

Cruz, Rebeca; Casal, Susana

2013-11-15

Vitamin E analysis in green vegetables is performed by an array of different methods, making it difficult to compare published data or choosing the adequate one for a particular sample. Aiming to achieve a consistent method with wide applicability, the current study reports the development and validation of a fast micro-method for quantification of vitamin E in green leafy vegetables. The methodology uses solid-liquid extraction based on the Folch method, with tocol as internal standard, and normal-phase HPLC with fluorescence detection. A large linear working range was confirmed, being highly reproducible, with inter-day precisions below 5% (RSD). Method sensitivity was established (below 0.02 μg/g fresh weight), and accuracy was assessed by recovery tests (>96%). The method was tested in different green leafy vegetables, evidencing diverse tocochromanol profiles, with variable ratios and amounts of α- and γ-tocopherol, and other minor compounds. The methodology is adequate for routine analyses, with a reduced chromatographic run (<7 min) and organic solvent consumption, and requires only standard chromatographic equipment available in most laboratories. Copyright © 2013 Elsevier Ltd. All rights reserved.

Ion chromatographic determination of sulfur in fuels

NASA Technical Reports Server (NTRS)

Mizisin, C. S.; Kuivinen, D. E.; Otterson, D. A.

1978-01-01

The sulfur content of fuels was determined using an ion chromatograph to measure the sulfate produced by a modified Parr bomb oxidation. Standard Reference Materials from the National Bureau of Standards, of approximately 0.2 + or - 0.004% sulfur, were analyzed resulting in a standard deviation no greater than 0.008. The ion chromatographic method can be applied to conventional fuels as well as shale-oil derived fuels. Other acid forming elements, such as fluorine, chlorine and nitrogen could be determined at the same time, provided that these elements have reached a suitable ionic state during the oxidation of the fuel.

Effects of Multidimensional Family Therapy (MDFT) on Nonopioid Drug Abuse: A Systematic Review and Meta-Analysis

ERIC Educational Resources Information Center

Filges, Trine; Andersen, Ditte; Jørgensen, Anne-Marie Klint

2018-01-01

Purpose: This review evaluates the evidence of the effects of multidimensional family therapy (MDFT) on drug use reduction in young people for the treatment of nonopioid drug use. Method: We followed Campbell Collaboration guidelines to conduct a systematic review of randomized and nonrandomized trials. Meta-analytic methods were used to…

Vacuum polarization in the field of a multidimensional global monopole

NASA Astrophysics Data System (ADS)

Grats, Yu. V.; Spirin, P. A.

2016-11-01

An approximate expression for the Euclidean Green function of a massless scalar field in the spacetime of a multidimensional global monopole has been derived. Expressions for the vacuum expectation values <ϕ2>ren and < T 00>ren have been derived by the dimensional regularization method. Comparison with the results obtained by alternative regularization methods is made.

The Versatility of SpAM: A Fast, Efficient, Spatial Method of Data Collection for Multidimensional Scaling

ERIC Educational Resources Information Center

Hout, Michael C.; Goldinger, Stephen D.; Ferguson, Ryan W.

2013-01-01

Although traditional methods to collect similarity data (for multidimensional scaling [MDS]) are robust, they share a key shortcoming. Specifically, the possible pairwise comparisons in any set of objects grow rapidly as a function of set size. This leads to lengthy experimental protocols, or procedures that involve scaling stimulus subsets. We…

Invited Article: Single-shot THz detection techniques optimized for multidimensional THz spectroscopy

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

Teo, Stephanie M.; Ofori-Okai, Benjamin K.; Werley, Christopher A.

Multidimensional spectroscopy at visible and infrared frequencies has opened a window into the transfer of energy and quantum coherences at ultrafast time scales. For these measurements to be performed in a manageable amount of time, one spectral axis is typically recorded in a single laser shot. An analogous rapid-scanning capability for THz measurements will unlock the multidimensional toolkit in this frequency range. Here, we first review the merits of existing single-shot THz schemes and discuss their potential in multidimensional THz spectroscopy. We then introduce improved experimental designs and noise suppression techniques for the two most promising methods: frequency-to-time encoding withmore » linear spectral interferometry and angle-to-time encoding with dual echelons. Both methods, each using electro-optic detection in the linear regime, were able to reproduce the THz temporal waveform acquired with a traditional scanning delay line. Although spectral interferometry had mediocre performance in terms of signal-to-noise, the dual echelon method was easily implemented and achieved the same level of signal-to-noise as the scanning delay line in only 4.5% of the laser pulses otherwise required (or 22 times faster). This reduction in acquisition time will compress day-long scans to hours and hence provides a practical technique for multidimensional THz measurements.« less

Invited Article: Single-shot THz detection techniques optimized for multidimensional THz spectroscopy.

PubMed

Teo, Stephanie M; Ofori-Okai, Benjamin K; Werley, Christopher A; Nelson, Keith A

2015-05-01

Multidimensional spectroscopy at visible and infrared frequencies has opened a window into the transfer of energy and quantum coherences at ultrafast time scales. For these measurements to be performed in a manageable amount of time, one spectral axis is typically recorded in a single laser shot. An analogous rapid-scanning capability for THz measurements will unlock the multidimensional toolkit in this frequency range. Here, we first review the merits of existing single-shot THz schemes and discuss their potential in multidimensional THz spectroscopy. We then introduce improved experimental designs and noise suppression techniques for the two most promising methods: frequency-to-time encoding with linear spectral interferometry and angle-to-time encoding with dual echelons. Both methods, each using electro-optic detection in the linear regime, were able to reproduce the THz temporal waveform acquired with a traditional scanning delay line. Although spectral interferometry had mediocre performance in terms of signal-to-noise, the dual echelon method was easily implemented and achieved the same level of signal-to-noise as the scanning delay line in only 4.5% of the laser pulses otherwise required (or 22 times faster). This reduction in acquisition time will compress day-long scans to hours and hence provides a practical technique for multidimensional THz measurements.

VALIDATION OF AN EPA METHOD FOR THE ION CHROMATOGRAPHIC DETERMINATION OF PERCHLORATE IN FERTILIZERS USING A POLYVINYL ALCOHOL GEL RESIN.

EPA Science Inventory

This paper summarizes the key points of a joint study between the EPA and Metrohm-Peak, Inc., on the use of polyvinyl alcohol [PVA] columns for the ion chromatographic determination of percholorate in aqueous leachates or solutions of fertilizers. A series of fertilizer samples ...

High-speed peak matching algorithm for retention time alignment of gas chromatographic data for chemometric analysis

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

Johnson, Kevin J.; Wright, Bob W.; Jarman, Kristin H.

2003-05-09

A rapid retention time alignment algorithm was developed as a preprocessing utility to be used prior to chemometric analysis of large datasets of diesel fuel gas chromatographic profiles. Retention time variation from chromatogram-to-chromatogram has been a significant impediment against the use of chemometric techniques in the analysis of chromatographic data due to the inability of current multivariate techniques to correctly model information that shifts from variable to variable within a dataset. The algorithm developed is shown to increase the efficacy of pattern recognition methods applied to a set of diesel fuel chromatograms by retaining chemical selectivity while reducing chromatogram-to-chromatogram retentionmore » time variations and to do so on a time scale that makes analysis of large sets of chromatographic data practical.« less

Increasing Accuracy of Tissue Shear Modulus Reconstruction Using Ultrasonic Strain Tensor Measurement

NASA Astrophysics Data System (ADS)

Sumi, C.

Previously, we developed three displacement vector measurement methods, i.e., the multidimensional cross-spectrum phase gradient method (MCSPGM), the multidimensional autocorrelation method (MAM), and the multidimensional Doppler method (MDM). To increase the accuracies and stabilities of lateral and elevational displacement measurements, we also developed spatially variant, displacement component-dependent regularization. In particular, the regularization of only the lateral/elevational displacements is advantageous for the lateral unmodulated case. The demonstrated measurements of the displacement vector distributions in experiments using an inhomogeneous shear modulus agar phantom confirm that displacement-component-dependent regularization enables more stable shear modulus reconstruction. In this report, we also review our developed lateral modulation methods that use Parabolic functions, Hanning windows, and Gaussian functions in the apodization function and the optimized apodization function that realizes the designed point spread function (PSF). The modulations significantly increase the accuracy of the strain tensor measurement and shear modulus reconstruction (demonstrated using an agar phantom).

Methods and apparatus for analysis of chromatographic migration patterns

DOEpatents

Stockham, Thomas G.; Ives, Jeffrey T.

1993-01-01

A method and apparatus for sharpening signal peaks in a signal representing the distribution of biological or chemical components of a mixture separated by a chromatographic technique such as, but not limited to, electrophoresis. A key step in the method is the use of a blind deconvolution technique, presently embodied as homomorphic filtering, to reduce the contribution of a blurring function to the signal encoding the peaks of the distribution. The invention further includes steps and apparatus directed to determination of a nucleotide sequence from a set of four such signals representing DNA sequence data derived by electrophoretic means.

Chromatographic determination of Fe chelated by ethylenediamine-N-(o-hydroxyphenylacetic)-N'-(p-hydroxyphenylacetic) acid in commercial EDDHA/Fe3+ fertilizers.

PubMed

García-Marco, Sonia; Torreblanca, Ana; Lucena, Juan J

2006-02-22

EDDHA/Fe3+ chelates are the most common fertilizers used to solve Fe chlorosis in established crops. Commercial products contain two regioisomers, ethylenediamine-N,N'-bis(o-hydroxyphenylacetic) acid (o,o-EDDHA)/Fe3+ and ethylenediamine-N-(o-hydroxyphenylacetic)-N'-(p-hydroxyphenylacetic) acid (o,p-EDDHA)/Fe3+. Although several chromatographic methods exist for the determination of Fe3+ chelated by the o,o-EDDHA isomer, no method has been described for the quantification of Fe3+ chelated by o,p-EDDHA. In this work, factors that affect the behavior of o,p-EDDHA/Fe3+ in ion pair chromatography are reviewed: pH, ion pair reagent, and organic modifier. The best chromatographic performance was obtained with an aqueous mobile phase at pH 6.0 containing 35% acetonitrile and 5 mM tetrabutylammonium hydroxide under isocratic elution conditions. This method was applied to the quantification of commercial samples.

Improved method for the extraction and chromatographic analysis on a fused-core column of ellagitannins found in oak-aged wine.

PubMed

Navarro, María; Kontoudakis, Nikolaos; Canals, Joan Miquel; García-Romero, Esteban; Gómez-Alonso, Sergio; Zamora, Fernando; Hermosín-Gutiérrez, Isidro

2017-07-01

A new method for the analysis of ellagitannins observed in oak-aged wine is proposed, exhibiting interesting advantages with regard to previously reported analytical methods. The necessary extraction of ellagitannins from wine was simplified to a single step of solid phase extraction (SPE) using size exclusion chromatography with Sephadex LH-20 without the need for any previous SPE of phenolic compounds using reversed-phase materials. The quantitative recovery of wine ellagitannins requires a combined elution with methanol and ethyl acetate, especially for increasing the recovery of the less polar acutissimins. The chromatographic method was performed using a fused-core C18 column, thereby avoiding the coelution of main ellagitannins, such as vescalagin and roburin E. However, the very polar ellagitannins, namely, the roburins A, B and C, still partially coeluted, and their quantification was assisted by the MS detector. This methodology also enabled the analysis of free gallic and ellagic acids in the same chromatographic run. Copyright © 2017 Elsevier Ltd. All rights reserved.

Multiresidue chromatographic method for the determination of macrolide residues in muscle by high-performance liquid chromatography with UV detection.

PubMed

Juhel-Gaugain, M; Anger, B; Laurentie, M

1999-01-01

A high-performance liquid chromatographic (HPLC) method for the simultaneous determination of tilmicosin, tylosin, spiramycin, and its major metabolite neospiramycin was developed that is suitable for porcine, bovine, and poultry muscles. Macrolide residues were extracted from muscle with acetonitrile, fat was removed by liquid-liquid extraction with isooctane, and the extract was then cleaned on Bond Elut C18 cartridges. The HPLC separation was performed on an Inertsil ODS3 C18 column (150 x 4 mm) with 0.05% trifluoroacetic acid-acetonitrile in a gradient mode. Two different chromatographic gradients were used for tilmicosin-tylosin and spiramycin-neospiramycin, and the detection wavelengths were 287 and 232 nm, respectively. The method was validated from 1/2 the maximum residue limit (MRL) to 4 times the MRL with pork muscle samples. Mean recoveries were 60, 63.5, 51, and 42% for tilmicosin, tylosin, spiramycin, and neospiramycin, respectively. The detection limits are 15 micrograms/kg for tilmicosin and tylosin, 30 micrograms/kg for spiramycin, and 25 micrograms/kg for neospiramycin. Linearity, precision, and accuracy of the method were also tested.

HPTLC method for the simultaneous determination of four indole alkaloids in Rauwolfia tetraphylla: a study of organic/green solvent and continuous/pulse sonication.

PubMed

Gupta, Shikha; Shanker, Karuna; Srivastava, Santosh K

2012-07-01

A new validated high-performance thin-layer chromatographic (HPTLC) method has been developed for the simultaneous quantitation of four antipsychotic indole alkaloids (IAs), reserpiline (RP, 1), α-yohimbine (YH, 2), isoreserpiline (IRP, 3) and 10-methoxy tetrahydroalstonine (MTHA, 4) as markers in the leaves of Rauwolfia tetraphylla. Extraction efficiency of the targeted IAs from the leaf matrix with organic and ecofriendly (green) solvents using percolation, ultrasonication and microwave techniques were studied. Non-ionic surfactants, viz. Triton X-100, Triton X-114 and Genapol X-80 were used for extraction and no back-extraction or liquid chromatographic steps were used to remove the targeted IAs from the surfactant-rich extractant phase. The optimized cloud point extraction was found a potentially useful methodology for the preconcentration of the targeted IAs. The separation was achieved on silica gel 60F(254) HPTLC plates using hexane-ethylacetate-methanol (5:4:1, v/v/v) as mobile phase. The quantitation of IAs (1-4) was carried out using the densitometric reflection/absorption mode at 520 nm after post chromatographic derivatization using Dragendorff's reagent. The method was validated for peak purity, precision, accuracy, robustness, limit of detection (LOD) and quantitation (LOQ). Method specificity was confirmed using retention factor (R(f)) and visible spectral (post chromatographic scan) correlation of marker compounds in the samples and standard tracks. Copyright © 2012 Elsevier B.V. All rights reserved.

Development and Validation of a Reversed Phase HPLC Method for Determination of Anacardic Acids in Cashew (Anacardium occidentale) Nut Shell Liquid.

PubMed

Oiram Filho, Francisco; Alcântra, Daniel Barbosa; Rodrigues, Tigressa Helena Soares; Alexandre E Silva, Lorena Mara; de Oliveira Silva, Ebenezer; Zocolo, Guilherme Julião; de Brito, Edy Sousa

2018-04-01

Cashew nut shell liquid (CNSL) contains phenolic lipids with aliphatic chains that are of commercial interest. In this work, a chromatographic method was developed to monitor and quantify anacardic acids (AnAc) in CNSL. Samples containing AnAc were analyzed on a high-performance liquid chromatograph coupled to a diode array detector, equipped with a reversed phase C18 (150 × 4.6 mm × 5 μm) column using acetonitrile and water as the mobile phase both acidified with acetic acid to pH 3.0 in an isocratic mode (80:20:1). The chromatographic method showed adequate selectivity, as it could clearly separate the different AnAc. To validate this method, AnAc triene was used as an external standard at seven different concentrations varying from 50 to 1,000 μg mL-1. The Student's t-test and F-test were applied to ensure high confidence for the obtained data from the analytical calibration curve. The results were satisfactory with respect to intra-day (relative standard deviation (RSD) = 0.60%) and inter-day (RSD = 0.67%) precision, linearity (y = 2,670.8x - 26,949, r2 > 0.9998), system suitability for retention time (RSD = 1.02%), area under the curve (RSD = 0.24%), selectivity and limits of detection (19.8 μg mg-1) and quantification (60.2 μg mg-1). The developed chromatographic method was applied for the analysis of different CNSL samples, and it was deemed suitable for the quantification of AnAc.

A validated high performance liquid chromatograph-photodiode array method for simultaneous determination of 10 bioactive components in compound hongdoushan capsule

PubMed Central

Zhu, Liancai; Yang, Xian; Tan, Jun; Wang, Bochu; Zhang, Xue

2014-01-01

Background: The compound Hongdoushan capsule (CHC) is widely known as compound herbal preparation and is often used to treat ovarian cancer and breast cancer, and to enhance the body immunity, etc., in clinical practice. Objective: To determine simultaneously 10 bioactive components from CHC, namely glycyrrhetinic acid, liquiritin, glycyrrhizin, baccatin III, 10-deacetylbaccatin III, cephalomannine, taxol, ginsenoside Rg1, ginsenoside Re, and ginsenoside Rb1. Materials and Methods: A high performance liquid chromatograph method coupled with photodiode array detector was developed and validated for the 1st time. Chromatographic analysis was performed on a SHIMADZU C18 by utilizing a gradient elution program. The mobile phase was acetonitrile (A)-water (B) at a flow rate of 0.8 mL/min. Results: The calibration curve was linear over the investigated concentration ranges with the values of r2 higher than 0.9993 for all the 10 bioactive components. The average recovery rates range from 98.4% to 100.5% with relative standard deviations ≤2.9%. The developed method was successfully applied to analyze 10 compounds in six CHC samples from different batches. In addition, the herbal sources of 32 chromatographic peaks were identified through comparative studying on chromatograms of standard, the respective extracts of Hongdoushan, RenShen, GanCao, and CHC. Conclusion: All the results imply that the accurate and reproducible method developed has high separation rate and enables the determination of 10 bioactive components in a single run for the quality control of CHC. PMID:24696551

[Fluorescent signal detection of chromatographic chip by algorithms of pyramid connection and Gaussian mixture model].

PubMed

Hu, Beibei; Zhang, Xueqing; Chen, Haopeng; Cui, Daxiang

2011-03-01

We proposed a new algorithm for automatic identification of fluorescent signal. Based on the features of chromatographic chips, mathematic morphology in RGB color space was used to filter and enhance the images, pyramid connection was used to segment the areas of fluorescent signal, and then the method of Gaussian Mixture Model was used to detect the fluorescent signal. Finally we calculated the average fluorescent intensity in obtained fluorescent areas. Our results show that the algorithm has a good efficacy to segment the fluorescent areas, can detect the fluorescent signal quickly and accurately, and finally realize the quantitative detection of fluorescent signal in chromatographic chip.

QUANTITATION OF PERCHLORATE ION BY ELECTROSPRAY IONIZATION MASS SPECTROMETRY (ESI-MS) USING STABLE ASSOCIATION COMPLEXES WITH ORGANIC CATIONS AND BASES TO ENHANCE SELECTIVITY

EPA Science Inventory

Quantitation of trace levels of perchlorate ion in water has become a key issue since this species was discovered in water supplies around the United States. Although ion chromatographic methods presently offer the lowest limit of detection, =40 nm (4ngm1-1), chromatographic ret...

Inner chromatogram projection (ICP) for resolution of GC-MS data with embedded chromatographic peaks.

PubMed

Wang, Zhi-Guo; Chen, Zeng-Ping; Gong, Fan; Wu, Hai-Long; Yu, Ru-Qin

2002-05-01

The chromatographic peak located inside another peak in the time direction is called an embedded or inner peak in contradistinction with the embedding peak, which is called an outer peak. The chemical components corresponding to inner and outer peaks are called inner and outer components, respectively. This special case of co-eluting chromatograms was investigated using chemometric approaches taking GC-MS as an example. A novel method, named inner chromatogram projection (ICP), for resolution of GC-MS data with embedded chromatographic peaks is derived. Orthogonal projection resolution is first utilized to obtain the chromatographic profile of the inner component. Projection of the two-way data matrix columnwise-normalized along the time direction to the normalized profile of the inner component found is subsequently performed to find the selective m/z points, if they exist, which represent the chromatogram of the outer component by itself. With the profiles obtained, the mass spectra can easily be found by means of a least-squares procedure. The results for both simulated data and real samples demonstrate that the proposed method is capable of achieving satisfactory resolution performance not affected by the shapes of chromatograms and the relative positions of the components involved.

Quality evaluation of extracted ion chromatograms and chromatographic peaks in liquid chromatography/mass spectrometry-based metabolomics data

PubMed Central

2014-01-01

Background Extracted ion chromatogram (EIC) extraction and chromatographic peak detection are two important processing procedures in liquid chromatography/mass spectrometry (LC/MS)-based metabolomics data analysis. Most commonly, the LC/MS technique employs electrospray ionization as the ionization method. The EICs from LC/MS data are often noisy and contain high background signals. Furthermore, the chromatographic peak quality varies with respect to its location in the chromatogram and most peaks have zigzag shapes. Therefore, there is a critical need to develop effective metrics for quality evaluation of EICs and chromatographic peaks in LC/MS based metabolomics data analysis. Results We investigated a comprehensive set of potential quality evaluation metrics for extracted EICs and detected chromatographic peaks. Specifically, for EIC quality evaluation, we analyzed the mass chromatographic quality index (MCQ index) and propose a novel quality evaluation metric, the EIC-related global zigzag index, which is based on an EIC's first order derivatives. For chromatographic peak quality evaluation, we analyzed and compared six metrics: sharpness, Gaussian similarity, signal-to-noise ratio, peak significance level, triangle peak area similarity ratio and the local peak-related local zigzag index. Conclusions Although the MCQ index is suited for selecting and aligning analyte components, it cannot fairly evaluate EICs with high background signals or those containing only a single peak. Our proposed EIC related global zigzag index is robust enough to evaluate EIC qualities in both scenarios. Of the six peak quality evaluation metrics, the sharpness, peak significance level, and zigzag index outperform the others due to the zigzag nature of LC/MS chromatographic peaks. Furthermore, using several peak quality metrics in combination is more efficient than individual metrics in peak quality evaluation. PMID:25350128

Quality evaluation of extracted ion chromatograms and chromatographic peaks in liquid chromatography/mass spectrometry-based metabolomics data.

PubMed

Zhang, Wenchao; Zhao, Patrick X

2014-01-01

Extracted ion chromatogram (EIC) extraction and chromatographic peak detection are two important processing procedures in liquid chromatography/mass spectrometry (LC/MS)-based metabolomics data analysis. Most commonly, the LC/MS technique employs electrospray ionization as the ionization method. The EICs from LC/MS data are often noisy and contain high background signals. Furthermore, the chromatographic peak quality varies with respect to its location in the chromatogram and most peaks have zigzag shapes. Therefore, there is a critical need to develop effective metrics for quality evaluation of EICs and chromatographic peaks in LC/MS based metabolomics data analysis. We investigated a comprehensive set of potential quality evaluation metrics for extracted EICs and detected chromatographic peaks. Specifically, for EIC quality evaluation, we analyzed the mass chromatographic quality index (MCQ index) and propose a novel quality evaluation metric, the EIC-related global zigzag index, which is based on an EIC's first order derivatives. For chromatographic peak quality evaluation, we analyzed and compared six metrics: sharpness, Gaussian similarity, signal-to-noise ratio, peak significance level, triangle peak area similarity ratio and the local peak-related local zigzag index. Although the MCQ index is suited for selecting and aligning analyte components, it cannot fairly evaluate EICs with high background signals or those containing only a single peak. Our proposed EIC related global zigzag index is robust enough to evaluate EIC qualities in both scenarios. Of the six peak quality evaluation metrics, the sharpness, peak significance level, and zigzag index outperform the others due to the zigzag nature of LC/MS chromatographic peaks. Furthermore, using several peak quality metrics in combination is more efficient than individual metrics in peak quality evaluation.

Gas chromatographic analysis of dimethyltryptamine and beta-carboline alkaloids in ayahuasca, an Amazonian psychoactive plant beverage.

PubMed

Pires, Ana Paula Salum; De Oliveira, Carolina Dizioli Rodrigues; Moura, Sidnei; Dörr, Felipe Augusto; Silva, Wagner Abreu E; Yonamine, Mauricio

2009-01-01

Ayahuasca is obtained by infusing the pounded stems of Banisteriopsis caapi in combination with the leaves of Psychotria viridis. P. viridis is rich in the psychedelic indole N,N-dimethyltryptamine, whereas B. caapi contains substantial amounts of beta-carboline alkaloids, mainly harmine, harmaline and tetrahydroharmine, which are monoamine-oxidase inhibitors. Because of differences in composition in ayahuasca preparations, a method to measure their main active constituents is needed. To develop a gas chromatographic method for the simultaneous determination of dimethyltryptamine and the main beta-carbolines found in ayahuasca preparations. The alkaloids were extracted by means of solid phase extraction (C(18)) and detected by gas chromatography with nitrogen/phosphorous detector. The lower limit of quantification (LLOQ) was 0.02 mg/mL for all analytes. The calibration curves were linear over a concentration range of 0.02-4.0 mg/mL (r(2 )> 0.99). The method was also precise (RSD < 10%). A simple gas chromatographic method to determine the main alkaloids found in ayahuasca was developed and validated. The method can be useful to estimate administered doses in animals and humans for further pharmacological and toxicological investigations of ayahuasca. Copyright (c) 2009 John Wiley & Sons, Ltd.

Leveraging probabilistic peak detection to estimate baseline drift in complex chromatographic samples.

PubMed

Lopatka, Martin; Barcaru, Andrei; Sjerps, Marjan J; Vivó-Truyols, Gabriel

2016-01-29

Accurate analysis of chromatographic data often requires the removal of baseline drift. A frequently employed strategy strives to determine asymmetric weights in order to fit a baseline model by regression. Unfortunately, chromatograms characterized by a very high peak saturation pose a significant challenge to such algorithms. In addition, a low signal-to-noise ratio (i.e. s/n<40) also adversely affects accurate baseline correction by asymmetrically weighted regression. We present a baseline estimation method that leverages a probabilistic peak detection algorithm. A posterior probability of being affected by a peak is computed for each point in the chromatogram, leading to a set of weights that allow non-iterative calculation of a baseline estimate. For extremely saturated chromatograms, the peak weighted (PW) method demonstrates notable improvement compared to the other methods examined. However, in chromatograms characterized by low-noise and well-resolved peaks, the asymmetric least squares (ALS) and the more sophisticated Mixture Model (MM) approaches achieve superior results in significantly less time. We evaluate the performance of these three baseline correction methods over a range of chromatographic conditions to demonstrate the cases in which each method is most appropriate. Copyright © 2016 Elsevier B.V. All rights reserved.

The space transformation in the simulation of multidimensional random fields

USGS Publications Warehouse

Christakos, G.

1987-01-01

Space transformations are proposed as a mathematically meaningful and practically comprehensive approach to simulate multidimensional random fields. Within this context the turning bands method of simulation is reconsidered and improved in both the space and frequency domains. ?? 1987.

Methods for estimating properties of hydrocarbons comprising asphaltenes based on their solubility

DOEpatents

Schabron, John F.; Rovani, Jr., Joseph F.

2016-10-04

Disclosed herein is a method of estimating a property of a hydrocarbon comprising the steps of: preparing a liquid sample of a hydrocarbon, the hydrocarbon having asphaltene fractions therein; precipitating at least some of the asphaltenes of a hydrocarbon from the liquid sample with one or more precipitants in a chromatographic column; dissolving at least two of the different asphaltene fractions from the precipitated asphaltenes during a successive dissolution protocol; eluting the at least two different dissolved asphaltene fractions from the chromatographic column; monitoring the amount of the fractions eluted from the chromatographic column; using detected signals to calculate a percentage of a peak area for a first of the asphaltene fractions and a peak area for a second of the asphaltene fractions relative to the total peak areas, to determine a parameter that relates to the property of the hydrocarbon; and estimating the property of the hydrocarbon.

Multidimensional Risk Analysis: MRISK

NASA Technical Reports Server (NTRS)

McCollum, Raymond; Brown, Douglas; O'Shea, Sarah Beth; Reith, William; Rabulan, Jennifer; Melrose, Graeme

2015-01-01

Multidimensional Risk (MRISK) calculates the combined multidimensional score using Mahalanobis distance. MRISK accounts for covariance between consequence dimensions, which de-conflicts the interdependencies of consequence dimensions, providing a clearer depiction of risks. Additionally, in the event the dimensions are not correlated, Mahalanobis distance reduces to Euclidean distance normalized by the variance and, therefore, represents the most flexible and optimal method to combine dimensions. MRISK is currently being used in NASA's Environmentally Responsible Aviation (ERA) project o assess risk and prioritize scarce resources.

Using a multidimensional unfolding approach to assess multiple sclerosis patient preferences for disease-modifying therapy: a pilot study

PubMed Central

Sempere, Angel Perez; Vera-Lopez, Vanesa; Gimenez-Martinez, Juana; Ruiz-Beato, Elena; Cuervo, Jesús; Maurino, Jorge

2017-01-01

Purpose Multidimensional unfolding is a multivariate method to assess preferences using a small sample size, a geometric model locating individuals and alternatives as points in a joint space. The objective was to evaluate relapsing–remitting multiple sclerosis (RRMS) patient preferences toward key disease-modifying therapy (DMT) attributes using multidimensional unfolding. Patients and methods A cross-sectional pilot study in RRMS patients was conducted. Drug attributes included relapse prevention, disease progression prevention, side-effect risk and route and schedule of administration. Assessment of preferences was performed through a five-card game. Patients were asked to value attributes from 1 (most preferred) to 5 (least preferred). Results A total of 37 patients were included; the mean age was 38.6 years, and 78.4% were female. Disease progression prevention was the most important factor (51.4%), followed by relapse prevention (40.5%). The frequency of administration had the lowest preference rating for 56.8% of patients. Finally, 19.6% valued the side-effect risk attribute as having low/very low importance. Conclusion Patients’ perspective for DMT attributes may provide valuable information to facilitate shared decision-making. Efficacy attributes were the most important drug characteristics for RRMS patients. Multidimensional unfolding seems to be a feasible approach to assess preferences in multiple sclerosis patients. Further elicitation studies using multidimensional unfolding with other stated choice methods are necessary to confirm these findings. PMID:28615928

Simple method for the extraction and reversed-phase high-performance liquid chromatographic analysis of carotenoid pigments from red yeasts (Basidiomycota, Fungi).

PubMed

Weber, Roland W S; Anke, Heidrun; Davoli, Paolo

2007-03-23

A simple method for the extraction of carotenoid pigments from frozen wet cells of red yeasts (Basidiomycota) and their analysis by reversed-phase HPLC using a C(18) column and a water/acetone solvent system is described. Typical red yeast carotenoids belonging to an oxidative series from the monocyclic gamma-carotene to 2-hydroxytorularhodin and from the bicyclic beta-carotene to astaxanthin were separated. Pigment identity was confirmed by LC-atmospheric pressure chemical ionisation (APCI) mass spectrometry using similar chromatographic conditions.

[Gas chromatographic isolation of chloropicrin in drinking water].

PubMed

Malysheva, A G; Sotnikov, E E; Moskovkin, A S; Kamenetskaia, D B

2004-01-01

Gas chromatographic method has been developed to identify chloropicrin in the drinking water, which is based on its separation from water by statistic gas extraction and on the analysis of equilibrium vapor phase on a capillary column with electron-capture and nitrogen-phosphorus detectors connected in series. The method allows chloropicrin to be detected at the level of 5 mg/dm3 with a total measurement error of +/- 10% at a confidence probability of 0.95. The paper shows that the sensitivity of identification can be significantly increased.

[Evaluation of fetal lung maturity using a modified lecithin-sphingomyelin determination and Clements' foam test].

PubMed

Neumann, G; Gartzke, J; Faber, G

1978-01-01

The modified thin layer chromatographic method for the determination of the phospholipids lecithin and sphingomyelin from amniotic fluid is useful in estimating fetal pulmonary maturity. The foam test of Clements is a simple rapid method for screening of suspicious cases of pregnancies at risk and of great value as bed side test even performing by the doctor. In comparing Clements-Test with thin layer chromatographic for L/S-Ratio determination we found a good correlation of 81,8% of all cases.

Determination of ethylene oxide, ethylene chlorohydrin, and ethylene glycol in aqueous solutions and ethylene oxide residues in associated plastics.

PubMed

Ball, N A

1984-09-01

A gas chromatographic (GC) method was developed for the determination of ethylene oxide and its two reaction products, ethylene chlorohydrin and ethylene glycol, in aqueous ophthalmic solutions. Propylene oxide was used as an internal standard. All three components were determined in one isothermal chromatographic analysis in less than 15 min. An extraction method for the determination of ethylene oxide residues in plastic components was also developed, and certain plastics with different ethylene oxide retention characteristics were identified.

Frequency-Comb Based Double-Quantum Two-Dimensional Spectrum Identifies Collective Hyperfine Resonances in Atomic Vapor Induced by Dipole-Dipole Interactions

NASA Astrophysics Data System (ADS)

Lomsadze, Bachana; Cundiff, Steven T.

2018-06-01

Frequency-comb based multidimensional coherent spectroscopy is a novel optical method that enables high-resolution measurement in a short acquisition time. The method's resolution makes multidimensional coherent spectroscopy relevant for atomic systems that have narrow resonances. We use double-quantum multidimensional coherent spectroscopy to reveal collective hyperfine resonances in rubidium vapor at 100 °C induced by dipole-dipole interactions. We observe tilted and elongated line shapes in the double-quantum 2D spectra, which have never been reported for Doppler-broadened systems. The elongated line shapes suggest that the signal is predominately from the interacting atoms that have a near zero relative velocity.

Liquid chromatographic determination of benzocaine and N-acetylbenzocaine in the edible fillet tissue from rainbow trout

USGS Publications Warehouse

Meinertz, J.R.; Stehly, G.R.; Hubert, T.D.; Bernardy, J.A.

1999-01-01

A method was developed for determining benzocaine and N-acetylbenzocaine concentrations in fillet tissue of rainbow trout. The method involves extracting the analytes with acetonitrile, removing lipids or hydrophobic compounds from the extract with hexane, and providing additional clean-up with solid-phase extraction techniques. Analyte concentrations are determined using reversed-phase high-performance liquid chromatographic techniques with an isocratic mobile phase and UV detection. The accuracy (range, 92 to 121%), precision (R.S.D., <14%), and sensitivity (method quantitation limit, <24 ng/g) for each analyte indicate the usefulness of this method for studies characterizing the depletion of benzocaine residues from fish exposed to benzocaine. Copyright (C) 1999.

Membership determination of open clusters based on a spectral clustering method

NASA Astrophysics Data System (ADS)

Gao, Xin-Hua

2018-06-01

We present a spectral clustering (SC) method aimed at segregating reliable members of open clusters in multi-dimensional space. The SC method is a non-parametric clustering technique that performs cluster division using eigenvectors of the similarity matrix; no prior knowledge of the clusters is required. This method is more flexible in dealing with multi-dimensional data compared to other methods of membership determination. We use this method to segregate the cluster members of five open clusters (Hyades, Coma Ber, Pleiades, Praesepe, and NGC 188) in five-dimensional space; fairly clean cluster members are obtained. We find that the SC method can capture a small number of cluster members (weak signal) from a large number of field stars (heavy noise). Based on these cluster members, we compute the mean proper motions and distances for the Hyades, Coma Ber, Pleiades, and Praesepe clusters, and our results are in general quite consistent with the results derived by other authors. The test results indicate that the SC method is highly suitable for segregating cluster members of open clusters based on high-precision multi-dimensional astrometric data such as Gaia data.

Rapid determination of phenolic compounds and alkaloids of carob flour by improved liquid chromatography tandem mass spectrometry.

PubMed

Ortega, Nàdia; Macià, Alba; Romero, Maria-Paz; Trullols, Esther; Morello, Jose-Ramón; Anglès, Neus; Motilva, Maria-Jose

2009-08-26

An improved chromatographic method was developed using ultra-performance liquid chromatography-tandem mass spectrometry to identify and quantify phenolic compounds and alkaloids, theobromine and caffeine, in carob flour samples. The developed method has been validated in terms of speed, sensitivity, selectivity, peak efficiency, linearity, reproducibility, limits of detection, and limits of quantification. The chromatographic method allows the identification and quantification of 20 phenolic compounds, that is, phenolic acids, flavonoids, and their aglycone and glucoside forms, together with the determination of the alkaloids, caffeine and theobromine, at low concentration levels all in a short analysis time of less than 20 min.

Determination of noscapine, hexylresorcinol and anethole in cough lozenges by liquid chromatography.

PubMed

Lucangioli, S; Fernández Otero, G; Rodríguez, V; Carducci, C N

1996-06-01

A liquid chromatographic method was developed for the simultaneous separation and determination of noscapine hydrochloride, hexylresorcinol and anethole in cough lozenges. Analysis was performed on a phenyl column with phosphate buffer- acetonitrile as mobile phase and the separated components were detected at 282 mm. Recoveries obtained for the analytes were of 94.6% for noscapine hydrochloride, 99.1% for hexylresorcinol and 96.3% for anethole. The values of the relative standard deviation were 0.8% for noscapine hydrochloride, 1.5% for hexylresorcinol and 1.1% for anethole. The analytical method was validated and a system suitability test was accomplished for the chromatographic method.

Methods and apparatus for analysis of chromatographic migration patterns

DOEpatents

Stockham, T.G.; Ives, J.T.

1993-12-28

A method and apparatus are presented for sharpening signal peaks in a signal representing the distribution of biological or chemical components of a mixture separated by a chromatographic technique such as, but not limited to, electrophoresis. A key step in the method is the use of a blind deconvolution technique, presently embodied as homomorphic filtering, to reduce the contribution of a blurring function to the signal encoding the peaks of the distribution. The invention further includes steps and apparatus directed to determination of a nucleotide sequence from a set of four such signals representing DNA sequence data derived by electrophoretic means. 16 figures.

High-performance liquid chromatographic method for guanylhydrazone compounds.

PubMed

Cerami, C; Zhang, X; Ulrich, P; Bianchi, M; Tracey, K J; Berger, B J

1996-01-12

A high-performance liquid chromatographic method has been developed for a series of aromatic guanylhydrazones that have demonstrated therapeutic potential as anti-inflammatory agents. The compounds were separated using octadecyl or diisopropyloctyl reversed-phase columns, with an acetonitrile gradient in water containing heptane sulfonate, tetramethylammonium chloride, and phosphoric acid. The method was used to reliably quantify levels of analyte as low as 785 ng/ml, and the detector response was linear to at least 50 micrograms/ml using a 100 microliters injection volume. The assay system was used to determine the basic pharmacokinetics of a lead compound, CNI-1493, from serum concentrations following a single intravenous injection in rats.

Validated chromatographic and spectrophotometric methods for analysis of some amoebicide drugs in their combined pharmaceutical preparation.

PubMed

Abdelaleem, Eglal Adelhamid; Abdelwahab, Nada Sayed

2013-01-01

This work is concerned with development and validation of chromatographic and spectrophotometric methods for analysis of mebeverine HCl (MEH), diloxanide furoate (DF) and metronidazole (MET) in Dimetrol® tablets - spectrophotometric and RP-HPLC methods using UV detection. The developed spectrophotometric methods depend on determination of MEH and DF in the combined dosage form using the successive derivative ratio spectra method which depends on derivatization of the obtained ratio spectra in two steps using methanol as a solvent and measuring MEH at 226.4-232.2 nm (peak to peak) and DF at 260.6-264.8 nm (peak to peak). While MET concentrations were determined using first derivative (1D) at λ = 327 nm using the same solvent. The chromatographic method depends on HPLC separation on ODS column and elution with a mobile phase consisting water: methanol: triethylamine (25: 75: 0.5, by volume, orthophosphoric acid to pH =4). Pumping the mobile phase at 0.7 ml min-1 with UV at 230 nm. Factors affecting the developed methods were studied and optimized, moreover, they have been validated as per ICH guideline and the results demonstrated that the suggested methods are reproducible, reliable and can be applied for routine use with short time of analysis. Statistical analysis of the two developed methods with each other using F and student's-t tests showed no significant difference.

Nitroguanidine Wastewater Pollution Control Technology: Phase 2 Wastewater Characterization and Analytical Methods Development for Organics

DTIC Science & Technology

1984-03-01

a....... .6 Thin Layer Chromatographic (TLC) Analyses... o................. ......a... 7 RESULTS AND DISCUSSIONo.....................o...Beckman 5230 UV/visible spectrophotometer was used for colorimetric determinations of urea and cyanamide. Urea was hydrolyzed by urease and...correlation coefficients were 0.9999. THIN LAYER CHROMATOGRAPHIC (TLC) ANALYSES Cellulose plates were used and were developed in the following systems: 3N

40 CFR 52.742 - Incorporation by reference.

Code of Federal Regulations, 2011 CFR

2011-07-01

... Water-Reducible Paints by Direct Injection into a Gas Chromatograph, for § 52.741(a)(4)(i)(B)(3)(iii... Chromatograph, for § 52.741(a)(4)(i)(B)(3)(v). (6) ASTM D2697-86, Standard Test Method for Volume Nonvolatile... Liquids by Isoteniscope, for § 52.741(a)(3), (a)(8)(ii), (a)(9)(iii), and (a)(10)(iii). (11) ASTM D323-82...

Optimal multi-dimensional poverty lines: The state of poverty in Iraq

NASA Astrophysics Data System (ADS)

Ameen, Jamal R. M.

2017-09-01

Poverty estimation based on calories intake is unrealistic. The established concept of multidimensional poverty has methodological weaknesses in the treatment of different dimensions and there is disagreement in methods of combining them into a single poverty line. This paper introduces a methodology to estimate optimal multidimensional poverty lines and uses the Iraqi household socio-economic survey data of 2012 to demonstrate the idea. The optimal poverty line for Iraq is found to be 170.5 Thousand Iraqi Dinars (TID).

Tensor-Train Split-Operator Fourier Transform (TT-SOFT) Method: Multidimensional Nonadiabatic Quantum Dynamics.

PubMed

Greene, Samuel M; Batista, Victor S

2017-09-12

We introduce the "tensor-train split-operator Fourier transform" (TT-SOFT) method for simulations of multidimensional nonadiabatic quantum dynamics. TT-SOFT is essentially the grid-based SOFT method implemented in dynamically adaptive tensor-train representations. In the same spirit of all matrix product states, the tensor-train format enables the representation, propagation, and computation of observables of multidimensional wave functions in terms of the grid-based wavepacket tensor components, bypassing the need of actually computing the wave function in its full-rank tensor product grid space. We demonstrate the accuracy and efficiency of the TT-SOFT method as applied to propagation of 24-dimensional wave packets, describing the S 1 /S 2 interconversion dynamics of pyrazine after UV photoexcitation to the S 2 state. Our results show that the TT-SOFT method is a powerful computational approach for simulations of quantum dynamics of polyatomic systems since it avoids the exponential scaling problem of full-rank grid-based representations.

Probabilistic classification method on multi wavelength chromatographic data for photosynthetic pigments identification

NASA Astrophysics Data System (ADS)

Prilianti, K. R.; Setiawan, Y.; Indriatmoko, Adhiwibawa, M. A. S.; Limantara, L.; Brotosudarmo, T. H. P.

2014-02-01

Environmental and health problem caused by artificial colorant encourages the increasing usage of natural colorant nowadays. Natural colorant refers to the colorant that is derivate from living organism or minerals. Extensive research topic has been done to exploit these colorant, but recent data shows that only 0.5% of the wide range of plant pigments in the earth has been exhaustively used. Hence development of the pigment characterization technique is an important consideration. High-performance liquid chromatography (HPLC) is a widely used technique to separate pigments in a mixture and identify it. In former HPLC fingerprinting, pigment characterization was based on a single chromatogram from a fixed wavelength (one dimensional) and discard the information contained at other wavelength. Therefore, two dimensional fingerprints have been proposed to use more chromatographic information. Unfortunately this method leads to the data processing problem due to the size of its data matrix. The other common problem in the chromatogram analysis is the subjectivity of the researcher in recognizing the chromatogram pattern. In this research an automated analysis method of the multi wavelength chromatographic data was proposed. Principal component analysis (PCA) was used to compress the data matrix and Maximum Likelihood (ML) classification was applied to identify the chromatogram pattern of the existing pigments in a mixture. Three photosynthetic pigments were selected to show the proposed method. Those pigments are β-carotene, fucoxanthin and zeaxanthin. The result suggests that the method could well inform the existence of the pigments in a particular mixture. A simple computer application was also developed to facilitate real time analysis. Input of the application is multi wavelength chromatographic data matrix and the output is information about the existence of the three pigments.

Validation of stationary phases in (111)In-pentetreotide planar chromatography.

PubMed

Moreno-Ortega, E; Mena-Bares, L M; Maza-Muret, F R; Hidalgo-Ramos, F J; Vallejo-Casas, J A

2013-01-01

Since Pall-German stopped manufacturing ITLC-SG, it has become necessary to validate alternative stationary phases. To validate different stationary phases versus ITLC-SG Pall-Gelman in the determination of the radiochemical purity (RCP) of (111)In-pentetreotide ((111)In-Octreoscan) by planar chromatography. We conducted a case-control study, which included 66 (111)In-pentetreotide preparations. We determined the RCP by planar chromatography, using a freshly prepared solution of 0,1M sodium citrate (pH 5) and the following stationary phases: ITLC-SG (Pall-Gelman) (reference method), iTLC-SG (Varian), HPTLC silica gel 60 (Merck), Whatman 1, Whatman 3MM and Whatman 17. For each of the methods, we calculated: PRQ, relative front values (RF) of the radiopharmaceutical and free (111)In, chromatographic development time, resolution between peaks. We compared the results obtained with the reference method. The statistical analysis was performed using the SPSS program. The p value was calculated for the study of statistical significance. The highest resolution is obtained with HPTLC silica gel 60 (Merck). However, the chromatographic development time is too long (mean=33.62minutes). Greater resolution is obtained with iTLC-SG (Varian) than with the reference method, with lower chromatographic development time (mean=3.61minutes). Very low resolutions are obtained with Whatman paper, essentially with Whatman 1 and 3MM. Therefore, we do not recommend their use. Although iTLC-SG (Varian) and HPTLC silica gel 60 (Merck) are suitable alternatives to ITLC-SG (Pall-Gelman) in determining the RCP of (111)In-pentetreotide, iTLC-SG (Varian) is the method of choice due to its lower chromatographic development time. Copyright © 2012 Elsevier España, S.L. and SEMNIM. All rights reserved.

Predicting the chromatographic retention of polymers: poly(methyl methacrylate)s and polyacryate blends.

