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Sample records for chromatography methods instrumentation

  1. Analytical chromatography. Methods, instrumentation and applications

    International Nuclear Information System (INIS)

    Yashin, Ya I; Yashin, A Ya

    2006-01-01

    The state-of-the-art and the prospects in the development of main methods of analytical chromatography, viz., gas, high performance liquid and ion chromatographic techniques, are characterised. Achievements of the past 10-15 years in the theory and general methodology of chromatography and also in the development of new sorbents, columns and chromatographic instruments are outlined. The use of chromatography in the environmental control, biology, medicine, pharmaceutics, and also for monitoring the quality of foodstuffs and products of chemical, petrochemical and gas industries, etc. is considered.

  2. Instrumental liquid chromatography: a practical manual on high-performance liquid chromatographic methods

    National Research Council Canada - National Science Library

    Parris, N. A

    1976-01-01

    Available texts on liquid chromatography have tended to emphasize the developments in the theoretical understanding of the technique and methodology or to list numerous applications, complete with experimental details...

  3. Constructing a LabVIEW-Controlled High-Performance Liquid Chromatography (HPLC) System: An Undergraduate Instrumental Methods Exercise

    Science.gov (United States)

    Smith, Eugene T.; Hill, Marc

    2011-01-01

    In this laboratory exercise, students develop a LabVIEW-controlled high-performance liquid chromatography system utilizing a data acquisition device, two pumps, a detector, and fraction collector. The programming experience involves a variety of methods for interface communication, including serial control, analog-to-digital conversion, and…

  4. Instrument platforms for nano liquid chromatography

    Czech Academy of Sciences Publication Activity Database

    Šesták, Jozef; Moravcová, Dana; Kahle, Vladislav

    2015-01-01

    Roč. 1421, NOV (2015), s. 2-17 ISSN 0021-9673 R&D Projects: GA MV VG20112015021 Institutional support: RVO:68081715 Keywords : nano liquid chromatography * splitless gradient generation * nano LC platforms Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.926, year: 2015 http://hdl.handle.net/11104/0250900

  5. Instrument platforms for nano liquid chromatography.

    Science.gov (United States)

    Šesták, Jozef; Moravcová, Dana; Kahle, Vladislav

    2015-11-20

    The history of liquid chromatography started more than a century ago and miniaturization and automation are two leading trends in this field. Nanocolumn liquid chromatography (nano LC) and largely synonymous capillary liquid chromatography (capillary LC) are the most recent results of this process where miniaturization of column dimensions and sorbent particle size play crucial role. Very interesting results achieved in the research of extremely miniaturized LC columns at the end of the last century lacked distinctive raison d'être and only advances in mass spectrometry brought a real breakthrough. Configuration of nano LC-electrospray ionization mass spectrometry (LC-ESI-MS) has become a basic tool in bioanalytical chemistry, especially in proteomics. This review discusses and summarizes past and current trends in the realization of nano liquid chromatography (nano LC) platforms. Special attention is given to the mobile phase delivery under nanoflow rates (isocratic, gradient) and sample injection to the nanocolumn. Available detection techniques applied in nano LC separations are also briefly discussed. We followed up the key themes from the original scientific reports over gradual improvements up to the contemporary commercial solutions. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Instrumentation for analytical scale supercritical fluid chromatography.

    Science.gov (United States)

    Berger, Terry A

    2015-11-20

    Analytical scale supercritical fluid chromatography (SFC) is largely a sub-discipline of high performance liquid chromatography (HPLC), in that most of the hardware and software can be used for either technique. The aspects that separate the 2 techniques stem from the use of carbon dioxide (CO2) as the main component of the mobile phase in SFC. The high compressibility and low viscosity of CO2 mean that pumps, and autosamplers designed for HPLC either need to be modified or an alternate means of dealing with compressibility needs to be found. The inclusion of a back pressure regulator and a high pressure flow cell for any UV-Vis detector are also necessary. Details of the various approaches, problems and solutions are described. Characteristics, such as adiabatic vs. isothermal compressibility, thermal gradients, and refractive index issues are dealt with in detail. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Robotic thin layer chromatography instrument for synthetic chemistry

    International Nuclear Information System (INIS)

    Corkan, L.A.; Haynes, E.; Kline, S.; Lindsey, J.S.

    1991-01-01

    We have constructed a second generation instrument for performing automated thin layer chromatography (TLC), The TLC instrument Consists of four dedicated stations for (1) plate dispensing, (2) sample application, (3) plate development, and (4) densitometry. A robot is used to move TLC plates among stations. The TLC instrument functions either as a stand-alone unit or as one analytical module in a robotic workstation for synthetic chemistry. An integrated hardware and software architecture enables automatic TLC analysis of samples produced concurrently from synthetic reactions in progress on the workstation. The combination of fixed automation and robotics gives a throughput of 12 TLC samples per hour. From these results a blueprint has emerged for an advanced automated TLC instrument with far greater throughput and analytical capabilities

  8. Gradient High Performance Liquid Chromatography Method ...

    African Journals Online (AJOL)

    Purpose: To develop a gradient high performance liquid chromatography (HPLC) method for the simultaneous determination of phenylephrine (PHE) and ibuprofen (IBU) in solid ..... nimesulide, phenylephrine. Hydrochloride, chlorpheniramine maleate and caffeine anhydrous in pharmaceutical dosage form. Acta Pol.

  9. Validated High Performance Liquid Chromatography Method for ...

    African Journals Online (AJOL)

    Purpose: To develop a simple, rapid and sensitive high performance liquid chromatography (HPLC) method for the determination of cefadroxil monohydrate in human plasma. Methods: Schimadzu HPLC with LC solution software was used with Waters Spherisorb, C18 (5 μm, 150mm × 4.5mm) column. The mobile phase ...

  10. Liquid chromatography detection unit, system, and method

    Science.gov (United States)

    Derenzo, Stephen E.; Moses, William W.

    2015-10-27

    An embodiment of a liquid chromatography detection unit includes a fluid channel and a radiation detector. The radiation detector is operable to image a distribution of a radiolabeled compound as the distribution travels along the fluid channel. An embodiment of a liquid chromatography system includes an injector, a separation column, and a radiation detector. The injector is operable to inject a sample that includes a radiolabeled compound into a solvent stream. The position sensitive radiation detector is operable to image a distribution of the radiolabeled compound as the distribution travels along a fluid channel. An embodiment of a method of liquid chromatography includes injecting a sample that comprises radiolabeled compounds into a solvent. The radiolabeled compounds are then separated. A position sensitive radiation detector is employed to image distributions of the radiolabeled compounds as the radiolabeled compounds travel along a fluid channel.

  11. Trace analysis of halogenated hydrocarbons in gaseous samples by on-line enrichment in an adsorption trap, on-column cold-trapping and capillary gas chromatography. I.Method and instrumentation

    NARCIS (Netherlands)

    Noij, T.H.M.; Fabian, P.; Borchers, R.; Janssen, F.; Cramers, C.A.M.G.; Rijks, J.A.

    1987-01-01

    A method is described for the determination of halocarbons in gaseous samples down to the ppt level (1:1012, v/v), consisting of successive on-line sub-ambient enrichment on an adsorbent, on-column cryofocusing, capillary gas chromatography and electron-capture detection. The quantitative aspects of

  12. Development of a new screening method for the detection of antibiotic residues in muscle tissues using liquid chromatography and high resolution mass spectrometry with a LC-LTQ-Orbitrap instrument.

    OpenAIRE

    2011-01-01

    Abstract In the present work, a liquid chromatography- high resolution mass spectrometry method was developed for the screening in meat of a wide range of antibiotics used in veterinary medicine. Full scan mode under high resolution mass spectral conditions using LTQ-Orbitrap mass spectrometer with resolving power 60.000 FWHM was applied for analysis of the samples. Samples were prepared using two extractions protocols prior to LC-MS analysis. The scope of the method focuses on the...

  13. Development of a high performance liquid chromatography method ...

    African Journals Online (AJOL)

    Development of a high performance liquid chromatography method for simultaneous ... Purpose: To develop and validate a new low-cost high performance liquid chromatography (HPLC) method for ..... Several papers have reported the use of ...

  14. Robotic thin layer chromatography instrument for synthetic chemistry

    International Nuclear Information System (INIS)

    Corkan, L.A.; Lindsey, J.S.

    1990-01-01

    One of our long-term goals is to develop robotic workstations for automated synthetic chemistry. Toward that goal we have constructed a 2nd generation instrument for performing TLC analysis. TLC has important advantages (over HPLC and GC) in analysis of crude reaction samples and parallel sample development. The TLC instrument consist of four dedicated stations for (1) plate dispensing, (2) sample application, (3) plate development, and (4) plate densitometry. A robot is used to move plates among stations. The combination of fixed automation and robotics gives high sample throughout (up to 10 samples per hour). A second robot performs reaction chemistry and feeds samples to the TLC instrument, thus enabling TLC analysis at the same time as synthetic reactions proceed on the workstation

  15. Schinus terebinthifolius countercurrent chromatography (Part III): Method transfer from small countercurrent chromatography column to preparative centrifugal partition chromatography ones as a part of method development.

    Science.gov (United States)

    das Neves Costa, Fernanda; Hubert, Jane; Borie, Nicolas; Kotland, Alexis; Hewitson, Peter; Ignatova, Svetlana; Renault, Jean-Hugues

    2017-03-03

    Countercurrent chromatography (CCC) and centrifugal partition chromatography (CPC) are support free liquid-liquid chromatography techniques sharing the same basic principles and features. Method transfer has previously been demonstrated for both techniques but never from one to another. This study aimed to show such a feasibility using fractionation of Schinus terebinthifolius berries dichloromethane extract as a case study. Heptane - ethyl acetate - methanol -water (6:1:6:1, v/v/v/v) was used as solvent system with masticadienonic and 3β-masticadienolic acids as target compounds. The optimized separation methodology previously described in Part I and II, was scaled up from an analytical hydrodynamic CCC column (17.4mL) to preparative hydrostatic CPC instruments (250mL and 303mL) as a part of method development. Flow-rate and sample loading were further optimized on CPC. Mobile phase linear velocity is suggested as a transfer invariant parameter if the CPC column contains sufficient number of partition cells. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Instrumental methods of analysis, 7th edition

    International Nuclear Information System (INIS)

    Willard, H.H.; Merritt, L.L. Jr.; Dean, J.A.; Settle, F.A. Jr.