PubMed

Bashir, Mubasher A; Radke, Wolfgang

2007-09-07

The suitability of a retention model especially designed for polymers is investigated to describe and predict the chromatographic retention behavior of poly(methyl methacrylate)s as a function of mobile phase composition and gradient steepness. It is found that three simple yet rationally chosen chromatographic experiments suffice to extract the analyte specific model parameters necessary to calculate the retention volumes. This allows predicting accurate retention volumes based on a minimum number of initial experiments. Therefore, methods for polymer separations can be developed in relatively short time. The suitability of the virtual chromatography approach to predict the separation of polymer blend is demonstrated for the first time using a blend of different polyacrylates.

Vacuum polarization in the field of a multidimensional global monopole

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

Grats, Yu. V., E-mail: grats@phys.msu.ru; Spirin, P. A.

2016-11-15

An approximate expression for the Euclidean Green function of a massless scalar field in the spacetime of a multidimensional global monopole has been derived. Expressions for the vacuum expectation values 〈ϕ{sup 2}〉{sub ren} and 〈T{sub 00}〉{sub ren} have been derived by the dimensional regularization method. Comparison with the results obtained by alternative regularization methods is made.

Positivity-preserving numerical schemes for multidimensional advection

NASA Technical Reports Server (NTRS)

Leonard, B. P.; Macvean, M. K.; Lock, A. P.

1993-01-01

This report describes the construction of an explicit, single time-step, conservative, finite-volume method for multidimensional advective flow, based on a uniformly third-order polynomial interpolation algorithm (UTOPIA). Particular attention is paid to the problem of flow-to-grid angle-dependent, anisotropic distortion typical of one-dimensional schemes used component-wise. The third-order multidimensional scheme automatically includes certain cross-difference terms that guarantee good isotropy (and stability). However, above first-order, polynomial-based advection schemes do not preserve positivity (the multidimensional analogue of monotonicity). For this reason, a multidimensional generalization of the first author's universal flux-limiter is sought. This is a very challenging problem. A simple flux-limiter can be found; but this introduces strong anisotropic distortion. A more sophisticated technique, limiting part of the flux and then restoring the isotropy-maintaining cross-terms afterwards, gives more satisfactory results. Test cases are confined to two dimensions; three-dimensional extensions are briefly discussed.

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

Ingebretsen, O.C.; Borgen, J.; Farstad, M.

A reversed-phase liquid-chromatographic procedure is presented for quantitation or uric acid in human serum, with absorbance measured at 292 nm. The mobile phase was sodium acetate (35 mmol/L, pH 5.0)/acetonitrile (9/1 by vol). Complete precipitation of serum proteins was obtained by mixing serum (50-500 microL) with an equal volume of acetonitrile, and the precipitate was removed by centrifugation. Aliquots (20 microL) of the supernate were injected directly into the liquid chromatograph, which was adjusted so that the absorbance reading of the uric acid peak was as high as possible. Routinely, a full-scale deflection of 1.28 absorbance units was used. Themore » within-run precision (CV) was 0.6% for a serum uric acid concentration of 227 mumol/L and day-to-day precision over a 15-day period was 0.8% for uric acid of 345 mumol/L. No interferences from related compounds were observed. Researchers compared results by this method with those by kinetic and equilibrium adaptations of uricase methods. The method reported is simple, and can be used in a fully automatic liquid-chromatographic system.« less

Development and validation of a high throughput assay for the quantification of multiple green tea-derived catechins in human plasma.

PubMed

Mawson, Deborah H; Jeffrey, Keon L; Teale, Philip; Grace, Philip B

2018-06-19

A rapid, accurate and robust method for the determination of catechin (C), epicatechin (EC), gallocatechin (GC), epigallocatechin (EGC), catechin gallate (Cg), epicatechin gallate (ECg), gallocatechin gallate (GCg) and epigallocatechin gallate (EGCg) concentrations in human plasma has been developed. The method utilises protein precipitation following enzyme hydrolysis, with chromatographic separation and detection using reversed-phase liquid chromatography - tandem mass spectrometry (LC-MS/MS). Traditional issues such as lengthy chromatographic run times, sample and extract stability, and lack of suitable internal standards have been addressed. The method has been evaluated using a comprehensive validation procedure, confirming linearity over appropriate concentration ranges, and inter/intra batch precision and accuracies within suitable thresholds (precisions within 13.8% and accuracies within 12.4%). Recoveries of analytes were found to be consistent between different matrix samples, compensated for using suitable internal markers and within the performance of the instrumentation used. Similarly, chromatographic interferences have been corrected using the internal markers selected. Stability of all analytes in matrix is demonstrated over 32 days and throughout extraction conditions. This method is suitable for high throughput sample analysis studies. This article is protected by copyright. All rights reserved.

Determination of losartan potassium, quinapril hydrochloride and hydrochlorothiazide in pharmaceutical preparations using derivative spectrophotometry and chromatographic-densitometric method.

PubMed

Stolarczyk, Mariusz; Maślanka, Anna; Apola, Anna; Krzek, Jan

2013-01-01

Two methods, spectrophotometric and chromatographic-densitometric ones, were developed for determination of losartan potassium, quinapril hydrochloride and hydrochlorothiazide in pharmaceutical preparations. Spectrophotometric method involved derivative spectrophotometry and zero order spectrophotometry. The measurements were carried out at lambda = 224.0 nm for quinapril, lambda = 261.0 nm for hydrochlorothiazide and lambda = 270.0 nm for losartan when the derivative spectrophotometry was applied and lambda = 317.0 nm when zero order spectrophotometry was applied for the determination of hydrochlorothiazide. In chromatographic-densitometric studies high performance thin layer chromatography (HPTLC) plates were used as stationary phase and a mixture of solvents n-butanol : acetic acid : water (15 : 5 : 1, v/v/v) as mobile phase. Under the established conditions good resolution of examined constituents was obtained. Retardation factor for quinapril hydrochloride was R(f) - 0.70, for losartan potassium R(f) - 0.85 and for hydrochlorothiazide R(f) - 0.78. The developed methods are characterized by high sensitivity and accuracy. For quantitative analysis, densitometric measurements were carried out at lambda = 218.0 nm for quinapril, lambda = 275.0 nm for hydrochlorothiazide and = 232.0 nm for losartan.

The Development and Validation of Novel, Simple High-Performance Liquid Chromatographic Method with Refractive Index Detector for Quantification of Memantine Hydrochloride in Dissolution Samples.

PubMed

Sawant, Tukaram B; Wakchaure, Vikas S; Rakibe, Udyakumar K; Musmade, Prashant B; Chaudhari, Bhata R; Mane, Dhananjay V

2017-07-01

The present study was aimed to develop an analytical method for quantification of memantine (MEM) hydrochloride in dissolution samples using high-performance liquid chromatography with refractive index (RI) detector. The chromatographic separation was achieved on C18 (250 × 4.5 mm, 5 μm) column using isocratic mobile phase comprises of buffer (pH 5.2):methanol (40:60 v/v) pumped at a flow rate of 1.0 mL/min. The column effluents were monitored using RI detector. The retention time of MEM was found to be ~6.5 ± 0.3 min. The developed chromatographic method was validated and found to be linear over the concentration range of 5.0-45.0 μg/mL for MEM. Mean recovery of MEM was found to be 99.2 ± 0.5% (w/w). The method was found to be simple, fast, precise and accurate, which can be utilized for the quantification of MEM in dissolution samples. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

On Multi-Dimensional Unstructured Mesh Adaption

NASA Technical Reports Server (NTRS)

Wood, William A.; Kleb, William L.

1999-01-01

Anisotropic unstructured mesh adaption is developed for a truly multi-dimensional upwind fluctuation splitting scheme, as applied to scalar advection-diffusion. The adaption is performed locally using edge swapping, point insertion/deletion, and nodal displacements. Comparisons are made versus the current state of the art for aggressive anisotropic unstructured adaption, which is based on a posteriori error estimates. Demonstration of both schemes to model problems, with features representative of compressible gas dynamics, show the present method to be superior to the a posteriori adaption for linear advection. The performance of the two methods is more similar when applied to nonlinear advection, with a difference in the treatment of shocks. The a posteriori adaption can excessively cluster points to a shock, while the present multi-dimensional scheme tends to merely align with a shock, using fewer nodes. As a consequence of this alignment tendency, an implementation of eigenvalue limiting for the suppression of expansion shocks is developed for the multi-dimensional distribution scheme. The differences in the treatment of shocks by the adaption schemes, along with the inherently low levels of artificial dissipation in the fluctuation splitting solver, suggest the present method is a strong candidate for applications to compressible gas dynamics.

Assessing Dimensionality of Noncompensatory Multidimensional Item Response Theory with Complex Structures

ERIC Educational Resources Information Center

Svetina, Dubravka

2013-01-01

The purpose of this study was to investigate the effect of complex structure on dimensionality assessment in noncompensatory multidimensional item response models using dimensionality assessment procedures based on DETECT (dimensionality evaluation to enumerate contributing traits) and NOHARM (normal ogive harmonic analysis robust method). Five…

A New Heterogeneous Multidimensional Unfolding Procedure

ERIC Educational Resources Information Center

Park, Joonwook; Rajagopal, Priyali; DeSarbo, Wayne S.

2012-01-01

A variety of joint space multidimensional scaling (MDS) methods have been utilized for the spatial analysis of two- or three-way dominance data involving subjects' preferences, choices, considerations, intentions, etc. so as to provide a parsimonious spatial depiction of the underlying relevant dimensions, attributes, stimuli, and/or subjects'…

Chromatographic fingerprinting: An innovative approach for food 'identitation' and food authentication - A tutorial.

PubMed

Cuadros-Rodríguez, Luis; Ruiz-Samblás, Cristina; Valverde-Som, Lucia; Pérez-Castaño, Estefanía; González-Casado, Antonio

2016-02-25

Fingerprinting methods describe a variety of analytical methods that provide analytical signals related to the composition of foodstuffs in a non-selective way such as by collecting a spectrum or a chromatogram. Mathematical processing of the information in such fingerprints may allow the characterisation and/or authentication of foodstuffs. In this context, the particular meaning of 'fingerprinting', in conjunction with 'profiling', is different from the original meanings used in metabolomics. This fact has produced some confusion with the use of these terms in analytical papers. Researchers coming from the metabolomic field could use 'profiling' or 'fingerprinting' on a different way to researchers who are devoted to food science. The arrival of an eclectic discipline, named 'foodomics' has not been enough to allay this terminological problem, since the authors keep on using the terms with both meanings. Thus, a first goal of this tutorial is to clarify the difference between both terms. In addition, the chemical approaches for food authentication, i.e., chemical markers, component profiling and instrumental fingerprinting, have been described. A new term, designated as 'food identitation', has been introduced in order to complete the life cycle of the chemical-based food authentication process. Chromatographic fingerprinting has been explained in detail and some strategies which could be applied has been clarified and discussed. Particularly, the strategies for chromatographic signals acquisition and chromatographic data handling are unified in a single framework. Finally, an overview about the applications of chromatographic (GC and LC) fingerprints in food authentication using different chemometric techniques has been included. Copyright © 2016 Elsevier B.V. All rights reserved.

Liquid chromatographic-tandem mass spectrometric method for the simultaneous determination of alkylphenols polyethoxylates, alkylphenoxy carboxylates and alkylphenols in wastewater and surface-water.

PubMed

Ciofi, L; Ancillotti, C; Chiuminatto, U; Fibbi, D; Checchini, L; Orlandini, S; Del Bubba, M

2014-10-03

Four different pellicular stationary phases (i.e. octadecylsilane, octasilane, Phenyl-Hexyl and pentafluorophenyl) were investigated for the chromatographic resolution of alkylphenols (APs), alkylphenols polyethoxylates (APnEOs) and alkylphenoxy carboxylates (APECs) using mixtures of water and organic solvents (i.e. methanol, acetonitrile and tetrahydrofuran) as eluents, in order to obtain their determination by a single LC-MS/MS run. In fact, alkylphenols and alkylphenoxy carboxylates must be analysed in negative ion mode, whereas alkylphenols polyethoxylates undergo ionisation only in positive ion mode, and therefore, two distinct LC-MS/MS analysis are commonly adopted. The best resolution among the aforementioned target analytes was achieved on the pentafluorophenyl column, eluting with an acidified water-acetonitrile-tetrahydrofuran mixture and using the post column addition of an ammonia solution in methanol for the detection of positively ionisable compounds. Under these optimized chromatographic conditions the investigated compounds were determined via a single chromatographic run, with only one polarity switch, in 15min, achieving the following instrumental detection limits: 600pg for AP1EOs, 0.8-14pg for AP2EOs, 10.4-150pg for APs and 4.4-4.8pg for APECs. The chromatographic method was coupled with solid-phase extraction and clean-up procedures and successfully applied to the analysis of wastewater and surface water samples, highlighting mean concentration ranging from 6ng/L for 4-t-OP1EC to 1434ng/L for 4-NP1121EC, depending on the sample analysed. Copyright © 2014 Elsevier B.V. All rights reserved.

Use of the Keele injector for sample introduction for gas chromatographic analysis of vinclozolin in lettuces.

PubMed

Shim, J H; Lee, Y S; Kim, M R; Lee, C J; Kim, I S

2003-10-10

We examined a Keele injector for sample introduction for gas chromatographic analysis of vinclozolin treated in lettuces. Samples in milligram quantity were introduced into a glass tube in a Keele injector at a gas chromatograph injection port. The glass tube was then crushed to allow the sample to carry onto a capillary column in a normal manner. The standard calibration curve for quantitative detection of vinclozolin was obtained by determining vinclozolin spiked in samples at variable concentrations. The calibration curve showed a linear response to vinclozolin ranging from 0.05 to 1.0 microg/g, giving a slope value of 174.8, the y-intercept value of -2.8146 and the mean r2-value of 0.9994. Limit of quantification for vinclozolin was 0.05 microg/g by this method, comparable to 0.01 microg/g by a normal injector. When samples treated previously with vinclozolin were determined by the Keele injector, vinclozolin was found to be about 30% lower as compared to a normal method, suggesting about 70% recovery of the spiked vinclozolin by the Keele injector. From these results, the Keele injector was suggested to be potential for sample introduction in gas chromatographic analysis of vinclozolin in lettuce samples.

Core-Shell in Liquid Chromatography: Application for Determining Sulphonamides in Feed and Meat Using Conventional Chromatographic Systems

PubMed Central

Armentano, Antonio; Summa, Simona; Magro, Sonia Lo; D’Antini, Pasquale; Palermo, Carmen; Muscarella, Marilena

2016-01-01

A C18 column packed with core-shell particles was used for the chromatographic separation of sulphonamides in feed and meat by a conventional high performance liquid chromatography system coupled with a diode array detector. Two analytical methods, already used in our laboratory, have been modified without any changes in the extraction and clean-up steps and in the liquid chromatography instrumentation. Chromatographic conditions applied on a traditional 5-µm column have been optimized on a column packed with 2.6 µm core-shell particles. A binary mobile phase [acetate buffer solution at pH 4.50 and a mixture of methanol acetonitrile 50: 50 (v/v)] was employed in gradient mode at the flow rate of 1.2 mL with an injection volume of 6 µL. These chromatographic conditions allow the separation of 13 sulphonamides with an entire run of 13 minutes. Preliminary studies have been carried out comparing blanks and spiked samples of feed and meat. A good resolution and the absence of interferences were achieved in chromatograms for both matrices. Since no change was made to the sample preparation, the optimized method does not require a complete revalidation and can be used to make routine analysis faster. PMID:28217560

Analyzing chromatographic data using multilevel modeling.

PubMed

Wiczling, Paweł

2018-06-01

It is relatively easy to collect chromatographic measurements for a large number of analytes, especially with gradient chromatographic methods coupled with mass spectrometry detection. Such data often have a hierarchical or clustered structure. For example, analytes with similar hydrophobicity and dissociation constant tend to be more alike in their retention than a randomly chosen set of analytes. Multilevel models recognize the existence of such data structures by assigning a model for each parameter, with its parameters also estimated from data. In this work, a multilevel model is proposed to describe retention time data obtained from a series of wide linear organic modifier gradients of different gradient duration and different mobile phase pH for a large set of acids and bases. The multilevel model consists of (1) the same deterministic equation describing the relationship between retention time and analyte-specific and instrument-specific parameters, (2) covariance relationships relating various physicochemical properties of the analyte to chromatographically specific parameters through quantitative structure-retention relationship based equations, and (3) stochastic components of intra-analyte and interanalyte variability. The model was implemented in Stan, which provides full Bayesian inference for continuous-variable models through Markov chain Monte Carlo methods. Graphical abstract Relationships between log k and MeOH content for acidic, basic, and neutral compounds with different log P. CI credible interval, PSA polar surface area.

[HPLC fingerprint of flavonoids in Sophora flavescens and determination of five components].

PubMed

Ma, Hong-Yan; Zhou, Wan-Shan; Chu, Fu-Jiang; Wang, Dong; Liang, Sheng-Wang; Li, Shao

2013-08-01

A simple and reliable method of high-performance liquid chromatography with photodiode array detection (HPLC-DAD) was developed to evaluate the quality of a traditional Chinese medicine Sophora flavescens through establishing chromatographic fingerprint and simultaneous determination of five flavonoids, including trifolirhizin, maackiain, kushenol I, kurarinone and sophoraflavanone G. The optimal conditions of separation and detection were achieved on an ULTIMATE XB-C18 column (4.6 mm x 250 mm, 5 microm) with a gradient of acetonitrile and water, detected at 295 nm. In the chromatographic fingerprint, 13 peaks were selected as the characteristic peaks to assess the similarities of different samples collected from different origins in China according to similarity evaluation for chromatographic fingerprint of traditional chinese medicine (2004AB) and principal component analysis (PCA) were used in data analysis. There were significant differences in the fingerprint chromatograms between S. flavescens and S. tonkinensis. Principal component analysis showed that kurarinone and sophoraflavanone G were the most important component. In quantitative analysis, the five components showed good regression (R > 0.999) with linear ranges, and their recoveries were in the range of 96.3% - 102.3%. This study indicated that the combination of quantitative and chromatographic fingerprint analysis can be readily utilized as a quality control method for S. flavescens and its related traditional Chinese medicinal preparations.

Simultaneous LC determination of paracetamol and related compounds in pharmaceutical formulations using a carbon-based column.

PubMed

Monser, Lotfi; Darghouth, Frida

2002-03-01

A simple, rapid and convenient high performance liquid chromatographic method, which permits the simultaneous determination of paracetamol, 4-aminophenol and 4-chloracetanilide in pharmaceutical preparation has been developed. The chromatographic separation was achieved on porous graphitized carbon (PGC) column using an isocratic mixture of 80/20 (v/v) acetonitrile/0.05 M potassium phosphate buffer (pH 5.5) and ultraviolet detection at 244 nm. Correlation coefficient for calibration curves in the ranges 1-50 microg ml(-1) for paracetamol and 5-40 microg ml(-1) for 4-aminophenol and 4-chloroacetanilide were >0.99. The sensitivity of detection is 0.1 microg ml(-1) for paracetamol and 0.5 microg ml(-1) for 4-aminophenol and 4-chloroacetanilide. The proposed liquid chromatographic method was successfully applied to the analysis of commercially available paracetamol dosage forms with recoveries of 98-103%. It is suggested that the proposed method should be used for routine quality control and dosage form assay of paracetamol in pharmaceutical preparations. The chromatographic behaviour of the three compounds was examined under variable mobile phase compositions and pH, the results revealed that selectivity was dependent on the organic solvent and pH used. The retention selectivity of these compounds on PGC was compared with those of octadecylsilica (ODS) packing materials in reversed phase liquid chromatography. The ODS column gave little separation for the degradation product (4-aminophenol) from paracetamol, whereas PGC column provides better separation in much shorter time.

Application of fast Fourier transform cross-correlation and mass spectrometry data for accurate alignment of chromatograms.

PubMed

Zheng, Yi-Bao; Zhang, Zhi-Min; Liang, Yi-Zeng; Zhan, De-Jian; Huang, Jian-Hua; Yun, Yong-Huan; Xie, Hua-Lin

2013-04-19

Chromatography has been established as one of the most important analytical methods in the modern analytical laboratory. However, preprocessing of the chromatograms, especially peak alignment, is usually a time-consuming task prior to extracting useful information from the datasets because of the small unavoidable differences in the experimental conditions caused by minor changes and drift. Most of the alignment algorithms are performed on reduced datasets using only the detected peaks in the chromatograms, which means a loss of data and introduces the problem of extraction of peak data from the chromatographic profiles. These disadvantages can be overcome by using the full chromatographic information that is generated from hyphenated chromatographic instruments. A new alignment algorithm called CAMS (Chromatogram Alignment via Mass Spectra) is present here to correct the retention time shifts among chromatograms accurately and rapidly. In this report, peaks of each chromatogram were detected based on Continuous Wavelet Transform (CWT) with Haar wavelet and were aligned against the reference chromatogram via the correlation of mass spectra. The aligning procedure was accelerated by Fast Fourier Transform cross correlation (FFT cross correlation). This approach has been compared with several well-known alignment methods on real chromatographic datasets, which demonstrates that CAMS can preserve the shape of peaks and achieve a high quality alignment result. Furthermore, the CAMS method was implemented in the Matlab language and available as an open source package at http://www.github.com/matchcoder/CAMS. Copyright © 2013. Published by Elsevier B.V.

Estimations of temperature deviations in chromatographic columns using isenthalpic plots. I. Theory for isocratic systems.

PubMed

Tarafder, Abhijit; Iraneta, Pamela; Guiochon, Georges; Kaczmarski, Krzysztof; Poe, Donald P

2014-10-31

We propose to use constant enthalpy or isenthalpic diagrams as a tool to estimate the extent of the temperature variations caused by the mobile phase pressure drop along a chromatographic column, e.g. of its cooling in supercritical fluid and its heating in ultra-performance liquid chromatography. Temperature strongly affects chromatographic phenomena. Any of its variations inside the column, whether intended or not, can lead to significant changes in separation performance. Although instruments use column ovens in order to keep constant the column temperature, operating conditions leading to a high pressure drop may cause significant variations of the column temperature, both in the axial and the radial directions, from the set value. Different ways of measuring these temperature variations are available but they are too inconvenient to be employed in many practical situations. In contrast, the thermodynamic plot-based method that we describe here can easily be used with only a ruler and a pencil. They should be helpful in developing methods or in analyzing results in analytical laboratories. Although the most effective application area for this approach should be SFC (supercritical fluid chromatography), it can be applied to any chromatographic conditions in which temperature variations take place along the column due to the pressure drop, e.g. in ultra-high pressure liquid chromatography (UHPLC). The method proposed here is applicable to isocractic conditions only. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparative purification of polyethylene glycol derivatives with polystyrene-divinylbenzene beads as chromatographic packing.

PubMed

Yu, Pengzhan; Li, Xingqi; Li, Xiunan; Lu, Xiuling; Ma, Guanghui; Su, Zhiguo

2007-10-15

A clear and powerful chromatographic approach to purify polyethylene glycol derivatives at a preparative scale was reported, which was based on the polystyrene-divinylbenzene beads with ethanol/water as eluants. The validity of this method was verified with the reaction mixture of mPEG-Glu and mPEG propionaldehyde diethylacetal (ALD-PEG) as the model. The target products were one-step achieved with the purity of >99% on the polymer resins column at gram scale. The method developed was free from such disadvantages as utility of toxic solvent and narrow application scope, which was combined with conventional approaches. The method developed provided an appealing and attractive alternative methods for purification of PEG derivatives at a preparative scale.

The Cognitive Visualization System with the Dynamic Projection of Multidimensional Data

NASA Astrophysics Data System (ADS)

Gorohov, V.; Vitkovskiy, V.

2008-08-01

The phenomenon of cognitive machine drawing consists in the generation on the screen the special graphic representations, which create in the brain of human operator entertainment means. These means seem man by aesthetically attractive and, thus, they stimulate its descriptive imagination, closely related to the intuitive mechanisms of thinking. The essence of cognitive effect lies in the fact that man receives the moving projection as pseudo-three-dimensional object characterizing multidimensional means in the multidimensional space. After the thorough qualitative study of the visual aspects of multidimensional means with the aid of the enumerated algorithms appears the possibility, using algorithms of standard machine drawing to paint the interesting user separate objects or the groups of objects. Then it is possible to again return to the dynamic behavior of the rotation of means for the purpose of checking the intuitive ideas of user about the clusters and the connections in multidimensional data. Is possible the development of the methods of cognitive machine drawing in combination with other information technologies, first of all with the packets of digital processing of images and multidimensional statistical analysis.

Application of an innovative design space optimization strategy to the development of liquid chromatographic methods to combat potentially counterfeit nonsteroidal anti-inflammatory drugs.

PubMed

Mbinze, J K; Lebrun, P; Debrus, B; Dispas, A; Kalenda, N; Mavar Tayey Mbay, J; Schofield, T; Boulanger, B; Rozet, E; Hubert, Ph; Marini, R D

2012-11-09

In the context of the battle against counterfeit medicines, an innovative methodology has been used to develop rapid and specific high performance liquid chromatographic methods to detect and determine 18 non-steroidal anti-inflammatory drugs, 5 pharmaceutical conservatives, paracetamol, chlorzoxazone, caffeine and salicylic acid. These molecules are commonly encountered alone or in combination on the market. Regrettably, a significant proportion of these consumed medicines are counterfeit or substandard, with a strong negative impact in countries of Central Africa. In this context, an innovative design space optimization strategy was successfully applied to the development of LC screening methods allowing the detection of substandard or counterfeit medicines. Using the results of a unique experimental design, the design spaces of 5 potentially relevant HPLC methods have been developed, and transferred to an ultra high performance liquid chromatographic system to evaluate the robustness of the predicted DS while providing rapid methods of analysis. Moreover, one of the methods has been fully validated using the accuracy profile as decision tool, and was then used for the quantitative determination of three active ingredients and one impurity in a common and widely used pharmaceutical formulation. The method was applied to 5 pharmaceuticals sold in the Democratic Republic of Congo. None of these pharmaceuticals was found compliant to the European Medicines Agency specifications. Copyright © 2012 Elsevier B.V. All rights reserved.

Simultaneous extraction and quantitation of several bioactive amines in cheese and chocolate.

PubMed

Baker, G B; Wong, J T; Coutts, R T; Pasutto, F M

1987-04-17

A method is described for simultaneous extraction and quantitation of the amines 2-phenylethylamine, tele-methylhistamine, histamine, tryptamine, m- and p-tyramine, 3-methoxytyramine, 5-hydroxytryptamine, cadaverine, putrescine, spermidine and spermine. This method is based on extractive derivatization of the amines with a perfluoroacylating agent, pentafluorobenzoyl chloride, under basic aqueous conditions. Analysis was done on a gas chromatograph equipped with an electron-capture detector and a capillary column system. The procedure is relatively rapid and provides derivatives with good chromatographic properties. Its application to analysis of the above amines in cheese and chocolate products is described.

Data Dependent Peak Model Based Spectrum Deconvolution for Analysis of High Resolution LC-MS Data

PubMed Central

2015-01-01

A data dependent peak model (DDPM) based spectrum deconvolution method was developed for analysis of high resolution LC-MS data. To construct the selected ion chromatogram (XIC), a clustering method, the density based spatial clustering of applications with noise (DBSCAN), is applied to all m/z values of an LC-MS data set to group the m/z values into each XIC. The DBSCAN constructs XICs without the need for a user defined m/z variation window. After the XIC construction, the peaks of molecular ions in each XIC are detected using both the first and the second derivative tests, followed by an optimized chromatographic peak model selection method for peak deconvolution. A total of six chromatographic peak models are considered, including Gaussian, log-normal, Poisson, gamma, exponentially modified Gaussian, and hybrid of exponential and Gaussian models. The abundant nonoverlapping peaks are chosen to find the optimal peak models that are both data- and retention-time-dependent. Analysis of 18 spiked-in LC-MS data demonstrates that the proposed DDPM spectrum deconvolution method outperforms the traditional method. On average, the DDPM approach not only detected 58 more chromatographic peaks from each of the testing LC-MS data but also improved the retention time and peak area 3% and 6%, respectively. PMID:24533635

Cuba: Multidimensional numerical integration library

NASA Astrophysics Data System (ADS)

Hahn, Thomas

2016-08-01

The Cuba library offers four independent routines for multidimensional numerical integration: Vegas, Suave, Divonne, and Cuhre. The four algorithms work by very different methods, and can integrate vector integrands and have very similar Fortran, C/C++, and Mathematica interfaces. Their invocation is very similar, making it easy to cross-check by substituting one method by another. For further safeguarding, the output is supplemented by a chi-square probability which quantifies the reliability of the error estimate.

The Multidimensionality of Child Poverty: Evidence from Afghanistan

ERIC Educational Resources Information Center

Trani, Jean-Francois; Biggeri, Mario; Mauro, Vincenzo

2013-01-01

This paper examines multidimensional poverty among children in Afghanistan using the Alkire-Foster method. Several previous studies have underlined the need to separate children from their adult nexus when studying poverty and treat them according to their own specificities. From the capability approach, child poverty is understood to be the lack…

Avoiding Degeneracy in Multidimensional Unfolding by Penalizing on the Coefficient of Variation

ERIC Educational Resources Information Center

Busing, Frank M. T. A.; Groenen, Patrick J. K.; Heiser, Willem J.

2005-01-01

Multidimensional unfolding methods suffer from the degeneracy problem in almost all circumstances. Most degeneracies are easily recognized: the solutions are perfect but trivial, characterized by approximately equal distances between points from different sets. A definition of an absolutely degenerate solution is proposed, which makes clear that…

Multidimensional Scaling of High School Students' Perceptions of Academic Dishonesty

ERIC Educational Resources Information Center

Schmelkin, Liora Pedhazur; Gilbert, Kimberly A.; Silva, Rebecca

2010-01-01

Although cheating on tests and other forms of academic dishonesty are considered rampant, no standard definition of academic dishonesty exists. The current study was conducted to investigate the perceptions of academic dishonesty in high school students, utilizing an innovative methodology, multidimensional scaling (MDS). Two methods were used to…

Transesterification of propylene glycol methyl ether in chromatographic reactors using anion exchange resin as a catalyst.

PubMed

Oh, Jungmin; Sreedhar, Balamurali; Donaldson, Megan E; Frank, Timothy C; Schultz, Alfred K; Bommarius, Andreas S; Kawajiri, Yoshiaki

2016-09-30

Reactive chromatography using an anion exchange resin is proposed for a transesterification reaction of propylene glycol methyl ether (DOWANOL™ PM) with ethyl acetate to produce propylene glycol methyl ether acetate (DOWANOL™ PMA). This reaction is studied in batch and chromatographic reactors catalyzed by an anion exchange resin. Several anion exchange resins are tested and compared based on the performance of resin as an adsorbent and a catalyst. A chromatographic column is packed with a selected catalyst, AMBERLITE™ IRA904, and both reaction and chromatographic elution are studied at different temperatures and feed concentrations. The resulting chromatograms are fitted to a mathematical model to obtain adsorption equilibrium and reaction kinetic parameters by the inverse method. Compared to esterification investigated in a previous study, transesterification has advantages such as a higher conversion at lower temperature and easy removal of the byproduct which may lead to higher productivity. Deactivation of anion exchange resins is observed and potential solutions are suggested. Copyright © 2016 Elsevier B.V. All rights reserved.

Development and validation of micellar liquid chromatographic methods for the determination of antibiotics in different matrixes.

PubMed

Rambla-Alegre, Maria; Esteve-Romero, Josep; Carda-Broch, Samuel

2011-01-01

Antibiotics are the most important bioactive and chemotherapeutic compounds to be produced by microbiological synthesis, and they have proved their worth in a variety of fields, such as medicinal chemistry, agriculture, and the food industry. Interest in antibiotics has grown in parallel with an increasingly high degree of productivity in the field of analytical applications. Therefore, it is necessary to develop chromatographic procedures capable of determining various drugs simultaneously in the shortest possible time. Micellar liquid chromatography (MLC) is an RP-HPLC technique that offers advantages over conventional HPLC as far as sample preparation, selectivity, and versatility are concerned. Its main advantage is that samples can be injected directly into the chromatographic system with no previous preparation step. This paper mainly focuses on the results of the authors' own recent research and reports the chromatographic conditions for determination of various antibiotics (penicillins, quinolones, and sulfonamides) in different matrixes (pharmaceuticals, biological fluids, and food). The work of other authors on MLC-based antibiotic determination has been included.

Avoiding Misannotation of In-Source Fragmentation Products as Cellular Metabolites in Liquid Chromatography–Mass Spectrometry-Based Metabolomics

DOE PAGES

Xu, Yi-Fan; Lu, Wenyun; Rabinowitz, Joshua D.

2015-01-15

Liquid chromatography–mass spectrometry (LC-MS) technology allows for rapid quantitation of cellular metabolites, with metabolites identified by mass spectrometry and chromatographic retention time. Recently, with the development of rapid scanning high-resolution high accuracy mass spectrometers and the desire for high throughput screening, minimal or no chromatographic separation has become increasingly popular. Furthermore, when analyzing complex cellular extracts, however, the lack of chromatographic separation could potentially result in misannotation of structurally related metabolites. Here, we show that, even using electrospray ionization, a soft ionization method, in-source fragmentation generates unwanted byproducts of identical mass to common metabolites. For example, nucleotide-triphosphates generate nucleotide-diphosphates, andmore » hexose-phosphates generate triose-phosphates. We also evaluated yeast intracellular metabolite extracts and found more than 20 cases of in-source fragments that mimic common metabolites. Finally and accordingly, chromatographic separation is required for accurate quantitation of many common cellular metabolites.« less

The spectrum-effect relationship-a rational approach to screening effective compounds, reflecting the internal quality of Chinese herbal medicine.

PubMed

Zhu, Chun-Sheng; Lin, Zhi-Jian; Xiao, Ming-Liang; Niu, Hong-Juan; Zhang, Bing

2016-03-01

Since the chromatographic fingerprint was introduced, it has been accepted by many countries to assess the quality and authenticity of Chinese herbal medicine (CHM). However, solely using the chromatographic fingerprint to assay numerous chemicals is not suitable for the assessment of the whole internal quality and pharmacodynamics of CHM. Consequently, it is necessary to develop a rational approach to connecting the chromatographic fingerprint with effective components to assess the internal quality of CHM. For this purpose, a spectrum-effect relationship theory was proposed and accepted as a new method for the assessment of CHM because of its potential use to screen effective components from CHM. In this paper, we systematically reviewed the application of the spectrum-effect relationship theory in the research of CHM, including research mentality, different chromatographic analysis techniques, data processing technologies, and structure determination. Copyright © 2016 China Pharmaceutical University. Published by Elsevier B.V. All rights reserved.

Detection and quantification of ginsenoside Re in ginseng samples by a chromatographic immunostaining method using monoclonal antibody against ginsenoside Re.

PubMed

Morinaga, Osamu; Tanaka, Hiroyuki; Shoyama, Yukihiro

2006-01-02

A chromatographic immunostaining method has been developed for the determination of ginsenoside Re (G-Re) in ginseng samples on a polyethersulphone (PES) membrane. G-Re standard and the extracts of ginseng roots were applied to a PES membrane and developed by methanol-water-acetic acid (45:55:1, by volume). G-Re was clearly detected by an immunostaining method using a monoclonal antibody against G-Re. The coloring spots of G-Re were analyzed quantitatively using NIH Image software indicating at least 0.125 microg of G-Re was detectable. G-Re can be analyzed quantitatively between 0.25 and 4.0 microg.

Application of Multi-Parameter Data Visualization by Means of Multidimensional Scaling to Evaluate Possibility of Coal Gasification

NASA Astrophysics Data System (ADS)

Jamróz, Dariusz; Niedoba, Tomasz; Surowiak, Agnieszka; Tumidajski, Tadeusz; Szostek, Roman; Gajer, Mirosław

2017-09-01

The application of methods drawing upon multi-parameter visualization of data by transformation of multidimensional space into two-dimensional one allow to show multi-parameter data on computer screen. Thanks to that, it is possible to conduct a qualitative analysis of this data in the most natural way for human being, i.e. by the sense of sight. An example of such method of multi-parameter visualization is multidimensional scaling. This method was used in this paper to present and analyze a set of seven-dimensional data obtained from Janina Mining Plant and Wieczorek Coal Mine. It was decided to examine whether the method of multi-parameter data visualization allows to divide the samples space into areas of various applicability to fluidal gasification process. The "Technological applicability card for coals" was used for this purpose [Sobolewski et al., 2012; 2017], in which the key parameters, important and additional ones affecting the gasification process were described.

Fast acquisition of multidimensional NMR spectra of solids and mesophases using alternative sampling methods.

PubMed

Lesot, Philippe; Kazimierczuk, Krzysztof; Trébosc, Julien; Amoureux, Jean-Paul; Lafon, Olivier

2015-11-01

Unique information about the atom-level structure and dynamics of solids and mesophases can be obtained by the use of multidimensional nuclear magnetic resonance (NMR) experiments. Nevertheless, the acquisition of these experiments often requires long acquisition times. We review here alternative sampling methods, which have been proposed to circumvent this issue in the case of solids and mesophases. Compared to the spectra of solutions, those of solids and mesophases present some specificities because they usually display lower signal-to-noise ratios, non-Lorentzian line shapes, lower spectral resolutions and wider spectral widths. We highlight herein the advantages and limitations of these alternative sampling methods. A first route to accelerate the acquisition time of multidimensional NMR spectra consists in the use of sparse sampling schemes, such as truncated, radial or random sampling ones. These sparsely sampled datasets are generally processed by reconstruction methods differing from the Discrete Fourier Transform (DFT). A host of non-DFT methods have been applied for solids and mesophases, including the G-matrix Fourier transform, the linear least-square procedures, the covariance transform, the maximum entropy and the compressed sensing. A second class of alternative sampling consists in departing from the Jeener paradigm for multidimensional NMR experiments. These non-Jeener methods include Hadamard spectroscopy as well as spatial or orientational encoding of the evolution frequencies. The increasing number of high field NMR magnets and the development of techniques to enhance NMR sensitivity will contribute to widen the use of these alternative sampling methods for the study of solids and mesophases in the coming years. Copyright © 2015 John Wiley & Sons, Ltd.

Chromatographic fingerprinting through chemometric techniques for herbal slimming pills: A way of adulterant identification.

PubMed

Shekari, Nafiseh; Vosough, Maryam; Tabar Heidar, Kourosh

2018-05-01

In the current study, gas chromatography-mass spectrometry (GC-MS) fingerprinting of herbal slimming pills assisted by chemometric methods has been presented. Deconvolution of two-way chromatographic signals of nine herbal slimming pills into pure chromatographic and spectral patterns was performed. The peak clusters were resolved using multivariate curve resolution-alternating least squares (MCR-ALS) by employing appropriate constraints. It was revealed that more useful chemical information about the composition of the slimming pills can be obtained by employing sophisticated GC-MS method coupled with proper chemometric tools yielding the extended number of identified constituents. The thorough fingerprinting of the complex mixtures proved the presence of some toxic or carcinogen components, such as toluene, furfural, furfuryl alcohol, styrene, itaconic anhydride, citraconic anhydride, trimethyl phosphate, phenol, pyrocatechol, p-propenylanisole and pyrogallol. In addition, some samples were shown to be adulterated with undeclared ingredients, including stimulants, anorexiant and laxatives such as phenolphthalein, amfepramone, caffeine and sibutramine. Copyright © 2018 Elsevier B.V. All rights reserved.

[The progress in speciation analysis of trace elements by atomic spectrometry].

PubMed

Wang, Zeng-Huan; Wang, Xu-Nuo; Ke, Chang-Liang; Lin, Qin

2013-12-01

The main purpose of the present work is to review the different non-chromatographic methods for the speciation analysis of trace elements in geological, environmental, biological and medical areas. In this paper, the sample processing methods in speciation analysis were summarized, and the main strategies for non-chromatographic technique were evaluated. The basic principles of the liquid extractions proposed in the published literatures recently and their advantages and disadvantages were discussed, such as conventional solvent extraction, cloud point extraction, single droplet microextraction, and dispersive liquid-liquid microextraction. Solid phase extraction, as a non-chromatographic technique for speciation analysis, can be used in batch or in flow detection, and especially suitable for the online connection to atomic spectrometric detector. The developments and applications of sorbent materials filled in the columns of solid phase extraction were reviewed. The sorbents include chelating resins, nanometer materials, molecular and ion imprinted materials, and bio-sorbents. Other techniques, e. g. hydride generation technique and coprecipitation, were also reviewed together with their main applications.

Sampling of atmospheric carbonyl compounds for determination by liquid chromatography after 2,4-dinitrophenylhydrazine labelling

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

Vairavamurthy, A.; Roberts, J.M.; Newman, L.

1991-06-01

Carbonyl compounds are both primary (directly emitted) and secondary (formed in situ) atmospheric species, which play a major role in tropospheric photochemistry. Because of trace concentrations (parts-per-billion and lower), ambient air measurements of carbonyls pose serious analytical problems. Generally, chromatographic approaches combined with chemical derivatization have been used to enhance sensitivity and selectivity in analysis. Currently, the liquid chromatographic method coupled to 2,4-dinitrophenylhydrazine derivatization (DNPH-LC) is in widespread use. Interferences arising from similar compounds are greatly minimized by chromatographic separation; however, those in the air sampling step, especially with ozone, continue to be problematic and remain to be resolved. Wemore » discuss here the different sampling techniques used for time-integrated collection of carbonyls in the DNPH-LC methods. Emphasis is placed on addressing: (1) the principles, advantages, and limitations of sampling techniques; (2) problems associated with reagent blank and sampling instrument; and (3) effects of atmospheric co-pollutants, especially ozone. 58 refs., 8 figs., 3 tabs.« less

Solvent-modified solid-phase microextraction for the determination of diazepam in human plasma samples by capillary gas chromatography.

PubMed

Krogh, M; Grefslie, H; Rasmussen, K E

1997-02-21

This paper describes microextraction and gas chromatographic analysis of diazepam from human plasma. The method was based on immobilisation of 1.5 microliters of 1-octanol on a polyacrylate-coated fiber designed for solid-phase microextraction. The solvent-modified fibre was used to extract diazepam from the samples. The plasma sample was pre-treated to release diazepam from the protein binding. The fibre was inserted into the modified plasma sample, adjusted to pH 5.5 an internal standard was added and the mixture was carefully stirred for 4 min. The fibre with the immobilised solvent and the enriched analytes was injected into the capillary gas chromatograph. The solvent and the extracted analytes were evaporated at 300 degrees C in the split-splitless injection port of the gas chromatograph, separated on a methylsilicon capillary column and detected with a nitrogen-phosphorus detector. The method was shown to be reproducible with a detection limit of 0.10 nmol/ml in human plasma.

Thermal Desorption Capability Development for Enhanced On-site Health Risk Assessment: HAPSITE (registered trademark) ER Passive Sampling in the Field

DTIC Science & Technology

2015-06-07

Field-Portable Gas Chromatograph-Mass Spectrometer.” Forensic Toxicol, 2006, 24, 17-22. Smith, P. “Person-Portable Gas Chromatography : Rapid Temperature...bench-top Gas Chromatograph-Mass Spectrometer (GC-MS) system (ISQ). Nine sites were sampled and analyzed for compounds using Environmental Protection...extraction methods for Liquid Chromatography -MS (LC- MS). Additionally, TD is approximately 1000X more sensitive, requires minimal sample preparation

Multidimensional effects in nonadiabatic statistical theories of spin- forbidden kinetics. A case study of 3O + CO → CO 2

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

Jasper, Ahren

2015-04-14

The appropriateness of treating crossing seams of electronic states of different spins as nonadiabatic transition states in statistical calculations of spin-forbidden reaction rates is considered. We show that the spin-forbidden reaction coordinate, the nuclear coordinate perpendicular to the crossing seam, is coupled to the remaining nuclear degrees of freedom. We found that this coupling gives rise to multidimensional effects that are not typically included in statistical treatments of spin-forbidden kinetics. Three qualitative categories of multidimensional effects may be identified: static multidimensional effects due to the geometry-dependence of the local shape of the crossing seam and of the spin–orbit coupling, dynamicalmore » multidimensional effects due to energy exchange with the reaction coordinate during the seam crossing, and nonlocal(history-dependent) multidimensional effects due to interference of the electronic variables at second, third, and later seam crossings. Nonlocal multidimensional effects are intimately related to electronic decoherence, where electronic dephasing acts to erase the history of the system. A semiclassical model based on short-time full-dimensional trajectories that includes all three multidimensional effects as well as a model for electronic decoherence is presented. The results of this multidimensional nonadiabatic statistical theory (MNST) for the 3O + CO → CO 2 reaction are compared with the results of statistical theories employing one-dimensional (Landau–Zener and weak coupling) models for the transition probability and with those calculated previously using multistate trajectories. The MNST method is shown to accurately reproduce the multistate decay-of-mixing trajectory results, so long as consistent thresholds are used. Furthermore, the MNST approach has several advantages over multistate trajectory approaches and is more suitable in chemical kinetics calculations at low temperatures and for complex systems. The error in statistical calculations that neglect multidimensional effects is shown to be as large as a factor of 2 for this system, with static multidimensional effects identified as the largest source of error.« less

A review of chromatographic methods for the determination of water- and fat-soluble vitamins in biological fluids.

PubMed

Karaźniewicz-Łada, Marta; Główka, Anna

2016-01-01

Vitamins are an essential element of nutrition and thus contribute to human health. Vitamins catalyze many biochemical reactions and their lack or excess can cause health problems. Therefore, monitoring vitamin concentrations in plasma or other biological fluids may be useful in the diagnosis of various disorders as well as in the treatment process. Several chromatographic methods have been developed for the determination of these compounds in biological samples, including high-performance liquid chromatography with UV and fluorescence detection. Recently, high-performance liquid chromatography with tandem mass spectrometry methods have been widely used for the determination of vitamins in complex matrices because of their high sensitivity and selectivity. This method requires preconditioning of samples for analysis, including protein precipitation and/or various extraction techniques. The choice of method may depend on the desired cost, convenience, turnaround time, specificity, and accuracy of the information to be obtained. This article reviews the recently reported chromatographic methods used for determination of vitamins in biological fluids. Relevant papers published mostly during the last 5 years were identified by an extensive PubMed search using appropriate keywords. Particular attention was given to the preparation steps and extraction techniques. This report may be helpful in the selection of procedures that are appropriate for certain types of biological materials and analytes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Validation of green-solvent extraction combined with chromatographic chemical fingerprint to evaluate quality of Stevia rebaudiana Bertoni.

PubMed

Teo, Chin Chye; Tan, Swee Ngin; Yong, Jean Wan Hong; Hew, Choy Sin; Ong, Eng Shi

2009-02-01

An approach that combined green-solvent methods of extraction with chromatographic chemical fingerprint and pattern recognition tools such as principal component analysis (PCA) was used to evaluate the quality of medicinal plants. Pressurized hot water extraction (PHWE) and microwave-assisted extraction (MAE) were used and their extraction efficiencies to extract two bioactive compounds, namely stevioside (SV) and rebaudioside A (RA), from Stevia rebaudiana Bertoni (SB) under different cultivation conditions were compared. The proposed methods showed that SV and RA could be extracted from SB using pure water under optimized conditions. The extraction efficiency of the methods was observed to be higher or comparable to heating under reflux with water. The method precision (RSD, n = 6) was found to vary from 1.91 to 2.86% for the two different methods on different days. Compared to PHWE, MAE has higher extraction efficiency with shorter extraction time. MAE was also found to extract more chemical constituents and provide distinctive chemical fingerprints for quality control purposes. Thus, a combination of MAE with chromatographic chemical fingerprints and PCA provided a simple and rapid approach for the comparison and classification of medicinal plants from different growth conditions. Hence, the current work highlighted the importance of extraction method in chemical fingerprinting for the classification of medicinal plants from different cultivation conditions with the aid of pattern recognition tools used.

Development and Validation of a Simultaneous RP-HPLCUV/DAD Method for Determination of Polyphenols in Gels Containing S. terebinthifolius Raddi (Anacardiaceae)

PubMed Central

Carvalho, Melina G.; Aragão, Cícero F. S; Raffin, Fernanda N.; de L. Moura, Túlio F. A.

2017-01-01

Topical gels containing extracts of Schinus terebinthifolius have been used to treat bacterial vaginosis. It has been reported that this species has antimicrobial, anti-inflammatory and anti-ulcerogenic properties, which can be attributed to the presence of phenolic compounds. In this work, a sensitive and selective reversed-phase HPLC-UV/DAD method for the simultaneous assay of six polyphenols that could be present in S. terebinthifolius was developed. The method was shown to be accurate and precise. Peak purity and similarity index both exceeded 0.99. Calibration curves were linear over the concentration range studied, with correlation coefficients between 0.9931 and 0.9974. This method was used to determine the polyphenol content of a hydroalcoholic extract and pharmacy-compounded vaginal gel. Although the method is useful to assess the 6 phenolic compounds, some compounds could not be detected in the products. SUMMARY A sensitive, selective, accurate and precise reversed-phase HPLC-UV/DAD method for the simultaneous assay of six polyphenols in S. terebinthifolius Raddi Abbreviations used: RP-HPLC-UV/DAD: Reverse Phase High Performance Liquid Chromatograph with Ultraviolet and Diode Array Detector, HPLC: High Performance Liquid Chromatograph, HPLC-UV: High Performance Liquid Chromatograph with Ultraviolet Detector, ANVISA: Brazilian National Health Surveillance Agency, LOD: Limit of detection, LOQ: Limit of quantitation PMID:28539726

The development of the simultaneous GC method of helium, argon and neon measurements for the groundwater dating.

NASA Astrophysics Data System (ADS)

Najman, Joanna; Śliwka, Ireneusz

2014-05-01

In this work we present a chromatographic method for simultaneous analysis of helium, neon and argon in groundwater from one water sample. The concentration of helium in groundwater may be a good environmental tracer for groundwater dating. Proper use of environmental tracers in hydrogeology for dating purpose, requires the knowledge of recharge temperature of the system and the so-called "Excess air". "Excess air" allows for the necessary correction of measured concentration of helium in water. Both parameters can be determined by measuring the concentration of argon and neon in groundwater. In the Department of Physicochemistry of Ecosystems from the Institute of Nuclear Physics Polish Academy of Sciences the chromatographic method for the simultaneous analysis of He, Ar and Ne from one groundwater sample for dating purposes was developed. Water samples are taken to the stainless steel vessels with a capacity of 2900 cc. Gases are extracted from water by headspace method (HS). Helium, neon and argon are analyzed on two gas chromatographs equipped with capillary and packed columns and three thermo-conductive detectors (TCD). The chromatographic method was applied to groundwater dating from areas of Podhalańska Basin, Kraków and Żarnowiec. The levels of detection LOD for each measurement systems for the tested compounds are: 1,9•10-8 cm3STP/cm3 for Ne, 3,1•10-6 cm3STP/cm3 for Ar and 1,2•10-8 cm3STP/cm3 for He. Work performed within the strategic research project "Technologies supporting the development of safe nuclear power" financed by the National Centre for Research and Development (NCBiR). Research Task "Development of methods to assure nuclear safety and radiation protection for current and future needs of nuclear power plants", contract No. SP/J/6/143339/11. This work was also supported by grant No. N N525 3488 38 from the Polish National Science Centre.

Different Spectrophotometric and Chromatographic Methods for Determination of Mepivacaine and Its Toxic Impurity.

PubMed

Abdelwahab, Nada S; Fared, Nehal F; Elagawany, Mohamed; Abdelmomen, Esraa H

2017-09-01

Stability-indicating spectrophotometric, TLC-densitometric, and ultra-performance LC (UPLC) methods were developed for the determination of mepivacaine HCl (MEP) in the presence of its toxic impurity, 2,6-dimethylanaline (DMA). Different spectrophotometric methods were developed for the determination of MEP and DMA. In a dual-wavelength method combined with direct spectrophotometric measurement, the absorbance difference between 221.4 and 240 nm was used for MEP measurements, whereas the absorbance at 283 nm was used for measuring DMA in the binary mixture. In the second-derivative method, amplitudes at 272.2 and 232.6 nm were recorded and used for the determination of MEP and DMA, respectively. The developed TLC-densitometric method depended on chromatographic separation using silica gel 60 F254 TLC plates as a stationary phase and methanol-water-acetic acid (9 + 1 + 0.1, v/v/v) as a developing system, with UV scanning at 230 nm. The developed UPLC method depended on separation using a C18 column (250 × 4.6 mm id, 5 μm particle size) as a stationary phase and acetonitrile-water (40 + 60, v/v; pH 4 with phosphoric acid) as a mobile phase at a flow rate of 0.4 mL/min, with UV detection at 215 nm. The chromatographic run time was approximately 1 min. The proposed methods were validated with respect to International Conference on Harmonization guidelines regarding precision, accuracy, ruggedness, robustness, and specificity.

The Evaluation of Classroom Social Structure by Three-Way Multidimensional Scaling of Sociometric Data.

ERIC Educational Resources Information Center

Langeheine, Rolf

1978-01-01

A three-way multidimensional scaling model is presented as a method for identifying classroom cliques, by simultaneous analysis of three variables (for example, chooser/choosen/criteria). Two scaling models--Carroll and Chang's INDSCAL and Lingoes' PINDIS--are presented and applied to two sets of empirical data. (CP)

Evaluating Change in Behavioral Preferences: Multidimensional Scaling Single-Ideal Point Model

ERIC Educational Resources Information Center

Ding, Cody

2016-01-01

The purpose of the article is to propose a multidimensional scaling single-ideal point model as a method to evaluate changes in individuals' preferences under the explicit methodological framework of behavioral preference assessment. One example is used to illustrate the approach for a clear idea of what this approach can accomplish.

Comparing the Performance of Five Multidimensional CAT Selection Procedures with Different Stopping Rules

ERIC Educational Resources Information Center

Yao, Lihua

2013-01-01

Through simulated data, five multidimensional computerized adaptive testing (MCAT) selection procedures with varying test lengths are examined and compared using different stopping rules. Fixed item exposure rates are used for all the items, and the Priority Index (PI) method is used for the content constraints. Two stopping rules, standard error…

Income and beyond: Multidimensional Poverty in Six Latin American Countries

ERIC Educational Resources Information Center

Battiston, Diego; Cruces, Guillermo; Lopez-Calva, Luis Felipe; Lugo, Maria Ana; Santos, Maria Emma

2013-01-01

This paper studies multidimensional poverty for Argentina, Brazil, Chile, El Salvador, Mexico and Uruguay for the period 1992-2006. The approach overcomes the limitations of the two traditional methods of poverty analysis in Latin America (income-based and unmet basic needs) by combining income with five other dimensions: school attendance for…

Comparing Voice-Therapy and Vocal-Hygiene Treatments in Dysphonia Using a Limited Multidimensional Evaluation Protocol

ERIC Educational Resources Information Center

Rodriguez-Parra, Maria J.; Adrian, Jose A.; Casado, Juan C.

2011-01-01

Purpose: This study evaluates the effectiveness of two different programs of voice-treatment on a heterogeneous group of dysphonic speakers and the stability of therapeutic progress for longterm follow-up post-treatment period, using a limited multidimensional protocol of evaluation. Method: Forty-two participants with voice disorders were…

Assessing Fit and Dimensionality in Least Squares Metric Multidimensional Scaling Using Akaike's Information Criterion

ERIC Educational Resources Information Center

Ding, Cody S.; Davison, Mark L.

2010-01-01

Akaike's information criterion is suggested as a tool for evaluating fit and dimensionality in metric multidimensional scaling that uses least squares methods of estimation. This criterion combines the least squares loss function with the number of estimated parameters. Numerical examples are presented. The results from analyses of both simulation…

A Multi-Method Multi-Analytic Approach to Establishing Internal Construct Validity Evidence: The Sport Multidimensional Perfectionism Scale 2

ERIC Educational Resources Information Center

Gotwals, John K.; Dunn, John G. H.

2009-01-01

This article presents a chronology of three empirical studies that outline the measurement process by which two new subscales ("Doubts about Actions" and "Organization") were developed and integrated into a revised version of Dunn, Causgrove Dunn, and Syrotuik's (2002) "Sport Multidimensional Perfectionism Scale"…

Heuristic Constraint Management Methods in Multidimensional Adaptive Testing

ERIC Educational Resources Information Center

Born, Sebastian; Frey, Andreas

2017-01-01

Although multidimensional adaptive testing (MAT) has been proven to be highly advantageous with regard to measurement efficiency when several highly correlated dimensions are measured, there are few operational assessments that use MAT. This may be due to issues of constraint management, which is more complex in MAT than it is in unidimensional…

Performance of chromatographic systems to model soil-water sorption.

PubMed

Hidalgo-Rodríguez, Marta; Fuguet, Elisabet; Ràfols, Clara; Rosés, Martí

2012-08-24

A systematic approach for evaluating the goodness of chromatographic systems to model the sorption of neutral organic compounds by soil from water is presented in this work. It is based on the examination of the three sources of error that determine the overall variance obtained when soil-water partition coefficients are correlated against chromatographic retention factors: the variance of the soil-water sorption data, the variance of the chromatographic data, and the variance attributed to the dissimilarity between the two systems. These contributions of variance are easily predicted through the characterization of the systems by the solvation parameter model. According to this method, several chromatographic systems besides the reference octanol-water partition system have been selected to test their performance in the emulation of soil-water sorption. The results from the experimental correlations agree with the predicted variances. The high-performance liquid chromatography system based on an immobilized artificial membrane and the micellar electrokinetic chromatography systems of sodium dodecylsulfate and sodium taurocholate provide the most precise correlation models. They have shown to predict well soil-water sorption coefficients of several tested herbicides. Octanol-water partitions and high-performance liquid chromatography measurements using C18 columns are less suited for the estimation of soil-water partition coefficients. Copyright © 2012 Elsevier B.V. All rights reserved.

Large-scale Instability during Gravitational Collapse with Neutrino Transport and a Core-Collapse Supernova

NASA Astrophysics Data System (ADS)

Aksenov, A. G.; Chechetkin, V. M.

2018-04-01

Most of the energy released in the gravitational collapse of the cores of massive stars is carried away by neutrinos. Neutrinos play a pivotal role in explaining core-collape supernovae. Currently, mathematical models of the gravitational collapse are based on multi-dimensional gas dynamics and thermonuclear reactions, while neutrino transport is considered in a simplified way. Multidimensional gas dynamics is used with neutrino transport in the flux-limited diffusion approximation to study the role of multi-dimensional effects. The possibility of large-scale convection is discussed, which is interesting both for explaining SN II and for setting up observations to register possible high-energy (≳10MeV) neutrinos from the supernova. A new multi-dimensional, multi-temperature gas dynamics method with neutrino transport is presented.

Multidimensional Recurrence Quantification Analysis (MdRQA) for the Analysis of Multidimensional Time-Series: A Software Implementation in MATLAB and Its Application to Group-Level Data in Joint Action

PubMed Central

Wallot, Sebastian; Roepstorff, Andreas; Mønster, Dan

2016-01-01

We introduce Multidimensional Recurrence Quantification Analysis (MdRQA) as a tool to analyze multidimensional time-series data. We show how MdRQA can be used to capture the dynamics of high-dimensional signals, and how MdRQA can be used to assess coupling between two or more variables. In particular, we describe applications of the method in research on joint and collective action, as it provides a coherent analysis framework to systematically investigate dynamics at different group levels—from individual dynamics, to dyadic dynamics, up to global group-level of arbitrary size. The Appendix in Supplementary Material contains a software implementation in MATLAB to calculate MdRQA measures. PMID:27920748

Multidimensional Recurrence Quantification Analysis (MdRQA) for the Analysis of Multidimensional Time-Series: A Software Implementation in MATLAB and Its Application to Group-Level Data in Joint Action.

PubMed

Wallot, Sebastian; Roepstorff, Andreas; Mønster, Dan

2016-01-01

We introduce Multidimensional Recurrence Quantification Analysis (MdRQA) as a tool to analyze multidimensional time-series data. We show how MdRQA can be used to capture the dynamics of high-dimensional signals, and how MdRQA can be used to assess coupling between two or more variables. In particular, we describe applications of the method in research on joint and collective action, as it provides a coherent analysis framework to systematically investigate dynamics at different group levels-from individual dynamics, to dyadic dynamics, up to global group-level of arbitrary size. The Appendix in Supplementary Material contains a software implementation in MATLAB to calculate MdRQA measures.

Human and methodological sources of variability in the measurement of urinary 8-oxo-7,8-dihydro-2'-deoxyguanosine.

PubMed

Barregard, Lars; Møller, Peter; Henriksen, Trine; Mistry, Vilas; Koppen, Gudrun; Rossner, Pavel; Sram, Radim J; Weimann, Allan; Poulsen, Henrik E; Nataf, Robert; Andreoli, Roberta; Manini, Paola; Marczylo, Tim; Lam, Patricia; Evans, Mark D; Kasai, Hiroshi; Kawai, Kazuaki; Li, Yun-Shan; Sakai, Kazuo; Singh, Rajinder; Teichert, Friederike; Farmer, Peter B; Rozalski, Rafal; Gackowski, Daniel; Siomek, Agnieszka; Saez, Guillermo T; Cerda, Concha; Broberg, Karin; Lindh, Christian; Hossain, Mohammad Bakhtiar; Haghdoost, Siamak; Hu, Chiung-Wen; Chao, Mu-Rong; Wu, Kuen-Yuh; Orhan, Hilmi; Senduran, Nilufer; Smith, Raymond J; Santella, Regina M; Su, Yali; Cortez, Czarina; Yeh, Susan; Olinski, Ryszard; Loft, Steffen; Cooke, Marcus S

2013-06-20

Urinary 8-oxo-7,8-dihydro-2'-deoxyguanosine (8-oxodG) is a widely used biomarker of oxidative stress. However, variability between chromatographic and ELISA methods hampers interpretation of data, and this variability may increase should urine composition differ between individuals, leading to assay interference. Furthermore, optimal urine sampling conditions are not well defined. We performed inter-laboratory comparisons of 8-oxodG measurement between mass spectrometric-, electrochemical- and ELISA-based methods, using common within-technique calibrants to analyze 8-oxodG-spiked phosphate-buffered saline and urine samples. We also investigated human subject- and sample collection-related variables, as potential sources of variability. Chromatographic assays showed high agreement across urines from different subjects, whereas ELISAs showed far more inter-laboratory variation and generally overestimated levels, compared to the chromatographic assays. Excretion rates in timed 'spot' samples showed strong correlations with 24 h excretion (the 'gold' standard) of urinary 8-oxodG (rp 0.67-0.90), although the associations were weaker for 8-oxodG adjusted for creatinine or specific gravity (SG). The within-individual excretion of 8-oxodG varied only moderately between days (CV 17% for 24 h excretion and 20% for first void, creatinine-corrected samples). This is the first comprehensive study of both human and methodological factors influencing 8-oxodG measurement, providing key information for future studies with this important biomarker. ELISA variability is greater than chromatographic assay variability, and cannot determine absolute levels of 8-oxodG. Use of standardized calibrants greatly improves intra-technique agreement and, for the chromatographic assays, importantly allows integration of results for pooled analyses. If 24 h samples are not feasible, creatinine- or SG-adjusted first morning samples are recommended.

The necessity-concerns framework: a multidimensional theory benefits from multidimensional analysis.

PubMed

Phillips, L Alison; Diefenbach, Michael A; Kronish, Ian M; Negron, Rennie M; Horowitz, Carol R

2014-08-01

Patients' medication-related concerns and necessity-beliefs predict adherence. Evaluation of the potentially complex interplay of these two dimensions has been limited because of methods that reduce them to a single dimension (difference scores). We use polynomial regression to assess the multidimensional effect of stroke-event survivors' medication-related concerns and necessity beliefs on their adherence to stroke-prevention medication. Survivors (n = 600) rated their concerns, necessity beliefs, and adherence to medication. Confirmatory and exploratory polynomial regression determined the best-fitting multidimensional model. As posited by the necessity-concerns framework (NCF), the greatest and lowest adherence was reported by those necessity weak concerns and strong concerns/weak Necessity-Beliefs, respectively. However, as could not be assessed using a difference-score model, patients with ambivalent beliefs were less adherent than those exhibiting indifference. Polynomial regression allows for assessment of the multidimensional nature of the NCF. Clinicians/Researchers should be aware that concerns and necessity dimensions are not polar opposites.

A 3D finite element ALE method using an approximate Riemann solution

DOE PAGES

Chiravalle, V. P.; Morgan, N. R.

2016-08-09

Arbitrary Lagrangian–Eulerian finite volume methods that solve a multidimensional Riemann-like problem at the cell center in a staggered grid hydrodynamic (SGH) arrangement have been proposed. This research proposes a new 3D finite element arbitrary Lagrangian–Eulerian SGH method that incorporates a multidimensional Riemann-like problem. Here, two different Riemann jump relations are investigated. A new limiting method that greatly improves the accuracy of the SGH method on isentropic flows is investigated. A remap method that improves upon a well-known mesh relaxation and remapping technique in order to ensure total energy conservation during the remap is also presented. Numerical details and test problemmore » results are presented.« less

A 3D finite element ALE method using an approximate Riemann solution

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

Chiravalle, V. P.; Morgan, N. R.

Arbitrary Lagrangian–Eulerian finite volume methods that solve a multidimensional Riemann-like problem at the cell center in a staggered grid hydrodynamic (SGH) arrangement have been proposed. This research proposes a new 3D finite element arbitrary Lagrangian–Eulerian SGH method that incorporates a multidimensional Riemann-like problem. Here, two different Riemann jump relations are investigated. A new limiting method that greatly improves the accuracy of the SGH method on isentropic flows is investigated. A remap method that improves upon a well-known mesh relaxation and remapping technique in order to ensure total energy conservation during the remap is also presented. Numerical details and test problemmore » results are presented.« less

Dual liquid and gas chromatograph system

DOEpatents

Gay, D.D.

A chromatographic system is described that utilizes one detection system for gas chromatographic and micro-liquid chromatographic determinations. The detection system is a direct-current, atmospheric-pressure, helium plasma emission spectrometer. The detector utilizes a nontransparent plasma source unit which contains the plasma region and two side-arms which receive effluents from the micro-liquid chromatograph and the gas chromatograph. The dual nature of this chromatographic system offers: (1) extreme flexibility in the samples to be examined; (2) extreme low sensitivity; (3) element selectivity; (4) long-term stability; (5) direct correlation of data from the liquid and gas samples; (6) simpler operation than with individual liquid and gas chromatographs, each with different detection systems; and (7) cheaper than a commercial liquid chromatograph and a gas chromatograph.

Dual liquid and gas chromatograph system

DOEpatents

Gay, Don D.

1985-01-01

A chromatographic system that utilizes one detection system for gas chromatographic and micro-liquid chromatographic determinations. The detection system is a direct-current, atmospheric-pressure, helium plasma emission spectrometer. The detector utilizes a non-transparent plasma source unit which contains the plasma region and two side-arms which receive effluents from the micro-liquid chromatograph and the gas chromatograph. The dual nature of this chromatographic system offers: (1) extreme flexibility in the samples to be examined; (2) extremely low sensitivity; (3) element selectivity; (4) long-term stability; (5) direct correlation of data from the liquid and gas samples; (6) simpler operation than with individual liquid and gas chromatographs, each with different detection systems; and (7) cheaper than a commercial liquid chromatograph and a gas chromatograph.

Generalizing DTW to the multi-dimensional case requires an adaptive approach

PubMed Central

Hu, Bing; Jin, Hongxia; Wang, Jun; Keogh, Eamonn

2017-01-01

In recent years Dynamic Time Warping (DTW) has emerged as the distance measure of choice for virtually all time series data mining applications. For example, virtually all applications that process data from wearable devices use DTW as a core sub-routine. This is the result of significant progress in improving DTW’s efficiency, together with multiple empirical studies showing that DTW-based classifiers at least equal (and generally surpass) the accuracy of all their rivals across dozens of datasets. Thus far, most of the research has considered only the one-dimensional case, with practitioners generalizing to the multi-dimensional case in one of two ways, dependent or independent warping. In general, it appears the community believes either that the two ways are equivalent, or that the choice is irrelevant. In this work, we show that this is not the case. The two most commonly used multi-dimensional DTW methods can produce different classifications, and neither one dominates over the other. This seems to suggest that one should learn the best method for a particular application. However, we will show that this is not necessary; a simple, principled rule can be used on a case-by-case basis to predict which of the two methods we should trust at the time of classification. Our method allows us to ensure that classification results are at least as accurate as the better of the two rival methods, and, in many cases, our method is significantly more accurate. We demonstrate our ideas with the most extensive set of multi-dimensional time series classification experiments ever attempted. PMID:29104448

Improving LC-MS sensitivity through increases in chromatographic performance: comparisons of UPLC-ES/MS/MS to HPLC-ES/MS/MS.

PubMed

Churchwell, Mona I; Twaddle, Nathan C; Meeker, Larry R; Doerge, Daniel R

2005-10-25

Recent technological advances have made available reverse phase chromatographic media with a 1.7 microm particle size along with a liquid handling system that can operate such columns at much higher pressures. This technology, termed ultra performance liquid chromatography (UPLC), offers significant theoretical advantages in resolution, speed, and sensitivity for analytical determinations, particularly when coupled with mass spectrometers capable of high-speed acquisitions. This paper explores the differences in LC-MS performance by conducting a side-by-side comparison of UPLC for several methods previously optimized for HPLC-based separation and quantification of multiple analytes with maximum throughput. In general, UPLC produced significant improvements in method sensitivity, speed, and resolution. Sensitivity increases with UPLC, which were found to be analyte-dependent, were as large as 10-fold and improvements in method speed were as large as 5-fold under conditions of comparable peak separations. Improvements in chromatographic resolution with UPLC were apparent from generally narrower peak widths and from a separation of diastereomers not possible using HPLC. Overall, the improvements in LC-MS method sensitivity, speed, and resolution provided by UPLC show that further advances can be made in analytical methodology to add significant value to hypothesis-driven research.

Characterization and analysis of structural isomers of dimethyl methoxypyrazines in cork stoppers and ladybugs (Harmonia axyridis and Coccinella septempunctata).

PubMed

Slabizki, Petra; Legrum, Charlotte; Meusinger, Reinhard; Schmarr, Hans-Georg

2014-10-01

The three constitutional isomers of dimethyl-substituted methoxypyrazines: 3,5-dimethyl-2-methoxypyrazine 1; 2,5-dimethyl-3-methoxypyrazine 2; and 2,3-dimethyl-5-methoxypyrazine 3 are potent flavor compounds with similar mass spectrometric, gas chromatographic, and nuclear magnetic resonance spectroscopic behavior. Therefore, unambiguous analytical determination is critical, particularly in complex matrices. The unequivocal identification of 1-3 could be achieved by homo- and heteronuclear NMR correlation experiments. The observed mass fragmentation for 1-3 is proposed and discussed, benefitting from synthesized partially deuterated 1 and 2. On common polar and apolar stationary phases used in gas chromatography (GC) 1 and 2 show similar behavior whereas 3 can be separated. In our focus on off-flavor analysis with respect to wine aroma, 1 has been described as a "moldy" off-flavor compound in cork and 2 as a constituent in Harmonia axyridis contributing to the so-called "ladybug taint," whereas 3 has not yet been described as a constituent of wine aroma. A successful separation of 1 and 2 could be achieved on octakis-(2,3-di-O-pentyl-6-O-methyl)-γ-cyclodextrin as stationary phase in GC. Applying heart-cut multidimensional GC analysis with tandem mass spectrometric detection we could confirm the presence of 1 as a "moldy" off-flavor compound in cork. However, in the case of Harmonia axyridis, a previous identification of 2 has to be reconsidered. In our experiments we identified the constitutional isomer 1, which was also found in Coccinella septempunctata, another species discussed with respect to the "ladybug taint." The analysis of such structurally related compounds is a demonstrative example for the importance of a chromatographic separation, as mass spectrometric data by itself could not guarantee the unequivocal identification.

Determination of new retention indices for quick identification of essential oils compounds.

PubMed

Hérent, Marie-France; De Bie, Véronique; Tilquin, Bernard

2007-02-19

The classical methods of chromatographic identification of compounds were based on calculation of retention indices by using different stationary phases. The aim of the work was to differentiate essential oils extracted from different plant species by identification of some of their major compounds. The method of identification was based on the calculation of new retention indices of essential oils compounds fractionated on a polar chromatographic column with temperature programming system. Similar chromatograms have been obtained on the same column for one plant family with two different temperature gradients allowing the rapid identification of essential oils of different species, sub-species or chemotypes of Citrus, Mentha and Thymus.

Chromatography in the detection and characterization of illegal pharmaceutical preparations.

PubMed

Deconinck, Eric; Sacré, Pierre-Yves; Courselle, Patricia; De Beer, Jacques O

2013-09-01

Counterfeit and illegal pharmaceutical products are an increasing worldwide problem and constitute a major challenge for analytical laboratories to detect and characterize them. Spectroscopic techniques such as infrared spectroscopy and Raman spectroscopy have always been the first methods of choice to detect counterfeits and illegal preparations, but due to the evolution in the seized products and the necessity of risk assessment, chromatographic methods are becoming more important in this domain. This review intends to give a general overview of the techniques described in literature to characterize counterfeit and illegal pharmaceutical preparations, focusing on the role of chromatographic techniques with different detection tools.

One-step liquid-liquid extraction of cocaine from urine samples for gas chromatographic analysis.

PubMed

Farina, Marcelo; Yonamine, Maurício; Silva, Ovandir A

2002-07-17

An improved technique for cocaine extraction from urine samples for gas chromatographic (GC) analysis is described. Employing a simple liquid-liquid extraction (LLE) of cocaine with a mixture of ethyl ether:isopropanol (9:1) the method presents a mean recovery of 74.49%. Limit of detection (LOD) and limit of quantification (LOQ) were 5 and 20 ng/ml, respectively. The method is highly precise (coefficient of variation (CV) <8%) and linear from 20 to 2000 ng/ml. It can he applied to detect the presence of cocaine in urine as a marker of its recent use in drug abuse treatment protocols.

Analysis of benzo(a)pyrene in airborne particulates by gas chromatography

NASA Technical Reports Server (NTRS)

Luedecke, E.

1976-01-01

A routine method was developed to measure benzo(a)pyrene in airborne particulates. Samples were collected on a filter and the organic portion was extracted with cyclohexane. The polynuclear hydrocarbon (PNHC) fraction was separated from the aliphatics by column chromatography. An internal standard was added to the extract and a portion of it was injected into a gas chromatograph. Although the gas chromatographic method has often been reported in the literature, satisfactory separation of benzo(a)pyrene and benzo(e)pyrene has not been achieved. With the introduction of a nematic liquid crystal as the stationary phase good separation is now possible.

Expedited Selection of NMR Chiral Solvating Agents for Determination of Enantiopurity

PubMed Central

2016-01-01

The use of NMR chiral solvating agents (CSAs) for the analysis of enantiopurity has been known for decades, but has been supplanted in recent years by chromatographic enantioseparation technology. While chromatographic methods for the analysis of enantiopurity are now commonplace and easy to implement, there are still individual compounds and entire classes of analytes where enantioseparation can prove extremely difficult, notably, compounds that are chiral by virtue of very subtle differences such as isotopic substitution or small differences in alkyl chain length. NMR analysis using CSAs can often be useful for such problems, but the traditional approach to selection of an appropriate CSA and the development of an NMR-based analysis method often involves a trial-and-error approach that can be relatively slow and tedious. In this study we describe a high-throughput experimentation approach to the selection of NMR CSAs that employs automation-enabled screening of prepared libraries of CSAs in a systematic fashion. This approach affords excellent results for a standard set of enantioenriched compounds, providing a valuable comparative data set for the effectiveness of CSAs for different classes of compounds. In addition, the technique has been successfully applied to challenging pharmaceutical development problems that are not amenable to chromatographic solutions. Overall, this methodology provides a rapid and powerful approach for investigating enantiopurity that compliments and augments conventional chromatographic approaches. PMID:27280168

A simple multi-scale Gaussian smoothing-based strategy for automatic chromatographic peak extraction.

PubMed

Fu, Hai-Yan; Guo, Jun-Wei; Yu, Yong-Jie; Li, He-Dong; Cui, Hua-Peng; Liu, Ping-Ping; Wang, Bing; Wang, Sheng; Lu, Peng

2016-06-24

Peak detection is a critical step in chromatographic data analysis. In the present work, we developed a multi-scale Gaussian smoothing-based strategy for accurate peak extraction. The strategy consisted of three stages: background drift correction, peak detection, and peak filtration. Background drift correction was implemented using a moving window strategy. The new peak detection method is a variant of the system used by the well-known MassSpecWavelet, i.e., chromatographic peaks are found at local maximum values under various smoothing window scales. Therefore, peaks can be detected through the ridge lines of maximum values under these window scales, and signals that are monotonously increased/decreased around the peak position could be treated as part of the peak. Instrumental noise was estimated after peak elimination, and a peak filtration strategy was performed to remove peaks with signal-to-noise ratios smaller than 3. The performance of our method was evaluated using two complex datasets. These datasets include essential oil samples for quality control obtained from gas chromatography and tobacco plant samples for metabolic profiling analysis obtained from gas chromatography coupled with mass spectrometry. Results confirmed the reasonability of the developed method. Copyright © 2016 Elsevier B.V. All rights reserved.

Direct screening and confirmation of priority volatile organic pollutants in drinking water.

PubMed

Caro, J; Serrano, A; Gallego, M

2007-01-05

A screening tool was proposed for the rapid detection of eight priority volatile organic pollutants according to European standards in drinking water. The method is based on the direct coupling of a headspace sampler with a mass spectrometer, using a chromatographic column heated to 175 degrees C as an interface. The water sample was subjected to the headspace extraction process and the volatile fraction was introduced directly into the mass spectrometer, without prior chromatographic separation, achieving low detection limits (0.6-1.2 ng/ml) for all compounds. The mass spectrum resulting from the simultaneous ionization and fragmentation of the mixture of molecules constitutes the volatile profile of each sample. An appropriate chemometric treatment of these signals permitted them to be classified, on the basis of their volatile composition, as contaminated or uncontaminated with respect to the legally established concentration levels for these compounds in drinking water, and providing no false negatives. A conventional confirmation method was carried out to analyze positive water samples by using the same instrumental setup as in the screening method, but using an appropriate temperature program in the chromatographic column to separate, identify and quantify each analyte.

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

PubMed

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

2006-03-07

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

[Application of robustness test for assessment of the measurement uncertainty at the end of development phase of a chromatographic method for quantification of water-soluble vitamins].

PubMed

Ihssane, B; Bouchafra, H; El Karbane, M; Azougagh, M; Saffaj, T

2016-05-01

We propose in this work an efficient way to evaluate the measurement of uncertainty at the end of the development step of an analytical method, since this assessment provides an indication of the performance of the optimization process. The estimation of the uncertainty is done through a robustness test by applying a Placquett-Burman design, investigating six parameters influencing the simultaneous chromatographic assay of five water-soluble vitamins. The estimated effects of the variation of each parameter are translated into standard uncertainty value at each concentration level. The values obtained of the relative uncertainty do not exceed the acceptance limit of 5%, showing that the procedure development was well done. In addition, a statistical comparison conducted to compare standard uncertainty after the development stage and those of the validation step indicates that the estimated uncertainty are equivalent. The results obtained show clearly the performance and capacity of the chromatographic method to simultaneously assay the five vitamins and suitability for use in routine application. Copyright © 2015 Académie Nationale de Pharmacie. Published by Elsevier Masson SAS. All rights reserved.

Chromatographic and electrophoretic approaches in ink analysis.

PubMed

Zlotnick, J A; Smith, F P

1999-10-15

Inks are manufactured from a wide variety of substances that exhibit very different chemical behaviors. Inks designed for use in different writing instruments or printing methods have quite dissimilar components. Since the 1950s chromatographic and electrophoretic methods have played important roles in the analysis of inks, where compositional information may have bearing on the investigation of counterfeiting, fraud, forgery, and other crimes. Techniques such as paper chromatography and electrophoresis, thin-layer chromatography, high-performance liquid chromatography, gas chromatography, gel electrophoresis, and the relatively new technique of capillary electrophoresis have all been explored as possible avenues for the separation of components of inks. This paper reviews the components of different types of inks and applications of the above separation methods are reviewed.

Development of liquid chromatographic methods for the determination of phytosterols in Standard Reference Materials containing saw palmetto.

PubMed

Bedner, Mary; Schantz, Michele M; Sander, Lane C; Sharpless, Katherine E

2008-05-23

Liquid chromatographic (LC) methods using atmospheric pressure chemical ionization/mass spectrometric (APCI-MS) detection were developed for the separation and analysis of the phytosterols campesterol, cycloartenol, lupenone, lupeol, beta-sitosterol, and stigmasterol. Brassicasterol and cholesterol were also included for investigation as internal standards. The methods were used to identify and quantify the phytosterols in each of two Serenoa repens (saw palmetto) Standard Reference Materials (SRMs) developed by the National Institute of Standards and Technology (NIST). Values obtained by LC-MS were compared to those obtained using the more traditional approach of gas chromatography with flame ionization detection. This is the first reported use of LC-MS to determine phytosterols in saw palmetto dietary supplement materials.

High performance liquid chromatographic hydrocarbon group-type analyses of mid-distillates employing fuel-derived fractions as standards

NASA Technical Reports Server (NTRS)

Seng, G. T.; Otterson, D. A.

1983-01-01

Two high performance liquid chromatographic (HPLC) methods have been developed for the determination of saturates, olefins and aromatics in petroleum and shale derived mid-distillate fuels. In one method the fuel to be analyzed is reacted with sulfuric acid, to remove a substantial portion of the aromatics, which provides a reacted fuel fraction for use in group type quantitation. The second involves the removal of a substantial portion of the saturates fraction from the HPLC system to permit the determination of olefin concentrations as low as 0.3 volume percent, and to improve the accuracy and precision of olefins determinations. Each method was evaluated using model compound mixtures and real fuel samples.

Determination and discrimination of biodiesel fuels by gas chromatographic and chemometric methods

NASA Astrophysics Data System (ADS)

Milina, R.; Mustafa, Z.; Bojilov, D.; Dagnon, S.; Moskovkina, M.

2016-03-01

Pattern recognition method (PRM) was applied to gas chromatographic (GC) data for a fatty acid methyl esters (FAME) composition of commercial and laboratory synthesized biodiesel fuels from vegetable oils including sunflower, rapeseed, corn and palm oils. Two GC quantitative methods to calculate individual fames were compared: Area % and internal standard. The both methods were applied for analysis of two certified reference materials. The statistical processing of the obtained results demonstrates the accuracy and precision of the two methods and allows them to be compared. For further chemometric investigations of biodiesel fuels by their FAME-profiles any of those methods can be used. PRM results of FAME profiles of samples from different vegetable oils show a successful recognition of biodiesels according to the feedstock. The information obtained can be used for selection of feedstock to produce biodiesels with certain properties, for assessing their interchangeability, for fuel spillage and remedial actions in the environment.

Validation of Ion Chromatographic Method for Determination of Standard Inorganic Anions in Treated and Untreated Drinking Water

NASA Astrophysics Data System (ADS)

Ivanova, V.; Surleva, A.; Koleva, B.

2018-06-01

An ion chromatographic method for determination of fluoride, chloride, nitrate and sulphate in untreated and treated drinking waters was described. An automated 850 IC Professional, Metrohm system equipped with conductivity detector and Metrosep A Supp 7-250 (250 x 4 mm) column was used. The validation of the method was performed for simultaneous determination of all studied analytes and the results have showed that the validated method fits the requirements of the current water legislation. The main analytical characteristics were estimated for each of studied analytes: limits of detection, limits of quantification, working and linear ranges, repeatability and intermediate precision, recovery. The trueness of the method was estimated by analysis of certified reference material for soft drinking water. Recovery test was performed on spiked drinking water samples. An uncertainty was estimated. The method was applied for analysis of drinking waters before and after chlorination.

[Recent advances in sample preparation methods of plant hormones].

PubMed

Wu, Qian; Wang, Lus; Wu, Dapeng; Duan, Chunfeng; Guan, Yafeng

2014-04-01

Plant hormones are a group of naturally occurring trace substances which play a crucial role in controlling the plant development, growth and environment response. With the development of the chromatography and mass spectroscopy technique, chromatographic analytical method has become a widely used way for plant hormone analysis. Among the steps of chromatographic analysis, sample preparation is undoubtedly the most vital one. Thus, a highly selective and efficient sample preparation method is critical for accurate identification and quantification of phytohormones. For the three major kinds of plant hormones including acidic plant hormones & basic plant hormones, brassinosteroids and plant polypeptides, the sample preparation methods are reviewed in sequence especially the recently developed methods. The review includes novel methods, devices, extractive materials and derivative reagents for sample preparation of phytohormones analysis. Especially, some related works of our group are included. At last, the future developments in this field are also prospected.

Development and validation of a generic high-performance liquid chromatography for the simultaneous separation and determination of six cough ingredients: Robustness study on core-shell particles.

PubMed

Yehia, Ali Mohamed; Essam, Hebatallah Mohamed

2016-09-01

A generally applicable high-performance liquid chromatographic method for the qualitative and quantitative determination of pharmaceutical preparations containing phenylephrine hydrochloride, paracetamol, ephedrine hydrochloride, guaifenesin, doxylamine succinate, and dextromethorphan hydrobromide is developed. Optimization of chromatographic conditions was performed for the gradient elution using different buffer pH values, flow rates and two C18 stationary phases. The method was developed using a Kinetex® C18 column as a core-shell stationary phase with a gradient profile using buffer pH 5.0 and acetonitrile at 2.0 mL/min flow rate. Detection was carried out at 220 nm and linear calibrations were obtained for all components within the studied ranges. The method was fully validated in agreement with ICH guidelines. The proposed method is specific, accurate and precise (RSD% < 3%). Limits of detection are lower than 2.0 μg/mL. Qualitative and quantitative responses were evaluated using experimental design to assist the method robustness. The method was proved to be highly robust against 10% change in buffer pH and flow rate (RSD% < 10%), however, the flow rate may significantly influence the quantitative responses of phenylephrine, paracetamol, and doxylamine (RSD% > 10%). Satisfactory results were obtained for commercial combinations analyses. Statistical comparison between the proposed chromatographic and official methods revealed no significant difference. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Validated Chromatographic Methods for the Analysis of Two Binary Mixtures Containing Pyridoxine Hydrochloride.

PubMed

Habib, Neven M; Abdelrahman, Maha M; Abdelwhab, Nada S; Ali, Nourudin W

2017-03-01

Accurate and precise TLC-densitometric and HPLC-diode-array detector (DAD) methods have been developed and validated to resolve two binary mixtures containing pyridoxine hydrochloride (PYH) with either cyclizine hydrochloride (CYH) or meclizine hydrochloride (MEH). In the developed TLC-densitometric method, chromatographic separation of the three studied drugs was carried out on silica gel 60 F254 plates using a developing system containing methylene chloride + acetone + methanol (7 + 1 + 0.5, v/v/v) scanning separated bands at 220 nm. Beer-Lambert law was obeyed in the ranges of 0.2-5, 0.2-4, and 0.2-4 µg/band for PYH, CYH, and MEH, respectively. On the other hand, the developed HPLC-DAD method depended on chromatographic separation on a Zorbax Eclipse C18 column using methanol-KH2PO4 (0.05 M; 90 + 10, v/v; pH 5, with H3PO4 and KOH) as the mobile phase, a flow rate of 1 mL/min, and UV scanning at 220 nm. A linear relationship was obtained between the integrated peak area and the concentration in the ranges of 10-50, 10-50, and 7-50 µg/mL for PYH, CYH, and MEH, respectively. The proposed methods were successfully applied for the determination of the cited drugs in their pharmaceutical formulations. Statistical comparison with the reported methods using Student's t- and F-tests found there were no significant differences between the proposed and reported methods for accuracy and precision.

Multidimensional signal modulation and/or demodulation for data communications

DOEpatents

Smith, Stephen F [London, TN; Dress, William B [Camas, WA

2008-03-04

Systems and methods are described for multidimensional signal modulation and/or demodulation for data communications. A method includes modulating a carrier signal in a first domain selected from the group consisting of phase, frequency, amplitude, polarization and spread; modulating the carrier signal in a second domain selected from the group consisting of phase, frequency, amplitude, polarization and spread; and modulating the carrier signal in a third domain selected from the group consisting of phase, frequency, amplitude, polarization and spread.

A Method for Generating Reduced-Order Linear Models of Multidimensional Supersonic Inlets

NASA Technical Reports Server (NTRS)

Chicatelli, Amy; Hartley, Tom T.

1998-01-01

Simulation of high speed propulsion systems may be divided into two categories, nonlinear and linear. The nonlinear simulations are usually based on multidimensional computational fluid dynamics (CFD) methodologies and tend to provide high resolution results that show the fine detail of the flow. Consequently, these simulations are large, numerically intensive, and run much slower than real-time. ne linear simulations are usually based on large lumping techniques that are linearized about a steady-state operating condition. These simplistic models often run at or near real-time but do not always capture the detailed dynamics of the plant. Under a grant sponsored by the NASA Lewis Research Center, Cleveland, Ohio, a new method has been developed that can be used to generate improved linear models for control design from multidimensional steady-state CFD results. This CFD-based linear modeling technique provides a small perturbation model that can be used for control applications and real-time simulations. It is important to note the utility of the modeling procedure; all that is needed to obtain a linear model of the propulsion system is the geometry and steady-state operating conditions from a multidimensional CFD simulation or experiment. This research represents a beginning step in establishing a bridge between the controls discipline and the CFD discipline so that the control engineer is able to effectively use multidimensional CFD results in control system design and analysis.

Method of multi-dimensional moment analysis for the characterization of signal peaks

DOEpatents

Pfeifer, Kent B; Yelton, William G; Kerr, Dayle R; Bouchier, Francis A

2012-10-23

A method of multi-dimensional moment analysis for the characterization of signal peaks can be used to optimize the operation of an analytical system. With a two-dimensional Peclet analysis, the quality and signal fidelity of peaks in a two-dimensional experimental space can be analyzed and scored. This method is particularly useful in determining optimum operational parameters for an analytical system which requires the automated analysis of large numbers of analyte data peaks. For example, the method can be used to optimize analytical systems including an ion mobility spectrometer that uses a temperature stepped desorption technique for the detection of explosive mixtures.

Renaissance of protein crystallization and precipitation in biopharmaceuticals purification.

PubMed

Dos Santos, Raquel; Carvalho, Ana Luísa; Roque, A Cecília A

The current chromatographic approaches used in protein purification are not keeping pace with the increasing biopharmaceutical market demand. With the upstream improvements, the bottleneck shifted towards the downstream process. New approaches rely in Anything But Chromatography methodologies and revisiting former techniques with a bioprocess perspective. Protein crystallization and precipitation methods are already implemented in the downstream process of diverse therapeutic biological macromolecules, overcoming the current chromatographic bottlenecks. Promising work is being developed in order to implement crystallization and precipitation in the purification pipeline of high value therapeutic molecules. This review focuses in the role of these two methodologies in current industrial purification processes, and highlights their potential implementation in the purification pipeline of high value therapeutic molecules, overcoming chromatographic holdups. Copyright © 2016 Elsevier Inc. All rights reserved.

A rapid gas chromatographic injection-port derivatization method for the tandem mass spectrometric determination of patulin and 5-hydroxymethylfurfural in fruit juices.

PubMed

Marsol-Vall, Alexis; Balcells, Mercè; Eras, Jordi; Canela-Garayoa, Ramon

2016-07-01

A novel method consisting of injection-port derivatization coupled to gas chromatography-tandem mass spectrometry is described. The method allows the rapid assessment of 5-hydroxymethylfurfural (HMF) and patulin content in apple and pear derivatives. The chromatographic separation of the compounds was achieved in a short chromatographic run (12.2min) suitable for routine controls of these compounds in the fruit juice industry. The optimal conditions for the injection-port derivatization were at 270°C, 0.5min purge-off, and a 1:2 sample:derivatization reagent ratio (v/v). These conditions represent an important saving in terms of derivatization reagent consumption and sample preparation time. Quality parameters were assessed for the target compounds, giving LOD of 0.7 and 1.6μg/kg and LOQ of 2 and 5μg/kg for patulin and HMF, respectively. These values are below the maximum patulin concentration in food products intended for infants and young children. Repeatability (%RSD n=5) was below 12% for both compounds. In addition, the method linearity ranged between 25 and 1000μg/kg and between 5 and 192μg/kg for HMF and patulin, respectively. Finally, the method was applied to study HMF and patulin content in various fruit juice samples. Copyright © 2016 Elsevier B.V. All rights reserved.