    1988-01-01

    The authors have prepared an organized and generally polished product. The book is fashioned to be used as a textbook for an undergraduate instrumental analysis course, a supporting textbook for graduate-level courses, and a general reference work on analytical instrumentation and techniques for professional chemists. Four major areas are emphasized: data collection and processing, spectroscopic instrumentation and methods, liquid and gas chromatographic methods, and electrochemical methods. Analytical instrumentation and methods have been updated, and a thorough citation of pertinent recent literature is included

  17. Instrument modifications that produced reduced plate heights supercritical fluid chromatography.

    Science.gov (United States)

    Berger, Terry A

    2016-04-29

    The concept of peak fidelity was shown to be helpful in modeling tubing and detector cell dimensions. Connection tubing and flow cell variances were modeled to determine appropriate internal ID's, lengths, and volumes. A low dispersion plumbing configuration, based on these calculations, was assembled to replace the standard plumbing and produced the reported results. The modifications made were straightforward using commercially available parts. The full theoretical efficiency of a 3×100 mm column packed with 1.8 μm totally porous particles was achieved for the first time in supercritical fluid chromatography (SFC). Peak fidelity of >0.95 was maintained to below k=2. A reduced plate height as low as 1.87 was measured. Thus, true "ultra high performance" SFC was achieved, with the results a major improvement from all previous SFC reports. Since there were no efficiency losses, none could be attributed to thermal gradients caused by the expansion of the fluid over large pressure drops, under the conditions used. Similarly, changes in diffusion coefficients caused by significant decreases in density during expansion are apparently balanced by the increase in linear velocity, keeping the ratio between the diffusion coefficient and the linear velocity a constant. Changing modifier concentration to change retention was shown to not be a significant problem. All these issues have been a concern in the past. Diffusion coefficients, and viscosity data needs to be collected at high pressures before the actual limits of SFC can be discovered. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Chromatography.

    Science.gov (United States)

    Brantley, L. Reed, Sr.; Demanche, Edna L.; Klemm, E. Barbara; Kyselka, Will; Phillips, Edwin A.; Pottenger, Francis M.; Yamamoto, Karen N.; Young, Donald B.

    This booklet presents some activities on chromatography. Directions for preparing leaf pigment extracts using alcohol are given, and paper chromatography and thin-layer chromatography are described as modifications of the basic principles of chromatography. (KHR)

  19. Plasma chromatography

    International Nuclear Information System (INIS)

    Anon.

    1984-01-01

    This book examines the fundamental theory and various applications of ion mobility spectroscopy. Plasma chromatography developed from research on the diffusion and mobility of ions. Topics considered include instrument design and description (e.g., performance, spectral interpretation, sample handling, mass spectrometry), the role of ion mobility in plasma chromatography (e.g., kinetic theory of ion transport), atmospheric pressure ionization (e.g., rate equations), the characterization of isomers by plasma chromatography (e.g., molecular ion characteristics, polynuclear aromatics), plasma chromatography as a gas chromatographic detection method (e.g., qualitative analysis, continuous mobility monitoring, quantitative analysis), the analysis of toxic vapors by plasma chromatography (e.g., plasma chromatograph calibration, instrument control and data processing), the analysis of semiconductor devices and microelectronic packages by plasma chromatography/mass spectroscopy (e.g., analysis of organic surface contaminants, analysis of water in sealed electronic packages), and instrument design and automation (hardware, software)

  20. Development of a new screening method for the detection of antibiotic residues in muscle tissues using liquid chromatography and high resolution mass spectrometry with a LC-LTQ-Orbitrap instrument.

    Science.gov (United States)

    Hurtaud-Pessel, D; Jagadeshwar-Reddy, T; Verdon, E

    2011-10-01

    A liquid chromatography-high resolution mass spectrometry (LC-HRMS) method was developed for screening meat for a wide range of antibiotics used in veterinary medicine. Full-scan mode under high resolution mass spectral conditions using an LTQ-Orbitrap mass spectrometer with resolving power 60,000 full width at half maximum (FWHM) was applied for analysis of the samples. Samples were prepared using two extraction protocols prior to LC-HRMS analysis. The scope of the method focuses on screening the following main families of antibacterial veterinary drugs: penicillins, cephalosporins, sulfonamides, macrolides, tetracyclines, aminoglucosides and quinolones. Compounds were successfully identified in spiked samples from their accurate mass and LC retention times from the acquired full-scan chromatogram. Automated data processing using ToxId software allowed rapid treatment of the data. Analyses of muscle tissues from real samples collected from antibiotic-treated animals was carried out using the above methodology and antibiotic residues were identified unambiguously. Further analysis of the data for real samples allowed the identification of the targeted antibiotic residues but also non-targeted compounds, such as some of their metabolites.

  1. Pixe method as microanalytical instrument

    International Nuclear Information System (INIS)

    Tabacniks, M.H.

    1986-02-01

    The PIXE method (Particle Induced X-Ray Emission) as analytical method presenting the evolution, the theoretical fundaments, the detection limit, the optimization for operational conditions is evaluated. The applications of the method to air pollution control and aerosol studies in regions such as Antartic, Amazon and other regions are analysed. (M.C.K.) [pt

  2. Computational and instrumental methods in EPR

    CERN Document Server

    Bender, Christopher J

    2006-01-01

    Computational and Instrumental Methods in EPR Prof. Bender, Fordham University Prof. Lawrence J. Berliner, University of Denver Electron magnetic resonance has been greatly facilitated by the introduction of advances in instrumentation and better computational tools, such as the increasingly widespread use of the density matrix formalism. This volume is devoted to both instrumentation and computation aspects of EPR, while addressing applications such as spin relaxation time measurements, the measurement of hyperfine interaction parameters, and the recovery of Mn(II) spin Hamiltonian parameters via spectral simulation. Key features: Microwave Amplitude Modulation Technique to Measure Spin-Lattice (T1) and Spin-Spin (T2) Relaxation Times Improvement in the Measurement of Spin-Lattice Relaxation Time in Electron Paramagnetic Resonance Quantitative Measurement of Magnetic Hyperfine Parameters and the Physical Organic Chemistry of Supramolecular Systems New Methods of Simulation of Mn(II) EPR Spectra: Single Cryst...

  3. Liquid chromatography method to determine polyamines in thermosetting polymers

    Energy Technology Data Exchange (ETDEWEB)

    Dopico-Garcia, M.S. [Laboratorio de Quimica - Centro de Investigacions Tecnoloxicas, Universidade da Coruna, Campus de Esteiro s/n, 15403 Ferrol (Spain); Centro Galego do Plastico, A Cabana s/n, 15590 Ferrol (Spain); Lopez-Vilarino, J.M. [Laboratorio de Quimica - Centro de Investigacions Tecnoloxicas, Universidade da Coruna, Campus de Esteiro s/n, 15403 Ferrol (Spain); Fernandez-Martinez, G. [Unidad de Tecnicas Cromatograficas, Servizos de Apoio a Investigacion, Edificio Servizos Centrais de Investigacion, Universidade da Coruna, Campus de Elvina s/n, 15071 A Coruna (Spain); Gonzalez-Rodriguez, M.V., E-mail: victoria@udc.es [Dpto. de Quimica Analitica - E.U. Politecnica, Universidade da Coruna, Avda. 19 de Febrero s/n, 15405 Ferrol (Spain)

    2010-05-14

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

  4. Liquid chromatography method to determine polyamines in thermosetting polymers.

    Science.gov (United States)

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

    2010-05-14

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

  5. Liquid chromatography method to determine polyamines in thermosetting polymers

    International Nuclear Information System (INIS)

    Dopico-Garcia, M.S.; Lopez-Vilarino, J.M.; Fernandez-Martinez, G.; Gonzalez-Rodriguez, M.V.

    2010-01-01

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

  6. Methods of uranium isotpic separation by chemical exchange chromatography

    International Nuclear Information System (INIS)

    Pena V, L.A.; Valle M, L.

    1985-01-01

    Chemical exchange chromatography as applied to isotope separation has undergone a constant development during the last few years. The results so far indicate that this method could eventually become commercially useful. This work presents a critical review of the experimental methods presently under study by principal research groups, and which have not get been compared. (Author)

  7. Instrumentation and quantitative methods of evaluation

    International Nuclear Information System (INIS)

    Beck, R.N.; Cooper, M.D.

    1991-01-01

    This report summarizes goals and accomplishments of the research program entitled Instrumentation and Quantitative Methods of Evaluation, during the period January 15, 1989 through July 15, 1991. This program is very closely integrated with the radiopharmaceutical program entitled Quantitative Studies in Radiopharmaceutical Science. Together, they constitute the PROGRAM OF NUCLEAR MEDICINE AND QUANTITATIVE IMAGING RESEARCH within The Franklin McLean Memorial Research Institute (FMI). The program addresses problems involving the basic science and technology that underlie the physical and conceptual tools of radiotracer methodology as they relate to the measurement of structural and functional parameters of physiologic importance in health and disease. The principal tool is quantitative radionuclide imaging. The objective of this program is to further the development and transfer of radiotracer methodology from basic theory to routine clinical practice. The focus of the research is on the development of new instruments and radiopharmaceuticals, and the evaluation of these through the phase of clinical feasibility. 234 refs., 11 figs., 2 tabs

  8. Method of decontaminating radioactive-contaminated instruments

    International Nuclear Information System (INIS)

    Urata, Megumu; Fujii, Masaaki; Kitaguchi, Hiroshi.

    1982-01-01

    Purpose: To enable safety processing of liquid wastes by recovering radioactive metal ions remaining in the electrolytes after the decontamination procedure thereby decreasing the radioactivity. Method: In a decontamination tank containing electrolytes consisting of diluted hydrochloric acid and diluted sulfuric acid, are provided a radioactive contaminated instrument connected to an anode and a collector electrode made of stainless steel connected to a cathode respectively. Upon applying electrical current, the portion of the mother material to be decontaminated is polished electrolytically into metal ions and they are deposited as metal on the collection electrode. After completion of the decontamination, an ultrasonic wave generator is operated to strip and remove the oxide films. Thereafter, the anode is replaced with the carbon electrode and electrical current is supplied continuously, whereby the remaining metal ions are deposited and recovered as the metal on the collection electrode. (Yoshino, Y.)