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

Kaczmarski, Krzysztof; Guiochon, Georges A

The adsorption isotherms of selected compounds are our main source of information on the mechanisms of adsorption processes. Thus, the selection of the methods used to determine adsorption isotherm data and to evaluate the errors made is critical. Three chromatographic methods were evaluated, frontal analysis (FA), frontal analysis by characteristic point (FACP), and the pulse or perturbation method (PM), and their accuracies were compared. Using the equilibrium-dispersive (ED) model of chromatography, breakthrough curves of single components were generated corresponding to three different adsorption isotherm models: the Langmuir, the bi-Langmuir, and the Moreau isotherms. For each breakthrough curve, the best conventionalmore » procedures of each method (FA, FACP, PM) were used to calculate the corresponding data point, using typical values of the parameters of each isotherm model, for four different values of the column efficiency (N = 500, 1000, 2000, and 10,000). Then, the data points were fitted to each isotherm model and the corresponding isotherm parameters were compared to those of the initial isotherm model. When isotherm data are derived with a chromatographic method, they may suffer from two types of errors: (1) the errors made in deriving the experimental data points from the chromatographic records; (2) the errors made in selecting an incorrect isotherm model and fitting to it the experimental data. Both errors decrease significantly with increasing column efficiency with FA and FACP, but not with PM.« less

Multidimensional poverty and child survival in India.

PubMed

Mohanty, Sanjay K

2011-01-01

Though the concept of multidimensional poverty has been acknowledged cutting across the disciplines (among economists, public health professionals, development thinkers, social scientists, policy makers and international organizations) and included in the development agenda, its measurement and application are still limited. OBJECTIVES AND METHODOLOGY: Using unit data from the National Family and Health Survey 3, India, this paper measures poverty in multidimensional space and examine the linkages of multidimensional poverty with child survival. The multidimensional poverty is measured in the dimension of knowledge, health and wealth and the child survival is measured with respect to infant mortality and under-five mortality. Descriptive statistics, principal component analyses and the life table methods are used in the analyses. The estimates of multidimensional poverty are robust and the inter-state differentials are large. While infant mortality rate and under-five mortality rate are disproportionately higher among the abject poor compared to the non-poor, there are no significant differences in child survival among educationally, economically and health poor at the national level. State pattern in child survival among the education, economical and health poor are mixed. Use of multidimensional poverty measures help to identify abject poor who are unlikely to come out of poverty trap. The child survival is significantly lower among abject poor compared to moderate poor and non-poor. We urge to popularize the concept of multiple deprivations in research and program so as to reduce poverty and inequality in the population.

From Molecules to Cells to Organisms: Understanding Health and Disease with Multidimensional Single-Cell Methods

NASA Astrophysics Data System (ADS)

Candia, Julián

2013-03-01

The multidimensional nature of many single-cell measurements (e.g. multiple markers measured simultaneously using Fluorescence-Activated Cell Sorting (FACS) technologies) offers unprecedented opportunities to unravel emergent phenomena that are governed by the cooperative action of multiple elements across different scales, from molecules and proteins to cells and organisms. We will discuss an integrated analysis framework to investigate multicolor FACS data from different perspectives: Singular Value Decomposition to achieve an effective dimensional reduction in the data representation, machine learning techniques to separate different patient classes and improve diagnosis, as well as a novel cell-similarity network analysis method to identify cell subpopulations in an unbiased manner. Besides FACS data, this framework is versatile: in this vein, we will demonstrate an application to the multidimensional single-cell shape analysis of healthy and prematurely aged cells.

A second-order cell-centered Lagrangian ADER-MOOD finite volume scheme on multidimensional unstructured meshes for hydrodynamics

NASA Astrophysics Data System (ADS)

Boscheri, Walter; Dumbser, Michael; Loubère, Raphaël; Maire, Pierre-Henri

2018-04-01

In this paper we develop a conservative cell-centered Lagrangian finite volume scheme for the solution of the hydrodynamics equations on unstructured multidimensional grids. The method is derived from the Eucclhyd scheme discussed in [47,43,45]. It is second-order accurate in space and is combined with the a posteriori Multidimensional Optimal Order Detection (MOOD) limiting strategy to ensure robustness and stability at shock waves. Second-order of accuracy in time is achieved via the ADER (Arbitrary high order schemes using DERivatives) approach. A large set of numerical test cases is proposed to assess the ability of the method to achieve effective second order of accuracy on smooth flows, maintaining an essentially non-oscillatory behavior on discontinuous profiles, general robustness ensuring physical admissibility of the numerical solution, and precision where appropriate.

Numerical Simulations of Multidimensional Flows in Presence of either Strong Shocks or Strong Gravitational Fields

NASA Astrophysics Data System (ADS)

Font, J. A.; Ibanez, J. M.; Marti, J. M.

1993-04-01

Some numerical solutions via local characteristic approach have been obtained describing multidimensional flows. These solutions have been used as tests of a two- dimensional code which extends some high-resolution shock-captunng methods, designed recently to solve nonlinear hyperbolic systems of conservation laws. K words: HYDRODYNAMICS - BLACK HOLE - RELATIVITY - SHOCK WAVES

Multidimensional CAT Item Selection Methods for Domain Scores and Composite Scores: Theory and Applications

ERIC Educational Resources Information Center

Yao, Lihua

2012-01-01

Multidimensional computer adaptive testing (MCAT) can provide higher precision and reliability or reduce test length when compared with unidimensional CAT or with the paper-and-pencil test. This study compared five item selection procedures in the MCAT framework for both domain scores and overall scores through simulation by varying the structure…

A Bifactor Multidimensional Item Response Theory Model for Differential Item Functioning Analysis on Testlet-Based Items

ERIC Educational Resources Information Center

Fukuhara, Hirotaka; Kamata, Akihito

2011-01-01

A differential item functioning (DIF) detection method for testlet-based data was proposed and evaluated in this study. The proposed DIF model is an extension of a bifactor multidimensional item response theory (MIRT) model for testlets. Unlike traditional item response theory (IRT) DIF models, the proposed model takes testlet effects into…

Students' Personal Connection with Science: Investigating the Multidimensional Phenomenological Structure of Self-Relevance

ERIC Educational Resources Information Center

Hartwell, Matthew; Kaplan, Avi

2018-01-01

This paper presents findings from a two-phase mixed methods study investigating the phenomenological structure of self-relevance among ninth-grade junior high school biology students (Phase 1: N = 118; Phase 2: N = 139). We begin with a phenomenological multidimensional definition of self-relevance as comprising three dimensions: the academic…

Effectiveness of Multidimensional Family Therapy with Higher Severity Substance-Abusing Adolescents: Report from Two Randomized Controlled Trials

ERIC Educational Resources Information Center

Henderson, Craig E.; Dakof, Gayle A.; Greenbaum, Paul E.; Liddle, Howard A.

2010-01-01

Objective: We used growth mixture modeling to examine heterogeneity in treatment response in a secondary analysis of 2 randomized controlled trials testing multidimensional family therapy (MDFT), an established evidence-based therapy for adolescent drug abuse and delinquency. Method: The first study compared 2 evidence-based adolescent substance…

Bayesian Analysis of Multidimensional Item Response Theory Models: A Discussion and Illustration of Three Response Style Models

ERIC Educational Resources Information Center

Leventhal, Brian C.; Stone, Clement A.

2018-01-01

Interest in Bayesian analysis of item response theory (IRT) models has grown tremendously due to the appeal of the paradigm among psychometricians, advantages of these methods when analyzing complex models, and availability of general-purpose software. Possible models include models which reflect multidimensionality due to designed test structure,…

Development and validation of a headspace gas chromatographic method for the determination of residual solvents in arterolane (RBx11160) maleate bulk drug

PubMed Central

Gupta, Abhishek; Singh, Yogendra; Srinivas, Kona S.; Jain, Garima; Sreekumar, V. B.; Semwal, Vinod Prasad

2010-01-01

Objective: Arterolane maleate is an antimalarial drug currently under Phase III clinical evaluation, and presents a simple, economical and scalable synthesis, and does not suffer from safety problems. Arterolane maleate is more active than artemisinin; and is cheap to produce. It has a longer lifetime in the plasma, so it stays active longer in the body. To provide quality control over the manufacture of any API, it is essential to develop highly selective analytical methods. In the current article we are reporting the development and validation of a rapid and specific Head space gas chromatographic (HSGC) method for the determination of organic volatile impurities (residual solvents) in Arterolane Maleate bulk drug. Materials and Methods: The method development and its validation were performed on Perkin Elmer's gas chromatographic system equipped with Flame Ionization detector and head space analyzer. The method involved a thermal gradient elution of ten residual solvents present in arterolane maleate salt in RTx-624, 30 m × 0.32 mm, 1.8 μ column using nitrogen gas as a carrier. The flow rate was 0.5 ml/min and flame ionization detector (FID) was used. Results: During method validation, parameters such as precision, linearity, accuracy, limit of quantification and detection and specificity were evaluated, which remained within acceptable limits. Conclusions: The method has been successfully applied for the quantification of the amount of residual solvents present in arterolane maleate bulk drug.The method presents a simple and reliable solution for the routine quantitative analysis of residual solvents in Arterolane maleate bulk drug. PMID:21814428

Organic Laboratory Experiments.

ERIC Educational Resources Information Center

Smith, Sherrel

1990-01-01

Detailed is a method in which short pieces of teflon tubing may be used for collection tubes for collecting preparative fractions from gas chromatographs. Material preparation, laboratory procedures, and results of this method are discussed. (CW)

Separation of Protactinium Employing Sulfur-Based Extraction Chromatographic Resins.

PubMed

Mastren, Tara; Stein, Benjamin W; Parker, T Gannon; Radchenko, Valery; Copping, Roy; Owens, Allison; Wyant, Lance E; Brugh, Mark; Kozimor, Stosh A; Nortier, F Meiring; Birnbaum, Eva R; John, Kevin D; Fassbender, Michael E

2018-06-05

Protactinium-230 ( t 1/2 = 17.4 d) is the parent isotope of 230 U ( t 1/2 = 20.8 d), a radionuclide of interest for targeted alpha therapy (TAT). Column chromatographic methods have been developed to separate no-carrier-added 230 Pa from proton irradiated thorium targets and accompanying fission products. Results reported within demonstrate the use of novel sulfur bearing chromatographic extraction resins for the selective separation of protactinium. The recovery yield of 230 Pa was 93 ± 4% employing a R 3 P═S type commercially available resin and 88 ± 4% employing a DGTA (diglycothioamide) containing custom synthesized extraction chromatographic resin. The radiochemical purity of the recovered 230 Pa was measured via high purity germanium γ-ray spectroscopy to be >99.5% with the remaining radioactive contaminant being 95 Nb due to its similar chemistry to protactinium. Measured equilibrium distribution coefficients for protactinium, thorium, uranium, niobium, radium, and actinium on both the R 3 P═S type and the DGTA resin in hydrochloric acid media are reported, to the best of our knowledge, for the first time.

Separation of Protactinium Employing Sulfur-Based Extraction Chromatographic Resins

DOE PAGES

Mastren, Tara; Stein, Benjamin W.; Parker, T. Gannon; ...

2018-05-14

Protactinium-230 (t 1/2 = 17.4 d) is the parent isotope of 230U (t 1/2 = 20.8 d), a radionuclide of interest for targeted alpha therapy (TAT). Column chromatographic methods have been developed to separate no-carrier-added 230Pa from proton irradiated thorium targets and accompanying fission products. Results reported within this paper demonstrate the use of novel sulfur bearing chromatographic extraction resins for the selective separation of protactinium. The recovery yield of 230Pa was 93 ± 4% employing a R 3P=S type commercially available resin and 88 ± 4% employing a DGTA (diglycothioamide) containing custom synthesized extraction chromatographic resin. The radiochemical puritymore » of the recovered 230Pa was measured via high purity germanium γ-ray spectroscopy to be >99.5% with the remaining radioactive contaminant being 95Nb due to its similar chemistry to protactinium. Finally, measured equilibrium distribution coefficients for protactinium, thorium, uranium, niobium, radium, and actinium on both the R 3P=S type and the DGTA resin in hydrochloric acid media are reported, to the best of our knowledge, for the first time.« less

Assessing the varietal origin of extra-virgin olive oil using liquid chromatography fingerprints of phenolic compound, data fusion and chemometrics.

PubMed

Bajoub, Aadil; Medina-Rodríguez, Santiago; Gómez-Romero, María; Ajal, El Amine; Bagur-González, María Gracia; Fernández-Gutiérrez, Alberto; Carrasco-Pancorbo, Alegría

2017-01-15

High Performance Liquid Chromatography (HPLC) with diode array (DAD) and fluorescence (FLD) detection was used to acquire the fingerprints of the phenolic fraction of monovarietal extra-virgin olive oils (extra-VOOs) collected over three consecutive crop seasons (2011/2012-2013/2014). The chromatographic fingerprints of 140 extra-VOO samples processed from olive fruits of seven olive varieties, were recorded and statistically treated for varietal authentication purposes. First, DAD and FLD chromatographic-fingerprint datasets were separately processed and, subsequently, were joined using "Low-level" and "Mid-Level" data fusion methods. After the preliminary examination by principal component analysis (PCA), three supervised pattern recognition techniques, Partial Least Squares Discriminant Analysis (PLS-DA), Soft Independent Modeling of Class Analogies (SIMCA) and K-Nearest Neighbors (k-NN) were applied to the four chromatographic-fingerprinting matrices. The classification models built were very sensitive and selective, showing considerably good recognition and prediction abilities. The combination "chromatographic dataset+chemometric technique" allowing the most accurate classification for each monovarietal extra-VOO was highlighted. Copyright © 2016 Elsevier Ltd. All rights reserved.

Separation of Protactinium Employing Sulfur-Based Extraction Chromatographic Resins

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

Mastren, Tara; Stein, Benjamin W.; Parker, T. Gannon

Protactinium-230 (t 1/2 = 17.4 d) is the parent isotope of 230U (t 1/2 = 20.8 d), a radionuclide of interest for targeted alpha therapy (TAT). Column chromatographic methods have been developed to separate no-carrier-added 230Pa from proton irradiated thorium targets and accompanying fission products. Results reported within this paper demonstrate the use of novel sulfur bearing chromatographic extraction resins for the selective separation of protactinium. The recovery yield of 230Pa was 93 ± 4% employing a R 3P=S type commercially available resin and 88 ± 4% employing a DGTA (diglycothioamide) containing custom synthesized extraction chromatographic resin. The radiochemical puritymore » of the recovered 230Pa was measured via high purity germanium γ-ray spectroscopy to be >99.5% with the remaining radioactive contaminant being 95Nb due to its similar chemistry to protactinium. Finally, measured equilibrium distribution coefficients for protactinium, thorium, uranium, niobium, radium, and actinium on both the R 3P=S type and the DGTA resin in hydrochloric acid media are reported, to the best of our knowledge, for the first time.« less

A versatile embedded boundary adaptive mesh method for compressible flow in complex geometry

NASA Astrophysics Data System (ADS)

Al-Marouf, M.; Samtaney, R.

2017-05-01

We present an embedded ghost fluid method for numerical solutions of the compressible Navier Stokes (CNS) equations in arbitrary complex domains. A PDE multidimensional extrapolation approach is used to reconstruct the solution in the ghost fluid regions and imposing boundary conditions on the fluid-solid interface, coupled with a multi-dimensional algebraic interpolation for freshly cleared cells. The CNS equations are numerically solved by the second order multidimensional upwind method. Block-structured adaptive mesh refinement, implemented with the Chombo framework, is utilized to reduce the computational cost while keeping high resolution mesh around the embedded boundary and regions of high gradient solutions. The versatility of the method is demonstrated via several numerical examples, in both static and moving geometry, ranging from low Mach number nearly incompressible flows to supersonic flows. Our simulation results are extensively verified against other numerical results and validated against available experimental results where applicable. The significance and advantages of our implementation, which revolve around balancing between the solution accuracy and implementation difficulties, are briefly discussed as well.

Self-Learning Adaptive Umbrella Sampling Method for the Determination of Free Energy Landscapes in Multiple Dimensions

PubMed Central

Wojtas-Niziurski, Wojciech; Meng, Yilin; Roux, Benoit; Bernèche, Simon

2013-01-01

The potential of mean force describing conformational changes of biomolecules is a central quantity that determines the function of biomolecular systems. Calculating an energy landscape of a process that depends on three or more reaction coordinates might require a lot of computational power, making some of multidimensional calculations practically impossible. Here, we present an efficient automatized umbrella sampling strategy for calculating multidimensional potential of mean force. The method progressively learns by itself, through a feedback mechanism, which regions of a multidimensional space are worth exploring and automatically generates a set of umbrella sampling windows that is adapted to the system. The self-learning adaptive umbrella sampling method is first explained with illustrative examples based on simplified reduced model systems, and then applied to two non-trivial situations: the conformational equilibrium of the pentapeptide Met-enkephalin in solution and ion permeation in the KcsA potassium channel. With this method, it is demonstrated that a significant smaller number of umbrella windows needs to be employed to characterize the free energy landscape over the most relevant regions without any loss in accuracy. PMID:23814508

Seismic interferometry by multidimensional deconvolution as a means to compensate for anisotropic illumination

NASA Astrophysics Data System (ADS)

Wapenaar, K.; van der Neut, J.; Ruigrok, E.; Draganov, D.; Hunziker, J.; Slob, E.; Thorbecke, J.; Snieder, R.

2008-12-01

It is well-known that under specific conditions the crosscorrelation of wavefields observed at two receivers yields the impulse response between these receivers. This principle is known as 'Green's function retrieval' or 'seismic interferometry'. Recently it has been recognized that in many situations it can be advantageous to replace the correlation process by deconvolution. One of the advantages is that deconvolution compensates for the waveform emitted by the source; another advantage is that it is not necessary to assume that the medium is lossless. The approaches that have been developed to date employ a 1D deconvolution process. We propose a method for seismic interferometry by multidimensional deconvolution and show that under specific circumstances the method compensates for irregularities in the source distribution. This is an important difference with crosscorrelation methods, which rely on the condition that waves are equipartitioned. This condition is for example fulfilled when the sources are regularly distributed along a closed surface and the power spectra of the sources are identical. The proposed multidimensional deconvolution method compensates for anisotropic illumination, without requiring knowledge about the positions and the spectra of the sources.

Tile-Based Fisher Ratio Analysis of Comprehensive Two-Dimensional Gas Chromatography Time-of-Flight Mass Spectrometry (GC × GC – TOFMS) Data using a Null Distribution Approach

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

Parsons, Brendon A.; Marney, Luke C.; Siegler, William C.

Multi-dimensional chromatographic instrumentation produces information-rich, and chemically complex data containing meaningful chemical signals and/or chemical patterns. Two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC × GC – TOFMS) is a prominent instrumental platform that has been applied extensively for discovery-based experimentation, where samples are sufficiently volatile or amenable to derivatization. Use of GC × GC – TOFMS and associated data analysis strategies aim to uncover meaningful chemical signals or chemical patterns. However, for complex samples, meaningful chemical information is often buried in a background of less meaningful chemical signal and noise. In this report, we utilize the tile-based F-ratiomore » software in concert with the standard addition method by spiking non-native chemicals into a diesel fuel matrix at low concentrations. While the previous work studied the concentration range of 100-1000 ppm, the current study focuses on the 0 ppm to 100 ppm analyte spike range. This study demonstrates the sensitivity and selectivity of the tile-based F-ratio software for discovery of true positives in the non-targeted analysis of a chemically complex and analytically challenging sample matrix. By exploring the low concentration spike levels, we gain a better understanding of the limit of detection (LOD) of the tile-based F-ratio software with GC × GC – TOFMS data.« less

Preliminary numerical analysis of improved gas chromatograph model

NASA Technical Reports Server (NTRS)

Woodrow, P. T.

1973-01-01

A mathematical model for the gas chromatograph was developed which incorporates the heretofore neglected transport mechanisms of intraparticle diffusion and rates of adsorption. Because a closed-form analytical solution to the model does not appear realizable, techniques for the numerical solution of the model equations are being investigated. Criteria were developed for using a finite terminal boundary condition in place of an infinite boundary condition used in analytical solution techniques. The class of weighted residual methods known as orthogonal collocation is presently being investigated and appears promising.

Simultaneous quantitative determination of fluorine and sodium monofluorophosphate in oral hygiene products.

PubMed

Wang, L H

2001-01-01

An ion chromatographic method for simultaneous quantitative determination of fluorine and sodium monofluorophosphate in oral hygiene products is described. The liquid chromatographic system consisted of an IC A1 polymethacrylate-based anion exchanger and carbonate buffer (pH 9.85) as the mobile phase with a conductive detector. Various excipient ions were investigated with respect to their interference with the determination of fluoride. Comparison with results obtained from a fluoride-ion electrode technique show good agreement.

CHROMATOGRAPHIC TECHNIQUES IN PHARMACEUTICAL ANALYSIS IN POIAND: HISTORY AND THE PRESENCE ON THE BASIS OF PAPERS PUBLISHED IN SELECTED POLISH PHARMACEUTICAL JOURNALS IN XX CENTURY.

PubMed

Bilek, Maciej; Namieśnik, Jacek

2016-01-01

For a long time, chromatographic techniques and techniques related to them have stimulated the development of new procedures in the field of pharmaceutical analysis. The newly developed methods, characterized by improved metrological parameters, allow for more accurate testing of, among others, the composition of raw materials, intermediates and final products. The chromatographic techniques also enable studies on waste generated in research laboratories and factories producing pharmaceuticals and parapharmaceuticals. Based on the review of reports published in Polish pharmaceutical journals, we assessed the impact of chromatographic techniques on the development of pharmaceutical analysis. The first chromatographic technique used in pharmaceutical analysis was a so-called capillary analysis. It was applied in the 1930s to control the identity of pharmaceutical formulations. In the 1940s and 1950s, the chromatographic techniques were mostly a subject of review publications, while their use in experimental work was rare. Paper chromatography and thin layer chromatography were introduced in the 1960s and 1970s, respectively. These new analytical tools have contributed to the intensive development of research in the field of phytochemistry and the analysis of herbal medicines. The development of colunm chromatography-based techniques, i.e., gas chromatography and high performance liquid chromatography took place in the end of 20th century. Both aforementioned techniques were widely applied in pharmaceutical analysis, for example, to assess the stability of drugs, test for impurities and degradation products as well as in pharmacokinetics studies. The first decade of 21" century was the time of new detection methods in gas and liquid chromatography. The information sources used to write this article were Polish pharmaceutical journals, both professional and scientific, originating from the interwar and post-war period, i.e., "Kronika Farmaceutyczna", "Farmacja Współczesna", "Wiadomości Farmaceutyczne", "Acta Poloniae Pharmaceutica", "Farmacja Polska", "Dissertationes Pharmaceuticae", "Annales UMCS sectio DDD Phamacia". The number of published works using various chromatography techniques was assessed based on the content description of individual issues of the journal "Acta Poloniae Pharmaceutica".

Fluorescent high-performance liquid chromatographic analysis of vigabatrin enantiomers after derivatizing with naproxen acyl chloride.

PubMed

Hsieh, Chun-Yu; Wang, Shing-Yaw; Kwan, Aij-Lie; Wu, Hsin-Lung

2008-01-18

Vigabatrin is widely used as an anticonvulsant in the treatment of seizures. Vigabatrin is usually supplied as racemate in formulation, but only the (S)-(+)-enantiomer of vigabatrin is pharmacologically active. A simple and sensitive liquid chromatographic method is described for the separation and quantification of vigabatrin enantiomers. The method is based on derivatizing racemic vigabatrin with a fluorescent chiral reagent (naproxen acyl chloride). The resulting diastereomeric derivatives are highly responsive to a fluorimetric detector (lambda(ex)=230 nm, lambda(em)=350 nm). The lower quantitation limit of the method is attainable at 25 nM for (S)-(+)-vigabatrin or (R)-(-)-vigabatrin with a detection limit of about 2.5 nM (S/N=3 with 10 microl injected). Application of the method to the analysis of vigabatrin in serum of dosed patients proved feasible.

Resolving and quantifying overlapped chromatographic bands by transmutation

PubMed

Malinowski

2000-09-15

A new chemometric technique called "transmutation" is developed for the purpose of sharpening overlapped chromatographic bands in order to quantify the components. The "transmutation function" is created from the chromatogram of the pure component of interest, obtained from the same instrument, operating under the same experimental conditions used to record the unresolved chromatogram of the sample mixture. The method is used to quantify mixtures containing toluene, ethylbenzene, m-xylene, naphthalene, and biphenyl from unresolved chromatograms previously reported. The results are compared to those obtained using window factor analysis, rank annihilation factor analysis, and matrix regression analysis. Unlike the latter methods, the transmutation method is not restricted to two-dimensional arrays of data, such as those obtained from HPLC/DAD, but is also applicable to chromatograms obtained from single detector experiments. Limitations of the method are discussed.

Analytical procedures for water-soluble vitamins in foods and dietary supplements: a review.

PubMed

Blake, Christopher J

2007-09-01

Water-soluble vitamins include the B-group vitamins and vitamin C. In order to correctly monitor water-soluble vitamin content in fortified foods for compliance monitoring as well as to establish accurate data banks, an accurate and precise analytical method is a prerequisite. For many years microbiological assays have been used for analysis of B vitamins. However they are no longer considered to be the gold standard in vitamins analysis as many studies have shown up their deficiencies. This review describes the current status of analytical methods, including microbiological assays and spectrophotometric, biosensor and chromatographic techniques. In particular it describes the current status of the official methods and highlights some new developments in chromatographic procedures and detection methods. An overview is made of multivitamin extractions and analyses for foods and supplements.

Theoretical study of the accuracy of the pulse method, frontal analysis, and frontal analysis by characteristic points for the determination of single component adsorption isotherms.

PubMed

Andrzejewska, Anna; Kaczmarski, Krzysztof; Guiochon, Georges

2009-02-13

The adsorption isotherms of selected compounds are our main source of information on the mechanisms of adsorption processes. Thus, the selection of the methods used to determine adsorption isotherm data and to evaluate the errors made is critical. Three chromatographic methods were evaluated, frontal analysis (FA), frontal analysis by characteristic point (FACP), and the pulse or perturbation method (PM), and their accuracies were compared. Using the equilibrium-dispersive (ED) model of chromatography, breakthrough curves of single components were generated corresponding to three different adsorption isotherm models: the Langmuir, the bi-Langmuir, and the Moreau isotherms. For each breakthrough curve, the best conventional procedures of each method (FA, FACP, PM) were used to calculate the corresponding data point, using typical values of the parameters of each isotherm model, for four different values of the column efficiency (N=500, 1000, 2000, and 10,000). Then, the data points were fitted to each isotherm model and the corresponding isotherm parameters were compared to those of the initial isotherm model. When isotherm data are derived with a chromatographic method, they may suffer from two types of errors: (1) the errors made in deriving the experimental data points from the chromatographic records; (2) the errors made in selecting an incorrect isotherm model and fitting to it the experimental data. Both errors decrease significantly with increasing column efficiency with FA and FACP, but not with PM.

Molecular Weights of Bovine and Porcine Heparin Samples: Comparison of Chromatographic Methods and Results of a Collaborative Survey.

PubMed

Bertini, Sabrina; Risi, Giulia; Guerrini, Marco; Carrick, Kevin; Szajek, Anita Y; Mulloy, Barbara

2017-07-19

In a collaborative study involving six laboratories in the USA, Europe, and India the molecular weight distributions of a panel of heparin sodium samples were determined, in order to compare heparin sodium of bovine intestinal origin with that of bovine lung and porcine intestinal origin. Porcine samples met the current criteria as laid out in the USP Heparin Sodium monograph. Bovine lung heparin samples had consistently lower average molecular weights. Bovine intestinal heparin was variable in molecular weight; some samples fell below the USP limits, some fell within these limits and others fell above the upper limits. These data will inform the establishment of pharmacopeial acceptance criteria for heparin sodium derived from bovine intestinal mucosa. The method for MW determination as described in the USP monograph uses a single, broad standard calibrant to characterize the chromatographic profile of heparin sodium on high-resolution silica-based GPC columns. These columns may be short-lived in some laboratories. Using the panel of samples described above, methods based on the use of robust polymer-based columns have been developed. In addition to the use of the USP's broad standard calibrant for heparin sodium with these columns, a set of conditions have been devised that allow light-scattering detected molecular weight characterization of heparin sodium, giving results that agree well with the monograph method. These findings may facilitate the validation of variant chromatographic methods with some practical advantages over the USP monograph method.

Development of sampling method and chromatographic analysis of volatile organic compounds emitted from human skin.

PubMed

Grabowska-Polanowska, Beata; Miarka, Przemysław; Skowron, Monika; Sułowicz, Joanna; Wojtyna, Katarzyna; Moskal, Karolina; Śliwka, Ireneusz

2017-10-01

The studies on volatile organic compounds emitted from skin are an interest for chemists, biologists and physicians due to their role in development of different scientific areas, including medical diagnostics, forensic medicine and the perfume design. This paper presents a proposal of two sampling methods applied to skin odor collection: the first one uses a bag of cellulose film, the second one, using cellulose sachets filled with active carbon. Volatile organic compounds were adsorbed on carbon sorbent, removed via thermal desorption and analyzed using gas chromatograph with mass spectrometer. The first sampling method allowed identification of more compounds (52) comparing to the second one (30). Quantitative analyses for acetone, butanal, pentanal and hexanal were done. The skin odor sampling method using a bag of cellulose film, allowed the identification of many more compounds when compared with the method using a sachet filled with active carbon.

Multidimensional poverty and catastrophic health spending in the mountainous regions of Myanmar, Nepal and India.

PubMed

Mohanty, Sanjay K; Agrawal, Nand Kishor; Mahapatra, Bidhubhusan; Choudhury, Dhrupad; Tuladhar, Sabarnee; Holmgren, E Valdemar

2017-01-18

Economic burden to households due to out-of-pocket expenditure (OOPE) is large in many Asian countries. Though studies suggest increasing household poverty due to high OOPE in developing countries, studies on association of multidimensional poverty and household health spending is limited. This paper tests the hypothesis that the multidimensionally poor are more likely to incur catastrophic health spending cutting across countries. Data from the Poverty and Vulnerability Assessment (PVA) Survey carried out by the International Center for Integrated Mountain Development (ICIMOD) has been used in the analyses. The PVA survey was a comprehensive household survey that covered the mountainous regions of India, Nepal and Myanmar. A total of 2647 households from India, 2310 households in Nepal and 4290 households in Myanmar covered under the PVA survey. Poverty is measured in a multidimensional framework by including the dimensions of education, income and energy, water and sanitation using the Alkire and Foster method. Health shock is measured using the frequency of illness, family sickness and death of any family member in a reference period of one year. Catastrophic health expenditure is defined as 40% above the household's capacity to pay. Results suggest that about three-fifths of the population in Myanmar, two-fifths of the population in Nepal and one-third of the population in India are multidimensionally poor. About 47% of the multidimensionally poor in India had incurred catastrophic health spending compared to 35% of the multidimensionally non-poor and the pattern was similar in both Nepal and Myanmar. The odds of incurring catastrophic health spending was 56% more among the multidimensionally poor than among the multidimensionally non-poor [95% CI: 1.35-1.76]. While health shocks to households are consistently significant predictors of catastrophic health spending cutting across country of residence, the educational attainment of the head of the household is not significant. The multidimensionally poor in the poorer regions are more likely to face health shocks and are less likely to afford professional health services. Increasing government spending on health and increasing households' access to health insurance can reduce catastrophic health spending and multidimensional poverty.

Fish contamination by polychlorobiphenyls: the mass spectrometric ortho effect in a new and easy gas chromatography-mass spectrometry method for the analysis of the seven indicators. The case of Bluefin Tuna.

PubMed

Masci, Maurizio; Orban, Elena; Nevigato, Teresina

2015-01-02

A simple instrumental procedure was developed to carry out the not simple analysis of PCBs in fish samples. PCBs with the same degree of chlorination (the isomers) are expected to be totally indistinguishable among them by all existing detectors and by all existing mass spectrometers, and there is no apparent solution in those frequent cases where two isomers chromatographically coelute. Generally such coelutions are solved by means of multidimensional GC, but it is a complex technique impractical for most laboratories. The present research focuses on the seven important "indicator PCBs" by using the mass spectrometer in an innovative way. The "mass spectrometric ortho effect" was usefully exploited in addressing coelutions between isomers. Other new important observations on mass spectra were decisive in solving the apparent problem arising from coelutions between higher chlorinated PCBs with the lower chlorinated ones when low-resolution MS is used. With the proposed procedure, the seven indicators are analyzed in a simple way and with a degree of accuracy never observed with the conventional gas chromatography. The method was applied to some Bluefin Tuna fish samples of big size suspected to have not negligible levels of PCBs due to the high position of this species in the food chain. The supposition was partly confirmed. On the basis of the results here obtained, the recently introduced EU Regulation on six of the seven indicators shows one critical point: in the present paper, an amendment to the Regulation is proposed. A number of important validation measures are reported. Copyright © 2014 Elsevier B.V. All rights reserved.

Proteome Analysis of Liver Cells Expressing a Full- Length Hepatitis C Virus (HCV) Replicon and Biopsy Specimens of Posttransplantation Liver from HCV-Infected Patients

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

Jacobs, Jon M.; Diamond, Deborah L.; Chan, Eric Y.

2005-06-01

The development of a reproducible model system for the study of Hepatitis C virus (HCV) infection has the potential to significantly enhance the study of virus-host interactions and provide future direction for modeling the pathogenesis of HCV. While there are studies describing global gene expression changes associated with HCV infection, changes in the proteome have not been characterized. We report the first large scale proteome analysis of the highly permissive Huh-7.5 cell line containing a full length HCV replicon. We detected > 4,400 proteins in this cell line, including HCV replicon proteins, using multidimensional liquid chromatographic (LC) separations coupled tomore » mass spectrometry (MS). The set of Huh-7.5 proteins confidently identified is, to our knowledge, the most comprehensive yet reported for a human cell line. Consistent with the literature, a comparison of Huh-7.5 cells (+) and (-) the HCV replicon identified expression changes of proteins involved in lipid metabolism. We extended these analyses to liver biopsy material from HCV-infected patients where > 1,500 proteins were detected from 2 {micro}g protein lysate using the Huh-7.5 protein database and the accurate mass and time (AMT) tag strategy. These findings demonstrate the utility of multidimensional proteome analysis of the HCV replicon model system for assisting the determination of proteins/pathways affected by HCV infection. Our ability to extend these analyses to the highly complex proteome of small liver biopsies with limiting protein yields offers the unique opportunity to begin evaluating the clinical significance of protein expression changes associated with HCV infection.« less

Screening of a Brassica napus bacterial artificial chromosome library using highly parallel single nucleotide polymorphism assays

PubMed Central

2013-01-01

Background Efficient screening of bacterial artificial chromosome (BAC) libraries with polymerase chain reaction (PCR)-based markers is feasible provided that a multidimensional pooling strategy is implemented. Single nucleotide polymorphisms (SNPs) can be screened in multiplexed format, therefore this marker type lends itself particularly well for medium- to high-throughput applications. Combining the power of multiplex-PCR assays with a multidimensional pooling system may prove to be especially challenging in a polyploid genome. In polyploid genomes two classes of SNPs need to be distinguished, polymorphisms between accessions (intragenomic SNPs) and those differentiating between homoeologous genomes (intergenomic SNPs). We have assessed whether the highly parallel Illumina GoldenGate® Genotyping Assay is suitable for the screening of a BAC library of the polyploid Brassica napus genome. Results A multidimensional screening platform was developed for a Brassica napus BAC library which is composed of almost 83,000 clones. Intragenomic and intergenomic SNPs were included in Illumina’s GoldenGate® Genotyping Assay and both SNP classes were used successfully for screening of the multidimensional BAC pools of the Brassica napus library. An optimized scoring method is proposed which is especially valuable for SNP calling of intergenomic SNPs. Validation of the genotyping results by independent methods revealed a success of approximately 80% for the multiplex PCR-based screening regardless of whether intra- or intergenomic SNPs were evaluated. Conclusions Illumina’s GoldenGate® Genotyping Assay can be efficiently used for screening of multidimensional Brassica napus BAC pools. SNP calling was specifically tailored for the evaluation of BAC pool screening data. The developed scoring method can be implemented independently of plant reference samples. It is demonstrated that intergenomic SNPs represent a powerful tool for BAC library screening of a polyploid genome. PMID:24010766

Acquisition and processing of data for isotope-ratio-monitoring mass spectrometry

NASA Technical Reports Server (NTRS)

Ricci, M. P.; Merritt, D. A.; Freeman, K. H.; Hayes, J. M.

1994-01-01

Methods are described for continuous monitoring of signals required for precise analyses of 13C, 18O, and 15N in gas streams containing varying quantities of CO2 and N2. The quantitative resolution (i.e. maximum performance in the absence of random errors) of these methods is adequate for determination of isotope ratios with an uncertainty of one part in 10(5); the precision actually obtained is often better than one part in 10(4). This report describes data-processing operations including definition of beginning and ending points of chromatographic peaks and quantitation of background levels, allowance for effects of chromatographic separation of isotopically substituted species, integration of signals related to specific masses, correction for effects of mass discrimination, recognition of drifts in mass spectrometer performance, and calculation of isotopic delta values. Characteristics of a system allowing off-line revision of parameters used in data reduction are described and an algorithm for identification of background levels in complex chromatograms is outlined. Effects of imperfect chromatographic resolution are demonstrated and discussed and an approach to deconvolution of signals from coeluting substances described.

Multivariate analysis of variance of designed chromatographic data. A case study involving fermentation of rooibos tea.

PubMed

Marini, Federico; de Beer, Dalene; Walters, Nico A; de Villiers, André; Joubert, Elizabeth; Walczak, Beata

2017-03-17

An ultimate goal of investigations of rooibos plant material subjected to different stages of fermentation is to identify the chemical changes taking place in the phenolic composition, using an untargeted approach and chromatographic fingerprints. Realization of this goal requires, among others, identification of the main components of the plant material involved in chemical reactions during the fermentation process. Quantitative chromatographic data for the compounds for extracts of green, semi-fermented and fermented rooibos form the basis of preliminary study following a targeted approach. The aim is to estimate whether treatment has a significant effect based on all quantified compounds and to identify the compounds, which contribute significantly to it. Analysis of variance is performed using modern multivariate methods such as ANOVA-Simultaneous Component Analysis, ANOVA - Target Projection and regularized MANOVA. This study is the first one in which all three approaches are compared and evaluated. For the data studied, all tree methods reveal the same significance of the fermentation effect on the extract compositions, but they lead to its different interpretation. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation and stability evaluation of extemporaneous oral suspension of valsartan using commercially available tablets.

PubMed

Zaid, Abdel Naser; Assali, Mohyeddin; Qaddomi, Aiman; Ghanem, Mashhour; Zaaror, Yara Abu

2014-01-01

The aim of this study was to develop an extemporaneous valsartan suspension (80 mg valsartan/5 mL) starting from commercial tablets (80-mg/ tablet). A high-performance liquid chromatographic system was used for the analysis and quantification of valsartan in the samples studied. Samples of valsartan suspension for analysis were prepared as reported by the validated high-performance liquid chromatographic method and the dissolution tests were performed according to the U.S. Food and Drug Administration's method. The high-performance liquid chromatographic assay indicated that the 80-mg/5-mL valsartan suspension was stable for 30 days when stored at long-term and accelerated storage conditions. Valsartan release profile showed that approximately 85% of valsartan dissolved after 10 minutes and, accordingly, the calculation of similarity factor was not necessary. It is possible for the pharmacist to crush valsartan 80-mg tablets and prepare a suspension which has dosage flexibility that can be calculated according to body-surface area, kidney, and liver functions, without affecting the chemical stability of the active ingredient nor its dissolution profile and also have a cost-effective dosage form.

[Study on the analysis of organogermanium compounds by ion chromatography].

PubMed

Chen, Q; Mou, S; Hou, X; Ni, Z

1997-05-01

A new high performance ion exchange chromatographic method for separation and determination of three organogermanium compounds beta-carboxyethylgermanium sesquioxide (I), beta-(alpha-methyl) carboxyethylgermanium sesquioxide (II) and di-(beta-carboxyethyl) germanium hydroxide (III) has been developed. A Dionex DX-300 Ion Chromatograph equipped with a Dionex PED-II pulsed electrochemical detector (conductivity mode), a Dionex AMMS-1 anion micromembrane suppressor, and a Dionex ACI advanced computer interface coupled with AI-450 chromatographic software was employed. The separation was achieved by using a Dionex IonPac AS4A-SC column as analytical column, sodium tetraborate solution as eluent, and sulfuric acid solution as regenerant. For reducing run time, a gradient program was chosen. The detection limits (S/N = 3, expressed as germanium) for the three compounds were 0.038mg/L (I), 0.035mg/L (II) and 0.025mg/L (III), respectively. The method has been applied to the analysis of two tonic oral drinks, and the average recoveries for the three compounds ranged from 95%-101%. The results obtained were in agreement with those of hydride generation atomic fluorescence spectrometry (HG-AFS).

A Multi-Dimensional Approach to Gradient Change in Phonological Acquisition: A Case Study of Disordered Speech Development

ERIC Educational Resources Information Center

Glaspey, Amy M.; MacLeod, Andrea A. N.

2010-01-01

The purpose of the current study is to document phonological change from a multidimensional perspective for a 3-year-old boy with phonological disorder by comparing three measures: (1) accuracy of consonant productions, (2) dynamic assessment, and (3) acoustic analysis. The methods included collecting a sample of the targets /s, [image omitted],…

The Synthesis Map Is a Multidimensional Educational Tool That Provides Insight into Students' Mental Models and Promotes Students' Synthetic Knowledge Generation

ERIC Educational Resources Information Center

Ortega, Ryan A.; Brame, Cynthia J.

2015-01-01

Concept mapping was developed as a method of displaying and organizing hierarchical knowledge structures. Using the new, multidimensional presentation software Prezi, we have developed a new teaching technique designed to engage higher-level skills in the cognitive domain. This tool, synthesis mapping, is a natural evolution of concept mapping,…

Fast-HPLC Fingerprinting to Discriminate Olive Oil from Other Edible Vegetable Oils by Multivariate Classification Methods.

PubMed

Jiménez-Carvelo, Ana M; González-Casado, Antonio; Pérez-Castaño, Estefanía; Cuadros-Rodríguez, Luis

2017-03-01

A new analytical method for the differentiation of olive oil from other vegetable oils using reversed-phase LC and applying chemometric techniques was developed. A 3 cm short column was used to obtain the chromatographic fingerprint of the methyl-transesterified fraction of each vegetable oil. The chromatographic analysis took only 4 min. The multivariate classification methods used were k-nearest neighbors, partial least-squares (PLS) discriminant analysis, one-class PLS, support vector machine classification, and soft independent modeling of class analogies. The discrimination of olive oil from other vegetable edible oils was evaluated by several classification quality metrics. Several strategies for the classification of the olive oil were used: one input-class, two input-class, and pseudo two input-class.

High performance liquid chromatographic determination of ambroxol in the presence of different preservatives in pharmaceutical formulations.

PubMed

Koundourellis, J E; Malliou, E T; Broussali, T A

2000-08-15

A high-performance chromatographic method is described for simultaneous determination of ambroxol in the presence of different preservatives in syrups. The method separates ambroxol from methyl- ethyl-, propyl- and butyl paraben and from other multi-component mixtures. The retention behaviour of ambroxol and parabens as a function of both pH and mobile phase composition was investigated. The eluents were monitored with a UV detector at 247 nm. Linear relationships between the amount of pharmaceutical compounds and peak heights were confirmed at the concentrations of 0.74-14.08 microg ml(-1). The high recovery (no extraction of the samples is required) and the low %RSD confirm the suitability of the proposed method for the determination of ambroxol in different pharmaceutical preparations.

High-performance liquid chromatographic method optimization for ondansetron assay in extemporaneous topical gel and in marketed products.

PubMed

Quamrun, Masuda; Mamoon, Rashid; Nasheed, Shams; Randy, Mullins

2014-01-01

The compounding and evaluation of ondansetron hydrochloride dihydrate topical gel, 2.5% w/w, were conducted in this study. The gelling agent was Carbopol 940. Ethanol 70% in purified water was used to dissolve the drug and disperse the gelling agent. A gel was formed by adding drops of 0.1 N sodium hydroxide solution. To assay this gel, we developed a simple and reproducible stability--indicating high-performance liquid chromatographic method. This method was validated for specificity, accuracy, and precision. The compounded gel was assayed in triplicate, and the average recovery was 98.3%. Ondansetron marketed products were analyzed for comparison with the compounded formulation. Assay, accuracy, and precision data of the compounded topical gel were comparable to the marketed products.

DEVELOPMENT AND PSYCHOMETRIC TESTING OF A MULTIDIMENSIONAL INSTRUMENT OF PERCEIVED DISCRIMINATION AMONG AFRICAN AMERICANS IN THE JACKSON HEART STUDY

PubMed Central

Sims, Mario; Wyatt, Sharon B.; Gutierrez, Mary Lou; Taylor, Herman A.; Williams, David R.

2009-01-01

Objective Assessing the discrimination-health disparities hypothesis requires psychometrically sound, multidimensional measures of discrimination. Among the available discrimination measures, few are multidimensional and none have adequate psychometric testing in a large, African American sample. We report the development and psychometric testing of the multidimensional Jackson Heart Study Discrimination (JHSDIS) Instrument. Methods A multidimensional measure assessing the occurrence, frequency, attribution, and coping responses to perceived everyday and lifetime discrimination; lifetime burden of discrimination; and effect of skin color was developed and tested in the 5302-member cohort of the Jackson Heart Study. Internal consistency was calculated by using Cronbach α. coefficient. Confirmatory factor analysis established the dimensions, and intercorrelation coefficients assessed the discriminant validity of the instrument. Setting Tri-county area of the Jackson, MS metropolitan statistical area. Results The JHSDIS was psychometrically sound (overall α=.78, .84 and .77, respectively, for the everyday and lifetime subscales). Confirmatory factor analysis yielded 11 factors, which confirmed the a priori dimensions represented. Conclusions The JHSDIS combined three scales into a single multidimensional instrument with good psychometric properties in a large sample of African Americans. This analysis lays the foundation for using this instrument in research that will examine the association between perceived discrimination and CVD among African Americans. PMID:19341164

The multidimensional perturbation value: a single metric to measure similarity and activity of treatments in high-throughput multidimensional screens.

PubMed

Hutz, Janna E; Nelson, Thomas; Wu, Hua; McAllister, Gregory; Moutsatsos, Ioannis; Jaeger, Savina A; Bandyopadhyay, Somnath; Nigsch, Florian; Cornett, Ben; Jenkins, Jeremy L; Selinger, Douglas W

2013-04-01

Screens using high-throughput, information-rich technologies such as microarrays, high-content screening (HCS), and next-generation sequencing (NGS) have become increasingly widespread. Compared with single-readout assays, these methods produce a more comprehensive picture of the effects of screened treatments. However, interpreting such multidimensional readouts is challenging. Univariate statistics such as t-tests and Z-factors cannot easily be applied to multidimensional profiles, leaving no obvious way to answer common screening questions such as "Is treatment X active in this assay?" and "Is treatment X different from (or equivalent to) treatment Y?" We have developed a simple, straightforward metric, the multidimensional perturbation value (mp-value), which can be used to answer these questions. Here, we demonstrate application of the mp-value to three data sets: a multiplexed gene expression screen of compounds and genomic reagents, a microarray-based gene expression screen of compounds, and an HCS compound screen. In all data sets, active treatments were successfully identified using the mp-value, and simulations and follow-up analyses supported the mp-value's statistical and biological validity. We believe the mp-value represents a promising way to simplify the analysis of multidimensional data while taking full advantage of its richness.

Microplate-Based Method for High-Throughput Screening (HTS) of Chromatographic Conditions Studies for Recombinant Protein Purification.

PubMed

Carvalho, Rimenys J; Cruz, Thayana A

2018-01-01

High-throughput screening (HTS) systems have emerged as important tools to provide fast and low cost evaluation of several conditions at once since it requires small quantities of material and sample volumes. These characteristics are extremely valuable for experiments with large number of variables enabling the application of design of experiments (DoE) strategies or simple experimental planning approaches. Once, the capacity of HTS systems to mimic chromatographic purification steps was established, several studies were performed successfully including scale down purification. Here, we propose a method for studying different purification conditions that can be used for any recombinant protein, including complex and glycosylated proteins, using low binding filter microplates.

Characterization of a chemical artifact in the liquid chromatographic determination of 3-butyn-2-one using the 2,4-dinitrophenylhydrazine method.

PubMed

Vogel, M; Pötter, W; Karst, U

2000-07-21

This study reports the identification of a chemical artifact occurring in the liquid chromatographic analysis of 3-butyn-2-one by means of the 2,4-dinitrophenylhydrazine (DNPH) method. Besides the expected derivatization reaction to the corresponding butynone DNPhydrazone, a rearrangement was observed, thus leading to the formation of 3-methyl-1-(2',4'-dinitrophenyl)pyrazol (DNPP). Although the rearrangement product and the hydrazone can easily be separated by means of liquid chromatography, problems arise from coelution of the pyrazol with the formaldehyde DNPhydrazone. Identification of the artifact by means of UV-Vis spectroscopy using dual wavelength or diode array detection is discussed.

Rapid thin-layer chromatographic photodensitometric method for the determination of metoclopramide and clebopride in the presence of some of their metabolic products.

PubMed

Huizing, G; Beckett, A H; Segura, J

1979-04-21

Metoclopramide and its newly developed analogue clebopride, together with some of their metabolic products are quantitated, following extraction from biological tissues and fluids, and subsequent separation on silica gel thin-layer chromatographic plates. Diazotisation, followed by coupling with N-(1-naphthyl)ethylenediammonium dichloride, carried out on the thin-layer plate, is utilised for visualisation. The intensity of the spots is measured by photodensitometric analysis. The effect of variation of various experimental conditions is studied. The method has proven to be satisfactory for the measurement of 20 ng/ml of these compounds in biological material; the results are well within the accepted limits of deviation.

A liquid chromatographic method for determination of theophylline in serum and capillary blood--a comparison.

PubMed

Gartzke, J; Jäger, H; Vins, I

1991-01-01

A simple, fast and reliable liquid chromatographic method for the determination of theophylline in serum and capillary blood after a solid phase extraction is described for therapeutic drug monitoring. The employment of capillary blood permits the determination of an individual drug profile and other pharmacokinetic studies in neonates and infants. There were no differences in venous- and capillary-blood levels but these values compared poorly with those in serum. An adjustment of the results by correction of the different volumes of serum and blood by haematocrit was unsuccessful. Differences in the binding of theophylline to erythrocytes could be an explanation for the differences in serum at blood levels of theophylline.

Refined separation of combined Fe–Hf from rock matrices for isotope analyses using AG-MP-1M and Ln-Spec chromatographic extraction resins

PubMed Central

Cheng, Ting; Nebel, Oliver; Sossi, Paolo A.; Chen, Fukun

2014-01-01

A combined procedure for separating Fe and Hf from a single rock digestion is presented. In a two-stage chromatographic extraction process, a purified Fe fraction is first quantitatively separated from the rock matrix using AG-MP-1M resin in HCl. Hafnium is subsequently isolated using a modified version of a commonly applied method using Eichrom LN-Spec resin. Our combined method includes:•Purification of Fe from the rock matrix using HCl, ready for mass spectrometric analysis.•Direct loading of the matrix onto the resin that is used for Hf purification.•Collection of a Fe-free Hf fraction. PMID:26150946

Fuels characterization studies. [jet fuels

NASA Technical Reports Server (NTRS)

Seng, G. T.; Antoine, A. C.; Flores, F. J.

1980-01-01

Current analytical techniques used in the characterization of broadened properties fuels are briefly described. Included are liquid chromatography, gas chromatography, and nuclear magnetic resonance spectroscopy. High performance liquid chromatographic ground-type methods development is being approached from several directions, including aromatic fraction standards development and the elimination of standards through removal or partial removal of the alkene and aromatic fractions or through the use of whole fuel refractive index values. More sensitive methods for alkene determinations using an ultraviolet-visible detector are also being pursued. Some of the more successful gas chromatographic physical property determinations for petroleum derived fuels are the distillation curve (simulated distillation), heat of combustion, hydrogen content, API gravity, viscosity, flash point, and (to a lesser extent) freezing point.

Approximate series solution of multi-dimensional, time fractional-order (heat-like) diffusion equations using FRDTM.

PubMed

Singh, Brajesh K; Srivastava, Vineet K

2015-04-01

The main goal of this paper is to present a new approximate series solution of the multi-dimensional (heat-like) diffusion equation with time-fractional derivative in Caputo form using a semi-analytical approach: fractional-order reduced differential transform method (FRDTM). The efficiency of FRDTM is confirmed by considering four test problems of the multi-dimensional time fractional-order diffusion equation. FRDTM is a very efficient, effective and powerful mathematical tool which provides exact or very close approximate solutions for a wide range of real-world problems arising in engineering and natural sciences, modelled in terms of differential equations.

Approximate series solution of multi-dimensional, time fractional-order (heat-like) diffusion equations using FRDTM

PubMed Central

Singh, Brajesh K.; Srivastava, Vineet K.

2015-01-01

The main goal of this paper is to present a new approximate series solution of the multi-dimensional (heat-like) diffusion equation with time-fractional derivative in Caputo form using a semi-analytical approach: fractional-order reduced differential transform method (FRDTM). The efficiency of FRDTM is confirmed by considering four test problems of the multi-dimensional time fractional-order diffusion equation. FRDTM is a very efficient, effective and powerful mathematical tool which provides exact or very close approximate solutions for a wide range of real-world problems arising in engineering and natural sciences, modelled in terms of differential equations. PMID:26064639

Manual method of visually identifying candidate signals for a targeted peptide.

PubMed

Filimonov, Aleksey; Kopylov, Arthur; Lisitsa, Andrey; Archakov, Alexander

2018-04-15

The purpose of this study is to improve peptide signal identification in groups of extracted ion chromatograms (XICs) obtained with the liquid chromatography-selected reaction monitoring (LC-SRM) technique and a triple quadrupole mass spectrometer (QqQ) operating in one of the supported multiple reaction monitoring (MRM) modes. The imperfection of quadrupole mass analyzers causes ion interference, which impedes the identification of peptide signals as chromatographic peak groups in relevant retention time intervals. To investigate this problem in depth, the QqQ conversion of the eluate into XIC groups was considered as the consecutive transformations of the particles' abundances as the corresponding functions of retention time. In this study, the hypothesis that, during this conversion, the same chromatographic profile should be preserved as an implicit sign in each chromatographic peak of the signal was confirmed for peptides. To examine chromatographic profiles, continuous transformations of XIC groups were derived and implemented in srm2prot Express software (s2pe, http://msr.ibmc.msk.ru/s2pe). Because of ion interference, several peptide-like signals may appear in one XIC group. Therefore, these signals must be considered candidates for a targeted peptide's signal and should be resolved after identification. The theoretical investigation of intensity functions as XICs that are not distorted by noise produced three rules for Identifying Candidate Signals for a targeted Peptide (ICSP, http://msr.ibmc.msk.ru/ICSP) that constitute the proposed manual visual method. We theoretically and experimentally compared this method with the conventional semiempirical intuitive technique and found that the former significantly streamlines peptide signal identification and avoids typical errors. Copyright © 2018 Elsevier B.V. All rights reserved.

Territories typification technique with use of statistical models

NASA Astrophysics Data System (ADS)

Galkin, V. I.; Rastegaev, A. V.; Seredin, V. V.; Andrianov, A. V.

2018-05-01

Territories typification is required for solution of many problems. The results of geological zoning received by means of various methods do not always agree. That is why the main goal of the research given is to develop a technique of obtaining a multidimensional standard classified indicator for geological zoning. In the course of the research, the probabilistic approach was used. In order to increase the reliability of geological information classification, the authors suggest using complex multidimensional probabilistic indicator P K as a criterion of the classification. The second criterion chosen is multidimensional standard classified indicator Z. These can serve as characteristics of classification in geological-engineering zoning. Above mentioned indicators P K and Z are in good correlation. Correlation coefficient values for the entire territory regardless of structural solidity equal r = 0.95 so each indicator can be used in geological-engineering zoning. The method suggested has been tested and the schematic map of zoning has been drawn.

Deterministic multidimensional nonuniform gap sampling.

PubMed

Worley, Bradley; Powers, Robert

2015-12-01

Born from empirical observations in nonuniformly sampled multidimensional NMR data relating to gaps between sampled points, the Poisson-gap sampling method has enjoyed widespread use in biomolecular NMR. While the majority of nonuniform sampling schemes are fully randomly drawn from probability densities that vary over a Nyquist grid, the Poisson-gap scheme employs constrained random deviates to minimize the gaps between sampled grid points. We describe a deterministic gap sampling method, based on the average behavior of Poisson-gap sampling, which performs comparably to its random counterpart with the additional benefit of completely deterministic behavior. We also introduce a general algorithm for multidimensional nonuniform sampling based on a gap equation, and apply it to yield a deterministic sampling scheme that combines burst-mode sampling features with those of Poisson-gap schemes. Finally, we derive a relationship between stochastic gap equations and the expectation value of their sampling probability densities. Copyright © 2015 Elsevier Inc. All rights reserved.

Multidimensional Poverty and Child Survival in India

PubMed Central

Mohanty, Sanjay K.

2011-01-01

Background Though the concept of multidimensional poverty has been acknowledged cutting across the disciplines (among economists, public health professionals, development thinkers, social scientists, policy makers and international organizations) and included in the development agenda, its measurement and application are still limited. Objectives and Methodology Using unit data from the National Family and Health Survey 3, India, this paper measures poverty in multidimensional space and examine the linkages of multidimensional poverty with child survival. The multidimensional poverty is measured in the dimension of knowledge, health and wealth and the child survival is measured with respect to infant mortality and under-five mortality. Descriptive statistics, principal component analyses and the life table methods are used in the analyses. Results The estimates of multidimensional poverty are robust and the inter-state differentials are large. While infant mortality rate and under-five mortality rate are disproportionately higher among the abject poor compared to the non-poor, there are no significant differences in child survival among educationally, economically and health poor at the national level. State pattern in child survival among the education, economical and health poor are mixed. Conclusion Use of multidimensional poverty measures help to identify abject poor who are unlikely to come out of poverty trap. The child survival is significantly lower among abject poor compared to moderate poor and non-poor. We urge to popularize the concept of multiple deprivations in research and program so as to reduce poverty and inequality in the population. PMID:22046384

Interactions across Multiple Stimulus Dimensions in Primary Auditory Cortex.

PubMed

Sloas, David C; Zhuo, Ran; Xue, Hongbo; Chambers, Anna R; Kolaczyk, Eric; Polley, Daniel B; Sen, Kamal

2016-01-01

Although sensory cortex is thought to be important for the perception of complex objects, its specific role in representing complex stimuli remains unknown. Complex objects are rich in information along multiple stimulus dimensions. The position of cortex in the sensory hierarchy suggests that cortical neurons may integrate across these dimensions to form a more gestalt representation of auditory objects. Yet, studies of cortical neurons typically explore single or few dimensions due to the difficulty of determining optimal stimuli in a high dimensional stimulus space. Evolutionary algorithms (EAs) provide a potentially powerful approach for exploring multidimensional stimulus spaces based on real-time spike feedback, but two important issues arise in their application. First, it is unclear whether it is necessary to characterize cortical responses to multidimensional stimuli or whether it suffices to characterize cortical responses to a single dimension at a time. Second, quantitative methods for analyzing complex multidimensional data from an EA are lacking. Here, we apply a statistical method for nonlinear regression, the generalized additive model (GAM), to address these issues. The GAM quantitatively describes the dependence between neural response and all stimulus dimensions. We find that auditory cortical neurons in mice are sensitive to interactions across dimensions. These interactions are diverse across the population, indicating significant integration across stimulus dimensions in auditory cortex. This result strongly motivates using multidimensional stimuli in auditory cortex. Together, the EA and the GAM provide a novel quantitative paradigm for investigating neural coding of complex multidimensional stimuli in auditory and other sensory cortices.

Partial least squares model and design of experiments toward the analysis of the metabolome of Jatropha gossypifolia leaves: Extraction and chromatographic fingerprint optimization.

PubMed

Pilon, Alan Cesar; Carnevale Neto, Fausto; Freire, Rafael Teixeira; Cardoso, Patrícia; Carneiro, Renato Lajarim; Da Silva Bolzani, Vanderlan; Castro-Gamboa, Ian

2016-03-01

A major challenge in metabolomic studies is how to extract and analyze an entire metabolome. So far, no single method was able to clearly complete this task in an efficient and reproducible way. In this work we proposed a sequential strategy for the extraction and chromatographic separation of metabolites from leaves Jatropha gossypifolia using a design of experiments and partial least square model. The effect of 14 different solvents on extraction process was evaluated and an optimized separation condition on liquid chromatography was estimated considering mobile phase composition and analysis time. The initial conditions of extraction using methanol and separation in 30 min between 5 and 100% water/methanol (1:1 v/v) with 0.1% of acetic acid, 20 μL sample volume, 3.0 mL min(-1) flow rate and 25°C column temperature led to 107 chromatographic peaks. After the optimization strategy using i-propanol/chloroform (1:1 v/v) for extraction, linear gradient elution of 60 min between 5 and 100% water/(acetonitrile/methanol 68:32 v/v with 0.1% of acetic acid), 30 μL sample volume, 2.0 mL min(-1) flow rate, and 30°C column temperature, we detected 140 chromatographic peaks, 30.84% more peaks compared to initial method. This is a reliable strategy using a limited number of experiments for metabolomics protocols. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

An improved UHPLC-UV method for separation and quantification of carotenoids in vegetable crops.

PubMed

Maurer, Megan M; Mein, Jonathan R; Chaudhuri, Swapan K; Constant, Howard L

2014-12-15

Carotenoid identification and quantitation is critical for the development of improved nutrition plant varieties. Industrial analysis of carotenoids is typically carried out on multiple crops with potentially thousands of samples per crop, placing critical needs on speed and broad utility of the analytical methods. Current chromatographic methods for carotenoid analysis have had limited industrial application due to their low throughput, requiring up to 60 min for complete separation of all compounds. We have developed an improved UHPLC-UV method that resolves all major carotenoids found in broccoli (Brassica oleracea L. var. italica), carrot (Daucus carota), corn (Zea mays), and tomato (Solanum lycopersicum). The chromatographic method is completed in 13.5 min allowing for the resolution of the 11 carotenoids of interest, including the structural isomers lutein/zeaxanthin and α-/β-carotene. Additional minor carotenoids have also been separated and identified with this method, demonstrating the utility of this method across major commercial food crops. Copyright © 2014 Elsevier Ltd. All rights reserved.

Visual modeling in an analysis of multidimensional data

NASA Astrophysics Data System (ADS)

Zakharova, A. A.; Vekhter, E. V.; Shklyar, A. V.; Pak, A. J.

2018-01-01

The article proposes an approach to solve visualization problems and the subsequent analysis of multidimensional data. Requirements to the properties of visual models, which were created to solve analysis problems, are described. As a perspective direction for the development of visual analysis tools for multidimensional and voluminous data, there was suggested an active use of factors of subjective perception and dynamic visualization. Practical results of solving the problem of multidimensional data analysis are shown using the example of a visual model of empirical data on the current state of studying processes of obtaining silicon carbide by an electric arc method. There are several results of solving this problem. At first, an idea of possibilities of determining the strategy for the development of the domain, secondly, the reliability of the published data on this subject, and changes in the areas of attention of researchers over time.

Unexpected retention behavior of baicalin: Hydrophilic interaction like properties of a reversed-phase column.

PubMed

Magda, Balázs; Márta, Zoltán; Imre, Tímea; Kalapos-Kovács, Bernadett; Klebovich, Imre; Fekete, Jenő; Szabó, Pál T

2015-01-01

The original aim of this study was to develop a method for the determination of baicalin from membrane vesicles. The unconventional chromatographic separation ("inverse gradient elution" on a reversed phase column) was due to a lucky chance, which is detailed and discussed in this study. The validated liquid chromatography-tandem mass spectrometry (LC-MS/MS) method is proved to be sensitive, rapid and selective. Chromatographic separation was performed on a Zorbax SB-C8 column (250 mm × 4.6 mm, i.d.; 5 μm) with 0.1% formic acid in water and methanol by linear gradient elution. Quantification of baicalin was determined by multiple reaction monitoring (MRM) mode using electrospray ionization (ESI). The calibration curve was linear (r = 0.9987) over the concentration range from 1 to 1000 nM. The coefficient of variation and relative error of baicalin for intra- and inter-assay at three quality control (QC) levels were 2.0-10.2% and -6.1 to 6.7%, respectively. The lower limit of quantification (LLOQ) for baicalin was 1 nM (0.446 ng/ml), without preconcentration of the sample. This method was subsequently applied to vesicular transport assays of baicalin in membrane vesicles successfully. The developed method can open up new area of research in the chromatographic separation of flavonoids and their glucuronides. Copyright © 2015. Published by Elsevier B.V.

Stability of suxamethonium in pharmaceutical solution for injection by validated stability-indicating chromatographic method.

PubMed

Beck, William; Kabiche, Sofiane; Balde, Issa-Bella; Carret, Sandra; Fontan, Jean-Eudes; Cisternino, Salvatore; Schlatter, Joël

2016-12-01

To assess the stability of pharmaceutical suxamethonium (succinylcholine) solution for injection by validated stability-indicating chromatographic method in vials stored at room temperature. The chromatographic assay was achieved by using a detector wavelength set at 218 nm, a C18 column, and an isocratic mobile phase (100% of water) at a flow rate of 0.6 mL/min for 5 minutes. The method was validated according to the International Conference on Harmonization guidelines with respect to the stability-indicating capacity of the method including linearity, limits of detection and quantitation, precision, accuracy, system suitability, robustness, and forced degradations. Linearity was achieved in the concentration range of 5 to 40 mg/mL with a correlation coefficient higher than 0.999. The limits of detection and quantification were 0.8 and 0.9 mg/mL, respectively. The percentage relative standard deviation for intraday (1.3-1.7) and interday (0.1-2.0) precision was found to be less than 2.1%. Accuracy was assessed by the recovery test of suxamethonium from solution for injection (99.5%-101.2%). Storage of suxamethonium solution for injection vials at ambient temperature (22°C-26°C) for 17 days demonstrated that at least 95% of original suxamethonium concentration remained stable. Copyright © 2016 Elsevier Inc. All rights reserved.

DEMONSTRATION BULLETIN: FIELD ANALYTICAL SCREENING PROGRAM: PCB METHOD - U.S. ENVIRONMENTAL PROTECTION AGENCY

EPA Science Inventory

The field analytical screening program (FASP) polychlorinated biphenyl (PCB) method uses a temperature-programmable gas chromatograph (GC) equipped with an electron capture detector (ECD) to identify and quantify PCBs. Gas chromatography is an EPA-approved method for determi...

FIELD ANALYTICAL SCREENING PROGRAM: PCP METHOD - INNOVATIVE TECHNOLOGY EVALUATION REPORT

EPA Science Inventory

The Field Analytical Screening Program (FASP) pentachlorophenol (PCP) method uses a gas chromatograph (GC) equipped with a megabore capillary column and flame ionization detector (FID) and electron capture detector (ECD) to identify and quantify PCP. The FASP PCP method is design...

Fluorescence-correlation spectroscopy study of molecular transport within reversed-phase chromatographic particles compared to planar model surfaces.

PubMed

Cooper, Justin; Harris, Joel M

2014-12-02

Reversed-phase liquid chromatography (RPLC) is a widely used technique for molecular separations. Stationary-phase materials for RPLC generally consist of porous silica-gel particles functionalized with n-alkane ligands. Understanding motions of molecules within the interior of these particles is important for developing efficient chromatographic materials and separations. To characterize these dynamics, time-resolved spectroscopic methods (photobleach recovery, fluorescence correlation, single-molecule imaging) have been adapted to measure molecular diffusion rates, typically at n-alkane-modified planar silica surfaces, which serve as models of chromatographic interfaces. A question arising from these studies is how dynamics of molecules on a planar surface relate to motions of molecules within the interior of a porous chromatographic particle. In this paper, imaging-fluorescence-correlation spectroscopy is used to measure diffusion rates of a fluorescent probe molecule 1,1'-dioctadecyl-3,3,3'3'-tetramethylindocarbocyanine perchlorate (DiI) within authentic RPLC porous silica particles and compared with its diffusion at a planar C18-modified surface. The results show that surface diffusion on the planar C18 substrate is much faster than the diffusion rate of the probe molecule through a chromatographic particle. Surface diffusion within porous particles, however, is governed by molecular trajectories along the tortuous contours of the interior surface of the particles. By accounting for the greater surface area that a molecule must explore to diffuse macroscopic distances through the particle, the molecular-scale diffusion rates on the two surfaces can be compared, and they are virtually identical. These results provide support for the relevance of surface-diffusion measurements made on planar model surfaces to the dynamic behavior of molecules on the internal surfaces of porous chromatographic particles.

Effectiveness of Multidimensional Cancer Survivor Rehabilitation and Cost-Effectiveness of Cancer Rehabilitation in General: A Systematic Review

PubMed Central

Mewes, Janne C.; IJzerman, Maarten J.; van Harten, Wim H.

2012-01-01

Introduction. Many cancer survivors suffer from a combination of disease- and treatment-related morbidities and complaints after primary treatment. There is a growing evidence base for the effectiveness of monodimensional rehabilitation interventions; in practice, however, patients often participate in multidimensional programs. This study systematically reviews evidence regarding effectiveness of multidimensional rehabilitation programs for cancer survivors and cost-effectiveness of cancer rehabilitation in general. Methods. The published literature was systematically reviewed. Data were extracted using standardized forms and were summarized narratively. Results. Sixteen effectiveness and six cost-effectiveness studies were included. Multidimensional rehabilitation programs were found to be effective, but not more effective than monodimensional interventions, and not on all outcome measures. Effect sizes for quality of life were in the range of −0.12 (95% confidence interval [CI], −0.45–0.20) to 0.98 (95% CI, 0.69–1.29). Incremental cost-effectiveness ratios ranged from −€16,976, indicating cost savings, to €11,057 per quality-adjusted life year. Conclusions. The evidence for multidimensional interventions and the economic impact of rehabilitation studies is scarce and dominated by breast cancer studies. Studies published so far report statistically significant benefits for multidimensional interventions over usual care, most notably for the outcomes fatigue and physical functioning. An additional benefit of multidimensional over monodimensional rehabilitation was not found, but this was also sparsely reported on. Available economic evaluations assessed very different rehabilitation interventions. Yet, despite low comparability, all showed favorable cost-effectiveness ratios. Future studies should focus their designs on the comparative effectiveness and cost-effectiveness of multidimensional programs. PMID:22982580

Supercritical fluid chromatography for lipid analysis in foodstuffs.

PubMed

Donato, Paola; Inferrera, Veronica; Sciarrone, Danilo; Mondello, Luigi

2017-01-01

The task of lipid analysis has always challenged separation scientists, and new techniques in chromatography were often developed for the separation of lipids; however, no single technique or methodology is yet capable of affording a comprehensive screening of all lipid species and classes. This review acquaints the role of supercritical fluid chromatography within the field of lipid analysis, from the early developed capillary separations based on pure CO 2 , to the most recent techniques employing packed columns under subcritical conditions, including the niche multidimensional techniques using supercritical fluids in at least one of the separation dimensions. A short history of supercritical fluid chromatography will be introduced first, from its early popularity in the late 1980s, to the sudden fall and oblivion until the last decade, experiencing a regain of interest within the chromatographic community. Afterwards, the subject of lipid nomenclature and classification will be briefly dealt with, before discussing the main applications of supercritical fluid chromatography for food analysis, according to the specific class of lipids. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ecto-Fc MS identifies ligand-receptor interactions through extracellular domain Fc fusion protein baits and shotgun proteomic analysis

PubMed Central

Savas, Jeffrey N.; De Wit, Joris; Comoletti, Davide; Zemla, Roland; Ghosh, Anirvan

2015-01-01

Ligand-receptor interactions represent essential biological triggers which regulate many diverse and important cellular processes. We have developed a discovery-based proteomic biochemical protocol which couples affinity purification with multidimensional liquid chromatographic tandem mass spectrometry (LCLC-MS/MS) and bioinformatic analysis. Compared to previous approaches, our analysis increases sensitivity, shortens analysis duration, and boosts comprehensiveness. In this protocol, receptor extracellular domains are fused with the Fc region of IgG to generate fusion proteins that are purified from transfected HEK293T cells. These “ecto-Fcs” are coupled to protein A beads and serve as baits for binding assays with prey proteins extracted from rodent brain. After capture, the affinity purified proteins are digested into peptides and comprehensively analyzed by LCLC-MS/MS with ion trap mass spectrometers. In four working days, this protocol can generate shortlists of candidate ligand-receptor protein-protein interactions. Our “Ecto-Fc MS” approach outperforms antibody-based approaches and provides a reproducible and robust framework to identify extracellular ligand – receptor interactions. PMID:25101821

Supervised Semi-Automated Data Analysis Software for Gas Chromatography / Differential Mobility Spectrometry (GC/DMS) Metabolomics Applications.

PubMed

Peirano, Daniel J; Pasamontes, Alberto; Davis, Cristina E

2016-09-01

Modern differential mobility spectrometers (DMS) produce complex and multi-dimensional data streams that allow for near-real-time or post-hoc chemical detection for a variety of applications. An active area of interest for this technology is metabolite monitoring for biological applications, and these data sets regularly have unique technical and data analysis end user requirements. While there are initial publications on how investigators have individually processed and analyzed their DMS metabolomic data, there are no user-ready commercial or open source software packages that are easily used for this purpose. We have created custom software uniquely suited to analyze gas chromatograph / differential mobility spectrometry (GC/DMS) data from biological sources. Here we explain the implementation of the software, describe the user features that are available, and provide an example of how this software functions using a previously-published data set. The software is compatible with many commercial or home-made DMS systems. Because the software is versatile, it can also potentially be used for other similarly structured data sets, such as GC/GC and other IMS modalities.

Green approach using monolithic column for simultaneous determination of coformulated drugs.

PubMed

Yehia, Ali M; Mohamed, Heba M

2016-06-01

Green chemistry and sustainability is now entirely encompassed across the majority of pharmaceutical companies and research labs. Researchers' attention is careworn toward implementing the green analytical chemistry principles for more eco-friendly analytical methodologies. Solvents play a dominant role in determining the greenness of the analytical procedure. Using safer solvents, the greenness profile of the methodology could be increased remarkably. In this context, a green chromatographic method has been developed and validated for the simultaneous determination of phenylephrine, paracetamol, and guaifenesin in their ternary pharmaceutical mixture. The chromatographic separation was carried out using monolithic column and green solvents as mobile phase. The use of monolithic column allows efficient separation protocols at higher flow rates, which results in short time of analysis. Two-factor three-level experimental design was used to optimize the chromatographic conditions. The greenness profile of the proposed methodology was assessed using eco-scale as a green metrics and was found to be an excellent green method with regard to the usage and production of hazardous chemicals and solvents, energy consumption, and amount of produced waste. The proposed method improved the environmental impact without compromising the analytical performance criteria and could be used as a safer alternate for the routine analysis of the studied drugs. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High sensitive analysis of steroids in doping control using gas chromatography/time-of-flight mass-spectrometry.

PubMed

Revelsky, A I; Samokhin, A S; Virus, E D; Rodchenkov, G M; Revelsky, I A

2011-04-01

The method of high sensitive gas chromatographic/time-of-flight mass-spectrometric (GC/TOF-MS) analysis of steroids was developed. Low-resolution TOF-MS instrument (with fast spectral acquisition rate) was used. This method is based on the formation of the silyl derivatives of steroids; exchange of the reagent mixture (pyridine and N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA)) for tert-butylmethylether; offline large sample volume injection of this solution based on sorption concentration of the respective derivatives from the vapour-gas mixture flow formed from the solution and inert gas flows; and entire analytes solvent-free concentrate transfer into the injector of the gas chromatograph. Detection limits for 100 µl sample solution volume were 0.5-2 pg/µl (depending on the component). Application of TOF-MS model 'TruTOF' (Leco, St Joseph, MO, USA) coupled with gas chromatograph and ChromaTOF software (Leco, St Joseph, MO, USA) allowed extraction of the full mass spectra and resolving coeluted peaks. Due to use of the proposed method (10 µl sample aliquot) and GC/TOF-MS, two times more steroid-like compounds were registered in the urine extract in comparison with the injection of 1 µl of the same sample solution. Copyright © 2010 John Wiley & Sons, Ltd.

Simple, fast and reliable liquid chromatographic and spectrophotometric methods for the determination of theophylline in urine, saliva and plasma samples.

PubMed

Charehsaz, Mohammad; Gürbay, Aylin; Aydin, Ahmet; Sahin, Gönül

2014-01-01

In this study, a high-performance liquid chromatographic method (HPLC) and UV spectrophotometric method were developed, validated and applied for the determination of theophylline in biological fluids. Liquid- liquid extraction is performed for isolation of the drug and elimination of plasma and saliva interferences. Urine samples were applied without any extraction. The chromatographic separation was achieved on a C18 column by using 60:40 methanol:water as mobile phase under isocratic conditions at a flow rate of 0.75 mL/min with UV detection at 280 nm in HPLC method. UV spectrophotometric analysis was performed at 275 nm. the limit of quantification: 1.1 µg/mL for urine, 1.9 µg/mL for saliva, 3.1 µg/mL for plasma; recovery: 94.85% for plasma, 100.45% for saliva, 101.39% for urine; intra-day precision: 0.22-2.33%, inter-day precision: 3.17-13.12%. Spectrophotometric analysis results were as follows: the limit of quantitation: 5.23 µg/mL for plasma, 8.7 µg/mL for urine; recovery: 98.27% for plasma, 95.25% for urine; intra-day precision: 2.37 - 3.00%, inter-day precision: 5.43-7.91%. It can be concluded that this validated HPLC method is easy, precise, accurate, sensitive and selective for determination of theophylline in biological samples. Also spectrophotometric analysis can be used where it can be applicable.

Development and Bioanalytical Validation of a Liquid Chromatographic-Tandem Mass Spectrometric (LC-MS/MS) Method for the Quantification of the CCR5 Antagonist Maraviroc in Human Plasma

PubMed Central

Emory, Joshua F.; Seserko, Lauren A.; Marzinke, Mark A.

2014-01-01

Background Maraviroc is a CCR5 antagonist that has been utilized as a viral entry inhibitor in the management of HIV-1. Current clinical trials are pursuing maraviroc drug efficacy in both oral and topical formulations. Therefore, in order to fully understand drug pharmacokinetics, a sensitive method is required to quantify plasma drug concentrations. Methods Maraviroc-spiked plasma was combined with acetonitrile containing an isotopically-labeled internal standard, and following protein precipitation, samples were evaporated to dryness and reconstituted for liquid chromatographic-tandem mass spectrometric (LC-MS/MS) analysis. Chromatographic separation was achieved on a Waters BEH C8, 50 × 2.1 mm UPLC column, with a 1.7 μm particle size and the eluent was analyzed using an API 4000 mass analyzer in selected reaction monitoring mode. The method was validated as per FDA Bioanalytical Method Validation guidelines. Results The analytical measuring range of the LC-MS/MS method is 0.5-1000 ng/ml. Calibration curves were generated using weighted 1/x2 quadratic regression. Inter-and intra-assay precision was ≤ 5.38% and ≤ 5.98%, respectively; inter-and intra-assay accuracy (%DEV) was ≤ 10.2% and ≤ 8.44%, respectively. Additional studies illustrated similar matrix effects between maraviroc and its internal standard, and that maraviroc is stable under a variety of conditions. Method comparison studies with a reference LC-MS/MS method show a slope of 0.948 with a Spearman coefficient of 0.98. Conclusions Based on the validation metrics, we have generated a sensitive and automated LC-MS/MS method for maraviroc quantification in human plasma. PMID:24561264

Method and apparatus for continuous annular electrochromatography

DOEpatents

Scott, Charles D.

1987-01-01

Separation of complex mixtures and solutions can be carried out using a method and apparatus for continuous annular electrochromatography. Solutes are diverted radially by an imposed electrical field as they move downward in a rotating chromatographic column.

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

PubMed

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

2017-09-01

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

Quantification of N-acetyl- and N-glycolylneuraminic acids by a stable isotope dilution assay using high-performance liquid chromatography-tandem mass spectrometry.

PubMed

Allevi, Pietro; Femia, Eti Alessandra; Costa, Maria Letizia; Cazzola, Roberta; Anastasia, Mario

2008-11-28

The present report describes a method for the quantification of N-acetyl- and N-glycolylneuraminic acids without any derivatization, using their (13)C(3)-isotopologues as internal standards and a C(18) reversed-phase column modified by decylboronic acid which allows for the first time a complete chromatographic separation between the two analytes. The method is based on high-performance liquid chromatographic coupled with electrospray ion-trap mass spectrometry. The limit of quantification of the method is 0.1mg/L (2.0ng on column) for both analytes. The calibration curves are linear for both sialic acids over the range of 0.1-80mg/L (2.0-1600ng on column) with a correlation coefficient greater than 0.997. The proposed method was applied to the quantitative determination of sialic acids released from fetuin as a model of glycoproteins.

Mass spectrometric-based stable isotopic 2-aminobenzoic acid glycan mapping for rapid glycan screening of biotherapeutics.

PubMed

Prien, Justin M; Prater, Bradley D; Qin, Qiang; Cockrill, Steven L

2010-02-15

Fast, sensitive, robust methods for "high-level" glycan screening are necessary during various stages of a biotherapeutic product's lifecycle, including clone selection, process changes, and quality control for lot release testing. Traditional glycan screening involves chromatographic or electrophoretic separation-based methods, and, although reproducible, these methods can be time-consuming. Even ultrahigh-performance chromatographic and microfluidic integrated LC/MS systems, which work on the tens of minute time scale, become lengthy when hundreds of samples are to be analyzed. Comparatively, a direct infusion mass spectrometry (MS)-based glycan screening method acquires data on a millisecond time scale, exhibits exquisite sensitivity and reproducibility, and is amenable to automated peak annotation. In addition, characterization of glycan species via sequential mass spectrometry can be performed simultaneously. Here, we demonstrate a quantitative high-throughput MS-based mapping approach using stable isotope 2-aminobenzoic acid (2-AA) for rapid "high-level" glycan screening.

Affiliation with Delinquent Peers as a Mediator of the Effects of Multidimensional Treatment Foster Care for Delinquent Girls

ERIC Educational Resources Information Center

Van Ryzin, Mark J.; Leve, Leslie D.

2012-01-01

Objective: This study evaluated the ability of delinquent peer affiliation to mediate the effects of multidimensional treatment foster care (MTFC; Chamberlain, 2003) on girls' delinquent behavior. Method: This study used a sample of girls from 2 cohorts (N = 166; M = 15.31 years old at baseline, range 13-17 years; 74% European American, 2% African…

Systematic evaluation of commercially available ultra-high performance liquid chromatography columns for drug metabolite profiling: optimization of chromatographic peak capacity.

PubMed

Dubbelman, Anne-Charlotte; Cuyckens, Filip; Dillen, Lieve; Gross, Gerhard; Hankemeier, Thomas; Vreeken, Rob J

2014-12-29

The present study investigated the practical use of modern ultra-high performance liquid chromatography (UHPLC) separation techniques for drug metabolite profiling, aiming to develop a widely applicable, high-throughput, easy-to-use chromatographic method, with a high chromatographic resolution to accommodate simultaneous qualitative and quantitative analysis of small-molecule drugs and metabolites in biological matrices. To this end, first the UHPLC system volume and variance were evaluated. Then, a mixture of 17 drugs and various metabolites (molecular mass of 151-749Da, logP of -1.04 to 6.7), was injected on six sub-2μm particle columns. Five newest generation core shell technology columns were compared and tested against one column packed with porous particles. Two aqueous (pH 2.7 and 6.8) and two organic mobile phases were evaluated, first with the same flow and temperature and subsequently at each column's individual limit of temperature and pressure. The results demonstrated that pre-column dead volume had negligible influence on the peak capacity and shape. In contrast, a decrease in post-column volume of 57% resulted in a substantial (47%) increase in median peak capacity and significantly improved peak shape. When the various combinations of stationary and mobile phases were used at the same flow rate (0.5mL/min) and temperature (45°C), limited differences were observed between the median peak capacities, with a maximum of 26%. At higher flow though (up to 0.9mL/min), a maximum difference of almost 40% in median peak capacity was found between columns. The finally selected combination of solid-core particle column and mobile phase composition was chosen for its selectivity, peak capacity, wide applicability and peak shape. The developed method was applied to rat hepatocyte samples incubated with the drug buspirone and demonstrated to provide a similar chromatographic resolution, but a 6 times higher signal-to-noise ratio than a more traditional UHPLC metabolite profiling method using a fully porous particle packed column, within one third of the analysis time. In conclusion, a widely applicable, selective and fast chromatographic method was developed that can be applied to perform drug metabolite profiling in the timeframe of a quantitative analysis. It is envisioned that this method will in future be used for simultaneous qualitative and quantitative analysis and can therefore be considered a first important step in the Quan/Qual workflow. Copyright © 2014 Elsevier B.V. All rights reserved.

Rapid fusion method for the determination of Pu, Np, and Am in large soil samples

DOE PAGES

Maxwell, Sherrod L.; Culligan, Brian; Hutchison, Jay B.; ...

2015-02-14

A new rapid sodium hydroxide fusion method for the preparation of 10-20 g soil samples has been developed by the Savannah River National Laboratory (SRNL). The method enables lower detection limits for plutonium, neptunium, and americium in environmental soil samples. The method also significantly reduces sample processing time and acid fume generation compared to traditional soil digestion techniques using hydrofluoric acid. Ten gram soil aliquots can be ashed and fused using the new method in 1-2 hours, completely dissolving samples, including refractory particles. Pu, Np and Am are separated using stacked 2mL cartridges of TEVA and DGA Resin and measuredmore » using alpha spectrometry. The method can be adapted for measurement by inductively-coupled plasma mass spectrometry (ICP-MS). Two 10 g soil aliquots of fused soil may be combined prior to chromatographic separations to further improve detection limits. Total sample preparation time, including chromatographic separations and alpha spectrometry source preparation, is less than 8 hours.« less

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.

Parsimony and goodness-of-fit in multi-dimensional NMR inversion

NASA Astrophysics Data System (ADS)

Babak, Petro; Kryuchkov, Sergey; Kantzas, Apostolos

2017-01-01

Multi-dimensional nuclear magnetic resonance (NMR) experiments are often used for study of molecular structure and dynamics of matter in core analysis and reservoir evaluation. Industrial applications of multi-dimensional NMR involve a high-dimensional measurement dataset with complicated correlation structure and require rapid and stable inversion algorithms from the time domain to the relaxation rate and/or diffusion domains. In practice, applying existing inverse algorithms with a large number of parameter values leads to an infinite number of solutions with a reasonable fit to the NMR data. The interpretation of such variability of multiple solutions and selection of the most appropriate solution could be a very complex problem. In most cases the characteristics of materials have sparse signatures, and investigators would like to distinguish the most significant relaxation and diffusion values of the materials. To produce an easy to interpret and unique NMR distribution with the finite number of the principal parameter values, we introduce a new method for NMR inversion. The method is constructed based on the trade-off between the conventional goodness-of-fit approach to multivariate data and the principle of parsimony guaranteeing inversion with the least number of parameter values. We suggest performing the inversion of NMR data using the forward stepwise regression selection algorithm. To account for the trade-off between goodness-of-fit and parsimony, the objective function is selected based on Akaike Information Criterion (AIC). The performance of the developed multi-dimensional NMR inversion method and its comparison with conventional methods are illustrated using real data for samples with bitumen, water and clay.

Chromatographic column evaluation for the untargeted profiling of glucosinolates in cauliflower by means of ultra-high performance liquid chromatography coupled to high resolution mass spectrometry.

PubMed

Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Montone, Carmela Maria; Piovesana, Susy; Zenezini Chiozzi, Riccardo; Laganà, Aldo

2018-03-01

The untargeted profiling is a promising approach for the characterization of secondary metabolites in biological matrices. Thanks to the recent rapid development of high-resolution mass spectrometry (HRMS) instrumentations, the number of applications by untargeted approaches for biological samples profiling has widely increased in the recent years. Despite the high potentialities of HRMS, however, a major issue in natural products analysis often arises in the upstream process of compounds separation. A separation technique is necessary to avoid phenomena such as signal suppression, and it is especially needed in the presence of isomeric metabolites, which are otherwise indistinguishable. Glucosinolates (GLSs), a group of secondary metabolites widely distributed among plants, resulted to be associated to the prevention of some serious diseases, such as cancer. This led to the development of several methods for the analysis of GLSs in vegetables tissues. The issue of GLSs chromatographic separation has been widely studied in the past because of the difficulty in the analysis of this highly polar and variable class of compounds. Several alternatives to reversed phase (RP) chromatography, sometimes not compatible with the coupling of liquid chromatography with mass spectrometry, have been tested for the analysis of intact GLSs. However, the availability of new stationary phases, in the last years, could allow the re-evaluation of RP chromatography for the analysis of intact GLSs. In this work, a thorough evaluation of four RP chromatographic columns for the analysis of GLSs in cauliflower (Brassica oleracea L. var. botrytis) extracts by an ultra-high performance liquid chromatographic system coupled via electrospray source to a hybrid quadrupole-Orbitrap mass spectrometer is presented. The columns tested were the following: one column Luna Omega polar C 18 , one column Kinetex Biphenyl, one column Kinetex core-shell XB-C 18 , two columns Kinetex core-shell XB-C 18 . After a previous optimization of the extraction method, cauliflower extracts were analyzed testing four different mobile phases onto the four columns for a total of sixteen different chromatographic conditions. The chromatographic systems were evaluated based on the number of detected and tentatively identified GLSs. Luna Polar stationary phase resulted to be the most suitable for the analysis of GLSs compared to Kinetex XB and Kinetex Biphenyl columns stationary phase. However, two in series Kinetex XB columns increased the number of tentatively identified GLSs compared to one Kinetex XB, showing the importance of column length in the analysis of complex mixtures. The data obtained with the best chromatographic system were deeply analyzed by MS/MS investigation for the final identification. Fiflty-one GLSs were tentatively identified, 24 of which have never been identified in cauliflower. Finally the linearity of the analytes response over the analyzed range of concentration was checked, suggesting that the developed method is suitable for both qualitative and quantitative analysis of GLSs in phytochemical mixtures. Copyright © 2017 Elsevier B.V. All rights reserved.

Factorial-design optimization of gas chromatographic analysis of tetrabrominated to decabrominated diphenyl ethers. Application to domestic dust.

PubMed

Regueiro, Jorge; Llompart, Maria; Garcia-Jares, Carmen; Cela, Rafael

2007-07-01

Gas chromatographic analysis of polybrominated diphenyl ethers (PBDEs) has been evaluated in an attempt to achieve better control of the separation process, especially for highly substituted congeners. Use of a narrow-bore capillary column enabled adequate determination of tetra, penta, hexa, hepta, octa, nona and decaBDE congeners in only one chromatographic run while maintaining resolution power similar to that of conventional columns. A micro electron-capture detector (GC-microECD) was used. Chromatographic conditions were optimized by multifactorial experimental design, with the objective of obtaining not only high sensitivity but also good precision. In this way two different approaches to maximizing response and minimizing variability were tested, and are fully discussed. These optimum chromatographic conditions were then used to determine PBDEs extracted from domestic dust samples by microwave-assisted solvent extraction (MASE). Quantitative recovery (90-108%) was achieved for all the PBDEs and method precision (RSD < 13%) was satisfactory. Accuracy was tested by use of the standard reference material SRM 2585, and sub-ng g(-1) limits of detection were obtained for all compounds except BDE-209 (1.44 ng g(-1)). Finally, several samples of house dust were analysed by use of the proposed method and all the target PBDEs were detected in all the samples. BDE-209 was the predominant congener. Amounts varied from 58 to 1615 ng g(-1) and the average contribution to the total PBDE burden of 52%. The main congeners of the octaBDE mixture (BDE-183, BDE-197, BDE-207 and BDE-196) also made an important contribution (29%) to the total. These are the first data about the presence of these compounds in European house-dust samples. Finally, the sum of the main congeners in the pentaBDE commercial mixture (BDE-47, BDE-99, and BDE-100) contributed 14% to the total. Figure Polybrominated diphenyl ethers in House Dust.