  9. Method of decontaminating radioactive-contaminated instruments

    Energy Technology Data Exchange (ETDEWEB)

    Urata, M; Fujii, M; Kitaguchi, H

    1982-03-29

    Purpose: To enable safety processing of liquid wastes by recovering radioactive metal ions remaining in the electrolytes after the decontamination procedure thereby decreasing the radioactivity. Method: In a decontamination tank containing electrolytes consisting of diluted hydrochloric acid and diluted sulfuric acid, are provided a radioactive contaminated instrument connected to an anode and a collector electrode made of stainless steel connected to a cathode respectively. Upon applying electrical current, the portion of the mother material to be decontaminated is polished electrolytically into metal ions and they are deposited as metal on the collection electrode. After completion of the decontamination, an ultrasonic wave generator is operated to strip and remove the oxide films. Thereafter, the anode is replaced with the carbon electrode and electrical current is supplied continuously, whereby the remaining metal ions are deposited and recovered as the metal on the collection electrode.

  10. Establishment of analysis method for methane detection by gas chromatography

    Science.gov (United States)

    Liu, Xinyuan; Yang, Jie; Ye, Tianyi; Han, Zeyu

    2018-02-01

    The study focused on the establishment of analysis method for methane determination by gas chromatography. Methane was detected by hydrogen flame ionization detector, and the quantitative relationship was determined by working curve of y=2041.2x+2187 with correlation coefficient of 0.9979. The relative standard deviation of 2.60-6.33% and the recovery rate of 96.36%∼105.89% were obtained during the parallel determination of standard gas. This method was not quite suitable for biogas content analysis because methane content in biogas would be over the measurement range in this method.

  11. Maximizing kinetic performance in supercritical fluid chromatography using state-of-the-art instruments.

    Science.gov (United States)

    Grand-Guillaume Perrenoud, Alexandre; Hamman, Chris; Goel, Meenakshi; Veuthey, Jean-Luc; Guillarme, Davy; Fekete, Szabolcs

    2013-11-01

    Recently, there has been a renewed interest in supercritical fluid chromatography (SFC), due to the introduction of state-of-the-art instruments and dedicated columns packed with small particles. However, the achievable kinetic performance and practical possibilities of such modern SFC instruments and columns has not been described in details until now. The goal of the present contribution was to provide some information about the optimal column dimensions (i.e. length, diameter and particle size) suitable for such state-of the-art systems, with respect to extra-column band broadening and system upper pressure limit. In addition, the reliability of the kinetic plot methodology, successfully applied in RPLC, was also evaluated under SFC conditions. Taking into account the system variance, measured at ∼85μL(2), on modern SFC instruments, a column of 3mm I.D. was ideally suited for the current technology, as the loss in efficiency remained reasonable (i.e. less than 10% decrease for k>6). Conversely, these systems struggle with 2.1mm I.D. columns (55% loss in N for k=5). Regarding particle size, columns packed with 5μm particles provided unexpectedly high minimum reduced plate height values (hmin=3.0-3.4), while the 3.5 and 1.7μm packing provided lower reduced plate heights hmin=2.2-2.4 and hmin=2.7-3.2, respectively. Considering the system upper pressure limit, it appears that columns packed with 1.7μm particles give the lowest analysis time for efficiencies up to 40,000-60,000 plates, if the mobile phase composition is in the range of 2-19% MeOH. The 3.5μm particles were attractive for higher efficiencies, particularly when the modifier percentage was above 20%, while 5μm was never kinetically relevant with modern SFC instruments, due to an obvious limitation in terms of upper flow rate value. The present work also confirms that the kinetic plot methodology could be successfully applied to SFC, without the need for isopycnic measurements, as the difference

  12. Airtight miniaturized chromatography: a safer method for radiopharmaceutical quality control

    International Nuclear Information System (INIS)

    Coupal, J.J.; Shih, W.J.; Ryo, U.Y.

    1988-01-01

    Miniaturized chromatography is widely used for quality control of radiopharmaceuticals. Recently, published chromatography procedures have illustrated or described chromatography chambers open to the air in use, suggesting that volatile toxic mobile phases are harmless to people in the vicinity. The authors describe the results of their search for an inexpensive closed chromatography chamber that can be used to derive safely the benefits from conventional miniaturized chromatography

  13. Instrumental neutron activation analysis - a routine method

    International Nuclear Information System (INIS)

    Bruin, M. de.

    1983-01-01

    This thesis describes the way in which at IRI instrumental neutron activation analysis (INAA) has been developed into an automated system for routine analysis. The basis of this work are 20 publications describing the development of INAA since 1968. (Auth.)

  14. A review of modern instrumental methods of elemental analysis of petroleum related material. Part 2

    International Nuclear Information System (INIS)

    Nadkarni, R.A.

    1991-01-01

    In this paper a review is presented of the state of the art in elemental analysis of petroleum-related materials (crude oil, gasoline, additives, and lubricants) using modern instrumental analysis techniques. The major instrumental techniques used for elemental analysis of petroleum products include atomic absorption spectrometry (both with flame and with graphite furnace atomizer), inductively coupled plasma atomic emission spectrometry, ion chromatography, microelemental methods, neutron activation, spark source mass spectrometry, and x-ray fluorescence. Each of these techniques is compared for its advantages, disadvantages, and typical applications in the petroleum field

  15. Modern Instrumental Methods in Forensic Toxicology*

    Science.gov (United States)

    Smith, Michael L.; Vorce, Shawn P.; Holler, Justin M.; Shimomura, Eric; Magluilo, Joe; Jacobs, Aaron J.; Huestis, Marilyn A.

    2009-01-01

    This article reviews modern analytical instrumentation in forensic toxicology for identification and quantification of drugs and toxins in biological fluids and tissues. A brief description of the theory and inherent strengths and limitations of each methodology is included. The focus is on new technologies that address current analytical limitations. A goal of this review is to encourage innovations to improve our technological capabilities and to encourage use of these analytical techniques in forensic toxicology practice. PMID:17579968

  16. Theories to support method development in comprehensive two-dimensional liquid chromatography - A review

    NARCIS (Netherlands)

    Bedani, F.; Schoenmakers, P.J.; Janssen, H.-G.

    2012-01-01

    On-line comprehensive two-dimensional liquid chromatography techniques promise to resolve samples that current one-dimensional liquid chromatography methods cannot adequately deal with. To make full use of the potential of two-dimensional liquid chromatography, optimization is required. Optimization

  17. Lipidomic analysis of biological samples: Comparison of liquid chromatography, supercritical fluid chromatography and direct infusion mass spectrometry methods.

    Science.gov (United States)

    Lísa, Miroslav; Cífková, Eva; Khalikova, Maria; Ovčačíková, Magdaléna; Holčapek, Michal

    2017-11-24

    Lipidomic analysis of biological samples in a clinical research represents challenging task for analytical methods given by the large number of samples and their extreme complexity. In this work, we compare direct infusion (DI) and chromatography - mass spectrometry (MS) lipidomic approaches represented by three analytical methods in terms of comprehensiveness, sample throughput, and validation results for the lipidomic analysis of biological samples represented by tumor tissue, surrounding normal tissue, plasma, and erythrocytes of kidney cancer patients. Methods are compared in one laboratory using the identical analytical protocol to ensure comparable conditions. Ultrahigh-performance liquid chromatography/MS (UHPLC/MS) method in hydrophilic interaction liquid chromatography mode and DI-MS method are used for this comparison as the most widely used methods for the lipidomic analysis together with ultrahigh-performance supercritical fluid chromatography/MS (UHPSFC/MS) method showing promising results in metabolomics analyses. The nontargeted analysis of pooled samples is performed using all tested methods and 610 lipid species within 23 lipid classes are identified. DI method provides the most comprehensive results due to identification of some polar lipid classes, which are not identified by UHPLC and UHPSFC methods. On the other hand, UHPSFC method provides an excellent sensitivity for less polar lipid classes and the highest sample throughput within 10min method time. The sample consumption of DI method is 125 times higher than for other methods, while only 40μL of organic solvent is used for one sample analysis compared to 3.5mL and 4.9mL in case of UHPLC and UHPSFC methods, respectively. Methods are validated for the quantitative lipidomic analysis of plasma samples with one internal standard for each lipid class. Results show applicability of all tested methods for the lipidomic analysis of biological samples depending on the analysis requirements

  18. Instrument design optimization with computational methods

    Energy Technology Data Exchange (ETDEWEB)

    Moore, Michael H. [Old Dominion Univ., Norfolk, VA (United States)

    2017-08-01

    Using Finite Element Analysis to approximate the solution of differential equations, two different instruments in experimental Hall C at the Thomas Jefferson National Accelerator Facility are analyzed. The time dependence of density uctuations from the liquid hydrogen (LH2) target used in the Qweak experiment (2011-2012) are studied with Computational Fluid Dynamics (CFD) and the simulation results compared to data from the experiment. The 2.5 kW liquid hydrogen target was the highest power LH2 target in the world and the first to be designed with CFD at Jefferson Lab. The first complete magnetic field simulation of the Super High Momentum Spectrometer (SHMS) is presented with a focus on primary electron beam deflection downstream of the target. The SHMS consists of a superconducting horizontal bending magnet (HB) and three superconducting quadrupole magnets. The HB allows particles scattered at an angle of 5:5 deg to the beam line to be steered into the quadrupole magnets which make up the optics of the spectrometer. Without mitigation, remnant fields from the SHMS may steer the unscattered beam outside of the acceptable envelope on the beam dump and limit beam operations at small scattering angles. A solution is proposed using optimal placement of a minimal amount of shielding iron around the beam line.