Human and Methodological Sources of Variability in the Measurement of Urinary 8-Oxo-7,8-dihydro-2′-deoxyguanosine

PubMed Central

Møller, Peter; Henriksen, Trine; Mistry, Vilas; Koppen, Gudrun; Rossner, Pavel; Sram, Radim J.; Weimann, Allan; Poulsen, Henrik E.; Nataf, Robert; Andreoli, Roberta; Manini, Paola; Marczylo, Tim; Lam, Patricia; Evans, Mark D.; Kasai, Hiroshi; Kawai, Kazuaki; Li, Yun-Shan; Sakai, Kazuo; Singh, Rajinder; Teichert, Friederike; Farmer, Peter B.; Rozalski, Rafal; Gackowski, Daniel; Siomek, Agnieszka; Saez, Guillermo T.; Cerda, Concha; Broberg, Karin; Lindh, Christian; Hossain, Mohammad Bakhtiar; Haghdoost, Siamak; Hu, Chiung-Wen; Chao, Mu-Rong; Wu, Kuen-Yuh; Orhan, Hilmi; Senduran, Nilufer; Smith, Raymond J.; Santella, Regina M.; Su, Yali; Cortez, Czarina; Yeh, Susan; Olinski, Ryszard; Loft, Steffen

2013-01-01

Abstract Aims: Urinary 8-oxo-7,8-dihydro-2′-deoxyguanosine (8-oxodG) is a widely used biomarker of oxidative stress. However, variability between chromatographic and ELISA methods hampers interpretation of data, and this variability may increase should urine composition differ between individuals, leading to assay interference. Furthermore, optimal urine sampling conditions are not well defined. We performed inter-laboratory comparisons of 8-oxodG measurement between mass spectrometric-, electrochemical- and ELISA-based methods, using common within-technique calibrants to analyze 8-oxodG-spiked phosphate-buffered saline and urine samples. We also investigated human subject- and sample collection-related variables, as potential sources of variability. Results: Chromatographic assays showed high agreement across urines from different subjects, whereas ELISAs showed far more inter-laboratory variation and generally overestimated levels, compared to the chromatographic assays. Excretion rates in timed ‘spot’ samples showed strong correlations with 24 h excretion (the ‘gold’ standard) of urinary 8-oxodG (rp 0.67–0.90), although the associations were weaker for 8-oxodG adjusted for creatinine or specific gravity (SG). The within-individual excretion of 8-oxodG varied only moderately between days (CV 17% for 24 h excretion and 20% for first void, creatinine-corrected samples). Innovation: This is the first comprehensive study of both human and methodological factors influencing 8-oxodG measurement, providing key information for future studies with this important biomarker. Conclusion: ELISA variability is greater than chromatographic assay variability, and cannot determine absolute levels of 8-oxodG. Use of standardized calibrants greatly improves intra-technique agreement and, for the chromatographic assays, importantly allows integration of results for pooled analyses. If 24 h samples are not feasible, creatinine- or SG-adjusted first morning samples are recommended. Antioxid. Redox Signal. 18, 2377–2391. PMID:23198723

High-pressure liquid chromatographic analysis of pramoxine hydrochloride in high lipoid aerosol foam dosage form.

PubMed

Weinberger, R; Mann, B; Posluszny, J

1980-04-01

A rapid and quantitative method for the determination of pramoxine hydrochloride by high-pressure liquid chromatography is presented. The drug is extracted as the salt from a preparation with a high lipoid composition by partitioning it to the aqueous phase of an ether-methanol-water-acetic acid system. The extract is chromatographed on an octadecylsilane bonded packing with a methanol-water-acetic acid-methanesulfonic acid mobile phase. The time required for each separation is approximately 6 min. Analytical recoveries of 100.4 +/- 1.5% were obtained.

High-performance liquid chromatographic characterization of some medical plant extracts used in cosmetic formulas.

PubMed

Schulz, H; Albroscheit, G

1988-06-17

Rapid and reliable methods are presented for the characterization of biologically active and/or characteristic constituents in aqueous extracts of Hamamelis virginiana, Matricaria chamomilla, Achillea millefolium, Thymus vulgaris, Althaea officinalis and Cinchonia spp. Prior to high-performance liquid chromatographic (HPLC) separation a clean-up step was performed using a solid-phase extraction system. The purified extracts were analysed by HPLC coupled with a diode-array detector and a fluorescence detector. In some instances, previously unreported components of the aqueous plant extracts were found.

Principal coordinate analysis assisted chromatographic analysis of bacterial cell wall collection: A robust classification approach.

PubMed

Kumar, Keshav; Cava, Felipe

2018-04-10

In the present work, Principal coordinate analysis (PCoA) is introduced to develop a robust model to classify the chromatographic data sets of peptidoglycan sample. PcoA captures the heterogeneity present in the data sets by using the dissimilarity matrix as input. Thus, in principle, it can even capture the subtle differences in the bacterial peptidoglycan composition and can provide a more robust and fast approach for classifying the bacterial collection and identifying the novel cell wall targets for further biological and clinical studies. The utility of the proposed approach is successfully demonstrated by analysing the two different kind of bacterial collections. The first set comprised of peptidoglycan sample belonging to different subclasses of Alphaproteobacteria. Whereas, the second set that is relatively more intricate for the chemometric analysis consist of different wild type Vibrio Cholerae and its mutants having subtle differences in their peptidoglycan composition. The present work clearly proposes a useful approach that can classify the chromatographic data sets of chromatographic peptidoglycan samples having subtle differences. Furthermore, present work clearly suggest that PCoA can be a method of choice in any data analysis workflow. Copyright © 2018 Elsevier Inc. All rights reserved.

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

PubMed

Plenis, Alina; Chmielewska, Aleksandra; Konieczna, Lucyna; Lamparczyk, Henryk

2007-09-01

A rapid and sensitive reversed-phase high-performance liquid chromatographic method (RP-HPLC) with ultraviolet detection has been developed for the determination of moclobemide and its metabolites, p-chloro-N-(-2-morpholinoethyl)benzamide N'-oxide (Ro 12-5637) and p-chloro-N-[2-(3-oxomorpholino)ethyl]-benzamide (Ro 12-8095), in human plasma. The assay was performed after single liquid-liquid extraction with dichloromethane at alkaline pH using phenacetin as the internal standard. Chromatographic separation was performed on a C(18) column using a mixture of acetonitrile and water (25:75, v/v), adjusted to pH 2.7 with ortho-phosphoric acid, as mobile phase. Spectrophotometric detection was performed at 239 nm. The method has been validated for accuracy, precision, selectivity, linearity, recovery and stability. The quantification limit for moclobemide and Ro 12-8095 was 10 ng/mL, and for Ro 12-5637 was 30 ng/mL. Linearity of the method was confirmed for the range 20-2500 ng/mL for moclobemide (r = 0.9998), 20-1750 ng/mL for Ro 12-8095 (r = 0.9996) and 30-350 ng/mL for Ro 12-5637 (r = 0.9991). Moreover, within-day and between-day precisions and accuracies of the method were established. The described method was successfully applied in pharmacokinetic studies of parent drug and its two metabolites after a single oral administration of 150 mg of moclobemide to 20 healthy volunteers. Copyright (c) 2007 John Wiley & Sons, Ltd.

A Review of Multidimensional, Multifluid Intermediate-scale Experiments: Flow Behavior, Saturation Imaging, and Tracer Detection and Quantification

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

Oostrom, Mart; Dane, J. H.; Wietsma, Thomas W.

2007-08-01

A review is presented of original multidimensional, intermediate-scale experiments involving non-aqueous phase liquid (NAPL) flow behavior, imaging, and detection/quantification with solute tracers. In a companion paper (Oostrom, M., J.H. Dane, and T.W. Wietsma. 2006. A review of multidimensional, multifluid intermediate-scale experiments: Nonaqueous phase dissolution and enhanced remediation. Vadose Zone Journal 5:570-598) experiments related to aqueous dissolution and enhanced remediation were discussed. The experiments investigating flow behavior include infiltration and redistribution experiments with both light and dense NAPLs in homogeneous and heterogeneous porous medium systems. The techniques used for NAPL saturation mapping for intermediate-scale experiments include photon-attenuation methods such as gammamore » and X-ray techniques, and photographic methods such as the light reflection, light transmission, and multispectral image analysis techniques. Solute tracer methods used for detection and quantification of NAPL in the subsurface are primarily limited to variations of techniques comparing the behavior of conservative and partitioning tracers. Besides a discussion of the experimental efforts, recommendations for future research at this laboratory scale are provided.« less

Monte Carlo methods for multidimensional integration for European option pricing

NASA Astrophysics Data System (ADS)

Todorov, V.; Dimov, I. T.

2016-10-01

In this paper, we illustrate examples of highly accurate Monte Carlo and quasi-Monte Carlo methods for multiple integrals related to the evaluation of European style options. The idea is that the value of the option is formulated in terms of the expectation of some random variable; then the average of independent samples of this random variable is used to estimate the value of the option. First we obtain an integral representation for the value of the option using the risk neutral valuation formula. Then with an appropriations change of the constants we obtain a multidimensional integral over the unit hypercube of the corresponding dimensionality. Then we compare a specific type of lattice rules over one of the best low discrepancy sequence of Sobol for numerical integration. Quasi-Monte Carlo methods are compared with Adaptive and Crude Monte Carlo techniques for solving the problem. The four approaches are completely different thus it is a question of interest to know which one of them outperforms the other for evaluation multidimensional integrals in finance. Some of the advantages and disadvantages of the developed algorithms are discussed.

Quantitative analysis of matrine in liquid crystalline nanoparticles by HPLC.

PubMed

Peng, Xinsheng; Li, Baohong; Hu, Min; Ling, Yahao; Tian, Yuan; Zhou, Yanxing; Zhou, Yanfang

2014-01-01

A reversed-phase high-performance liquid chromatographic method has been developed to quantitatively determine matrine in liquid crystal nanoparticles. The chromatographic method is carried out using an isocratic system. The mobile phase was composed of methanol-PBS(pH6.8)-triethylamine (50 : 50 : 0.1%) with a flow rate of 1 mL/min with SPD-20A UV/vis detector and the detection wavelength was at 220 nm. The linearity of matrine is in the range of 1.6 to 200.0  μ g/mL. The regression equation is y = 10706x - 2959 (R (2) = 1.0). The average recovery is 101.7%; RSD = 2.22%  (n = 9). This method provides a simple and accurate strategy to determine matrine in liquid crystalline nanoparticle.

Method for digesting spent ion exchange resins and recovering actinides therefrom using microwave radiation

DOEpatents

Maxwell, III, Sherrod L.; Nichols, Sheldon T.

1999-01-01

The present invention relates to methods for digesting diphosphonic acid substituted cation exchange resins that have become loaded with actinides, rare earth metals, or heavy metals, in a way that allows for downstream chromatographic analysis of the adsorbed species without damage to or inadequate elution from the downstream chromatographic resins. The methods of the present invention involve contacting the loaded diphosphonic acid resin with concentrated oxidizing acid in a closed vessel, and irradiating this mixture with microwave radiation. This efficiently increases the temperature of the mixture to a level suitable for digestion of the resin without the use of dehydrating acids that can damage downstream analytical resins. In order to ensure more complete digestion, the irradiated mixture can be mixed with hydrogen peroxide or other oxidant, and reirradiated with microwave radiation.

Adsorption behavior of plasmid DNA onto perfusion chromatographic matrix.

PubMed

Limonta, Miladys; Zumalacárregui, Lourdes; Soler, Dayana

2012-05-01

Anion exchange chromatography is the most popular chromatographic method for plasmid separation. POROS RI 50 is a perfusion chromatographic support which is a reversed phase matrix and is an alternative to conventional ones due to its mass transfer properties. The adsorption and elution of the pIDKE2 plasmid onto reversed phase POROS R1 50 was studied. Langmuir isotherm model was adjusted in order to get the maximum adsorption capacity and the dissociation constant for POROS R1 50-plasmid DNA (pDNA) system. Breakthrough curves were obtained for volumetric flows between 0.69-3.33 mL/min, given dynamic capacity up to 2.3 times higher than those reported for ionic exchange matrix used during the purification process of plasmids with similar size to that of pIDKE2. The efficiency was less than 45% for the flow conditions and initial concentration studied, which means that the support will not be operated under saturation circumstances.

Liquid chromatographic determination of benzo(a)pyrene in total particulate matter of cigarette smoke

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

Tomkins, B.A.; Jenkins, R.A.; Griest, W.H.

The benzo(a)pyrene (BaP) delivery of reference and commercially available tobacco cigarettes, as well as reference and placebo marijuana cigarettes, is determined using a sequential liquid chromatographic/liquid chromatographic procedure. The total particulate matter of sample cigarette smoke is collected using a Cambridge filter pad, which is ultrasonically extracted with acetone. The resulting extract is filtered, then fractionated using semipreparative-scale normal phase liquid chromatography (LC). Quantitative determination is achieved using analytical-scale reverse phase LC equipped with a fluorescence detector. The method is precise (+/- 10-15% relative standard deviation) and yields 85% or better BaP recovery at the ng/cig. level. A single padmore » may be analyzed in 8 person-hours, while a more typical lot of 12 pads (6 pads each for 2 cigarette brands) may be analyzed in 10 person-days.« less

Influence of Multidimensionality on Convergence of Sampling in Protein Simulation

NASA Astrophysics Data System (ADS)

Metsugi, Shoichi

2005-06-01

We study the problem of convergence of sampling in protein simulation originating in the multidimensionality of protein’s conformational space. Since several important physical quantities are given by second moments of dynamical variables, we attempt to obtain the time of simulation necessary for their sufficient convergence. We perform a molecular dynamics simulation of a protein and the subsequent principal component (PC) analysis as a function of simulation time T. As T increases, PC vectors with smaller amplitude of variations are identified and their amplitudes are equilibrated before identifying and equilibrating vectors with larger amplitude of variations. This sequential identification and equilibration mechanism makes protein simulation a useful method although it has an intrinsic multidimensional nature.

Microfluidic thread based electroanalytical system for green chromatographic separations.

PubMed

Agustini, Deonir; Fedalto, Lucas; Bergamini, Márcio F; Marcolino-Junior, Luiz Humberto

2018-02-13

The use of miniaturized chromatographic systems is an important strategy for reducing the consumption of supplies related to separations, allowing the development of more sustainable analytical methodologies. However, the high cost and complexity in the production of these systems combined with the operational difficulties and the need for the use of solvent and sample pretreatment are challenges to be overcome in order to make the chromatographic methods greener. Here, we report the construction and development of a low cost microfluidic system for green and solvent-free chromatographic separations with electrochemical detection integrated into cotton threads without the use of any mechanical pumping to transport the solutions. The manufacture of the proposed system was performed by simple assembly of the components, with the separation of the species based on an ion exchange mechanism and detection using gold electrodes manufactured directly on the cotton threads. A linear range of 0.025-5.0 mM was obtained for the effective separation of ascorbic acid (AA) and dopamine (DA) with detection limits of 2.89 μM (for AA) and 4.41 μM (for DA). Each analysis was performed at a low cost (less than 0.01 dollars), and with a small volume of waste generated (107.1 μL). So, the proposed system was successfully employed to determine the levels of AA and DA present in the tears of healthy volunteers without sample pretreatment, indicating the good analytical performance of the system and the possibility of performing greener chromatographic separations.

Fingerprint of Hedyotis diffusa Willd. by HPLC-MS.

PubMed

Yang, Ting; Yang, Yi-Hua; Yang, Ju-Yun; Chen, Ben-Mei; Duan, Ju-Ping; Yu, Shu-Yi; Ouyang, Hong-Tao; Cheng, Jun-Ping; Chen, Yu-Xiang

2008-01-01

A HPLC-MS fingerprint method has been developed based on the consistent chromatographic features of the major chemical constituents among 10 batches of Hedyotis diffusa Willd. Chromatographic separation was conducted on a Hypersil-Keystone Hypurity C(18) column using methanol:water:acetic acid as the mobile phase. Major compounds, including oleanolic acid, ursolic acid and ferulic acid, were analysed by HPLC-MS. Their analysis was ascertained by comparison with data derived from the standard compounds. The HPLC-MS fingerprint was successfully applied to analyse and differentiate samples from different geographical origins, or processing methods. H. diffusa was well distinguished from Hedyotis chrysotricha by HPLC-MS. Therefore the establishment of fingerprint of H. diffusa is critical in assessing and controlling its overall quality.

Static headspace gas chromatographic method for quantitative determination of residual solvents in pharmaceutical drug substances according to european pharmacopoeia requirements.

PubMed

Otero, Raquel; Carrera, Guillem; Dulsat, Joan Francesc; Fábregas, José Luís; Claramunt, Juan

2004-11-19

A static headspace (HS) gas chromatographic method for quantitative determination of residual solvents in a drug substance has been developed according to European Pharmacopoeia general procedure. A water-dimethylformamide mixture is proposed as sample solvent to obtain good sensitivity and recovery. The standard addition technique with internal standard quantitation was used for ethanol, tetrahydrofuran and toluene determination. Validation was performed within the requirements of ICH validation guidelines Q2A and Q2B. Selectivity was tested for 36 solvents, and system suitability requirements described in the European Pharmacopoeia were checked. Limits of detection and quantitation, precision, linearity, accuracy, intermediate precision and robustness were determined, and excellent results were obtained.

Quantification of urinary uric acid in the presence of thymol and thimerosal by high-performance liquid chromatography

NASA Technical Reports Server (NTRS)

Chen, Y.; Pietrzyk, R. A.; Whitson, P. A.

1997-01-01

A high-performance liquid chromatographic method was developed as an alternative to automated enzymatic analysis of uric acid in human urine preserved with thymol and/or thimerosal. Uric acid (tR = 10 min) and creatinine (tR = 5 min) were separated and quantified during isocratic elution (0.025 M acetate buffer, pH 4.5) from a mu Bondapak C18 column. The uric-acid peak was identified chemically by incubating urine samples with uricase. The thymol/thimerosal peak appeared at 31 min during the washing step and did not interfere with the analysis. We validated the high-performance liquid chromatographic method for linearity, precision and accuracy, and the results were found to be excellent.

COMPARISON OF METHODS TO DETERMINE OXYGEN DEMAND FOR BIOREMEDIATION OF A FUEL CONTAMINATED AQUIFER

EPA Science Inventory

Four analytical methods were compared for estimating concentrations of fuel contaminants in subsurface core samples. The methods were total organic carbon, chemical oxygen demand, oil and grease, and a solvent extraction of fuel hydrocarbons combined with a gas chromatographic te...

Efficient implementation of multidimensional fast fourier transform on a distributed-memory parallel multi-node computer

DOEpatents

Bhanot, Gyan V [Princeton, NJ; Chen, Dong [Croton-On-Hudson, NY; Gara, Alan G [Mount Kisco, NY; Giampapa, Mark E [Irvington, NY; Heidelberger, Philip [Cortlandt Manor, NY; Steinmacher-Burow, Burkhard D [Mount Kisco, NY; Vranas, Pavlos M [Bedford Hills, NY

2012-01-10

The present in invention is directed to a method, system and program storage device for efficiently implementing a multidimensional Fast Fourier Transform (FFT) of a multidimensional array comprising a plurality of elements initially distributed in a multi-node computer system comprising a plurality of nodes in communication over a network, comprising: distributing the plurality of elements of the array in a first dimension across the plurality of nodes of the computer system over the network to facilitate a first one-dimensional FFT; performing the first one-dimensional FFT on the elements of the array distributed at each node in the first dimension; re-distributing the one-dimensional FFT-transformed elements at each node in a second dimension via "all-to-all" distribution in random order across other nodes of the computer system over the network; and performing a second one-dimensional FFT on elements of the array re-distributed at each node in the second dimension, wherein the random order facilitates efficient utilization of the network thereby efficiently implementing the multidimensional FFT. The "all-to-all" re-distribution of array elements is further efficiently implemented in applications other than the multidimensional FFT on the distributed-memory parallel supercomputer.

Efficient implementation of a multidimensional fast fourier transform on a distributed-memory parallel multi-node computer

DOEpatents

Bhanot, Gyan V [Princeton, NJ; Chen, Dong [Croton-On-Hudson, NY; Gara, Alan G [Mount Kisco, NY; Giampapa, Mark E [Irvington, NY; Heidelberger, Philip [Cortlandt Manor, NY; Steinmacher-Burow, Burkhard D [Mount Kisco, NY; Vranas, Pavlos M [Bedford Hills, NY

2008-01-01

The present in invention is directed to a method, system and program storage device for efficiently implementing a multidimensional Fast Fourier Transform (FFT) of a multidimensional array comprising a plurality of elements initially distributed in a multi-node computer system comprising a plurality of nodes in communication over a network, comprising: distributing the plurality of elements of the array in a first dimension across the plurality of nodes of the computer system over the network to facilitate a first one-dimensional FFT; performing the first one-dimensional FFT on the elements of the array distributed at each node in the first dimension; re-distributing the one-dimensional FFT-transformed elements at each node in a second dimension via "all-to-all" distribution in random order across other nodes of the computer system over the network; and performing a second one-dimensional FFT on elements of the array re-distributed at each node in the second dimension, wherein the random order facilitates efficient utilization of the network thereby efficiently implementing the multidimensional FFT. The "all-to-all" re-distribution of array elements is further efficiently implemented in applications other than the multidimensional FFT on the distributed-memory parallel supercomputer.

Application of the method of steepest descent to laminated shield weight optimization with several constraints: Theory

NASA Technical Reports Server (NTRS)

Lahti, G. P.

1971-01-01

The method of steepest descent used in optimizing one-dimensional layered radiation shields is extended to multidimensional, multiconstraint situations. The multidimensional optimization algorithm and equations are developed for the case of a dose constraint in any one direction being dependent only on the shield thicknesses in that direction and independent of shield thicknesses in other directions. Expressions are derived for one-, two-, and three-dimensional cases (one, two, and three constraints). The precedure is applicable to the optimization of shields where there are different dose constraints and layering arrangements in the principal directions.

Detection of explosives in soils

DOEpatents

Chambers, William B.; Rodacy, Philip J.; Phelan, James M.; Woodfin, Ronald L.

2002-01-01

An apparatus and method for detecting explosive-indicating compounds in subsurface soil. The apparatus has a probe with an adsorbent material on some portion of its surface that can be placed into soil beneath the ground surface, where the adsorbent material can adsorb at least one explosive-indicating compound. The apparatus additional has the capability to desorb the explosive-indicating compound through heating or solvent extraction. A diagnostic instrument attached to the probe detects the desorbed explosive-indicating compound. In the method for detecting explosive-indicating compounds in soil, the sampling probe with an adsorbent material on at least some portion of a surface of the sampling probe is inserted into the soil to contact the adsorbent material with the soil. The explosive-indicating compounds are then desorbed and transferred as either a liquid or gas sample to a diagnostic tool for analysis. The resulting gas or liquid sample is analyzed using at least one diagnostic tool selected from the group consisting of an ion-mobility spectrometer, a gas chromatograph, a high performance liquid chromatograph, a capillary electrophoresis chromatograph, a mass spectrometer, a Fourier-transform infrared spectrometer and a Raman spectrometer to detect the presence of explosive-indicating compounds.

Headspace solid-phase microextraction and gas chromatographic analysis of low-molecular-weight sulfur volatiles with pulsed flame photometric detection and quantification by a stable isotope dilution assay.

PubMed

Ullrich, Sebastian; Neef, Sylvia K; Schmarr, Hans-Georg

2018-02-01

Low-molecular-weight volatile sulfur compounds such as thiols, sulfides, disulfides as well as thioacetates cause a sulfidic off-flavor in wines even at low concentration levels. The proposed analytical method for quantification of these compounds in wine is based on headspace solid-phase microextraction, followed by gas chromatographic analysis with sulfur-specific detection using a pulsed flame photometric detector. Robust quantification was achieved via a stable isotope dilution assay using commercial and synthesized deuterated isotopic standards. The necessary chromatographic separation of analytes and isotopic standards benefits from the inverse isotope effect realized on an apolar polydimethylsiloxane stationary phase of increased film thickness. Interferences with sulfur-specific detection in wine caused by sulfur dioxide were minimized by addition of propanal. The method provides adequate validation data, with good repeatability and limits of detection and quantification. It suits the requirements of wine quality management, allowing the control of oenological treatments to counteract an eventual formation of excessively high concentration of such malodorous compounds. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Studies on Chromatographic Fingerprint and Fingerprinting Profile-Efficacy Relationship of Polygoni Perfoliati Herba

PubMed Central

Tian, Li; Chen, Hua-Guo; Zhao, Chao; Gong, Xiao-Jian

2013-01-01

Polygoni Perfoliati Herba is widely used in China with antibacterium, anti-inflammatory, expectorant, antitumor, and antivirus activities. To reveal the mechanisms of the activities of Polygoni Perfoliati Herba, the relationship between the fingerprinting profile and its bioactivities was investigated. In the present study, high-performance liquid chromatographic (HPLC) fingerprinting method was developed. The established method was applied to analyze 51 batches of Polygoni Perfoliati Herba samples collected from different locations or in different harvesting times in China. Chemometrics, including similarity analysis, hierarchical clustering analysis, and principal component analysis, were used to express their similarities. It was found that similarity values of the samples were in the range of 0.432–0.998. The results of analgesic tests indicated that Polygoni Perfoliati Herba could significantly inhibit pain induced by hot plate and acetic acid in mice. The results of anti-inflammatory tests showed that Polygoni Perfoliati Herba had good anti-inflammatory effects (P < 0.01) in two models including dimethyl benzene-induced ear edema and acetic acid-induced peritoneal permeability in mice. Combining the results from chromatographic fingerprints with those from bioactivities, we found that seven peaks from Polygoni Perfoliati Herba were mainly responsible for analgesic and anti-inflammatory activities. PMID:24023580

Protein Stable Isotope Fingerprinting (P-SIF): Multidimensional Protein Chromatography Coupled to Stable Isotope-Ratio Mass Spectrometry

NASA Astrophysics Data System (ADS)

Pearson, A.; Bovee, R. J.; Mohr, W.; Tang, T.

2012-12-01

As metagenomics increases our insight into microbial community diversity and metabolic potential, new approaches are required to determine the biogeochemical expression of this potential within ecosystems. Because stable isotopic analysis of the major bioactive elements (C, N) has been used historically to map flows of substrates and energy among macroscopic food webs, similar principles may apply to microbes. To address this challenge, we have developed a new analytical approach called Protein Stable Isotope Fingerprinting (P-SIF). P-SIF generates natural stable isotopic fingerprints of microbial individual or community proteomes. The main advantage of P-SIF is the potential to bridge the gap between diversity and function, thereby providing a window into the "black box" of environmental microbiology and helping to decipher the roles of uncultivated species. Our method implements a three-way, orthogonal scheme to separate mixtures of whole proteins into subfractions dominated by single or closely-related proteins. Protein extracts first are isoelectrically focused in a gel-free technique that yields 12 fractions separated over a gradient of pH 3-10. Each fraction then is separated by size-exclusion chromatography into 20 pools, ranging from >100kD to ~10kD. Finally, each of these pools is subjected to HPLC and collected in 40 time-slices based on protein hydrophobicity. Theoretical calculation reveals that the true chromatographic resolution of the total scheme is 5000, somewhat less than the 9600 resulting fractions. High-yielding fractions are subjected to δ13C analysis by spooling-wire microcombustion irMS (SWiM-irMS) optimized for samples containing 1-5 nmol carbon. Here we will present the method, results for a variety of pure cultures, and preliminary data for a sample of mixed environmental proteins. The data show the promise of this method for unraveling the metabolic complexity hidden within microbial communities.

A New Computational Method to Fit the Weighted Euclidean Distance Model.

ERIC Educational Resources Information Center

De Leeuw, Jan; Pruzansky, Sandra

1978-01-01

A computational method for weighted euclidean distance scaling (a method of multidimensional scaling) which combines aspects of an "analytic" solution with an approach using loss functions is presented. (Author/JKS)

A comparative study of Conroy and Monte Carlo methods applied to multiple quadratures and multiple scattering

NASA Technical Reports Server (NTRS)

Deepak, A.; Fluellen, A.

1978-01-01

An efficient numerical method of multiple quadratures, the Conroy method, is applied to the problem of computing multiple scattering contributions in the radiative transfer through realistic planetary atmospheres. A brief error analysis of the method is given and comparisons are drawn with the more familiar Monte Carlo method. Both methods are stochastic problem-solving models of a physical or mathematical process and utilize the sampling scheme for points distributed over a definite region. In the Monte Carlo scheme the sample points are distributed randomly over the integration region. In the Conroy method, the sample points are distributed systematically, such that the point distribution forms a unique, closed, symmetrical pattern which effectively fills the region of the multidimensional integration. The methods are illustrated by two simple examples: one, of multidimensional integration involving two independent variables, and the other, of computing the second order scattering contribution to the sky radiance.

On-line solid-phase extraction coupled to liquid chromatography tandem mass spectrometry for the analysis of cyanotoxins in algal blooms.

PubMed

Fayad, Paul B; Roy-Lachapelle, Audrey; Duy, Sung Vo; Prévost, Michèle; Sauvé, Sébastien

2015-12-15

An analytical method based on on-line SPE-LC-HESI-MS/MS has been developed for the detection and quantification of eight selected cyanotoxins in algal bloom waters that include mycrocystins, anatoxin-a and cylindrospermopsin. The injection volume was 2 mL according to the expected concentration of cyanotoxins in matrix. The method provides an analysis time of 7 min per sample, acceptable recovery values (91-101%), good precision (RSD < 13%) and method limits of detection at the sub-microgram per liter levels (0.01-0.02 μg L(-1)). A detailed discussion on optimization parameters that have an impact on the overall performance of the method are presented. In particular, method optimization permitted the chromatographic separation of anatoxin-a and phenylalanine, an isobaric interference with a similar chromatographic characteristics. All optimization and validation experiments for the on-line SPE method and chromatographic separation were performed in environmentally relevant algal bloom water matrices. The applicability of the method was tested on several algal bloom water samples from monitored lakes across the province of Québec (Québec, Canada) known to produce cyanotoxins. All of the targeted cyanotoxins were detected with the exception of cylindrospermopsin. In addition, it was found that total microcystin concentrations in several surface water samples exceeded the proposed guidelines established by the province of Québec in Canada of 1.5 μg L(-1) as well as the World Health Organization of 1 μg L(-1) for both free and cell-bound microcystin-LR equivalent. Copyright © 2015 Elsevier Ltd. All rights reserved.

Analysis of imazaquin in soybeans by solid-phase extraction and high-performance liquid chromatography.

PubMed

Guo, C; Hu, J-Y; Chen, X-Y; Li, J-Z

2008-02-01

An analytical method for the determination imazaquin residues in soybeans was developed. The developed liquid/liquid partition and strong anion exchange solid-phase extraction procedures provide the effective cleanup, removing the greatest number of sample matrix interferences. By optimizing mobile-phase pH water/acetonitrile conditions with phosphoric acid, using a C-18 reverse-phase chromatographic column and employing ultraviolet detection, excellent peak resolution was achieved. The combined cleanup and chromatographic method steps reported herein were sensitive and reliable for determining the imazaquin residues in soybean samples. This method is characterized by recovery >88.4%, precision <6.7% CV, and sensitivity of 0.005 ppm, in agreement with directives for method validation in residue analysis. Imazaquin residues in soybeans were further confirmed by high performance liquid chromatography-mass spectrometry (LC-MS). The proposed method was successfully applied to the analysis of imazaquin residues in soybean samples grown in an experimental field after treatments of imazaquin formulation.

A high-throughput headspace gas chromatographic technique for the determination of nitrite content in water samples.

PubMed

Zhang, Shu-Xin; Peng, Rong; Jiang, Ran; Chai, Xin-Sheng; Barnes, Donald G

2018-02-23

This paper reports on a high-throughput headspace gas chromatographic method (HS-GC) for the determination of nitrite content in water sample, based on GC measurement of cyclohexene produced from the reaction between nitrite and cyclamate in a closed vial. The method has a relative standard deviation of <3.5%; The differences between the results of the nitrite measurements obtained by this method and those of a reference method were less than 5.8% and the recoveries of the method were in the range of 94.8-102% (for a spiked nitrite content range from 0.002 to 0.03 mg/L). The limit of detection of the method was 0.46 μg L -1 . Due to an overlapping mode in the headspace auto-sampler system, the method can provide an automated and high-throughput nitrite analysis for the surface water samples. In short, the present HS-GC method is simple, accurate, and sensitive, and it is very suitable to be used in the batch sample testing. Copyright © 2018 Elsevier B.V. All rights reserved.

Quantitative LC-MS of polymers: determining accurate molecular weight distributions by combined size exclusion chromatography and electrospray mass spectrometry with maximum entropy data processing.

PubMed

Gruendling, Till; Guilhaus, Michael; Barner-Kowollik, Christopher

2008-09-15

We report on the successful application of size exclusion chromatography (SEC) combined with electrospray ionization mass spectrometry (ESI-MS) and refractive index (RI) detection for the determination of accurate molecular weight distributions of synthetic polymers, corrected for chromatographic band broadening. The presented method makes use of the ability of ESI-MS to accurately depict the peak profiles and retention volumes of individual oligomers eluting from the SEC column, whereas quantitative information on the absolute concentration of oligomers is obtained from the RI-detector only. A sophisticated computational algorithm based on the maximum entropy principle is used to process the data gained by both detectors, yielding an accurate molecular weight distribution, corrected for chromatographic band broadening. Poly(methyl methacrylate) standards with molecular weights up to 10 kDa serve as model compounds. Molecular weight distributions (MWDs) obtained by the maximum entropy procedure are compared to MWDs, which were calculated by a conventional calibration of the SEC-retention time axis with peak retention data obtained from the mass spectrometer. Comparison showed that for the employed chromatographic system, distributions below 7 kDa were only weakly influenced by chromatographic band broadening. However, the maximum entropy algorithm could successfully correct the MWD of a 10 kDa standard for band broadening effects. Molecular weight averages were between 5 and 14% lower than the manufacturer stated data obtained by classical means of calibration. The presented method demonstrates a consistent approach for analyzing data obtained by coupling mass spectrometric detectors and concentration sensitive detectors to polymer liquid chromatography.

A validated chiral liquid chromatographic method for the enantiomeric separation of safinamide mesilate, a new anti-Parkinson drug.

PubMed

Zhang, Kai; Xue, Na; Shi, Xiaowei; Liu, Weina; Meng, Jing; Du, Yumin

2011-04-28

A enantioselective reversed-phase high performance liquid chromatographic method was developed for the enantiomeric resolution of safinamide mesilate, 2(S)-[4-(3-fluorobenzyloxy)benzylamino] propionamide methanesulfonate, a neuroprotectant with antiparkinsonian and anticonvulsant activity for the treatment of Parkinson disease. The enantiomers of safinamide mesilate were baseline resolved on a Chiralcel OD-RH (150mm×4.6mm, 5μm) column using a mobile phase system containing 300mM sodium di-hydrogen phosphate buffer (pH 3.0):methanol:acetonitrile (65:25:10, v/v/v). The resolution between the enantiomers was not less than 3.0. The pH value of buffer solution in the mobile phase has played a key role in enhancing chromatographic efficiency and resolution between the enantiomers. The developed method was validated and proved to be robust. The limit of detection and limit of quantification of (R)-enantiomer were found to be 15 and 50ng/mL, respectively, for 20μL injection volume. The percentage recovery of (R)-enantiomer was ranged from 94.2 to 103.7 in bulk drug samples of safinamide mesilate. The sample solution and mobile phase were found to be stable at least for 48h. The final optimized method was successfully applied to separate (R)-enantiomer from safinamide mesilate and was proven to be reproducible and accurate for the quantitative determination of (R)-enantiomer in bulk drugs. Copyright © 2010 Elsevier B.V. All rights reserved.

Detection of monohydroxylated polycyclic aromatic hydrocarbons in urine and particulate matter using LC separations coupled with integrated SPE and fluorescence detection or coupled with high-resolution time-of-flight mass spectrometry.

PubMed

Lintelmann, Jutta; Wu, Xiao; Kuhn, Evelyn; Ritter, Sebastian; Schmidt, Claudia; Zimmermann, Ralf

2018-05-01

A high-performance liquid chromatographic (HPLC) method with integrated solid-phase extraction for the determination of 1-hydroxypyrene and 1-, 2-, 3-, 4- and 9-hydroxyphenanthrene in urine was developed and validated. After enzymatic treatment and centrifugation of 500 μL urine, 100 μL of the sample was directly injected into the HPLC system. Integrated solid-phase extraction was performed on a selective, copper phthalocyanine modified packing material. Subsequent chromatographic separation was achieved on a pentafluorophenyl core-shell column using a methanol gradient. For quantification, time-programmed fluorescence detection was used. Matrix-dependent recoveries were between 94.8 and 102.4%, repeatability and reproducibility ranged from 2.2 to 17.9% and detection limits lay between 2.6 and 13.6 ng/L urine. A set of 16 samples from normally exposed adults was analyzed using this HPLC-fluorescence detection method. Results were comparable with those reported in other studies. The chromatographic separation of the method was transferred to an ultra-high-performance liquid chromatography pentafluorophenyl core-shell column and coupled to a high-resolution time-of-flight mass spectrometer (HR-TOF-MS). The resulting method was used to demonstrate the applicability of LC-HR-TOF-MS for simultaneous target and suspect screening of monohydroxylated polycyclic aromatic hydrocarbons in extracts of urine and particulate matter. Copyright © 2018 John Wiley & Sons, Ltd.

A versatile liquid chromatographic technique for pharmacokinetic estimation of curcumin in human plasma.

PubMed

Gugulothu, Dalapathi; Desai, Preshita; Patravale, Vandana

2014-09-01

A simple, rapid, sensitive and specific liquid chromatographic method was developed and validated for the determination of curcumin in human plasma. Berberine was used as the internal standard. Chromatographic separation was achieved on a Zorbax Eclipse C18 column at 40 °C, with a mobile phase consisting of 1% acetic acid (pH 3 adjusted with 50% triethanolamine): acetonitrile (55:45), at a flow rate of 1.25 mL/min. The method was validated for precision, accuracy, linearity, lower limit of quantification (LLOQ) and extraction efficiency according to the International Conference on Harmonization guidelines. The method was successfully developed with an LLOQ of 10 ng/mL and a runtime of 9 min. Linearity range was from 10 to 1000 ng/mL. Curcumin and Berberine were well separated with retention times of 8.2 ± 0.2 and 1.4 ± 0.1 min, respectively. Further, the method was successfully employed to study the pharmacokinetic parameters of curcumin, following oral administration of curcumin-loaded hydroxy propyl cellulose (HPC) nanoparticles and curcumin suspension in female Wistar rats. Curcumin-loaded HPC nanoparticles (Cmax: 106.01 ± 20.11 ng/mL) showed significant improvement in pharmacokinetic parameters when compared with curcumin suspension (Cmax: 30.13 ± 0.47 ng/mL) indicating 43.73-fold increase in relative bioavailability. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

A new high-performance thin-layer chromatographic method for determining bile salt hydrolase activity.

PubMed

Rohawi, Nur Syakila; Ramasamy, Kalavathy; Agatonovic-Kustrin, Snezana; Lim, Siong Meng

2018-06-05

A quantitative assay using high-performance thin-layer chromatography (HPTLC) was developed to investigate bile salt hydrolase (BSH) activity in Pediococcus pentosaceus LAB6 and Lactobacillus plantarum LAB12 probiotic bacteria isolated from Malaysian fermented food. Lactic acid bacteria (LAB) were cultured in de Man Rogosa and Sharpe (MRS) broth containing 1 mmol/L of sodium-based glyco- and tauro-conjugated bile salts for 24 h. The cultures were centrifuged and the resultant cell free supernatant was subjected to chromatographic separation on a HPTLC plate. Conjugated bile salts were quantified by densitometric scans at 550 nm and results were compared to digital image analysis of chromatographic plates after derivatisation with anisaldehyde/sulfuric acid. Standard curves for bile salts determination with both methods show good linearity with high coefficient of determination (R 2 ) between 0.97 and 0.99. Method validation indicates good sensitivity with low relative standard deviation (RSD) (<10%), low limits of detection (LOD) of 0.4 versus 0.2 μg and limit of quantification (LOQ) of 1.4 versus 0.7 μg, for densitometric vs digital image analysis method, respectively. The bile salt hydrolase activity was found to be higher against glyco- than tauro-conjugated bile salts (LAB6; 100% vs >38%: LAB12; 100% vs >75%). The present findings strongly show that quantitative analysis via digitally-enhanced HPTLC offers a rapid quantitative analysis for deconjugation of bile salts by probiotics. Copyright © 2018. Published by Elsevier B.V.

Development and validation of a high performance liquid chromatographic method for the separation of exo and endo isomers of granatamine (9-methyl-9-azabicyclo[3.3.1]nonan-3-amine); a key intermediate of granisetron.

PubMed

Krishna, S Radha; Babu, P Suresh; Rao, B M; Rao, N Someswara

2009-12-01

A simple and accurate high-performance liquid chromatographic method was developed for the determination of exo-9-methyl-9-azabicyclo[3.3.1]nonan-3-amine in endo-9-methyl-9-azabicyclo[3.3.1]nonan-3-amine, commercially known as grantamine and used as a key intermediate in the preparation of granisetron bulk drug. Chromatographic separation of the exo and endo isomers of 9-methyl-9-azabicyclo[3.3.1]nonan-3-amine was achieved on an Inertsil C8 column using a mobile phase containing 0.3% trifluoroacetic acid. The resolution between the two isomers was found to be more than 4. The limit of detection (LOD) and limit of quantification (LOQ) of exo isomer were 0.8 and 2.5 microg x mL(-1) respectively, for a 10 microL injection volume. The percentage recovery of exo-isomer ranged from 99 to 102% w/w in the endo-9-methyl-9-azabicyclo[3.3.1]nonan-3-amine sample. The test solution and mobile phase were observed to be stable up to 48 h after preparation. The validated method yielded good results for precision, linearity, accuracy, robustness and ruggedness. The proposed method was found to be suitable and accurate for the quantitative determination of exo-isomer in bulk samples of endo-9-methyl-9-azabicyclo[3.3.1]nonan-3-amine.

Comparison between micellar liquid chromatography and capillary zone electrophoresis for the determination of hydrophobic basic drugs in pharmaceutical preparations.

PubMed

Torres-Cartas, S; Martín-Biosca, Y; Sagrado, S; Villanueva-Camañas, R M; Medina-Hernández, M J

2007-01-01

The determination of highly hydrophobic basic compounds by means of conventional reversed-phase liquid chromatographic methods has several drawbacks. Owing to the characteristics of micellar liquid chromatography (MLC) and capillary electrophoresis (CE), these techniques could be advantageous alternatives to reversed-phase chromatographic methods for the determination of these kinds of compounds. The objective of this study was to develop and compare MLC and CE methods for the determination of antipsychotic basic drugs (amitryptiline, haloperidol, perphenazine and thioridazine) in pharmaceutical preparations. The chromatographic determination of the analytes was performed on a Kromasil C(18) analytical column; the mobile phase was 0.04 m cetyltrimethylammonium bromide (CTAB), at pH 3, containing 5% 1-butanol, at a flow rate of 1 mL/min. The CE separation was performed in a fused-silica capillary with a 50 mm tris-(hydroxymethyl)-aminomethane buffer, pH 7, at an applied voltage of 20 kV, using barbital as internal stardard. The proposed methods are suitable for a reliable quantitation of these compounds in the commercial tablets and drops in terms of accuracy and precision and require a very simple pre-treatment of the samples. By comparing the performance characteristics and experimental details of the MLC and CE methods we conclude that CE seems to be slightly better than MLC in the determination of highly hydrophobic compounds in pharmaceuticals in terms of resolution and economy, taking into account that the limits of detection are not a handicap in pharmaceutical samples. Copyright 2006 John Wiley & Sons, Ltd.

Simultaneous gas chromatographic determination of four toxic gases generally present in combustion atmospheres.

PubMed

Endecott, B R; Sanders, D C; Chaturvedi, A K

1996-01-01

The measurement of combustion gases produced by burning aircraft cabin materials poses a continuing limitation for smoke toxicity research. Because toxic effects of gases depend on both their concentrations and the duration of exposure, frequent atmosphere sampling is necessary to define the gas concentration-exposure time curve. A gas chromatographic (GC) method was developed for the simultaneous analyses of carbon monoxide (CO), hydrogen sulfide (H2S), sulfur dioxide (SO2), and hydrogen cyanide (HCN). The method used an MTI M200 dual-column gas chromatograph equipped with 4-m molecular sieve-5A and 8-m PoraPlot-U wall-coated capillary columns and two low-volume, high-sensitivity thermal conductivity detectors. Detectability (in parts per million [ppm]) and retention times (in seconds) for the gases were as follows: CO, 100 ppm, 28 s; H2S, 50 ppm, 26 s; SO2, 125 ppm, 76 s; and HCN, 60 ppm, 108 s. The method was effective for determining these gases in mixtures and in the combustion atmospheres generated by burning wool (CO, HCN, and H2S) and modacrylic fabrics (CO and HCN). Common atmospheric gaseous or combustion products (oxygen, carbon dioxide, nitrogen, water vapor, and other volatiles) did not interfere with the analyses. However, filtration of the combustion atmospheres was necessary to prevent restriction of the GC sampling inlet by smoke particulates. The speed, sensitivity, and selectivity of this method make it suitable for smoke toxicity research and for evaluating performance of passenger protective breathing equipment. Also, this method can potentially be modified to analyze these gases when they are liberated from biosamples.

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

PubMed

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

2007-01-01

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

Glyphosate analysis using sensors and electromigration separation techniques as alternatives to gas or liquid chromatography.

PubMed

Gauglitz, Günter; Wimmer, Benedikt; Melzer, Tanja; Huhn, Carolin

2018-01-01

Since its introduction in 1974, the herbicide glyphosate has experienced a tremendous increase in use, with about one million tons used annually today. This review focuses on sensors and electromigration separation techniques as alternatives to chromatographic methods for the analysis of glyphosate and its metabolite aminomethyl phosphonic acid. Even with the large number of studies published, glyphosate analysis remains challenging. With its polar and depending on pH even ionic functional groups lacking a chromophore, it is difficult to analyze with chromatographic techniques. Its analysis is mostly achieved after derivatization. Its purification from food and environmental samples inevitably results incoextraction of ionic matrix components, with a further impact on analysis derivatization. Its purification from food and environmental samples inevitably results in coextraction of ionic matrix components, with a further impact on analysis and also derivatization reactions. Its ability to form chelates with metal cations is another obstacle for precise quantification. Lastly, the low limits of detection required by legislation have to be met. These challenges preclude glyphosate from being analyzed together with many other pesticides in common multiresidue (chromatographic) methods. For better monitoring of glyphosate in environmental and food samples, further fast and robust methods are required. In this review, analytical methods are summarized and discussed from the perspective of biosensors and various formats of electromigration separation techniques, including modes such as capillary electrophoresis and micellar electrokinetic chromatography, combined with various detection techniques. These methods are critically discussed with regard to matrix tolerance, limits of detection reached, and selectivity.