  19. Improved GLR method to instrument failure detection

    International Nuclear Information System (INIS)

    Jeong, Hak Yeoung; Chang, Soon Heung

    1985-01-01

    The generalized likehood radio(GLR) method performs statistical tests on the innovations sequence of a Kalman-Buchy filter state estimator for system failure detection and its identification. However, the major drawback of the convensional GLR is to hypothesize particular failure type in each case. In this paper, a method to solve this drawback is proposed. The improved GLR method is applied to a PWR pressurizer and gives successful results in detection and identification of any failure. Furthmore, some benefit on the processing time per each cycle of failure detection and its identification can be accompanied. (Author)

  20. Radioactive standards and calibration methods for contamination monitoring instruments

    Energy Technology Data Exchange (ETDEWEB)

    Yoshida, Makoto [Japan Atomic Energy Research Inst., Tokai, Ibaraki (Japan). Tokai Research Establishment

    1997-06-01

    Contamination monitoring in the facilities for handling unsealed radioactive materials is one of the most important procedures for radiation protection as well as radiation dose monitoring. For implementation of the proper contamination monitoring, radiation measuring instruments should not only be suitable to the purpose of monitoring, but also be well calibrated for the objective qualities of measurement. In the calibration of contamination monitoring instruments, quality reference activities need to be used. They are supplied in different such as extended sources, radioactive solutions or radioactive gases. These reference activities must be traceable to the national standards or equivalent standards. On the other hand, the appropriate calibration methods must be applied for each type of contamination monitoring instruments. In this paper, the concepts of calibration for contamination monitoring instruments, reference sources, determination methods of reference quantities and practical calibration methods of contamination monitoring instruments, including the procedures carried out in Japan Atomic Energy Research Institute and some relevant experimental data. (G.K.)

  1. Application of Instrumented Charpy Method in Characterisation of Materials

    OpenAIRE

    Alar, Željko; Mandić, Davor; Dugorepec, Andrija; Sakoman, Matija

    2015-01-01

    Testing of absorbed impact energy according to the Charpy method is carried out to determine the behaviour of a material under the impact load. Instrumented Charpy method allows getting the force displacement curve through the entire test, That curve can be related to force-displacement curve which is obtained by the static tensile test. The purpose of this study was to compare the results of forces obtained by the static tensile test with the forces obtained by the instrumented Charpy method...

  2. Chromatography methods and chemometrics for determination of milk fat adulterants

    Science.gov (United States)

    Trbović, D.; Petronijević, R.; Đorđević, V.

    2017-09-01

    Milk and milk-based products are among the leading food categories according to reported cases of food adulteration. Although many authentication problems exist in all areas of the food industry, adequate control methods are required to evaluate the authenticity of milk and milk products in the dairy industry. Moreover, gas chromatography (GC) analysis of triacylglycerols (TAGs) or fatty acid (FA) profiles of milk fat (MF) in combination with multivariate statistical data processing have been used to detect adulterations of milk and dairy products with foreign fats. The adulteration of milk and butter is a major issue for the dairy industry. The major adulterants of MF are vegetable oils (soybean, sunflower, groundnut, coconut, palm and peanut oil) and animal fat (cow tallow and pork lard). Multivariate analysis enables adulterated MF to be distinguished from authentic MF, while taking into account many analytical factors. Various multivariate analysis methods have been proposed to quantitatively detect levels of adulterant non-MFs, with multiple linear regression (MLR) seemingly the most suitable. There is a need for increased use of chemometric data analyses to detect adulterated MF in foods and for their expanded use in routine quality assurance testing.

  3. Turbidity threshold sampling: Methods and instrumentation

    Science.gov (United States)

    Rand Eads; Jack Lewis

    2001-01-01

    Traditional methods for determining the frequency of suspended sediment sample collection often rely on measurements, such as water discharge, that are not well correlated to sediment concentration. Stream power is generally not a good predictor of sediment concentration for rivers that transport the bulk of their load as fines, due to the highly variable routing of...

  4. High Performance Liquid Chromatography of Some Analgesic Compounds: An Instrumental Analysis Experiment.

    Science.gov (United States)

    Haddad, Paul; And Others

    1983-01-01

    Background information, procedures, and results are provided for an experiment demonstrating techniques of solvent selection, gradient elution, pH control, and ion-pairing in the analysis of an analgesic mixture using reversed-phase liquid chromatography on an octadecylsilane column. Although developed using sophisticated/expensive equipment, less…

  5. Application of an online ion-chromatography-based instrument for gradient flux measurements of speciated nitrogen and sulfur

    Science.gov (United States)

    Rumsey, Ian C.; Walker, John T.

    2016-06-01

    The dry component of total nitrogen and sulfur atmospheric deposition remains uncertain. The lack of measurements of sufficient chemical speciation and temporal extent make it difficult to develop accurate mass budgets and sufficient process level detail is not available to improve current air-surface exchange models. Over the past decade, significant advances have been made in the development of continuous air sampling measurement techniques, resulting with instruments of sufficient sensitivity and temporal resolution to directly quantify air-surface exchange of nitrogen and sulfur compounds. However, their applicability is generally restricted to only one or a few of the compounds within the deposition budget. Here, the performance of the Monitor for AeRosols and GAses in ambient air (MARGA 2S), a commercially available online ion-chromatography-based analyzer is characterized for the first time as applied for air-surface exchange measurements of HNO3, NH3, NH4+, NO3-, SO2 and SO42-. Analytical accuracy and precision are assessed under field conditions. Chemical concentrations gradient precision are determined at the same sampling site. Flux uncertainty measured by the aerodynamic gradient method is determined for a representative 3-week period in fall 2012 over a grass field. Analytical precision and chemical concentration gradient precision were found to compare favorably in comparison to previous studies. During the 3-week period, percentages of hourly chemical concentration gradients greater than the corresponding chemical concentration gradient detection limit were 86, 42, 82, 73, 74 and 69 % for NH3, NH4+, HNO3, NO3-, SO2 and SO42-, respectively. As expected, percentages were lowest for aerosol species, owing to their relatively low deposition velocities and correspondingly smaller gradients relative to gas phase species. Relative hourly median flux uncertainties were 31, 121, 42, 43, 67 and 56 % for NH3, NH4+, HNO3, NO3-, SO2 and SO42-, respectively. Flux

  6. Analytical techniques for instrument design - matrix methods

    International Nuclear Information System (INIS)

    Robinson, R.A.

    1997-01-01

    We take the traditional Cooper-Nathans approach, as has been applied for many years for steady-state triple-axis spectrometers, and consider its generalisation to other inelastic scattering spectrometers. This involves a number of simple manipulations of exponentials of quadratic forms. In particular, we discuss a toolbox of matrix manipulations that can be performed on the 6- dimensional Cooper-Nathans matrix: diagonalisation (Moller-Nielsen method), coordinate changes e.g. from (Δk I ,Δk F to ΔE, ΔQ ampersand 2 dummy variables), integration of one or more variables (e.g. over such dummy variables), integration subject to linear constraints (e.g. Bragg's Law for analysers), inversion to give the variance-covariance matrix, and so on. We show how these tools can be combined to solve a number of important problems, within the narrow-band limit and the gaussian approximation. We will argue that a generalised program that can handle multiple different spectrometers could (and should) be written in parallel to the Monte-Carlo packages that are becoming available. We will also discuss the complementarity between detailed Monte-Carlo calculations and the approach presented here. In particular, Monte-Carlo methods traditionally simulate the real experiment as performed in practice, given a model scattering law, while the Cooper-Nathans method asks the inverse question: given that a neutron turns up in a particular spectrometer configuration (e.g. angle and time of flight), what is the probability distribution of possible scattering events at the sample? The Monte-Carlo approach could be applied in the same spirit to this question

  7. Methods and instrumentation for positron emission tomography

    International Nuclear Information System (INIS)

    Mandelkern, M.A.; Phelps, M.E.

    1988-01-01

    This paper reports on positron emission tomography (PET), a technique for the noninvasive measurement of local tissue concentrations of injected radioactive tracers. Tracer kinetics techniques can be applied to this information to quantify physiologic function in human tissue. In the tracer method, a pharmaceutical is labeled by a radioactive atom. When introduced into the subject that molecule follows a physiologic pathway. The space- and time-dependent distribution of the radionuclide is obtained via an imaging technique. If the radiopharmaceutical is sufficiently analogous to a natural substrate or other substance of interest, a quantitative image can be translated into a physiologic measurement

  8. Instrumentation

    International Nuclear Information System (INIS)

    Umminger, K.

    2008-01-01

    A proper measurement of the relevant single and two-phase flow parameters is the basis for the understanding of many complex thermal-hydraulic processes. Reliable instrumentation is therefore necessary for the interaction between analysis and experiment especially in the field of nuclear safety research where postulated accident scenarios have to be simulated in experimental facilities and predicted by complex computer code systems. The so-called conventional instrumentation for the measurement of e. g. pressures, temperatures, pressure differences and single phase flow velocities is still a solid basis for the investigation and interpretation of many phenomena and especially for the understanding of the overall system behavior. Measurement data from such instrumentation still serves in many cases as a database for thermal-hydraulic system codes. However some special instrumentation such as online concentration measurement for boric acid in the water phase or for non-condensibles in steam atmosphere as well as flow visualization techniques were further developed and successfully applied during the recent years. Concerning the modeling needs for advanced thermal-hydraulic codes, significant advances have been accomplished in the last few years in the local instrumentation technology for two-phase flow by the application of new sensor techniques, optical or beam methods and electronic technology. This paper will give insight into the current state of instrumentation technology for safety-related thermohydraulic experiments. Advantages and limitations of some measurement processes and systems will be indicated as well as trends and possibilities for further development. Aspects of instrumentation in operating reactors will also be mentioned.

  9. Analytical techniques for instrument design - Matrix methods

    International Nuclear Information System (INIS)

    Robinson, R.A.

    1997-01-01

    The authors take the traditional Cooper-Nathans approach, as has been applied for many years for steady-state triple-axis spectrometers, and consider its generalization to other inelastic scattering spectrometers. This involves a number of simple manipulations of exponentials of quadratic forms. In particular, they discuss a toolbox of matrix manipulations that can be performed on the 6-dimensional Cooper-Nathans matrix. They show how these tools can be combined to solve a number of important problems, within the narrow-band limit and the gaussian approximation. They will argue that a generalized program that can handle multiple different spectrometers could (and should) be written in parallel to the Monte-Carlo packages that are becoming available. They also discuss the complementarity between detailed Monte-Carlo calculations and the approach presented here. In particular, Monte-Carlo methods traditionally simulate the real experiment as performed in practice, given a model scattering law, while the Cooper-Nathans method asks the inverse question: given that a neutron turns up in a particular spectrometer configuration (e.g. angle and time of flight), what is the probability distribution of possible scattering events at the sample? The Monte-Carlo approach could be applied in the same spirit to this question

  10. Method to deterministically study photonic nanostructures in different experimental instruments

    NARCIS (Netherlands)

    Husken, B.H.; Woldering, L.A.; Blum, Christian; Tjerkstra, R.W.; Vos, Willem L.

    2009-01-01

    We describe an experimental method to recover a single, deterministically fabricated nanostructure in various experimental instruments without the use of artificially fabricated markers, with the aim to study photonic structures. Therefore, a detailed map of the spatial surroundings of the

  11. Method and apparatus for continuous fluid leak monitoring and detection in analytical instruments and instrument systems

    Science.gov (United States)

    Weitz, Karl K [Pasco, WA; Moore, Ronald J [West Richland, WA

    2010-07-13

    A method and device are disclosed that provide for detection of fluid leaks in analytical instruments and instrument systems. The leak detection device includes a collection tube, a fluid absorbing material, and a circuit that electrically couples to an indicator device. When assembled, the leak detection device detects and monitors for fluid leaks, providing a preselected response in conjunction with the indicator device when contacted by a fluid.

  12. Advanced Measuring (Instrumentation Methods for Nuclear Installations: A Review

    Directory of Open Access Journals (Sweden)

    Wang Qiu-kuan

    2012-01-01

    Full Text Available The nuclear technology has been widely used in the world. The research of measurement in nuclear installations involves many aspects, such as nuclear reactors, nuclear fuel cycle, safety and security, nuclear accident, after action, analysis, and environmental applications. In last decades, many advanced measuring devices and techniques have been widely applied in nuclear installations. This paper mainly introduces the development of the measuring (instrumentation methods for nuclear installations and the applications of these instruments and methods.

  13. Analytical method for high resolution liquid chromatography for quality control French Macaw

    International Nuclear Information System (INIS)

    Garcia Penna, Caridad M; Torres Amaro, Leonid; Menendez Castillo, Rosa; Sanchez, Esther; Martinez Espinosa, Vivian; Gonzalez, Maria Lidia; Rodriguez, Carlos

    2007-01-01

    Was developed and validated an analytical method for high resolution liquid chromatography applicable to quality control of drugs dry French Macaw (Senna alata L. Roxb.) With ultraviolet detection at 340 nm. The method for high resolution liquid chromatography used to quantify the sennosides A and B, main components, was validated and proved to be specific, linear, precise and accurate. (Author)

  14. Falsification Testing of Instrumental Variables Methods for Comparative Effectiveness Research.

    Science.gov (United States)

    Pizer, Steven D

    2016-04-01

    To demonstrate how falsification tests can be used to evaluate instrumental variables methods applicable to a wide variety of comparative effectiveness research questions. Brief conceptual review of instrumental variables and falsification testing principles and techniques accompanied by an empirical application. Sample STATA code related to the empirical application is provided in the Appendix. Comparative long-term risks of sulfonylureas and thiazolidinediones for management of type 2 diabetes. Outcomes include mortality and hospitalization for an ambulatory care-sensitive condition. Prescribing pattern variations are used as instrumental variables. Falsification testing is an easily computed and powerful way to evaluate the validity of the key assumption underlying instrumental variables analysis. If falsification tests are used, instrumental variables techniques can help answer a multitude of important clinical questions. © Health Research and Educational Trust.

  15. Repairing method of color TV with measuring instrument

    International Nuclear Information System (INIS)

    1996-01-01

    This book concentrates on repairing method of color TV with measuring instrument, which deals with direction and sorts of measuring instrument for service, application and basic technique of an oscilloscope and a synchroscope, constituent of TV and wave reading, everything for test skill for service man, service technique by electronic voltmeter, service technique by sweep generator and maker generator, dot-bar generator and support skill for color TV and color bar generator and application technology of color circuit.

  16. Pre-staining thin layer chromatography method for amino acid ...

    African Journals Online (AJOL)

    Jane

    2010-12-13

    Dec 13, 2010 ... inexpensive and the results obtained were clean and reproducible. However, it is suitable for the high throughput screening of amino acid-producing strains. Key words: Thin layer chromatography, pre-staining, amino acid detection. INTRODUCTION. Several analytical techniques have been often used for.

  17. Instrumentation

    International Nuclear Information System (INIS)

    Muehllehner, G.; Colsher, J.G.

    1982-01-01

    This chapter reviews the parameters which are important to positron-imaging instruments. It summarizes the options which various groups have explored in designing tomographs and the methods which have been developed to overcome some of the limitations inherent in the technique as well as in present instruments. The chapter is not presented as a defense of positron imaging versus single-photon or other imaging modality, neither does it contain a description of various existing instruments, but rather stresses their common properties and problems. Design parameters which are considered are resolution, sampling requirements, sensitivity, methods of eliminating scattered radiation, random coincidences and attenuation. The implementation of these parameters is considered, with special reference to sampling, choice of detector material, detector ring diameter and shielding and variations in point spread function. Quantitation problems discussed are normalization, and attenuation and random corrections. Present developments mentioned are noise reduction through time-of-flight-assisted tomography and signal to noise improvements through high intrinsic resolution. Extensive bibliography. (U.K.)

  18. A Mixed Methods Portrait of Urban Instrumental Music Teaching

    Science.gov (United States)

    Fitzpatrick, Kate R.

    2011-01-01

    The purpose of this mixed methods study was to learn about the ways that instrumental music teachers in Chicago navigated the urban landscape. The design of the study most closely resembles Creswell and Plano Clark's (2007) two-part Triangulation Convergence Mixed Methods Design, with the addition of an initial exploratory focus group component.…

  19. Evolution in miniaturized column liquid chromatography instrumentation and applications: An overview.

    Science.gov (United States)

    Nazario, Carlos E D; Silva, Meire R; Franco, Maraíssa S; Lanças, Fernando M

    2015-11-20

    The purpose of this article is to underline the miniaturized LC instrumental system and describe the evolution of commercially available systems by discussing their advantages and drawbacks. Nowadays, there are already many miniaturized LC systems available with a great variety of pump design, interface and detectors as well as efficient columns technologies and reduced connections devices. The solvent delivery systems are able to drive the mobile phase without flow splitters and promote gradient elution using either dual piston reciprocating or syringe-type pumps. The mass spectrometry as detection system is the most widely used detection system; among many alternative ionization sources direct-EI LC-MS is a promising alternative to APCI. In addition, capillary columns are now available showing many possibilities of stationary phases, inner diameters and hardware materials. This review provides a discussion about miniaturized LC demonstrating fundamentals and instrumentals' aspects of the commercially available miniaturized LC instrumental system mainly nano and micro LC formats. This review also covers the recent developments and trends in instrumentation, capillary and nano columns, and several applications of this very important and promising field. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. Instrumental and statistical methods for the comparison of class evidence

    Science.gov (United States)

    Liszewski, Elisa Anne

    Trace evidence is a major field within forensic science. Association of trace evidence samples can be problematic due to sample heterogeneity and a lack of quantitative criteria for comparing spectra or chromatograms. The aim of this study is to evaluate different types of instrumentation for their ability to discriminate among samples of various types of trace evidence. Chemometric analysis, including techniques such as Agglomerative Hierarchical Clustering, Principal Components Analysis, and Discriminant Analysis, was employed to evaluate instrumental data. First, automotive clear coats were analyzed by using microspectrophotometry to collect UV absorption data. In total, 71 samples were analyzed with classification accuracy of 91.61%. An external validation was performed, resulting in a prediction accuracy of 81.11%. Next, fiber dyes were analyzed using UV-Visible microspectrophotometry. While several physical characteristics of cotton fiber can be identified and compared, fiber color is considered to be an excellent source of variation, and thus was examined in this study. Twelve dyes were employed, some being visually indistinguishable. Several different analyses and comparisons were done, including an inter-laboratory comparison and external validations. Lastly, common plastic samples and other polymers were analyzed using pyrolysis-gas chromatography/mass spectrometry, and their pyrolysis products were then analyzed using multivariate statistics. The classification accuracy varied dependent upon the number of classes chosen, but the plastics were grouped based on composition. The polymers were used as an external validation and misclassifications occurred with chlorinated samples all being placed into the category containing PVC.

  1. Application of Instrumented Charpy Method in Characterisation of Materials

    Directory of Open Access Journals (Sweden)

    Željko Alar

    2015-07-01

    Full Text Available Testing of absorbed impact energy according to the Charpy method is carried out to determine the behaviour of a material under the impact load. Instrumented Charpy method allows getting the force displacement curve through the entire test, That curve can be related to force-displacement curve which is obtained by the static tensile test. The purpose of this study was to compare the results of forces obtained by the static tensile test with the forces obtained by the instrumented Charpy method. Experimental part of the work contains testing of the mechanical properties of S275J0 steel by the static tensile test and Impact test on instrumented Charpy pendulum.

  2. Use of laminar chromatographic methods for determination of separation conditions in column extraction chromatography

    International Nuclear Information System (INIS)

    Ghersini, G.; Cerrai, E.

    1978-01-01

    Possibilities of using laminar chromatographic methods (paper and thin-layer chromatography) to determine optimal separation conditions in column extraction chromatography are analysed. Most of the given laminar methods are presented as Rf-spectra, i.e. as dependences of Rf found experimentally on eluating solution component concentration. Interrelation between Rf and distribution coefficients of corresponding liquid extraction systems and retention volumes of chromatographic columns is considered. Literature data on extraction paper and thin-layer chromatography of elements with various immovable phases are presented

  3. Qualitative and quantitative determination of ubiquinones by the method of high-efficiency liquid chromatography

    International Nuclear Information System (INIS)

    Yanotovskii, M.T.; Mogilevskaya, M.P.; Obol'nikova, E.A.; Kogan, L.M.; Samokhvalov, G.I.