Multi-dimensional construction of a novel active yolk@conductive shell nanofiber web as a self-standing anode for high-performance lithium-ion batteries

NASA Astrophysics Data System (ADS)

Liu, Hao; Chen, Luyi; Liang, Yeru; Fu, Ruowen; Wu, Dingcai

2015-11-01

A novel active yolk@conductive shell nanofiber web with a unique synergistic advantage of various hierarchical nanodimensional objects including the 0D monodisperse SiO2 yolks, the 1D continuous carbon shell and the 3D interconnected non-woven fabric web has been developed by an innovative multi-dimensional construction method, and thus demonstrates excellent electrochemical properties as a self-standing LIB anode.A novel active yolk@conductive shell nanofiber web with a unique synergistic advantage of various hierarchical nanodimensional objects including the 0D monodisperse SiO2 yolks, the 1D continuous carbon shell and the 3D interconnected non-woven fabric web has been developed by an innovative multi-dimensional construction method, and thus demonstrates excellent electrochemical properties as a self-standing LIB anode. Electronic supplementary information (ESI) available: Experimental details and additional information about material characterization. See DOI: 10.1039/c5nr06531c

High-frequency stock linkage and multi-dimensional stationary processes

NASA Astrophysics Data System (ADS)

Wang, Xi; Bao, Si; Chen, Jingchao

2017-02-01

In recent years, China's stock market has experienced dramatic fluctuations; in particular, in the second half of 2014 and 2015, the market rose sharply and fell quickly. Many classical financial phenomena, such as stock plate linkage, appeared repeatedly during this period. In general, these phenomena have usually been studied using daily-level data or minute-level data. Our paper focuses on the linkage phenomenon in Chinese stock 5-second-level data during this extremely volatile period. The method used to select the linkage points and the arbitrage strategy are both based on multi-dimensional stationary processes. A new program method for testing the multi-dimensional stationary process is proposed in our paper, and the detailed program is presented in the paper's appendix. Because of the existence of the stationary process, the strategy's logarithmic cumulative average return will converge under the condition of the strong ergodic theorem, and this ensures the effectiveness of the stocks' linkage points and the more stable statistical arbitrage strategy.

Principles of qualitative analysis in the chromatographic context.

PubMed

Valcárcel, M; Cárdenas, S; Simonet, B M; Carrillo-Carrión, C

2007-07-27

This article presents the state of the art of qualitative analysis in the framework of the chromatographic analysis. After establishing the differences between two main classes of qualitative analysis (analyte identification and sample classification/qualification) the particularities of instrumental qualitative analysis are commented on. Qualitative chromatographic analysis for sample classification/qualification through the so-called chromatographic fingerprint (for complex samples) or the volatiles profile (through the direct coupling headspace-mass spectrometry using the chromatograph as interface) is discussed. Next, more technical exposition of the qualitative chromatographic information is presented supported by a variety of representative examples.

Scope of partial least-squares regression applied to the enantiomeric composition determination of ketoprofen from strongly overlapped chromatographic profiles.

PubMed

Padró, Juan M; Osorio-Grisales, Jaiver; Arancibia, Juan A; Olivieri, Alejandro C; Castells, Cecilia B

2015-07-01

Valuable quantitative information could be obtained from strongly overlapped chromatographic profiles of two enantiomers by using proper chemometric methods. Complete separation profiles where the peaks are fully resolved are difficult to achieve in chiral separation methods, and this becomes a particularly severe problem in case that the analyst needs to measure the chiral purity, i.e., when one of the enantiomers is present in the sample in very low concentrations. In this report, we explore the scope of a multivariate chemometric technique based on unfolded partial least-squares regression, as a mathematical tool to solve this quite frequent difficulty. This technique was applied to obtain quantitative results from partially overlapped chromatographic profiles of R- and S-ketoprofen, with different values of enantioresolution factors (from 0.81 down to less than 0.2 resolution units), and also at several different S:R enantiomeric ratios. Enantiomeric purity below 1% was determined with excellent precision even from almost completely overlapped signals. All these assays were tested on the most demanding condition, i.e., when the minor peak elutes immediately after the main peak. The results were validated using univariate calibration of completely resolved profiles and the method applied to the determination of enantiomeric purity of commercial pharmaceuticals. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

PubMed

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

2016-11-01

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

Development and evaluation of a hydrophilic interaction liquid chromatography-MS/MS method to quantify 19 nucleobases and nucleosides in rat plasma.

PubMed

Du, Yan; Li, Yin-Jie; Hu, Xun-Xiu; Deng, Xu; Qian, Zeng-Ting; Li, Zheng; Guo, Meng-Zhe; Tang, Dao-Quan

2017-04-01

As essential endogenous compounds, nucleobases and nucleosides fulfill various functions in living organisms. This study presents the development and validation of a new hydrophilic interaction liquid chromatography tandem mass spectrometry method for simultaneous quantification of 19 nucleobases and nucleosides in rat plasma. For the sample preparation, 15 kinds of protein precipitants were evaluated according to the chromatographic profile and ion response of analytes. The optimization of chromatographic separation was respectively performed using reversed-phase liquid chromatography and hydrophilic interaction liquid chromatography mode; each separation mode included two test columns with different stationary phases. The chromatographic profile and parameters such as half-width (W 1/2 ), capacity factor (K') and tailing factor (f t ) were used to evaluate the separation efficiencies. Furthermore, the adopted composition of two mobile phase systems and the concentrations of the additives in the optimum buffer system were also investigated. The developed method was fully validated and successfully applied quantitatively to determine 19 nucleobases and nucleosides in plasma from normal and diabetic nephropathy (DN) rats. Significant differences between normal and DN rats were found in plasma levels of cytosine, xanthine, thymidine, adenosine, guanosine, inosine and 8-hydroxy-2'-deoxyguanosine. This information may provide a useful reference for the discovery of potential biomarkers of DN. Copyright © 2016 John Wiley & Sons, Ltd.

Retrovirus purification: method that conserves envelope glycoprotein and maximizes infectivity.

PubMed Central

McGrath, M; Witte, O; Pincus, T; Weissman, I L

1978-01-01

A Sepharose 4B chromatographic method for purification of retroviruses is described which was less time consuming, increased purified virus yields, conserved viral glycoprotein, and increased recovery of biological infectivity in comparison with conventional sucrose gradient ultracentrifugation techniques. Images PMID:205680

Discrete models for the numerical analysis of time-dependent multidimensional gas dynamics

NASA Technical Reports Server (NTRS)

Roe, P. L.

1984-01-01

A possible technique is explored for extending to multidimensional flows some of the upwind-differencing methods that are highly successful in the one-dimensional case. Emphasis is on the two-dimensional case, and the flow domain is assumed to be divided into polygonal computational elements. Inside each element, the flow is represented by a local superposition of elementary solutions consisting of plane waves not necessarily aligned with the element boundaries.

Current Applications of Chromatographic Methods in the Study of Human Body Fluids for Diagnosing Disorders.

PubMed

Jóźwik, Jagoda; Kałużna-Czaplińska, Joanna

2016-01-01

Currently, analysis of various human body fluids is one of the most essential and promising approaches to enable the discovery of biomarkers or pathophysiological mechanisms for disorders and diseases. Analysis of these fluids is challenging due to their complex composition and unique characteristics. Development of new analytical methods in this field has made it possible to analyze body fluids with higher selectivity, sensitivity, and precision. The composition and concentration of analytes in body fluids are most often determined by chromatography-based techniques. There is no doubt that proper use of knowledge that comes from a better understanding of the role of body fluids requires the cooperation of scientists of diverse specializations, including analytical chemists, biologists, and physicians. This article summarizes current knowledge about the application of different chromatographic methods in analyses of a wide range of compounds in human body fluids in order to diagnose certain diseases and disorders.

A review on creatinine measurement techniques.

PubMed

Mohabbati-Kalejahi, Elham; Azimirad, Vahid; Bahrami, Manouchehr; Ganbari, Ahmad

2012-08-15

This paper reviews the entire recent global tendency for creatinine measurement. Creatinine biosensors involve complex relationships between biology and micro-mechatronics to which the blood is subjected. Comparison between new and old methods shows that new techniques (e.g. Molecular Imprinted Polymers based algorithms) are better than old methods (e.g. Elisa) in terms of stability and linear range. All methods and their details for serum, plasma, urine and blood samples are surveyed. They are categorized into five main algorithms: optical, electrochemical, impedometrical, Ion Selective Field-Effect Transistor (ISFET) based technique and chromatography. Response time, detection limit, linear range and selectivity of reported sensors are discussed. Potentiometric measurement technique has the lowest response time of 4-10 s and the lowest detection limit of 0.28 nmol L(-1) belongs to chromatographic technique. Comparison between various techniques of measurements indicates that the best selectivity belongs to MIP based and chromatographic techniques. Copyright © 2012 Elsevier B.V. All rights reserved.

Chromatographic determination of aliphatic aldehydes in human serum after pre-column derivatization using 2,2'-furil, a novel fluorogenic reagent.

PubMed

Fathy Bakr Ali, Marwa; Kishikawa, Naoya; Ohyama, Kaname; Abdel-Mageed Mohamed, Horria; Mohamed Abdel-Wadood, Hanaa; Mohamed Mohamed, Ashraf; Kuroda, Naotaka

2013-07-26

A novel, highly sensitive and selective fluorimetric liquid chromatographic method for simultaneous determination of medium chain aliphatic aldehydes was developed. The method was based on the derivatization of aliphatic aldehydes with 1,2-di(2-furyl)-1,2-ethanedione (2,2'-furil), a novel fluorogenic reagent, to form highly fluorescent difurylimidazole derivatives. The fluorescence derivatives were separated in less than 20min on a reversed-phase ODS column using an isocratic elution with a mixture of methanol-water (80:20, v/v%). The detection limits were from 0.19 to 0.50nM (1-10fmol/injection) at a signal-to-noise ratio (S/N) of 3. This method was successfully applied for monitoring of aliphatic aldehydes in healthy human sera by a simple pretreatment procedure without interferences from serum constituents. Copyright © 2013 Elsevier B.V. All rights reserved.

Chapter 3. A multidimensional model for narrative analysis of substance use-related dependency.

PubMed

Larsson, Sam; von Braun, Therese; Lilja, John

2013-11-01

This chapter examines the possibilities and limitations of using a narrative method as a framework within a multidimensional model for exploring and analyzing the use and misuse of alcohol and drugs. It is posited that a multidimensional model, based on narrative reasoning, can give a more detailed and specific understanding of substance users, who represent a heterogeneous population of people, and of substance use-related dependency problems. Such a model describes and analyses the drug-use related problems in a manner that provides holistic and important information and knowledge about the person by contextual and situation interaction processes which are involved in the use/misuse of alcohol and drugs. Tentative conclusions and unresolved critical issues are considered.

Fuzzy Regression Prediction and Application Based on Multi-Dimensional Factors of Freight Volume

NASA Astrophysics Data System (ADS)

Xiao, Mengting; Li, Cheng

2018-01-01

Based on the reality of the development of air cargo, the multi-dimensional fuzzy regression method is used to determine the influencing factors, and the three most important influencing factors of GDP, total fixed assets investment and regular flight route mileage are determined. The system’s viewpoints and analogy methods, the use of fuzzy numbers and multiple regression methods to predict the civil aviation cargo volume. In comparison with the 13th Five-Year Plan for China’s Civil Aviation Development (2016-2020), it is proved that this method can effectively improve the accuracy of forecasting and reduce the risk of forecasting. It is proved that this model predicts civil aviation freight volume of the feasibility, has a high practical significance and practical operation.

The PedsQL in pediatric cancer: reliability and validity of the Pediatric Quality of Life Inventory Generic Core Scales, Multidimensional Fatigue Scale, and Cancer Module.

PubMed

Varni, James W; Burwinkle, Tasha M; Katz, Ernest R; Meeske, Kathy; Dickinson, Paige

2002-04-01

The Pediatric Quality of Life Inventory (PedsQL) is a modular instrument designed to measure health-related quality of life (HRQOL) in children and adolescents ages 2-18 years. The PedsQL 4.0 Generic Core Scales are multidimensional child self-report and parent proxy-report scales developed as the generic core measure to be integrated with the PedsQL disease specific modules. The PedsQL Multidimensional Fatigue Scale was designed to measure fatigue in pediatric patients. The PedsQL 3.0 Cancer Module was designed to measure pediatric cancer specific HRQOL. The PedsQL Generic Core Scales, Multidimensional Fatigue Scale, and Cancer Module were administered to 339 families (220 child self-reports; 337 parent proxy-reports). Internal consistency reliability for the PedsQL Generic Core Total Scale Score (alpha = 0.88 child, 0.93 parent report), Multidimensional Fatigue Total Scale Score (alpha = 0.89 child, 0.92 parent report) and most Cancer Module Scales (average alpha = 0.72 child, 0.87 parent report) demonstrated reliability acceptable for group comparisons. Validity was demonstrated using the known-groups method. The PedsQL distinguished between healthy children and children with cancer as a group, and among children on-treatment versus off-treatment. The validity of the PedsQL Multidimensional Fatigue Scale was further demonstrated through hypothesized intercorrelations with dimensions of generic and cancer specific HRQOL. The results demonstrate the reliability and validity of the PedsQL Generic Core Scales, Multidimensional Fatigue Scale, and Cancer Module in pediatric cancer. The PedsQL may be utilized as an outcome measure in clinical trials, research, and clinical practice. Copyright 2002 American Cancer Society.

The PedsQL Multidimensional Fatigue Scale in pediatric rheumatology: reliability and validity.

PubMed

Varni, James W; Burwinkle, Tasha M; Szer, Ilona S

2004-12-01

. The PedsQL (Pediatric Quality of Life Inventory) is a modular instrument designed to measure health related quality of life (HRQOL) in children and adolescents ages 2-18 years. The recently developed 18-item PedsQL Multidimensional Fatigue Scale was designed to measure fatigue in pediatric patients and comprises the General Fatigue Scale (6 items), Sleep/Rest Fatigue Scale (6 items), and Cognitive Fatigue Scale (6 items). The PedsQL 4.0 Generic Core Scales were developed as the generic core measure to be integrated with the PedsQL Disease-Specific Modules. The PedsQL 3.0 Rheumatology Module was designed to measure pediatric rheumatology-specific HRQOL. Methods. The PedsQL Multidimensional Fatigue Scale, Generic Core Scales, and Rheumatology Module were administered to 163 children and 154 parents (183 families accrued overall) recruited from a pediatric rheumatology clinic. Results. Internal consistency reliability for the PedsQL Multidimensional Fatigue Scale Total Score (a = 0.95 child, 0.95 parent report), General Fatigue Scale (a = 0.93 child, 0.92 parent), Sleep/Rest Fatigue Scale (a = 0.88 child, 0.90 parent), and Cognitive Fatigue Scale (a = 0.93 child, 0.96 parent) were excellent for group and individual comparisons. The validity of the PedsQL Multidimensional Fatigue Scale was confirmed through hypothesized intercorrelations with dimensions of generic and rheumatology-specific HRQOL. The PedsQL Multidimensional Fatigue Scale distinguished between healthy children and children with rheumatic diseases as a group, and was associated with greater disease severity. Children with fibromyalgia manifested greater fatigue than children with other rheumatic diseases. The results confirm the initial reliability and validity of the PedsQL Multidimensional Fatigue Scale in pediatric rheumatology.

Rapid and Convenient Separation of Chitooligosaccharides by Ion-Exchange Chromatography

NASA Astrophysics Data System (ADS)

Wu, Yuxiao; Lu, Wei-Peng; Wang, Jianing; Gao, Yunhua; Guo, Yanchuan

2017-12-01

Pervious methods for separation of highly purified chitooligosaccharides was time-consuming and labor-intensive, which limited the large-scale production. This study developed a convenient ion-exchange chromatography using the ÄKTA™ avant 150 chromatographic system. Five fractions were automatically collected under detecting the absorption at 210 nm. The fractions were analyzed by high-performance liquid chromatography. It proved that they primarily comprised chitobiose, chitotriose, chitotetraose, chitopentaose, and chitohexaose, respectively, with chromatographic purities over 90%. The separation process was rapid, convenient and could be monitored on-line, which would be benefit for the mass production of chitooligosaccharides.

Odor intensity and characterization studies of exhaust from a turbojet engine combustor

NASA Technical Reports Server (NTRS)

Butze, H. F.; Kendall, D. A.

1973-01-01

Sensory odor tests of the exhaust from a turbojet combustor operating at simulated idle conditions were made by a human panel sniffing diluted exhaust gas. Simultaneously, samples of undiluted exhaust gas were collected on adsorbent substrates, subsequently removed by solvent flushing, and analyzed chemically by liquid chromatographic methods. The concentrations of the principal malodorous species, the aromatic (unburned fuel-related) and the oxygenated (partially burned fuel) fractions, as determined chromatographically, correlated well with the intensity of the odor as determined by sniffing. Odor intensity increased as combustion efficiency decreased. Combustor modifications which increased combustion efficiency decreased odor intensity.

Liquid chromatographic characterization of PMR-15 resin and prepreg

NASA Technical Reports Server (NTRS)

Reed, K. E.

1980-01-01

A liquid chromatographic method has been developed capable of providing a chemical fingerprint of PMR-15 resin solutions and prepreg. The amounts of two of the monomers can be quantified so their experimentally determined molar ratio can be compared to the formulated one. Only the monomers were detected in fresh resin solution, whereas several additional components, resulting from an association or reaction between the norbornenyl endcap and the amine, were detected in a resin solution aged for three days. Two commercial prepregs exhibited fingerprints similar to that of laboratory material, but three others contained additional components corresponding to higher esters and nadimides.

Inactivation of aflatoxin B1 by using the synergistic effect of hydrogen peroxide and gamma radiation

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

Patel, U.D.; Govindarajan, P.; Dave, P.J.

Inactivation of aflatoxin B1 was studied by using gamma radiation and hydrogen peroxide. A 100-krad dose of gamma radiation was sufficient to inactivate 50 micrograms of aflatoxin B1 in the presence of 5% hydrogen peroxide, and 400 krad was required for total degradation of 100 micrograms of aflatoxin in the same system. Degradation of aflatoxin B1 was confirmed by high-pressure liquid chromatographic and thin-layer chromatographic analysis. Ames microsomal mutagenicity test showed loss of aflatoxin activity. This method of detoxification also reduces the toxin levels effectively in artificially contaminated groundnuts.

Novel Chromatographic Methods for Simultaneous Quantification of Fish and Wheat Germ Oils Mixture in Pharmaceutical Dosage Forms.

PubMed

El-Yazbi, Amira F; El-Hawiet, Amr

2017-05-01

Two simple, direct and environment-friendly chromatographic methods, high-performance liquid chromatography (HPLC) and high-performance thin layer chromatographic (HPTLC), were developed for the determination of a binary mixture of fish oil (FO) and wheat germ oil (WGO), for the first time, in their pharmaceutical dosage forms with no need for any sample pretreatment. The HPLC separation was carried out using C-18 stationary phase with mobile phase of 15% formic acid (pH 6), methanol and acetonitrile through gradient-elution, 1.5 mL min-1 flow-rate and detection at 215 nm for FO and 280 nm for WGO. HPTLC separation was carried out on silica-coated plates using diethyl ether-petroleum ether (0.5:9.5, v/v) as mobile phase. Detection was at 215 nm for FO and 240 nm for WGO. Regression analysis showed good linear relationship with r > 0.999 in the concentration-ranges of 0.2-2 mg mL-1 and 2.5-20 μg band-1 for WGO by HPLC and HPTLC methods, respectively, and 0.4-10 mg mL-1 and 25-200 μg band-1 for FO by HPLC and HPTLC methods, respectively. The methods were validated, showed good analytical performance and were successfully applied for the analysis of pharmaceutical formulations and synthetic mixtures of the analytes with good recoveries. Therefore, the two methods could be conveniently adopted for routine analysis of similar products in quality control laboratories of pharmaceutical industries especially that simultaneous determination of FO-WGO mixture has not been reported previously. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

A multi-method approach toward de novo glycan characterization: a Man-5 case study.

PubMed

Prien, Justin M; Prater, Bradley D; Cockrill, Steven L

2010-05-01

Regulatory agencies' expectations for biotherapeutic approval are becoming more stringent with regard to product characterization, where minor species as low as 0.1% of a given profile are typically identified. The mission of this manuscript is to demonstrate a multi-method approach toward de novo glycan characterization and quantitation, including minor species at or approaching the 0.1% benchmark. Recently, unexpected isomers of the Man(5)GlcNAc(2) (M(5)) were reported (Prien JM, Ashline DJ, Lapadula AJ, Zhang H, Reinhold VN. 2009. The high mannose glycans from bovine ribonuclease B isomer characterization by ion trap mass spectrometry (MS). J Am Soc Mass Spectrom. 20:539-556). In the current study, quantitative analysis of these isomers found in commercial M(5) standard demonstrated that they are in low abundance (<1% of the total) and therefore an exemplary "litmus test" for minor species characterization. A simple workflow devised around three core well-established analytical procedures: (1) fluorescence derivatization; (2) online rapid resolution reversed-phase separation coupled with negative-mode sequential mass spectrometry (RRRP-(-)-MS(n)); and (3) permethylation derivatization with nanospray sequential mass spectrometry (NSI-MS(n)) provides comprehensive glycan structural determination. All methods have limitations; however, a multi-method workflow is an at-line stopgap/solution which mitigates each method's individual shortcoming(s) providing greater opportunity for more comprehensive characterization. This manuscript is the first to demonstrate quantitative chromatographic separation of the M(5) isomers and the use of a commercially available stable isotope variant of 2-aminobenzoic acid to detect and chromatographically resolve multiple M(5) isomers in bovine ribonuclease B. With this multi-method approach, we have the capabilities to comprehensively characterize a biotherapeutic's glycan array in a de novo manner, including structural isomers at >/=0.1% of the total chromatographic peak area.

Determination of teicoplanin concentrations in serum by high-pressure liquid chromatography.

PubMed Central

Joos, B; Lüthy, R

1987-01-01

An isocratic reversed-phase high-pressure liquid chromatographic method for the determination of six components of the teicoplanin complex in biological fluid was developed. By using fluorescence detection after precolumn derivatization with fluorescamine, the assay is specific and highly sensitive, with reproducibility studies yielding coefficients of variation ranging from 1.5 to 8.5% (at 5 to 80 micrograms/ml). Response was linear from 2.5 to 80 micrograms/ml (r = 0.999); the recovery from spiked human serum was 76%. An external quality control was performed to compare this high-pressure liquid chromatographic method (H) with a standard microbiological assay (M); no significant deviation from slope = 1 and intercept = 0 was found by regression analysis (H = 1.03M - 0.45; n = 15). PMID:2957953

Isocratic non-aqueous reversed-phase high-performance liquid chromatographic separation of capsanthin and capsorubin in red peppers (Capsicum annuum L.), paprika and oleoresin.

PubMed

Weissenberg, M; Schaeffler, I; Menagem, E; Barzilai, M; Levy, A

1997-01-03

A simple, rapid high-performance liquid chromatography method has been devised in order to separate and quantify the xanthophylls capsorubin and capasanthin present in red pepper (Capsicum annuum L.) fruits and preparations made from them (paprika and oleoresin). A reversed-phase isocratic non-aqueous system allows the separation of xanthophylls within a few minutes, with detection at 450 nm, using methyl red as internal standard to locate the various carotenoids and xanthophylls found in plant extracts. The selection of extraction solvents, mild saponification conditions, and chromatographic features is evaluated and discussed. The method is proposed for rapid screening of large plant populations, plant selection, as well as for paprika products and oleoresin, and also for nutrition and quality control studies.

Application of a 1,1,3,3-tetramethylguanidine (TMG)/MeOH-CO2 in situ derivatization procedure for the gas chromatographic characterization of the fatty acid profile in olive oil.

PubMed

Saliu, F; Anzano, M; Franzetti, A

2015-03-01

1,1,3,3-Tetramethylguanidine (TMG), methanol and carbon dioxide were investigated as switchable polarity solvents (SPS) in the simultaneous derivatization and extraction of triacylglycerols for the gas chromatographic (GC) characterization of olive oil. Three commercial olive oils were used as test samples. Results of the developed method did not differ statistically from those provided by reference derivatization procedures. The transesterification reaction was carried out under a very mild condition, one step and in situ, and no particular matrix interferences were evidenced. The method represented the first example of the use of a switchable polarity mixture for the preparation of methyl ester derivatives of fatty acids (FAME).

Gas chromatographic determination of fumigant residues in stored grains, using isooctane partitioning and dual column packings.

PubMed

Daft, J L

1983-03-01

A gas chromatographic (GC) procedure for determining fumigants in grains was developed. Fumigants were leached from grain samples with the official AOAC method using acetone-water (5 + 1). They were then partitioned from the leachate with isooctane, yielding a dry, stable extract that was analyzed by GC. Fortified sample recoveries ranged from 90 to 100%. Two GC columns were used, 20% OV-101 and 20% OV-225/20% OV-17 (2 + 1). These columns gave dissimilar retention profiles and baseline resolution for the 7 fumigants investigated: chloroform, ethylene dichloride, carbon tetrachloride, trichloroethylene, chloropicrin, ethylene dibromide, and tetrachloroethylene. Further tests showed that grain samples could be screened for fumigant residues by direct injection of the acetone-water leachates obtained using the AOAC method.

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

PubMed

Wiczling, Paweł; Kaliszan, Roman

2016-01-05

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

Assessment of the chromatographic lipophilicity of eight cephalosporins on different stationary phases.

PubMed

Dąbrowska, Monika; Starek, Małgorzata; Komsta, Łukasz; Szafrański, Przemysław; Stasiewicz-Urban, Anna; Opoka, Włodzimierz

2017-04-01

The retention behaviors were investigated for a series of eight cephalosporins in thin-layer chromatography (TLC) using stationary phases of RP-2, RP-8, RP-18, NH 2 , DIOL, and CN chemically bonded silica gel. Additionally, various binary mobile phases (water/methanol and water/acetone) were used in different volume proportions. The retention behavior of the analyzed molecules was defined by R M0 constant. In addition, reversed phase high performance liquid chromatography (RP-HPLC) was performed in lipophilicity studies by using immobilized artificial membrane (IAM) stationary phase. Obtained chromatographic data (R M0 and logk' IAM ) were correlated with the lipophilicity, expressed as values of the log calculated (logP calc ) and experimental (logP exp(shake-flask) ) partition coefficient. Principal component analysis (PCA) was applied in order to obtain an overview of similarity or dissimilarity among the analyzed compounds. Hierarchical cluster analysis (HCA) was performed to compare the separation characteristics of the applied stationary phases. This study was undertaken to identify the best chromatographic system and chromatographic data processing method to enable the prediction of logP values. A comprehensive chromatographic investigation into the retention of the analyzed cephalosporins revealed a similar behavior on RP-18, RP-8 and CN stationary phases. The weak correlations obtained between experimental and certain computed lipophilicity indices revealed that R M0 and PC1/RM are relevant lipophilicity parameters and the RP-8, CN and RP-18 plates are appropriate stationary phases for lipophilicity investigation, whereas computational approaches still cannot fully replace experimentation. Copyright © 2017 Elsevier B.V. All rights reserved.

Implication of PKS type I gene and chromatographic strategy for the biodiscovery of antimicrobial polyketide metabolites from endosymbiotic Nocardiopsis prasina CLA68

NASA Astrophysics Data System (ADS)

Rao, H. C. Yashavantha; Rakshith, Devaraju; Gurudatt, D. M.; Satish, Sreedharamurthy

2016-06-01

Advanced approach in probing for polyketide antimicrobials requires novel genomics and chromatographic strategies. An endophytic strain CLA68 was isolated from the root of Combretum latifolium Blume (Combretaceae) collected from the Western Ghats of Southern India. Strain CLA68 was then identified as Nocardiopsis prasina by its characteristic culture morphology and analysis of 16S rRNA gene sequence. Biosynthetic polyketide synthase genes were investigated using two pairs of degenerate primers. Ethyl acetate extract of CLA68 exhibited broad spectrum activity against a panel of test human pathogens. PKS type-I gene detection and chromatographic strategy yielded a robust polyketide antimicrobial compound which identified as nocapyrone E. Minimum inhibitory concentration of the purified compound against MRSA and other human pathogens ranged between 25 and 100 μg/ml. The present work highlights the utility of N. prasina CLA68 as potential source for antimicrobial polyketide nocapyrone E which could help to combat multidrug-resistant pathogens. This study demonstrates feasibility of PKS type-I gene-based molecular approach and chemical investigation by chromatographic approach is the best method for prediction and rapid discovery of novel polyketides from endosymbiotic actinomycetes. The sequence data of this endosymbiotic actinomycete is deposited in GenBank under the accession no. KP269077.

Standardisation of Gymnema sylvestre R.Br. by high-performance thin-layer chromatography: an improved method.

PubMed

Raju, Valivarthi S R; Kannababu, S; Subbaraju, Gottumukkala V

2006-01-01

An improved high-performance thin-layer chromatographic (HPTLC) method for the standardisation of Gymnema sylvestre is reported. The method involves the initial hydrolysis of gymnemic acids, the active ingredients, to a common aglycone followed by the quantitative estimation of gymnemagenin. The present method rectifies an error found in an HPTLC method reported recently.

Path integral learning of multidimensional movement trajectories

NASA Astrophysics Data System (ADS)

André, João; Santos, Cristina; Costa, Lino

2013-10-01

This paper explores the use of Path Integral Methods, particularly several variants of the recent Path Integral Policy Improvement (PI2) algorithm in multidimensional movement parametrized policy learning. We rely on Dynamic Movement Primitives (DMPs) to codify discrete and rhythmic trajectories, and apply the PI2-CMA and PIBB methods in the learning of optimal policy parameters, according to different cost functions that inherently encode movement objectives. Additionally we merge both of these variants and propose the PIBB-CMA algorithm, comparing all of them with the vanilla version of PI2. From the obtained results we conclude that PIBB-CMA surpasses all other methods in terms of convergence speed and iterative final cost, which leads to an increased interest in its application to more complex robotic problems.

A two-dimensional Riemann solver with self-similar sub-structure - Alternative formulation based on least squares projection

NASA Astrophysics Data System (ADS)

Balsara, Dinshaw S.; Vides, Jeaniffer; Gurski, Katharine; Nkonga, Boniface; Dumbser, Michael; Garain, Sudip; Audit, Edouard

2016-01-01

Just as the quality of a one-dimensional approximate Riemann solver is improved by the inclusion of internal sub-structure, the quality of a multidimensional Riemann solver is also similarly improved. Such multidimensional Riemann problems arise when multiple states come together at the vertex of a mesh. The interaction of the resulting one-dimensional Riemann problems gives rise to a strongly-interacting state. We wish to endow this strongly-interacting state with physically-motivated sub-structure. The self-similar formulation of Balsara [16] proves especially useful for this purpose. While that work is based on a Galerkin projection, in this paper we present an analogous self-similar formulation that is based on a different interpretation. In the present formulation, we interpret the shock jumps at the boundary of the strongly-interacting state quite literally. The enforcement of the shock jump conditions is done with a least squares projection (Vides, Nkonga and Audit [67]). With that interpretation, we again show that the multidimensional Riemann solver can be endowed with sub-structure. However, we find that the most efficient implementation arises when we use a flux vector splitting and a least squares projection. An alternative formulation that is based on the full characteristic matrices is also presented. The multidimensional Riemann solvers that are demonstrated here use one-dimensional HLLC Riemann solvers as building blocks. Several stringent test problems drawn from hydrodynamics and MHD are presented to show that the method works. Results from structured and unstructured meshes demonstrate the versatility of our method. The reader is also invited to watch a video introduction to multidimensional Riemann solvers on http://www.nd.edu/ dbalsara/Numerical-PDE-Course.

Chemical compositions, chromatographic fingerprints and antioxidant activities of Andrographis Herba.

PubMed

Zhao, Yang; Kao, Chun-Pin; Wu, Kun-Chang; Liao, Chi-Ren; Ho, Yu-Ling; Chang, Yuan-Shiun

2014-11-10

This paper describes the development of an HPLC-UV-MS method for quantitative determination of andrographolide and dehydroandrographolide in Andrographis Herba and establishment of its chromatographic fingerprint. The method was validated for linearity, limit of detection and quantification, inter- and intra-day precisions, repeatability, stability and recovery. All the validation results of quantitative determination and fingerprinting methods were satisfactory. The developed method was then applied to assay the contents of andrographolide and dehydroandrographolide and to acquire the fingerprints of all the collected Andrographis Herba samples. Furthermore, similarity analysis and principal component analysis were used to reveal the similarities and differences between the samples on the basis of the characteristic peaks. More importantly, the DPPH free radical-scavenging and ferric reducing capacities of the Andrographis Herba samples were assayed. By bivariate correlation analysis, we found that six compounds are positively correlated to DPPH free radical scavenging and ferric reducing capacities, and four compounds are negatively correlated to DPPH free radical scavenging and ferric reducing capacities.

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

PubMed

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

2001-12-01

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

Rapid and sensitive method for determination of withaferin-A in human plasma by HPLC.

PubMed

Patial, Pankaj; Gota, Vikram

2011-02-01

To develop and validate a rapid and sensitive high-performance liquid chromatographic method for determination of withaferin-A in human plasma. Withaferin-A, the active molecule of a traditional Indian herb, has demonstrated several biological activities in preclinical models. A validated bioassay is not available for its pharmacokinetic evaluation. The chromatographic system used a reverse-phase C18 column with UV-visible detection at 225 nm. The mobile phase consisted of water and acetonitrile applied in a gradient flow. Withaferin-A was extracted by simple protein-precipitation technique. The calibration curve was linear in the concentration range of 0.05-1.6 µg/ml. The method has the desired sensitivity to detect the plasma concentration range of withaferin-A that is likely to show biological activity based on in vitro data. This is the first HPLC method ever described for the estimation of withaferin-A in human plasma which could be applied for pharmacokinetic studies.

Comparison of various extraction methods for policosanol from rice bran wax and establishment of chromatographic fingerprint of policosanol.

PubMed

Wang, Mei-Fei; Lian, Hong-Zhen; Mao, Li; Zhou, Jing-Ping; Gong, Hui-Juan; Qian, Bao-Yong; Fang, Yan; Li, Jie

2007-07-11

A capillary gas chromatographic (GC) method has been developed for the separation and determination of policosanol components extracted from rice bran wax. A Varian CP-sil 8 CB column was employed, and an oven temperature was programmed. Gas chromatography-mass spectrometry (GC-MS) was used to identify the composition of policosanol. Quantitative analysis was carried out by means of hydrogen flame ionization detector (FID) with dinonyl phthalate (DNP) as internal standard. The results indicated that the extract obtained by dry saponification has the highest contents of octacosanol and triacontanol among extracts by all used extraction methods including dry saponification, saponification in alcohol, saponification in water (neutralized and non-neutralized), and transesterification. Meanwhile, the GC-MS fingerprint of policosanol extracted by dry saponification has been established. Euclidean distance similarity calculation showed remarkable consistency of compositions and contents among 12 batches of policosanol from a rice bran wax variety. This protocol provided a rapid and feasible method for quality control of policosanol products.

Simple gas chromatographic method for furfural analysis.

PubMed

Gaspar, Elvira M S M; Lopes, João F

2009-04-03

A new, simple, gas chromatographic method was developed for the direct analysis of 5-hydroxymethylfurfural (5-HMF), 2-furfural (2-F) and 5-methylfurfural (5-MF) in liquid and water soluble foods, using direct immersion SPME coupled to GC-FID and/or GC-TOF-MS. The fiber (DVB/CAR/PDMS) conditions were optimized: pH effect, temperature, adsorption and desorption times. The method is simple and accurate (RSD<8%), showed good recoveries (77-107%) and good limits of detection (GC-FID: 1.37 microgL(-1) for 2-F, 8.96 microgL(-1) for 5-MF, 6.52 microgL(-1) for 5-HMF; GC-TOF-MS: 0.3, 1.2 and 0.9 ngmL(-1) for 2-F, 5-MF and 5-HMF, respectively). It was applied to different commercial food matrices: honey, white, demerara, brown and yellow table sugars, and white and red balsamic vinegars. This one-step, sensitive and direct method for the analysis of furfurals will contribute to characterise and quantify their presence in the human diet.

A NEW HPLC METHOD FOR SEPARATION OF PHYTOPLANKTON PIGMENTS IN NATURAL SAMPLES

EPA Science Inventory

A new high-performance liquid chromatographic (HPLC) method was developed to analyze, in a single run, most polar and non-polar chlorophylls and carotenoids from marine phytoplankton. The method is based on a reverse-phase amide C16 (RP-amide C16) column and an elution gradient o...

Study of multi-dimensional radiative energy transfer in molecular gases

NASA Technical Reports Server (NTRS)

Liu, Jiwen; Tiwari, S. N.

1993-01-01

The Monte Carlo method (MCM) is applied to analyze radiative heat transfer in nongray gases. The nongray model employed is based on the statistical arrow band model with an exponential-tailed inverse intensity distribution. Consideration of spectral correlation results in some distinguishing features of the Monte Carlo formulations. Validation of the Monte Carlo formulations has been conducted by comparing results of this method with other solutions. Extension of a one-dimensional problem to a multi-dimensional problem requires some special treatments in the Monte Carlo analysis. Use of different assumptions results in different sets of Monte Carlo formulations. The nongray narrow band formulations provide the most accurate results.

Real-time monitoring and visualization of the multi-dimensional motion of an anisotropic nanoparticle

NASA Astrophysics Data System (ADS)

Go, Gi-Hyun; Heo, Seungjin; Cho, Jong-Hoi; Yoo, Yang-Seok; Kim, Minkwan; Park, Chung-Hyun; Cho, Yong-Hoon

2017-03-01

As interest in anisotropic particles has increased in various research fields, methods of tracking such particles have become increasingly desirable. Here, we present a new and intuitive method to monitor the Brownian motion of a nanowire, which can construct and visualize multi-dimensional motion of a nanowire confined in an optical trap, using a dual particle tracking system. We measured the isolated angular fluctuations and translational motion of the nanowire in the optical trap, and determined its physical properties, such as stiffness and torque constants, depending on laser power and polarization direction. This has wide implications in nanoscience and nanotechnology with levitated anisotropic nanoparticles.

Electrochemical force microscopy

DOEpatents

Kalinin, Sergei V.; Jesse, Stephen; Collins, Liam F.; Rodriguez, Brian J.

2017-01-10

A system and method for electrochemical force microscopy are provided. The system and method are based on a multidimensional detection scheme that is sensitive to forces experienced by a biased electrode in a solution. The multidimensional approach allows separation of fast processes, such as double layer charging, and charge relaxation, and slow processes, such as diffusion and faradaic reactions, as well as capturing the bias dependence of the response. The time-resolved and bias measurements can also allow probing both linear (small bias range) and non-linear (large bias range) electrochemical regimes and potentially the de-convolution of charge dynamics and diffusion processes from steric effects and electrochemical reactivity.

Using multi-dimensional Smolyak interpolation to make a sum-of-products potential

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

Avila, Gustavo, E-mail: Gustavo-Avila@telefonica.net; Carrington, Tucker, E-mail: Tucker.Carrington@queensu.ca

2015-07-28

We propose a new method for obtaining potential energy surfaces in sum-of-products (SOP) form. If the number of terms is small enough, a SOP potential surface significantly reduces the cost of quantum dynamics calculations by obviating the need to do multidimensional integrals by quadrature. The method is based on a Smolyak interpolation technique and uses polynomial-like or spectral basis functions and 1D Lagrange-type functions. When written in terms of the basis functions from which the Lagrange-type functions are built, the Smolyak interpolant has only a modest number of terms. The ideas are tested for HONO (nitrous acid)

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

PubMed

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

2006-06-01

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

Real-time object recognition in multidimensional images based on joined extended structural tensor and higher-order tensor decomposition methods

NASA Astrophysics Data System (ADS)

Cyganek, Boguslaw; Smolka, Bogdan

2015-02-01

In this paper a system for real-time recognition of objects in multidimensional video signals is proposed. Object recognition is done by pattern projection into the tensor subspaces obtained from the factorization of the signal tensors representing the input signal. However, instead of taking only the intensity signal the novelty of this paper is first to build the Extended Structural Tensor representation from the intensity signal that conveys information on signal intensities, as well as on higher-order statistics of the input signals. This way the higher-order input pattern tensors are built from the training samples. Then, the tensor subspaces are built based on the Higher-Order Singular Value Decomposition of the prototype pattern tensors. Finally, recognition relies on measurements of the distance of a test pattern projected into the tensor subspaces obtained from the training tensors. Due to high-dimensionality of the input data, tensor based methods require high memory and computational resources. However, recent achievements in the technology of the multi-core microprocessors and graphic cards allows real-time operation of the multidimensional methods as is shown and analyzed in this paper based on real examples of object detection in digital images.

Multidimensional NMR inversion without Kronecker products: Multilinear inversion

NASA Astrophysics Data System (ADS)

Medellín, David; Ravi, Vivek R.; Torres-Verdín, Carlos

2016-08-01

Multidimensional NMR inversion using Kronecker products poses several challenges. First, kernel compression is only possible when the kernel matrices are separable, and in recent years, there has been an increasing interest in NMR sequences with non-separable kernels. Second, in three or more dimensions, the singular value decomposition is not unique; therefore kernel compression is not well-defined for higher dimensions. Without kernel compression, the Kronecker product yields matrices that require large amounts of memory, making the inversion intractable for personal computers. Finally, incorporating arbitrary regularization terms is not possible using the Lawson-Hanson (LH) or the Butler-Reeds-Dawson (BRD) algorithms. We develop a minimization-based inversion method that circumvents the above problems by using multilinear forms to perform multidimensional NMR inversion without using kernel compression or Kronecker products. The new method is memory efficient, requiring less than 0.1% of the memory required by the LH or BRD methods. It can also be extended to arbitrary dimensions and adapted to include non-separable kernels, linear constraints, and arbitrary regularization terms. Additionally, it is easy to implement because only a cost function and its first derivative are required to perform the inversion.

Differentially Private Synthesization of Multi-Dimensional Data using Copula Functions

PubMed Central

Li, Haoran; Xiong, Li; Jiang, Xiaoqian

2014-01-01

Differential privacy has recently emerged in private statistical data release as one of the strongest privacy guarantees. Most of the existing techniques that generate differentially private histograms or synthetic data only work well for single dimensional or low-dimensional histograms. They become problematic for high dimensional and large domain data due to increased perturbation error and computation complexity. In this paper, we propose DPCopula, a differentially private data synthesization technique using Copula functions for multi-dimensional data. The core of our method is to compute a differentially private copula function from which we can sample synthetic data. Copula functions are used to describe the dependence between multivariate random vectors and allow us to build the multivariate joint distribution using one-dimensional marginal distributions. We present two methods for estimating the parameters of the copula functions with differential privacy: maximum likelihood estimation and Kendall’s τ estimation. We present formal proofs for the privacy guarantee as well as the convergence property of our methods. Extensive experiments using both real datasets and synthetic datasets demonstrate that DPCopula generates highly accurate synthetic multi-dimensional data with significantly better utility than state-of-the-art techniques. PMID:25405241

Investigation of multidimensional control systems in the state space and wavelet medium

NASA Astrophysics Data System (ADS)

Fedosenkov, D. B.; Simikova, A. A.; Fedosenkov, B. A.

2018-05-01

The notions are introduced of “one-dimensional-point” and “multidimensional-point” automatic control systems. To demonstrate the joint use of approaches based on the concepts of state space and wavelet transforms, a method for optimal control in a state space medium represented in the form of time-frequency representations (maps), is considered. The computer-aided control system is formed on the basis of the similarity transformation method, which makes it possible to exclude the use of reduced state variable observers. 1D-material flow signals formed by primary transducers are converted by means of wavelet transformations into multidimensional concentrated-at-a point variables in the form of time-frequency distributions of Cohen’s class. The algorithm for synthesizing a stationary controller for feeding processes is given here. The conclusion is made that the formation of an optimal control law with time-frequency distributions available contributes to the improvement of transient processes quality in feeding subsystems and the mixing unit. Confirming the efficiency of the method presented is illustrated by an example of the current registration of material flows in the multi-feeding unit. The first section in your paper.

High-performance Thin-layer Chromatographic-densitometric Quantification and Recovery of Bioactive Compounds for Identification of Elite Chemotypes of Gloriosa superba L. Collected from Sikkim Himalayas (India)

PubMed Central

Misra, Ankita; Shukla, Pushpendra Kumar; Kumar, Bhanu; Chand, Jai; Kushwaha, Poonam; Khalid, Md.; Singh Rawat, Ajay Kumar; Srivastava, Sharad

2017-01-01

Background: Gloriosa superba L. (Colchicaceae) is used as adjuvant therapy in gout for its potential antimitotic activity due to high colchicine(s) alkaloids. Objective: This study aimed to develop an easy, cheap, precise, and accurate high-performance thin-layer chromatographic (HPTLC) validated method for simultaneous quantification of bioactive alkaloids (colchicine and gloriosine) in G. superba L. and to identify its elite chemotype(s) from Sikkim Himalayas (India). Methods: The HPTLC chromatographic method was developed using mobile phase of chloroform: acetone: diethyl amine (5:4:1) at λmax of 350 nm. Results: Five germplasms were collected from targeted region, and on morpho-anatomical inspection, no significant variation was observed among them. Quantification data reveal that content of colchicine (Rf: 0.72) and gloriosine (Rf: 0.61) varies from 0.035%–0.150% to 0.006%–0.032% (dry wt. basis). Linearity of method was obtained in the concentration range of 100–400 ng/spot of marker(s), exhibiting regression coefficient of 0.9987 (colchicine) and 0.9983 (gloriosine) with optimum recovery of 97.79 ± 3.86 and 100.023% ± 0.01%, respectively. Limit of detection and limit of quantification were analyzed, respectively, as 6.245, 18.926 and 8.024, 24.316 (ng). Two germplasms, namely NBG-27 and NBG-26, were found to be elite chemotype of both the markers. Conclusion: The developed method is validated in terms of accuracy, recovery, and precision studies as per the ICH guidelines (2005) and can be adopted for the simultaneous quantification of colchicine and gloriosine in phytopharmaceuticals. In addition, this study is relevant to explore the chemotypic variability in metabolite content for commercial and medicinal purposes. SUMMARY An easy, cheap, precise, and accurate high performance thin layer chromatographic (HPTLC) validated method for simultaneous quantification of bioactive alkaloids (colchicine and gloriosine) in G. superba L.Five germplasms were collected from targeted region, and on morpho anatomical inspection, no significant variation was observed among themQuantification data reveal that content of colchicine (Rf: 0.72) and gloriosine (Rf: 0.61) varies from 0.035%–0.150% to 0.006%–0.032% (dry wt. basis)Two germplasms, namely NBG 27 and NBG 26, were found to be elite chemotype of both the markers. PMID:29142436

Development of a green chromatographic method for determination of fat-soluble vitamins in food and pharmaceutical supplement.