    1986-01-01

    A method has been developed for the qualitative and quantitative determination of ubiquinones CoQ 6 -CoQ 10 , using high-efficiency reversed-phase liquid chromatography. Tocopherol acetate was used as the internal standard

  4. Fast methods for screening of trichothecenes in fungal cultures using gas chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Nielsen, Kristian Fog; Thrane, Ulf

    2001-01-01

    The paper presents a fast method for trichothecene profiling and chemotaxonomic studies in species of Fusarium, Stachybotrys, Trichoderma and Memnoniella. Micro scale extracted crude Fusarium extracts were derivatised using pentafluoropropionic anhydride and analysed by gas chromatography...

  5. Evaluation between ultrahigh pressure liquid chromatography and high-performance liquid chromatography analytical methods for characterizing natural dyestuffs.

    Science.gov (United States)

    Serrano, Ana; van Bommel, Maarten; Hallett, Jessica

    2013-11-29

    An evaluation was undertaken of ultrahigh pressure liquid chromatography (UHPLC) in comparison to high-performance liquid chromatography (HPLC) for characterizing natural dyes in cultural heritage objects. A new UHPLC method was optimized by testing several analytical parameters adapted from prior UHPLC studies developed in diverse fields of research. Different gradient elution programs were tested on seven UHPLC columns with different dimensions and stationary phase compositions by applying several mobile phases, flow rates, temperatures, and runtimes. The UHPLC method successfully provided more improved data than that achieved by the HPLC method. Indeed, even though carminic acid has shown circa 146% higher resolution with HPLC, UHPLC resulted in an increase of 41-61% resolution and a decrease of 91-422% limit of detection, depending on the dye compound. The optimized method was subsequently assigned to analyse 59 natural reference materials, in which 85 different components were ascribed with different physicochemical properties, in order to create a spectral database for future characterization of dyes in cultural heritage objects. The majority of these reference samples could be successfully distinguished with one single method through the examination of these compounds' retention times and their spectra acquired with a photodiode array detector. These results demonstrate that UHPLC analyses are extremely valuable for the acquisition of more precise chromatographic information concerning natural dyes with complex mixtures of different and/or closely related physicochemical properties, essential for distinguishing similar species of plants and animals used to colour cultural heritage objects. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Performance evaluation methods and instrumentation for mine ventilation fans

    Institute of Scientific and Technical Information of China (English)

    LI Man; WANG Xue-rong

    2009-01-01

    Ventilation fans are one of the most important pieces of equipment in coal mines. Their performance plays an important role in the safety of staff and production. Given the actual requirements of coal mine production, we instituted a research project on the measurement methods of key performance parameters such as wind pressure, amount of ventilation and power. At the end a virtual instrument for mine ventilation fans performance evaluation was developed using a USB interface. The practical perform-ance and analytical results of our experiments show that it is feasible, reliable and effective to use the proposed instrumentation for mine ventilation performance evaluation.

  7. Instrumentation and measurement method for the ATLAS test facility

    Energy Technology Data Exchange (ETDEWEB)

    Yun, Byong Jo; Chu, In Chul; Eu, Dong Jin; Kang, Kyong Ho; Kim, Yeon Sik; Song, Chul Hwa; Baek, Won Pil

    2007-03-15

    An integral effect test loop for pressurized water reactors (PWRs), the ATLAS is constructed by thermal-hydraulic safety research division in KAERI. The ATLAS facility has been designed to have the length scale of 1/2 and area scale of 1/144 compared with the reference plant, APR1400 which is a Korean evolution type nuclear reactors. A total 1300 instrumentations is equipped in the ATLAS test facility. In this report, the instrumentation of ATLAS test facility and related measurement methods were introduced.

  8. Instrumental variable methods in comparative safety and effectiveness research.

    Science.gov (United States)

    Brookhart, M Alan; Rassen, Jeremy A; Schneeweiss, Sebastian

    2010-06-01

    Instrumental variable (IV) methods have been proposed as a potential approach to the common problem of uncontrolled confounding in comparative studies of medical interventions, but IV methods are unfamiliar to many researchers. The goal of this article is to provide a non-technical, practical introduction to IV methods for comparative safety and effectiveness research. We outline the principles and basic assumptions necessary for valid IV estimation, discuss how to interpret the results of an IV study, provide a review of instruments that have been used in comparative effectiveness research, and suggest some minimal reporting standards for an IV analysis. Finally, we offer our perspective of the role of IV estimation vis-à-vis more traditional approaches based on statistical modeling of the exposure or outcome. We anticipate that IV methods will be often underpowered for drug safety studies of very rare outcomes, but may be potentially useful in studies of intended effects where uncontrolled confounding may be substantial.

  9. Instrumental variable methods in comparative safety and effectiveness research†

    Science.gov (United States)

    Brookhart, M. Alan; Rassen, Jeremy A.; Schneeweiss, Sebastian

    2010-01-01

    Summary Instrumental variable (IV) methods have been proposed as a potential approach to the common problem of uncontrolled confounding in comparative studies of medical interventions, but IV methods are unfamiliar to many researchers. The goal of this article is to provide a non-technical, practical introduction to IV methods for comparative safety and effectiveness research. We outline the principles and basic assumptions necessary for valid IV estimation, discuss how to interpret the results of an IV study, provide a review of instruments that have been used in comparative effectiveness research, and suggest some minimal reporting standards for an IV analysis. Finally, we offer our perspective of the role of IV estimation vis-à-vis more traditional approaches based on statistical modeling of the exposure or outcome. We anticipate that IV methods will be often underpowered for drug safety studies of very rare outcomes, but may be potentially useful in studies of intended effects where uncontrolled confounding may be substantial. PMID:20354968

  10. Instrument for Solvent Extraction and Analysis (ISEE) of Organics from Regolith Simulant Using Supercritical Fluid Extraction and Chromatography

    Science.gov (United States)

    Franco, Carolina; Hintze, Paul E.

    2017-01-01

    ISEE is an instrument with the potential to perform extractions from regolith found on the surface of asteroids and planets, followed by characterization and quantitation of the extracts using supercritical fluid extraction (SFE) and chromatography (SFC). SFE is a developed technique proven to extract a wide range of organic compounds. SFC is similar to High Performance Liquid Chromatography (HPLC) but has the advantage of performing chiral separations without needing to derivatize the chiral compounds. CO2 will be the solvent for both stages as it is readily available in the Mars atmosphere. ISEE will capture CO2 from the environment, and use it for SFE and SFC. If successful, this would allow ISEE to perform analysis of organic compounds without using consumables. This paper will present results on a preliminary, proof-of-principle effort to use SFE and SFC to extract and analyze lunar regolith simulant spiked with organic compounds representing a range of organics that ISEE would expect to characterize. An optimization of variables for the extraction of the organics from the spiked regolith was successfully developed, using 138 bar pressure and 40 C temperature. The extraction flow rate was optimized at 2% SLPM with 30% methanol modifier. The extractions were successful with a value of 77.3+/- 0.9% of organics extracted. However, the recovery of organics after the extraction was very low with only 48.5+/-14.2%. Moreover, three columns were selected to analyze multiple samples at a time; two of them are Viridis HSS C18 SB and Torus DIOL, and the third column, specific for chiral separations, has not yet been selected yet.

  11. Determination of Alternaria mycotoxins in wine and juice using ionic liquid modified countercurrent chromatography as a pretreatment method followed by high-performance liquid chromatography.

    Science.gov (United States)

    Fan, Chen; Cao, Xueli; Liu, Man; Wang, Wei

    2016-03-04

    Alternariol (AOH), alternariol monomethyl ether (AME), and tenuazonic acid (TeA) are some of the main Alternaria mycotoxins that can be found as contaminants in food materials. The objective of this study was to develop a pretreatment method with countercurrent chromatography (CCC) for enrichment and cleanup of trace Alternaria mycotoxins in food samples prior to high-performance liquid chromatography (HPLC) analysis. An Analytical CCC instrument with a column volume 22.5mL was used, and a two-phase solvent system composed of ethyl acetate and water modified with 6% [HOOMIM][Cl] in mass to volume ratio was selected. Under the optimized CCC operation conditions, trace amounts of AOH, AME, and TeA in large volume of liquid sample were efficiently extracted and enriched in the stationary phase, and then eluted out just by reversing the stationary phase as mobile phase in the opposite flowing direction tail-to-head. The enrichment and elution strategies are unique and can be fulfilled online with high enrichment factors (87-114) and high recoveries (81.14-110.94%). The method has been successively applied to the determination of Alternaria mycotoxins in real apple juice and wine samples with the limits of detection (LOD) in the range of 0.03-0.14μgL(-1). Totally 12 wine samples and 15 apple juice samples from the local market were analyzed. The detection rate of AOH and AME in both kinds of the samples were more than 50%, while TeA was found in relatively high level of 1.75-49.61μgL(-1) in some of the apple juice samples. The proposed method is simple, rapid, and sensitive and could also be used for the analysis and monitoring of Alternaria mycotoxin in other food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Hybrid Instruments and the Indirect Credit Method - Does it work?

    OpenAIRE

    Wiedermann-Ondrej, Nadine

    2007-01-01

    This paper analyses the possibility of double non-taxation of hybrid instruments in cross border transactions where the country of the investor has implemented the indirect credit method for mitigation or elimination of double taxation. From an isolated perspective a double non-taxation cannot be obtained because typically no taxes are paid in the foreign country due to the classification as debt and therefore even in the case of a classification as a dividend in the country of the investor n...

  13. Instrumentation

    International Nuclear Information System (INIS)

    Prieur, G.; Nadi, M.; Hedjiedj, A.; Weber, S.

    1995-01-01

    This second chapter on instrumentation gives little general consideration on history and classification of instrumentation, and two specific states of the art. The first one concerns NMR (block diagram of instrumentation chain with details on the magnets, gradients, probes, reception unit). The first one concerns precision instrumentation (optical fiber gyro-meter and scanning electron microscope), and its data processing tools (programmability, VXI standard and its history). The chapter ends with future trends on smart sensors and Field Emission Displays. (D.L.). Refs., figs

  14. Solvent Front Position Extraction procedure with thin-layer chromatography as a mode of multicomponent sample preparation for quantitative analysis by instrumental technique.

    Science.gov (United States)

    Klimek-Turek, A; Sikora, E; Dzido, T H

    2017-12-29

    A concept of using thin-layer chromatography to multicomponent sample preparation for quantitative determination of solutes followed by instrumental technique is presented. Thin-layer chromatography (TLC) is used to separate chosen substances and their internal standard from other components (matrix) and to form a single spot/zone containing them at the solvent front position. The location of the analytes and internal standard in the solvent front zone allows their easy extraction followed by quantitation by HPLC. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2012-05-07

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

  16. Instrumentation

    International Nuclear Information System (INIS)

    Decreton, M.

    2000-01-01

    SCK-CEN's research and development programme on instrumentation aims at evaluating the potentials of new instrumentation technologies under the severe constraints of a nuclear application. It focuses on the tolerance of sensors to high radiation doses, including optical fibre sensors, and on the related intelligent data processing needed to cope with the nuclear constraints. Main achievements in these domains in 1999 are summarised

  17. Instrumentation

    Energy Technology Data Exchange (ETDEWEB)

    Decreton, M

    2001-04-01

    SCK-CEN's research and development programme on instrumentation involves the assessment and the development of sensitive measurement systems used within a radiation environment. Particular emphasis is on the assessment of optical fibre components and their adaptability to radiation environments. The evaluation of ageing processes of instrumentation in fission plants, the development of specific data evaluation strategies to compensate for ageing induced degradation of sensors and cable performance form part of these activities. In 2000, particular emphasis was on in-core reactor instrumentation applied to fusion, accelerator driven and water-cooled fission reactors. This involved the development of high performance instrumentation for irradiation experiments in the BR2 reactor in support of new instrumentation needs for MYRRHA, and for diagnostic systems for the ITER reactor.

  18. Instrumentation

    International Nuclear Information System (INIS)

    Decreton, M.

    2001-01-01

    SCK-CEN's research and development programme on instrumentation involves the assessment and the development of sensitive measurement systems used within a radiation environment. Particular emphasis is on the assessment of optical fibre components and their adaptability to radiation environments. The evaluation of ageing processes of instrumentation in fission plants, the development of specific data evaluation strategies to compensate for ageing induced degradation of sensors and cable performance form part of these activities. In 2000, particular emphasis was on in-core reactor instrumentation applied to fusion, accelerator driven and water-cooled fission reactors. This involved the development of high performance instrumentation for irradiation experiments in the BR2 reactor in support of new instrumentation needs for MYRRHA, and for diagnostic systems for the ITER reactor

  19. Purification of flavonoids from licorice using an off-line preparative two-dimensional normal-phase liquid chromatography/reversed-phase liquid chromatography method.

    Science.gov (United States)

    Fan, Yunpeng; Fu, Yanhui; Fu, Qing; Cai, Jianfeng; Xin, Huaxia; Dai, Mei; Jin, Yu

    2016-07-01

    An orthogonal (71.9%) off-line preparative two-dimensional normal-phase liquid chromatography/reversed-phase liquid chromatography method coupled with effective sample pretreatment was developed for separation and purification of flavonoids from licorice. Most of the nonflavonoids were firstly removed using a self-made Click TE-Cys (60 μm) solid-phase extraction. In the first dimension, an industrial grade preparative chromatography was employed to purify the crude flavonoids. Click TE-Cys (10 μm) was selected as the stationary phase that provided an excellent separation with high reproducibility. Ethyl acetate/ethanol was selected as the mobile phase owing to their excellent solubility for flavonoids. Flavonoids co-eluted in the first dimension were selected for further purification using reversed-phase liquid chromatography. Multiple compounds could be isolated from one normal-phase fraction and some compounds with bad resolution in one-dimensional liquid chromatography could be prepared in this two-dimensional system owing to the orthogonal separation. Moreover, this two-dimensional liquid chromatography method was beneficial for the preparation of relatively trace flavonoid compounds, which were enriched in the first dimension and further purified in the second dimension. Totally, 24 flavonoid compounds with high purity were obtained. The results demonstrated that the off-line two-dimensional liquid chromatography method was effective for the preparative separation and purification of flavonoids from licorice. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Ion Chromatography Applications in Wastewater Analysis

    Directory of Open Access Journals (Sweden)

    Rajmund Michalski

    2018-02-01

    Full Text Available Wastewater analysis is an important area in analytical and environmental chemistry. It can be performed with both the classic wet methods and instrumental techniques. The development of new methods, and modification of the existing ones, constitute a major task for researchers. Ion chromatography plays a predominant role in ion determinations with the instrumental methods. It offers several advantages over the conventional methods, such as simultaneous determinations of alkali and alkaline earth cations and ammonia. Ammonium ions cannot be determined by spectroscopic methods. Ion chromatography has been accepted world-wide as a reference method for analyzing anions and cations in water and wastewater due to the fact that it enables the replacement of several individual wet chemistry methods for common ions with one instrumental technique. The following article describes the principles of ion chromatography, such as stationary phases, eluents, detectors, and sample preparation methods. Moreover, the applications of ion chromatography in wastewater analyses and international standards are presented.

  1. Pesticides amenable to liquid chromatography: Multi Residue Method 2

    NARCIS (Netherlands)

    Baumann RA; Hogendoorn EA; van Zoonen P; LOC

    1996-01-01

    In dit rapport wordt een multiresidue methode voor de bepaling van bestrijdingsmiddelen met behulp van vloeistof-chromatografie in een grote verscheidenheid aan voedingsprodukten beschreven. De methode omvat N-methylcarbamaat pesticiden, fenylureum herbiciden en chloorfenoxy-azijnzuur herbiciden.

  2. Ion counting method and it's operational characteristics in gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Fujii, Toshihiro

    1976-01-01

    Ion counting method with continuous channel electron multiplier which affords the direct detection of very small ion currents and it's operational characteristics were studied in gas chromatography-mass spectrometry. Then this method was applied to the single ion detection technique of GC-MS. A detection limit was measured, using various standard samples of low level concentration. (auth.)

  3. Instrumentation

    International Nuclear Information System (INIS)

    Decreton, M.

    2002-01-01

    SCK-CEN's R and D programme on instrumentation involves the development of advanced instrumentation systems for nuclear applications as well as the assessment of the performance of these instruments in a radiation environment. Particular emphasis is on the use of optical fibres as umbilincal links of a remote handling unit for use during maintanance of a fusion reacor, studies on the radiation hardening of plasma diagnostic systems; investigations on new instrumentation for the future MYRRHA accelerator driven system; space applications related to radiation-hardened lenses; the development of new approaches for dose, temperature and strain measurements; the assessment of radiation-hardened sensors and motors for remote handling tasks and studies of dose measurement systems including the use of optical fibres. Progress and achievements in these areas for 2001 are described

  4. Instrumentation

    Energy Technology Data Exchange (ETDEWEB)

    Decreton, M

    2002-04-01

    SCK-CEN's R and D programme on instrumentation involves the development of advanced instrumentation systems for nuclear applications as well as the assessment of the performance of these instruments in a radiation environment. Particular emphasis is on the use of optical fibres as umbilincal links of a remote handling unit for use during maintanance of a fusion reacor, studies on the radiation hardening of plasma diagnostic systems; investigations on new instrumentation for the future MYRRHA accelerator driven system; space applications related to radiation-hardened lenses; the development of new approaches for dose, temperature and strain measurements; the assessment of radiation-hardened sensors and motors for remote handling tasks and studies of dose measurement systems including the use of optical fibres. Progress and achievements in these areas for 2001 are described.

  5. Instrumentation

    Energy Technology Data Exchange (ETDEWEB)

    Decreton, M

    2000-07-01

    SCK-CEN's research and development programme on instrumentation aims at evaluating the potentials of new instrumentation technologies under the severe constraints of a nuclear application. It focuses on the tolerance of sensors to high radiation doses, including optical fibre sensors, and on the related intelligent data processing needed to cope with the nuclear constraints. Main achievements in these domains in 1999 are summarised.

  6. Buffer-Free High Performance Liquid Chromatography Method for ...

    African Journals Online (AJOL)

    Purpose: To develop and validate a simple, economical and reproducible high performance liquid chromatographic (HPLC) method for the determination of theophylline in pharmaceutical dosage forms. Method: Caffeine was used as the internal standard and reversed phase C-18 column was used to elute the drug and ...

  7. Liquid chromatography coupled to on-line post column derivatization for the determination of organic compounds: A review on instrumentation and chemistries

    International Nuclear Information System (INIS)

    Zacharis, Constantinos K.; Tzanavaras, Paraskevas D.

    2013-01-01

    Graphical abstract: -- Highlights: •Review on liquid chromatography coupled to post-column derivatization. •Overview of instrumentation for post-column derivatization. •Post-column chemistries for analysis of organic compounds. -- Abstract: Analytical derivatization either in pre or post column modes is one of the most widely used sample pretreatment techniques coupled to liquid chromatography. In the present review article we selected to discuss the post column derivatization mode for the analysis of organic compounds. The first part of the review focuses to the instrumentation of post-column setups including not only fundamental components such as pumps and reactors but also less common parts such as static mixers and back-pressure regulators; the second part of the article discusses the most popular “chemistries” that are involved in post column applications, including reagent-less approaches and new sensing platforms such as the popular gold nanoparticles. Some representative recent applications are also presented as tables

  8. Liquid chromatography coupled to on-line post column derivatization for the determination of organic compounds: A review on instrumentation and chemistries

    Energy Technology Data Exchange (ETDEWEB)

    Zacharis, Constantinos K., E-mail: zacharis@chem.auth.gr [Laboratory of Analytical Chemistry, Department of Chemistry, Aristotelian University of Thessaloniki, GR-54124 Thessaloniki (Greece); Department of Food Technology, School of Food Technology and Nutrition, Alexander Technological Educational Institute (ATEI) of Thessaloniki, 57400 Thessaloniki (Greece); Tzanavaras, Paraskevas D., E-mail: ptzanava@chem.auth.gr [Laboratory of Analytical Chemistry, Department of Chemistry, Aristotelian University of Thessaloniki, GR-54124 Thessaloniki (Greece)

    2013-10-10

    Graphical abstract: -- Highlights: •Review on liquid chromatography coupled to post-column derivatization. •Overview of instrumentation for post-column derivatization. •Post-column chemistries for analysis of organic compounds. -- Abstract: Analytical derivatization either in pre or post column modes is one of the most widely used sample pretreatment techniques coupled to liquid chromatography. In the present review article we selected to discuss the post column derivatization mode for the analysis of organic compounds. The first part of the review focuses to the instrumentation of post-column setups including not only fundamental components such as pumps and reactors but also less common parts such as static mixers and back-pressure regulators; the second part of the article discusses the most popular “chemistries” that are involved in post column applications, including reagent-less approaches and new sensing platforms such as the popular gold nanoparticles. Some representative recent applications are also presented as tables.