PubMed

Kienen, Vanessa; Costa, Willian F; Visentainer, Jesuí V; Souza, Nilson E; Oliveira, Cláudio C

2008-03-15

A green chromatographic analytical method for determination of fat-soluble vitamins (A, E, D3 and K1) in food and pharmaceutical supplement samples is proposed. The method is based on the modification of a C18 column with a 3.00% (w/v) sodium dodecyl sulphate (SDS) aqueous solution at pH 7 (0.02 mol L(-1) phosphate buffer solution) and in the usage of the same surfactant solution as mobile phase with the presence of 15.0% (v/v) butyl alcohol as an organic solvent modifier. After the separation process, the vitamins are detected at 230 nm (K1, D3 and E), 280 nm (A, E, D3 and K1) and 300 nm (K1, D3 and E). The chromatographic procedure yielded precise results (better than 5%) and is able to run one sample in 25 min, consuming 1.5 g of SDS, 90 mg of phosphate and 7.5 mL of butyl alcohol. When the flow rate of the mobile phase is 2 mL min(-1) the retention times are 4.0, 9.6, 13.0 and 22.7 min for D3, A, E and K1 vitamins, respectively; and all peak resolutions are higher than 2. The analytical curves present the following linear equations: area=6290+34852 (vitamin A), R2=0.9998; area=4092+36333 (vitamin E), R2=0.9997; area=-794+30382 (vitamin D3) R2=0.9998 and area=-7175+82621 (vitamin K1), R2=0.9996. The limits of detection and quantification for vitamins A, E, D(3) and K(1) were estimated for a test pharmaceutical vitamin supplement sample as 0.81, 1.12, 0.91 and 0.83 mg L(-1) and 2.43, 3.36, 2.73 and 2.49, respectively. When the proposed method was applied to food and pharmaceutical sample analysis, precise results were obtained (R.S.D.<5% and n=3) and in agreement with those obtained by using the classical chromatographic method that uses methanol and acetonitrile as mobile phase. Here, the traditional usage of toxic organic solvent as mobile phase is avoided, which permits to classify the present method as green.

21 CFR 177.1820 - Styrene-maleic anhydride copolymers.

Code of Federal Regulations, 2010 CFR

2010-04-01

... maleic anhydride monomer content shall be determined by a gas chromatographic method titled “Determination of Residual Maleic Anhydride in Polymers by Gas Chromatography,” which is incorporated by...

21 CFR 177.1820 - Styrene-maleic anhydride copolymers.

Code of Federal Regulations, 2011 CFR

2011-04-01

... maleic anhydride monomer content shall be determined by a gas chromatographic method titled “Determination of Residual Maleic Anhydride in Polymers by Gas Chromatography,” which is incorporated by...

Multi-dimensional Fokker-Planck equation analysis using the modified finite element method

NASA Astrophysics Data System (ADS)

Náprstek, J.; Král, R.

2016-09-01

The Fokker-Planck equation (FPE) is a frequently used tool for the solution of cross probability density function (PDF) of a dynamic system response excited by a vector of random processes. FEM represents a very effective solution possibility, particularly when transition processes are investigated or a more detailed solution is needed. Actual papers deal with single degree of freedom (SDOF) systems only. So the respective FPE includes two independent space variables only. Stepping over this limit into MDOF systems a number of specific problems related to a true multi-dimensionality must be overcome. Unlike earlier studies, multi-dimensional simplex elements in any arbitrary dimension should be deployed and rectangular (multi-brick) elements abandoned. Simple closed formulae of integration in multi-dimension domain have been derived. Another specific problem represents the generation of multi-dimensional finite element mesh. Assembling of system global matrices should be subjected to newly composed algorithms due to multi-dimensionality. The system matrices are quite full and no advantages following from their sparse character can be profited from, as is commonly used in conventional FEM applications in 2D/3D problems. After verification of partial algorithms, an illustrative example dealing with a 2DOF non-linear aeroelastic system in combination with random and deterministic excitations is discussed.

Assessment of health surveys: fitting a multidimensional graded response model.

PubMed

Depaoli, Sarah; Tiemensma, Jitske; Felt, John M

The multidimensional graded response model, an item response theory (IRT) model, can be used to improve the assessment of surveys, even when sample sizes are restricted. Typically, health-based survey development utilizes classical statistical techniques (e.g. reliability and factor analysis). In a review of four prominent journals within the field of Health Psychology, we found that IRT-based models were used in less than 10% of the studies examining scale development or assessment. However, implementing IRT-based methods can provide more details about individual survey items, which is useful when determining the final item content of surveys. An example using a quality of life survey for Cushing's syndrome (CushingQoL) highlights the main components for implementing the multidimensional graded response model. Patients with Cushing's syndrome (n = 397) completed the CushingQoL. Results from the multidimensional graded response model supported a 2-subscale scoring process for the survey. All items were deemed as worthy contributors to the survey. The graded response model can accommodate unidimensional or multidimensional scales, be used with relatively lower sample sizes, and is implemented in free software (example code provided in online Appendix). Use of this model can help to improve the quality of health-based scales being developed within the Health Sciences.

The Effect of Multidimensional Motivation Interventions on Cognitive and Behavioral Components of Motivation: Testing Martin's Model

PubMed Central

Pooragha Roodbarde, Fatemeh; Talepasand, Siavash; Rahimian Boogar, Issac

2017-01-01

Objective: The present study aimed at examining the effect of multidimensional motivation interventions based on Martin's model on cognitive and behavioral components of motivation. Method: The research design was prospective with pretest, posttest, and follow-up, and 2 experimental groups. In this study, 90 students (45 participants in the experimental group and 45 in the control group) constituted the sample of the study, and they were selected by available sampling method. Motivation interventions were implemented for fifteen 60-minute sessions 3 times a week, which lasted for about 2 months. Data were analyzed using repeated measures multivariate variance analysis test. Results: The findings revealed that multidimensional motivation interventions resulted in a significant increase in the scores of cognitive components such as self-efficacy, mastery goal, test anxiety, and feeling of lack of control, and behavioral components such as task management. The results of one-month follow-up indicated the stability of the created changes in test anxiety and cognitive strategies; however, no significant difference was found between the 2 groups at the follow-up in self-efficacy, mastery goals, source of control, and motivation. Conclusion: The research evidence indicated that academic motivation is a multidimensional component and is affected by cognitive and behavioral factors; therefore, researchers, teachers, and other authorities should attend to these factors to increase academic motivation. PMID:28659984

The Effect of Multidimensional Motivation Interventions on Cognitive and Behavioral Components of Motivation: Testing Martin's Model.

PubMed

Pooragha Roodbarde, Fatemeh; Talepasand, Siavash; Rahimian Boogar, Issac

2017-04-01

Objective: The present study aimed at examining the effect of multidimensional motivation interventions based on Martin's model on cognitive and behavioral components of motivation. Method: The research design was prospective with pretest, posttest, and follow-up, and 2 experimental groups. In this study, 90 students (45 participants in the experimental group and 45 in the control group) constituted the sample of the study, and they were selected by available sampling method. Motivation interventions were implemented for fifteen 60-minute sessions 3 times a week, which lasted for about 2 months. Data were analyzed using repeated measures multivariate variance analysis test. Results: The findings revealed that multidimensional motivation interventions resulted in a significant increase in the scores of cognitive components such as self-efficacy, mastery goal, test anxiety, and feeling of lack of control, and behavioral components such as task management. The results of one-month follow-up indicated the stability of the created changes in test anxiety and cognitive strategies; however, no significant difference was found between the 2 groups at the follow-up in self-efficacy, mastery goals, source of control, and motivation. Conclusion: The research evidence indicated that academic motivation is a multidimensional component and is affected by cognitive and behavioral factors; therefore, researchers, teachers, and other authorities should attend to these factors to increase academic motivation.

Improved δ(13)C analysis of amino sugars in soil by ion chromatography-oxidation-isotope ratio mass spectrometry.

PubMed

Dippold, Michaela A; Boesel, Stefanie; Gunina, Anna; Kuzyakov, Yakov; Glaser, Bruno

2014-03-30

Amino sugars build up microbial cell walls and are important components of soil organic matter. To evaluate their sources and turnover, δ(13)C analysis of soil-derived amino sugars by liquid chromatography was recently suggested. However, amino sugar δ(13)C determination remains challenging due to (1) a strong matrix effect, (2) CO2 -binding by alkaline eluents, and (3) strongly different chromatographic behavior and concentrations of basic and acidic amino sugars. To overcome these difficulties we established an ion chromatography-oxidation-isotope ratio mass spectrometry method to improve and facilitate soil amino sugar analysis. After acid hydrolysis of soil samples, the extract was purified from salts and other components impeding chromatographic resolution. The amino sugar concentrations and δ(13)C values were determined by coupling an ion chromatograph to an isotope ratio mass spectrometer. The accuracy and precision of quantification and δ(13)C determination were assessed. Internal standards enabled correction for losses during analysis, with a relative standard deviation <6%. The higher magnitude peaks of basic than of acidic amino sugars required an amount-dependent correction of δ(13)C values. This correction improved the accuracy of the determination of δ(13)C values to <1.5‰ and the precision to <0.5‰ for basic and acidic amino sugars in a single run. This method enables parallel quantification and δ(13)C determination of basic and acidic amino sugars in a single chromatogram due to the advantages of coupling an ion chromatograph to the isotope ratio mass spectrometer. Small adjustments of sample amount and injection volume are necessary to optimize precision and accuracy for individual soils. Copyright © 2014 John Wiley & Sons, Ltd.

High-resolution hydrodynamic chromatographic separation of large DNA using narrow, bare open capillaries: a rapid and economical alternative technology to pulsed-field gel electrophoresis?

PubMed

Liu, Lei; Veerappan, Vijaykumar; Pu, Qiaosheng; Cheng, Chang; Wang, Xiayan; Lu, Liping; Allen, Randy D; Guo, Guangsheng

2014-01-07

A high-resolution, rapid, and economical hydrodynamic chromatographic (HDC) method for large DNA separations in free solution was developed using narrow (5 μm diameter), bare open capillaries. Size-based separation was achieved in a chromatographic format with larger DNA molecules being eluting faster than smaller ones. Lambda DNA Mono Cut Mix was baseline-separated with the percentage resolutions generally less than 9.0% for all DNA fragments (1.5 to 48.5 kbp) tested in this work. High efficiencies were achieved for large DNA from this chromatographic technique, and the number of theoretical plates reached 3.6 × 10(5) plates for the longest (48.5 kbp) and 3.7 × 10(5) plates for the shortest (1.5 kbp) fragments. HDC parameters and performances were also discussed. The method was further applied for fractionating large DNA fragments from real-world samples (SacII digested Arabidopsis plant bacterial artificial chromosome (BAC) DNA and PmeI digested Rice BAC DNA) to demonstrate its feasibility for BAC DNA finger printing. Rapid separation of PmeI digested Rice BAC DNA covering from 0.44 to 119.041 kbp was achieved in less than 26 min. All DNA fragments of these samples were baseline separated in narrow bare open capillaries, while the smallest fragment (0.44 kbp) was missing in pulsed-field gel electrophoresis (PFGE) separation mode. It is demonstrated that narrow bare open capillary chromatography can realize a rapid separation for a wide size range of DNA mixtures that contain both small and large DNA fragments in a single run.

Current trends in green liquid chromatography for the analysis of pharmaceutically active compounds in the environmental water compartments.

PubMed

Shaaban, Heba; Górecki, Tadeusz

2015-01-01

Green analytical chemistry is an aspect of green chemistry which introduced in the late nineties. The main objectives of green analytical chemistry are to obtain new analytical technologies or to modify an old method to incorporate procedures that use less hazardous chemicals. There are several approaches to achieve this goal such as using environmentally benign solvents and reagents, reducing the chromatographic separation times and miniaturization of analytical devices. Traditional methods used for the analysis of pharmaceutically active compounds require large volumes of organic solvents and generate large amounts of waste. Most of them are volatile and harmful to the environment. With the awareness about the environment, the development of green technologies has been receiving increasing attention aiming at eliminating or reducing the amount of organic solvents consumed everyday worldwide without loss in chromatographic performance. This review provides the state of the art of green analytical methodologies for environmental analysis of pharmaceutically active compounds in the aquatic environment with special emphasis on strategies for greening liquid chromatography (LC). The current trends of fast LC applied to environmental analysis, including elevated mobile phase temperature, as well as different column technologies such as monolithic columns, fully porous sub-2 μm and superficially porous particles are presented. In addition, green aspects of gas chromatography (GC) and supercritical fluid chromatography (SFC) will be discussed. We pay special attention to new green approaches such as automation, miniaturization, direct analysis and the possibility of locating the chromatograph on-line or at-line as a step forward in reducing the environmental impact of chromatographic analyses. Copyright © 2014 Elsevier B.V. All rights reserved.

[Development of an automatic vacuum liquid chromatographic device and its application in the separation of the components from Schisandra chinensis (Turz) Baill].

PubMed

Zhu, Jingbo; Liu, Baoyue; Shan, Shibo; Ding, Yanl; Kou, Zinong; Xiao, Wei

2015-08-01

In order to meet the needs of efficient purification of products from natural resources, this paper developed an automatic vacuum liquid chromatographic device (AUTO-VLC) and applied it to the component separation of petroleum ether extracts of Schisandra chinensis (Turcz) Baill. The device was comprised of a solvent system, a 10-position distribution valve, a 3-position changes valve, dynamic axis compress chromatographic columns with three diameters, and a 10-position fraction valve. The programmable logic controller (PLC) S7- 200 was adopted to realize the automatic control and monitoring of the mobile phase changing, column selection, separation time setting and fraction collection. The separation results showed that six fractions (S1-S6) of different chemical components from 100 g Schisandra chinensis (Turcz) Baill. petroleum ether phase were obtained by the AUTO-VLC with 150 mm diameter dynamic axis compress chromatographic column. A new method used for the VLC separation parameters screened by using multiple development TLC was developed and confirmed. The initial mobile phase of AUTO-VLC was selected by taking Rf of all the target compounds ranging from 0 to 0.45 for fist development on the TLC; gradient elution ratio was selected according to k value (the slope of the linear function of Rf value and development times on the TLC) and the resolution of target compounds; elution times (n) were calculated by the formula n ≈ ΔRf/k. A total of four compounds with the purity more than 85% and 13 other components were separated from S5 under the selected conditions for only 17 h. Therefore, the development of the automatic VLC and its method are significant to the automatic and systematic separation of traditional Chinese medicines.

Three-way principal component analysis of the volatile fraction by HS-SPME/GC of aceto balsamico tradizionale of modena.

PubMed

Cocchi, Marina; Durante, Caterina; Grandi, Margherita; Manzini, Daniela; Marchetti, Andrea

2008-01-15

The present research is aimed at monitoring the evolution of the volatile organic compounds of different samples of aceto balsamico tradizionale of modena (ABTM) during ageing. The flavouring compounds, headspace fraction, of the vinegars of four batterie were sampled by solid phase microextraction technique (SPME), and successively analysed by gas chromatography. Obtaining a data set characterized by different sources of variability such as, different producers, samples of different age and chromatographic profile. The gas chromatographic signals were processed by a three-way data analysis method (Tucker3), which allows an easy visualisation of the data by furnishing a distinct set of graphs for each source of variability. The obtained results indicate that the samples can be separated according to their age highlighting the chemical constituents, which play a major role for their differentiation. The present study represents an example of how the application of Tucker3 models, on gas chromatographic signals may help to follow the transformation processes of food products.

Analytical instrument with apparatus and method for sample concentrating

DOEpatents

Zaromb, S.

1986-08-04

A system for analysis of trace concentrations of contaminants in air includes a portable liquid chromatograph and a preconcentrator for the contaminants to be analyzed. The preconcentrator includes a sample bag having an inlet valve and an outlet valve for collecting an air sample. When the sample is collected the sample bag is connected in series with a sorbing apparatus in a recirculation loop. The sorbing apparatus has an inner gas-permeable container containing a sorbent material and an outer gas-impermeable container. The sample is circulated through the outer container and around the inner container for trapping and preconcentrating the contaminants in the sorbent material. The sorbent material may be a liquid having the same composition as the mobile phase of the chromatograph for direct injection thereinto. Alternatively, the sorbent material may be a porous, solid body, to which mobile phase liquid is added after preconcentration of the contaminants for dissolving the contaminants, the liquid solution then being withdrawn for injection into the chromatograph.

Method for preconcentrating a sample for subsequent analysis

DOEpatents

Zaromb, Solomon

1990-01-01

A system for analysis of trace concentration of contaminants in air includes a portable liquid chromatograph and a preconcentrator for the contaminants to be analyzed. The preconcentrator includes a sample bag having an inlet valve and an outlet valve for collecting an air sample. When the sample is collected the sample bag is connected in series with a sorbing apparatus in a recirculation loop. The sorbing apparatus has an inner gas-permeable container containing a sorbent material and an outer gas-impermeable container. The sample is circulated through the outer container and around the inner container for trapping and preconcentrating the contaminants in the sorbent material. The sorbent material may be a liquid having the same composition as the mobile phase of the chromatograph for direct injection thereinto. Alternatively, the sorbent material may be a porous, solid body, to which mobile phase liquid is added after preconcentration of the contaminants for dissolving the contaminants, the liquid solution then being withdrawn for injection into the chromatograph.

Portable system and method combining chromatography and array of electrochemical sensors

DOEpatents

Zaromb, Solomon; Stetter, Joseph R.

1989-01-01

A portable system for analyzing a fluid sample includes a small, portable, low-pressure and low-power chromatographic analyzer and a chemical parameter spectrometry monitor including an array of sensors for detecting, identifying and measuring the concentrations of a variety of components in the eluent from the chromatographic analyzer. The monitor includes one or more operating condition controllers which may be used to change one or more of the operating conditions during exposure of the sensors to the eluent from the chromatography analyzer to form a response pattern which is then compared with a library of previously established patterns. Gas and liquid chromatographic embodiments are disclosed. In the gas embodiment, the operating condition controllers include heated filaments which may convert electrochemically inactive components to electrochemically active products. In the liquid chromatography embodiment, low-power, liquid-phase equivalents of heated filaments are used with appropriate sensors. The library response patterns may be divided into subsets and the formed pattern may be assigned for comparison only with the patterns of a particular subset.

[Quantitative structure-gas chromatographic retention relationship of polycyclic aromatic sulfur heterocycles using molecular electronegativity-distance vector].

PubMed

Li, Zhenghua; Cheng, Fansheng; Xia, Zhining

2011-01-01

The chemical structures of 114 polycyclic aromatic sulfur heterocycles (PASHs) have been studied by molecular electronegativity-distance vector (MEDV). The linear relationships between gas chromatographic retention index and the MEDV have been established by a multiple linear regression (MLR) model. The results of variable selection by stepwise multiple regression (SMR) and the powerful predictive abilities of the optimization model appraised by leave-one-out cross-validation showed that the optimization model with the correlation coefficient (R) of 0.994 7 and the cross-validated correlation coefficient (Rcv) of 0.994 0 possessed the best statistical quality. Furthermore, when the 114 PASHs compounds were divided into calibration and test sets in the ratio of 2:1, the statistical analysis showed our models possesses almost equal statistical quality, the very similar regression coefficients and the good robustness. The quantitative structure-retention relationship (QSRR) model established may provide a convenient and powerful method for predicting the gas chromatographic retention of PASHs.

Chromatographic background drift correction coupled with parallel factor analysis to resolve coelution problems in three-dimensional chromatographic data: quantification of eleven antibiotics in tap water samples by high-performance liquid chromatography coupled with a diode array detector.

PubMed

Yu, Yong-Jie; Wu, Hai-Long; Fu, Hai-Yan; Zhao, Juan; Li, Yuan-Na; Li, Shu-Fang; Kang, Chao; Yu, Ru-Qin

2013-08-09

Chromatographic background drift correction has been an important field of research in chromatographic analysis. In the present work, orthogonal spectral space projection for background drift correction of three-dimensional chromatographic data was described in detail and combined with parallel factor analysis (PARAFAC) to resolve overlapped chromatographic peaks and obtain the second-order advantage. This strategy was verified by simulated chromatographic data and afforded significant improvement in quantitative results. Finally, this strategy was successfully utilized to quantify eleven antibiotics in tap water samples. Compared with the traditional methodology of introducing excessive factors for the PARAFAC model to eliminate the effect of background drift, clear improvement in the quantitative performance of PARAFAC was observed after background drift correction by orthogonal spectral space projection. Copyright © 2013 Elsevier B.V. All rights reserved.

Fluorescence polarization immunoassays for rapid, accurate, and sensitive determination of mycotoxins

USDA-ARS?s Scientific Manuscript database

Analytical methods for the determination of mycotoxins in foods are commonly based on chromatographic techniques (GC, HPLC or LC-MS). Although these methods permit a sensitive and accurate determination of the analyte, they require skilled personnel and are time-consuming, expensive, and unsuitable ...

Microfabricated capillary electrophoresis chip and method for simultaneously detecting multiple redox labels

DOEpatents

Mathies, Richard A.; Singhal, Pankaj; Xie, Jin; Glazer, Alexander N.

2002-01-01

This invention relates to a microfabricated capillary electrophoresis chip for detecting multiple redox-active labels simultaneously using a matrix coding scheme and to a method of selectively labeling analytes for simultaneous electrochemical detection of multiple label-analyte conjugates after electrophoretic or chromatographic separation.

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.

Bayesian reconstruction of projection reconstruction NMR (PR-NMR).

PubMed

Yoon, Ji Won

2014-11-01

Projection reconstruction nuclear magnetic resonance (PR-NMR) is a technique for generating multidimensional NMR spectra. A small number of projections from lower-dimensional NMR spectra are used to reconstruct the multidimensional NMR spectra. In our previous work, it was shown that multidimensional NMR spectra are efficiently reconstructed using peak-by-peak based reversible jump Markov chain Monte Carlo (RJMCMC) algorithm. We propose an extended and generalized RJMCMC algorithm replacing a simple linear model with a linear mixed model to reconstruct close NMR spectra into true spectra. This statistical method generates samples in a Bayesian scheme. Our proposed algorithm is tested on a set of six projections derived from the three-dimensional 700 MHz HNCO spectrum of a protein HasA. Copyright © 2014 Elsevier Ltd. All rights reserved.

Solution of system of multidimensional differential equations in X for identification of gold nanoparticles on fibers with elimination of uncertainty

NASA Astrophysics Data System (ADS)

Dobrovolskaya, T. A.; Emelyanov, V. M.; Emelyanov, V. V.

2018-05-01

There are the results of the compilation and solution of a system of multidimensional differential correlation equations of distribution ellipses in the identification of colloidal gold nanoparticles on polyester fibers with multi-dimensional correlation components of Raman polarization spectra. A proposed method is to increase the accuracy and speed of identification of silver nanoparticles on polyester fibers, taking into account the longitudinal and transverse polarization of laser radiation over the entire spectral range, analyzing in sequence and in order simultaneously two peaks along the X-transverse and along the Y-along the fibers. During a solution of the system using a nonlinear quadratic and differential equation with respect to X, an uncertainty arises, the elimination of which is numerical addition Δ = + 0.02985

Lithium, magnesium and sulfur purification from seawater using an ion chromatograph with a fraction collector system for stable isotope measurements.

PubMed

Yoshimura, Toshihiro; Araoka, Daisuke; Tamenori, Yusuke; Kuroda, Junichiro; Kawahata, Hodaka; Ohkouchi, Naohiko

2018-01-05

We describe the mass descrimination and validation of an offline method for purification of Li, Mg and S with an ion chromatograph coupled to an automated fraction collector for use prior to stable isotope measurements. Significant sub-fraction mass fractionation was observed for both the Li and the Mg stable isotope ratios. The lighter Li and heavier Mg isotopes were preferentially retained by the column, resulting in 7 Li/ 6 Li and 26 Mg/ 24 Mg biases up to 85.8‰ and 0.95‰, respectively. The isotopic compositions of Li, Mg, and S separated from seawater were δ 7 Li L-SVEC  = +30.9‰, δ 26 Mg DSM3  = -0.83 ± 0.10‰, and δ 34 S VCDT  = +19.4 ± 0.6‰; each chromatographic peak was completely recovered, and the results were in good agreement with the published values regardless of whether or not chemical suppressor was used. The purification method enables multi-isotope analysis of a sample using various mass spectrometry techniques, such as multiple-collector inductively coupled plasma and thermal ionization mass spectrometry. Copyright © 2017 Elsevier B.V. All rights reserved.

Alternative measures of lipophilicity: from octanol-water partitioning to IAM retention.

PubMed

Giaginis, Costas; Tsantili-Kakoulidou, Anna

2008-08-01

This review describes lipophilicity parameters currently used in drug design and QSAR studies. After a short historical overview, the complex nature of lipophilicity as the outcome of polar/nonpolar inter- and intramolecular interactions is analysed and considered as the background for the discussion of the different lipophilicity descriptors. The first part focuses on octanol-water partitioning of neutral and ionisable compounds, evaluates the efficiency of predictions and provides a short description of the experimental methods for the determination of distribution coefficients. A next part is dedicated to reversed-phase chromatographic techniques, HPLC and TLC in lipophilicity assessment. The two methods are evaluated for their efficiency to simulate octanol-water and the progress achieved in the refinement of suitable chromatographic conditions, in particular in the field of HPLC, is outlined. Liposomes as direct models of biological membranes are examined and phospolipophilicity is compared to the traditional lipophilicity concept. Difficulties associated with liposome-water partitioning are discussed. The last part focuses on Immobilised Artificial Membrane (IAM) chromatography as an alternative which combines membrane simulation with rapid measurements. IAM chromatographic retention is compared to octanol-water and liposome-water partitioning as well as to reversed-phase retention and its potential to predict biopartitioning and biological activities is discussed.

[Quantitative relationship between gas chromatographic retention time and structural parameters of alkylphenols].

PubMed

Ruan, Xiaofang; Zhang, Ruisheng; Yao, Xiaojun; Liu, Mancang; Fan, Botao

2007-03-01

Alkylphenols are a group of permanent pollutants in the environment and could adversely disturb the human endocrine system. It is therefore important to effectively separate and measure the alkylphenols. To guide the chromatographic analysis of these compounds in practice, the development of quantitative relationship between the molecular structure and the retention time of alkylphenols becomes necessary. In this study, topological, constitutional, geometrical, electrostatic and quantum-chemical descriptors of 44 alkylphenols were calculated using a software, CODESSA, and these descriptors were pre-selected using the heuristic method. As a result, three-descriptor linear model (LM) was developed to describe the relationship between the molecular structure and the retention time of alkylphenols. Meanwhile, the non-linear regression model was also developed based on support vector machine (SVM) using the same three descriptors. The correlation coefficient (R(2)) for the LM and SVM was 0.98 and 0. 92, and the corresponding root-mean-square error was 0. 99 and 2. 77, respectively. By comparing the stability and prediction ability of the two models, it was found that the linear model was a better method for describing the quantitative relationship between the retention time of alkylphenols and the molecular structure. The results obtained suggested that the linear model could be applied for the chromatographic analysis of alkylphenols with known molecular structural parameters.

A novel liquid chromatography method using diode-array detector for the determination of oleuropein in dietary supplements.

PubMed

Bertolini, Tiziana; Vicentini, Lorenza; Boschetti, Silvia; Andreatta, Paolo; Gatti, Rita

2016-09-10

A simple and fast chromatographic method using ultraviolet diode-array detector (UV-DAD) was developed for the automatic high performance liquid chromatography (HPLC) determination of the title of oleuropein in a new dietary supplements in form of effervescent granules. The chromatographic separations were performed on a C18 core-shell column with detection at λ=232nm. The mobile phase consisted of deionized water with 0.1% TFA and acetonitrile under gradient conditions at a flow-rate of 0.8mL/min. Oleuropein and oleuroside present in the raw material were characterized by high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS). The validation of the analytical procedure has been performed determining the following parameters: specificity, linearity, repeatability, reproducibility, accuracy, limit of quantification (LOQ), stability of the standard and sample solutions. Linear response was observed in fortified placebo solutions (determination coefficient: 0.9998). Intra-day precision (relative standard deviation, RSD) was ≤5.0% for peak area and for retention times (tR) without significant differences between intra- and inter-day data. The limits of quantitation (LOQ) was about 5μg/mL and 9pmol/inject. Oleuropein recovery studies gave good results (99.9%) with a R.S.D. of 0.5%. The speed of analysis and the stability of the solutions with a fluctuation Δ (%) ≤2.0 at room temperature means an undoubted advantage of the method allowing the simultaneous preparation of many samples and consecutive chromatographic analyses by using an autosampler. The developed method is suitable for the quality control of oleuropein in raw material and industrial products. The method can be applied in any analytical laboratory not requiring a sophisticated instrumentation. Copyright © 2016 Elsevier B.V. All rights reserved.

Analysis of amide compounds in different parts of Piper ovatum Vahl by high-performance liquid chromatographic

PubMed Central

Silva, Daniel R.; Brenzan, Mislaine A.; Kambara, Lauro M.; Cortez, Lucia E. R.; Cortez, Diógenes A. G.

2013-01-01

Background: Piper ovatum (Piperaceae) has been used in traditional medicine for the treatment of inflammations and as an analgesic. Previous studies have showed important biological activities of the extracts and amides from P. ovatum leaves. Objective: In this study, a high-performance liquid chromatographic (HPLC) method was developed and validated for quantitative determination of the amides in different parts of Piper ovatum. Materials and Methods: The analysis was carried out on a Metasil ODS column (150 × 4.6 mm, 5μm) at room temperature. HPLC conditions were as follows: acetonitrile (A), and water (B), 1.0% acetic acid. The gradient elution used was 0–30 min, 0-60% A; 30–40 min, 60% A. Flow rate used was 1.0mL/min, and detection at 280nm. Results: The validation using piperlonguminine, as the standard, demonstrated that the method shows linearity (linear correlation coefficient = 0.998), precision (relative standard deviation <5%) and accuracy (mean recovery = 103.78%) in the concentration range 31.25 – 500μg/mL. The limit of detection and quantification were 1.21 and 4.03μg/mL, respectively. This method allowed the identification and quantification of piperlonguminine and piperovatine in the hydroethanolic extracts of P. ovatum obtained from the leaves, stems and roots. All the extracts showed the same chromatographic profile. The leaves and roots contained the highest concentrations of piperlonguminine and the stems and leaves showed the most concentrations of piperovatine. Conclusion: This HPLC method is suitable for routine quantitative analysis of amides in extracts of Piper ovatum and phytopharmaceuticals containing this herb. PMID:24174818

UPLC and LC-MS studies on degradation behavior of irinotecan hydrochloride and development of a validated stability-indicating ultra-performance liquid chromatographic method for determination of irinotecan hydrochloride and its impurities in pharmaceutical dosage forms.

PubMed

Kumar, Navneet; Sangeetha, Dhanaraj; Reddy, Sunil P

2012-10-01

The objective of the current investigation was to study the degradation behavior of irinotecan hydrochloride under different International Conference on Harmonization (ICH) recommended stress conditions using ultra-performance liquid chromatography and liquid chromatography-mass spectrometry and to establish a validated stability-indicating reverse-phase ultra-performance liquid chromatographic method for the quantitative determination of irinotecan hydrochloride and its seven impurities and degradation products in pharmaceutical dosage forms. Irinotecan hydrochloride was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. Irinotecan hydrochloride was found to degrade significantly in oxidative and base hydrolysis and photolytic degradation conditions. The degradation products were well resolved from the main peak and its impurities, thus proving the stability-indicating power of the method. Chromatographic separation was achieved on a Waters Acquity BEH C8 (100 × 2.1 mm) 1.7-µm column with a mobile phase containing a gradient mixture of solvent A (0.02M KH(2)PO(4) buffer, pH 3.4) and solvent B (a mixture of acetonitrile and methanol in the ratio of 62:38 v/v). The mobile phase was delivered at a flow rate of 0.3 mL/min with ultraviolet detection at 220 nm. The run time was 8 min, within which irinotecan and its seven impurities and degradation products were satisfactorily separated. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness. This method was also suitable for the assay determination of irinotecan hydrochloride in pharmaceutical dosage forms.

COREPA-M: NEW MULTI-DIMENSIONAL FUNCTIONALITY OF THE COREPA METHOD

EPA Science Inventory

The COmmon REactivity PAttern (COREPA) method is a recently developed pattern recognition technique accounting for conformational flexibility of chemicals in 3-D quantitative structure-activity relationships (QSARs). The method is based on the assumption that non-congeneric chemi...

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.

[The elaboration of gas chromatographic method of the determination of N-nitrosamines (N-nitrosodimethylamine, N-nitrosodiethylamine) in biological samples (urine)].

PubMed

Zaytseva, N V; Ulanova, T S; Nurislamova, T V; Popova, N A

2014-01-01

The issues of the elaboration of a method for the determination of N-nitrosamines (N-nitrosodimethylamine, N-nitrosodiethylamine) in urine by means of the method of capillary gas chromatography with the use of a thermionic detector are considered. There were performed investigations on the study of the efficacy of the extraction of N-nitrosamines from the urine by steam distillation and gas chromatographic detection of headspace. With the aim of the maximal recovery of N-nitrosamines from the urine and setting parameters of the extraction two method were used to prepare the bioassay for the analysis the alkalization with potassium hydroxide and the addition of salting out reagent--neutral salts of alkali and alkaline earth metals. During the process of performed studies there was found that the greatest degree of extraction of N-nitrosamines from the urine by the method of headspace analysis is achieved if using the salting-out agent in an amount of 16 g of sodium sulfate and for N-nitrosodimethylamine is 99%, for N-nitrosodiethylamine--100%.

Determination of lysine content based on an in situ pretreatment and headspace gas chromatographic measurement technique.

PubMed

Wan, Xiao-Fang; Liu, Bao-Lian; Yu, Teng; Yan, Ning; Chai, Xin-Sheng; Li, You-Ming; Chen, Guang-Xue

2018-05-01

This work reports on a simple method for the determination of lysine content by an in situ sample pretreatment and headspace gas chromatographic measurement (HS-GC) technique, based on carbon dioxide (CO 2 ) formation from the pretreatment reaction (between lysine and ninhydrin solution) in a closed vial. It was observed that complete lysine conversion to CO 2 could be achieved within 60 min at 60 °C in a phosphate buffer medium (pH = 4.0), with a minimum molar ratio of ninhydrin/lysine of 16. The results showed that the method had a good precision (RSD < 5.23%) and accuracy (within 6.80%), compared to the results measured by a reference method (ninhydrin spectroscopic method). Due to the feature of in situ sample pretreatment and headspace measurement, the present method becomes very simple and particularly suitable to be used for batch sample analysis in lysine-related research and applications. Graphical abstract The flow path of the reaction and HS-GC measurement for the lysine analysis.

Simplified multiple headspace extraction gas chromatographic technique for determination of monomer solubility in water.

PubMed

Chai, X S; Schork, F J; DeCinque, Anthony

2005-04-08

This paper reports an improved headspace gas chromatographic (GC) technique for determination of monomer solubilities in water. The method is based on a multiple headspace extraction GC technique developed previously [X.S. Chai, Q.X. Hou, F.J. Schork, J. Appl. Polym. Sci., in press], but with the major modification in the method calibration technique. As a result, only a few iterations of headspace extraction and GC measurement are required, which avoids the "exhaustive" headspace extraction, and thus the experimental time for each analysis. For highly insoluble monomers, effort must be made to minimize adsorption in the headspace sampling channel, transportation conduit and capillary column by using higher operating temperature and a short capillary column in the headspace sampler and GC system. For highly water soluble monomers, a new calibration method is proposed. The combinations of these technique modifications results in a method that is simple, rapid and automated. While the current focus of the authors is on the determination of monomer solubility in aqueous solutions, the method should be applicable to determination of solubility of any organic in water.

Determination of naltrexone and 6beta-naltrexol in human blood: comparison of high-performance liquid chromatography with spectrophotometric and tandem-mass-spectrometric detection.

PubMed

Brünen, Sonja; Krüger, Ralf; Finger, Susann; Korf, Felix; Kiefer, Falk; Wiedemann, Klaus; Lackner, Karl J; Hiemke, Christoph

2010-02-01

We present data for a comparison of a liquid-chromatographic method coupled with tandem mass spectrometry (LC-MS/MS) and a high-performance liquid-chromatographic method with column switching and UV spectrophotometric detection. The two methods were developed for determination of naltrexone and 6beta-naltrexol in blood serum or plasma aiming to be used for therapeutic drug monitoring to guide the treatment of patients with naltrexone. For the high-performance liquid chromatography (HPLC)/UV detection, online sample cleanup was conducted on Perfect Bond C(18) material with 2% (vol/vol) acetonitrile in deionized water. Drugs were separated on a C(18) column using 11.5% (vol/vol) acetonitrile and 0.4% (vol/vol) N,N,N,N-tetramethylethylenediamine within 20 min. LC-MS/MS used naltrexone-d (3) and 6beta-naltrexol-d (4) as internal standards. After protein precipitation, the chromatographic separation was performed on a C(18) column by applying a methanol gradient (5-100%, vol/vol) with 0.1% formic acid over 9.5 min. The HPLC/UV method was found to be linear for concentrations ranging from 2 to 100 ng/ml, with a regression correlation coefficient of r (2) > 0.998 for naltrexone and 6beta-naltrexol. The limit of quantification was 2 ng/ml for naltrexone and 6beta-naltrexol. For the LC-MS/MS method the calibration curves were linear (r(2) > 0.999) from 0.5 to 200 ng/ml for both substances, and the limit of quantification was 0.5 ng/ml. The concentrations measured by the two methods correlated significantly for both substances (r(2) > 0.967; p < 0.001). Both methods could be used for therapeutic drug monitoring. The HPLC/UV method was advantageous regarding automatization and costs, whereas LC-MS/MS was superior with regard to sensitivity.

Identification of marker proteins for the adulteration of meat products with soybean proteins by multidimensional liquid chromatography-tandem mass spectrometry.

PubMed

Leitner, Alexander; Castro-Rubio, Florentina; Marina, Maria Luisa; Lindner, Wolfgang

2006-09-01

Soybean proteins are frequently added to processed meat products for economic reasons and to improve their functional properties. Monitoring of the addition of soybean protein to meat products is of high interest due to the existence of regulations forbidding or limiting the amount of soybean proteins that can be added during the processing of meat products. We have used chromatographic prefractionation on the protein level by perfusion liquid chromatography to isolate peaks of interest from extracts of soybean protein isolate (SPI) and of meat products containing SPI. After enzymatic digestion using trypsin, the collected fractions were analyzed by nanoflow liquid chromatography-tandem mass spectrometry. Several variants and subunits of the major seed proteins, glycinin and beta-conglycinin, were identified in SPI, along with two other proteins. In soybean-protein-containing meat samples, different glycinin A subunits could be identified from the peak discriminating between samples with and without soybean proteins added. Among those, glycinin G4 subunit A4 was consistently found in all samples. Consequently, this protein (subunit) can be used as a target for new analytical techniques in the course of identifying the addition of soybean protein to meat products.

A high-throughput 2D-analytical technique to obtain single protein parameters from complex cell lysates for in silico process development of ion exchange chromatography.

PubMed

Kröner, Frieder; Elsäßer, Dennis; Hubbuch, Jürgen

2013-11-29

The accelerating growth of the market for biopharmaceutical proteins, the market entry of biosimilars and the growing interest in new, more complex molecules constantly pose new challenges for bioseparation process development. In the presented work we demonstrate the application of a multidimensional, analytical separation approach to obtain the relevant physicochemical parameters of single proteins in a complex mixture for in silico chromatographic process development. A complete cell lysate containing a low titre target protein was first fractionated by multiple linear salt gradient anion exchange chromatography (AEC) with varying gradient length. The collected fractions were subsequently analysed by high-throughput capillary gel electrophoresis (HT-CGE) after being desalted and concentrated. From the obtained data of the 2D-separation the retention-volumes and the concentration of the single proteins were determined. The retention-volumes of the single proteins were used to calculate the related steric-mass action model parameters. In a final evaluation experiment the received parameters were successfully applied to predict the retention behaviour of the single proteins in salt gradient AEC. Copyright © 2013 Elsevier B.V. All rights reserved.

The NOSAMS sample preparation laboratory in the next millenium: Progress after the WOCE program

NASA Astrophysics Data System (ADS)

Gagnon, Alan R.; McNichol, Ann P.; Donoghue, Joanne C.; Stuart, Dana R.; von Reden, Karl; Nosams

2000-10-01

Since 1991, the primary charge of the National Ocean Sciences AMS (NOSAMS) facility at the Woods Hole Oceanographic Institution has been to supply high throughput, high precision AMS 14C analyses for seawater samples collected as part of the World Ocean Circulation Experiment (WOCE). Approximately 13,000 samples taken as part of WOCE should be fully analyzed by the end of Y2K. Additional sample sources and techniques must be identified and incorporated if NOSAMS is to continue in its present operation mode. A trend in AMS today is the ability to routinely process and analyze radiocarbon samples that contain tiny amounts (<100 μg) of carbon. The capability to mass-produce small samples for 14C analysis has been recognized as a major facility goal. The installation of a new 134-position MC-SNICS ion source, which utilizes a smaller graphite target cartridge than presently used, is one step towards realizing this goal. New preparation systems constructed in the sample preparation laboratory (SPL) include an automated bank of 10 small-volume graphite reactors, an automated system to process organic carbon samples, and a multi-dimensional preparative capillary gas chromatograph (PCGC).

Multi-Dimensional Asymptotically Stable 4th Order Accurate Schemes for the Diffusion Equation

NASA Technical Reports Server (NTRS)

Abarbanel, Saul; Ditkowski, Adi

1996-01-01

An algorithm is presented which solves the multi-dimensional diffusion equation on co mplex shapes to 4th-order accuracy and is asymptotically stable in time. This bounded-error result is achieved by constructing, on a rectangular grid, a differentiation matrix whose symmetric part is negative definite. The differentiation matrix accounts for the Dirichlet boundary condition by imposing penalty like terms. Numerical examples in 2-D show that the method is effective even where standard schemes, stable by traditional definitions fail.

Paired-ion chromatography and high performance liquid chromatography of labetalol in feeds.

PubMed

Townley, E R; Ross, B

1980-11-01

A high performance liquid chromatographic (HPLC) method using reverse phase paired-ion chromatography and ultraviolet detection at 280 nm has been developed to determine labetalol, an alpha and beta adrenoceptor blocking agent, in Purina No. 5001 rodent chow. The method is simple and rapid, and demonstrates a separation technique applicable to other acidic and basic drugs. It requires only extraction of the drug with methanol--water--acetic acid (66 + 33 + 1) and separation of insoluble material by filtration before HPLC. Labetalol, is chromatographically separated from soluble feed components by means of a microBondapak C18 column and methanol--water--acetic acid (66 + 33 + 1) mobile phase, 0.005M with respect to sodium dioctylsulfosuccinate paired-ion reagent. Average recovery is 98.7% with a relative standard deviation of +/- 2.3% for the equipment described.

Determination of ammonium in a buddingtonite sample by ion-chromatography

USGS Publications Warehouse

Klock, P.R.; Lamothe, P.J.

1986-01-01

An ion-chromatographic method for the direct determination of ammonium, potassium, and sodium in geologic materials is described. Samples are decomposed with a mixture of hydrofluoric and hydrochloric acids in a sealed polycarbonate bottle heated in a microwave oven. The ion-chromatograph separates the cations and determines them by conductivity measurement. The ammonium concentrations thus determined have been verified by use of an ammonia-specific electrode. A total of 32 analyses of ammonium salts by both techniques showed an average error of -4%, with a relative standard deviation (RSD) of 6%. The ammonium concentrations found in a buddingtonite sample had an RSD of 2.2% and their mean agreed with that obtained by the Kjeldahl method. By use of the prescribed dilution of the sample, detection limits of 0.1% can be achieved for all three cations. ?? 1986.

Synthesis and chromatographic characterization of dextran-coated zirconia high-performance liquid chromatographic stationary phases.

PubMed

Dunlap, C J; Carr, P W

1996-10-11

Porous zirconia particles made by the oil emulsion (OE) method and the polymerization-induced colloid aggregation (PICA) method have been coated with a small, carboxymethylated (approximately 5%) dextran polymer and crosslinked in place. The parameters of the coating process (dextran concentration, adsorption time and crosslinker concentration) have all been examined and an optimum value for each determined. The coated and uncoated materials were characterized by nitrogen sorptometry and size-exclusion chromatography (SEC) using solutes (polystyrenes and dextrans) of well-defined molecular masses. Nitrogen sorptometry results show that the PICA material has a much lower pore volume and smaller pore diameter than do the OE materials. Despite this, the elution volumes of the SEC probes change very little upon polymer coating the PICA material while the OE material shows a very large change upon coating.

Determination of hydroxytyrosol and tyrosol by liquid chromatography for the quality control of cosmetic products based on olive extracts.

PubMed

Miralles, Pablo; Chisvert, Alberto; Salvador, Amparo

2015-01-01

An analytical method for the simultaneous determination of hydroxytyrosol and tyrosol in different types of olive extract raw materials and cosmetic cream samples has been developed. The determination was performed by liquid chromatography with UV spectrophotometric detection. Different chromatographic parameters, such as mobile phase pH and composition, oven temperature and different sample preparation variables were studied. The best chromatographic separation was obtained under the following conditions: C18 column set at 35°C and isocratic elution of a mixture ethanol: 1% acetic acid solution at pH 5 (5:95, v/v) as mobile phase pumped at 1 mL min(-1). The detection wavelength was set at 280 nm and the total run time required for the chromatographic analysis was 10 min, except for cosmetic cream samples where 20 min runtime was required (including a cleaning step). The method was satisfactorily applied to 23 samples including solid, water-soluble and fat-soluble olive extracts and cosmetic cream samples containing hydroxytyrosol and tyrosol. Good recoveries (95-107%) and repeatability (1.1-3.6%) were obtained, besides of limits of detection values below the μg mL(-1) level. These good analytical features, as well as its environmentally-friendly characteristics, make the presented method suitable to carry out both the control of the whole manufacture process of raw materials containing the target analytes and the quality control of the finished cosmetic products. Copyright © 2014 Elsevier B.V. All rights reserved.

40 CFR 60.583 - Test methods and procedures.

Code of Federal Regulations, 2012 CFR

2012-07-01

...) as follows: (1) Method 24 for analysis of inks. If nonphotochemically reactive solvents are used in the inks, standard gas chromatographic techniques may be used to identify and quantify these solvents... of an affected facility shall determine the weighted average VOC content of the inks according to the...