  9. Extending the frontiers of mass spectrometric instrumentation and methods

    Energy Technology Data Exchange (ETDEWEB)

    Schieffer, Gregg Martin [Iowa State Univ., Ames, IA (United States)

    2010-01-01

    The focus of this dissertation is two-fold: developing novel analysis methods using mass spectrometry and the implementation and characterization of a novel ion mobility mass spectrometry instrumentation. The novel mass spectrometry combines ion trap for ion/ion reactions coupled to an ion mobility cell. The long term goal of this instrumentation is to use ion/ion reactions to probe the structure of gas phase biomolecule ions. The three ion source - ion trap - ion mobility - qTOF mass spectrometer (IT - IM - TOF MS) instrument is described. The analysis of the degradation products in coal (Chapter 2) and the imaging plant metabolites (Appendix III) fall under the methods development category. These projects use existing commercial instrumentation (JEOL AccuTOF MS and Thermo Finnigan LCQ IT, respectively) for the mass analysis of the degraded coal products and the plant metabolites, respectively. The coal degradation paper discusses the use of the DART ion source for fast and easy sample analysis. The sample preparation consisted of a simple 50 fold dilution of the soluble coal products in water and placing the liquid in front of the heated gas stream. This is the first time the DART ion source has been used for analysis of coal. Steven Raders under the guidance of John Verkade came up with the coal degradation projects. Raders performed the coal degradation reactions, worked up the products, and sent them to me. Gregg Schieffer developed the method and wrote the paper demonstrating the use of the DART ion source for the fast and easy sample analysis. The plant metabolite imaging project extends the use of colloidal graphite as a sample coating for atmospheric pressure LDI. DC Perdian and I closely worked together to make this project work. Perdian focused on building the LDI setup whereas Schieffer focused on the MSn analysis of the metabolites. Both Perdian and I took the data featured in the paper. Perdian was the primary writer of the paper and used it as a

  10. Schinus terebinthifolius countercurrent chromatography (Part II): Intra-apparatus scale-up and inter-apparatus method transfer.

    Science.gov (United States)

    Costa, Fernanda das Neves; Vieira, Mariana Neves; Garrard, Ian; Hewitson, Peter; Jerz, Gerold; Leitão, Gilda Guimarães; Ignatova, Svetlana

    2016-09-30

    Countercurrent chromatography (CCC) is being widely used across the world for purification of various materials, especially in natural product research. The predictability of CCC scale-up has been successfully demonstrated using specially designed instruments of the same manufacturer. The reality is that the most of CCC users do not have access to such instruments and do not have enough experience to transfer methods from one CCC column to another. This unique study of three international teams is based on innovative approach to simplify the scale-up between different CCC machines using fractionation of Schinus terebinthifolius berries dichloromethane extract as a case study. The optimized separation methodology, recently developed by the authors (Part I), was repeatedly performed on CCC columns of different design available at most research laboratories across the world. Hexane - ethyl acetate - methanol - water (6:1:6:1, v/v/v/v) was used as solvent system with masticadienonic and 3β-masticadienolic acids as target compounds to monitor stationary phase retention and calculate peak resolution. It has been demonstrated that volumetric, linear and length scale-up transfer factors based on column characteristics can be directly applied to different i.d., volume and length columns independently on instrument make in an intra-apparatus scale-up and inter-apparatus method transfer. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Determination of the Antibiotic Oxytetracycline in Commercial Milk by Solid-Phase Extraction: A High-Performance Liquid Chromatography (HPLC) Experiment for Quantitative Instrumental Analysis

    Science.gov (United States)

    Mei-Ratliff, Yuan

    2012-01-01

    Trace levels of oxytetracylcine spiked into commercial milk samples are extracted, cleaned up, and preconcentrated using a C[subscript 18] solid-phase extraction column. The extract is then analyzed by a high-performance liquid chromatography (HPLC) instrument equipped with a UV detector and a C[subscript 18] column (150 mm x 4.6 mm x 3.5 [mu]m).…

  12. New methods of magnet-based instrumentation for NOTES.

    Science.gov (United States)

    Magdeburg, Richard; Hauth, Daniel; Kaehler, Georg

    2013-12-01

    Laparoscopic surgery has displaced open surgery as the standard of care for many clinical conditions. NOTES has been described as the next surgical frontier with the objective of incision-free abdominal surgery. The principal challenge of NOTES procedures is the loss of triangulation and instrument rigidity, which is one of the fundamental concepts of laparoscopic surgery. To overcome these problems necessitates the development of new instrumentation. material and methods: We aimed to assess the use of a very simple combination of internal and external magnets that might allow the vigorous multiaxial traction/counter-traction required in NOTES procedures. The magnet retraction system consisted of an external magnetic assembly and either small internal magnets attached by endoscopic clips to the designated tissue (magnet-clip-approach) or an endoscopic grasping forceps in a magnetic deflector roll (magnet-trocar-approach). We compared both methods regarding precision, time and efficacy by performing transgastric partial uterus resections with better results for the magnet-trocar-approach. This proof-of-principle animal study showed that the combination of external and internal magnets generates sufficient coupling forces at clinically relevant abdominal wall thicknesses, making them suitable for use and evaluation in NOTES procedures, and provides the vigorous multiaxial traction/counter-traction required by the lack of additional abdominal trocars.

  13. Simultaneous determination of seven flavonoids in Epimedium by liquid chromatography-tandem mass spectrometry method

    Institute of Scientific and Technical Information of China (English)

    Cai Sheng Wu; Bao Lin Guo; Yu Xin Sheng; Jin Lan Zhang

    2008-01-01

    In this paper, a sensitive and specific liquid chromatography-electrospray ionisation-mass spectrometry (LC-ESI-MS) method has been developed and validated for the identification and determination of seven flavonoids, namely epimedin A, epimedin B, epimedin C, icariin, sagittatoside B, 2"-0-rhamnosyl icariside II, and baohuoside I in Epimedium from different sources.

  14. Methods and instrumentation for quantitative microchip capillary electrophoresis

    NARCIS (Netherlands)

    Revermann, T.

    2007-01-01

    The development of novel instrumentation and analytical methodology for quantitative microchip capillary electrophoresis (MCE) is described in this thesis. Demanding only small quantities of reagents and samples, microfluidic instrumentation is highly advantageous. Fast separations at high voltages

  15. Downstream processing and chromatography based analytical methods for production of vaccines, gene therapy vectors, and bacteriophages

    Science.gov (United States)

    Kramberger, Petra; Urbas, Lidija; Štrancar, Aleš

    2015-01-01

    Downstream processing of nanoplexes (viruses, virus-like particles, bacteriophages) is characterized by complexity of the starting material, number of purification methods to choose from, regulations that are setting the frame for the final product and analytical methods for upstream and downstream monitoring. This review gives an overview on the nanoplex downstream challenges and chromatography based analytical methods for efficient monitoring of the nanoplex production. PMID:25751122

  16. Instruments

    International Nuclear Information System (INIS)

    Buehrer, W.

    1996-01-01

    The present paper mediates a basic knowledge of the most commonly used experimental techniques. We discuss the principles and concepts necessary to understand what one is doing if one performs an experiment on a certain instrument. (author) 29 figs., 1 tab., refs

  17. Setting up of a liquid chromatography-high resolution tandem mass spectrometry method for the detection of caseins in food. A comparison with ELISA method

    Directory of Open Access Journals (Sweden)

    Daniela Gastaldi

    2013-06-01

    Full Text Available Determination of caseins in food matrices is usually performed by using the competitiveenzyme- linked immunosorbent assay (ELISA technique. However such a technique suffers from a number of limitations. Among these, the applicability to a narrow concentration range, a non linear (logarithmic response, a non-negligible cross-reactivity and a high cost per kit. At the time of the completion of this study, in case of ELISA positive feedback, there was poor availability in the literature of finding reliable instrumental methods able to determine both qualitatively and quantitatively this class of substances. In the present study, a liquid chromatography-high resolution tandem mass spectrometry (HPLC-HRMS/MS instrumental method was developed with a high resolution mass spectrometer (Orbitrap. Real samples of sausages in which caseins were detected by ELISA technique were analysed. A casein-free sample of ham was used as a blank. The analytical characteristics of the instrumental method were compared with those of a commercial ELISA test, declared specific for α- and β-casein.

  18. Cromatografia unificada Unified chromatography

    Directory of Open Access Journals (Sweden)

    Carin von Mühlen

    2004-10-01

    Full Text Available The scope of this study encompasses an overview of the principles of unified chromatography as well as the principles of chromatographic techniques as applied to unified systems, which include gas chromatography, liquid chromatography, supercritical fluid chromatography, high temperature and high pressure liquid chromatography, micro-liquid chromatography, enhanced fluidity chromatography, and solvating gas chromatography. Theoretical considerations and individual instrumental parameters such as mobile phase, sample introduction system, columns, and detection system are also discussed. Future applications of this separation approach are discussed.

  19. Method to deterministically study photonic nanostructures in different experimental instruments.

    Science.gov (United States)

    Husken, B H; Woldering, L A; Blum, C; Vos, W L

    2009-01-01

    We describe an experimental method to recover a single, deterministically fabricated nanostructure in various experimental instruments without the use of artificially fabricated markers, with the aim to study photonic structures. Therefore, a detailed map of the spatial surroundings of the nanostructure is made during the fabrication of the structure. These maps are made using a series of micrographs with successively decreasing magnifications. The graphs reveal intrinsic and characteristic geometric features that can subsequently be used in different setups to act as markers. As an illustration, we probe surface cavities with radii of 65 nm on a silica opal photonic crystal with various setups: a focused ion beam workstation; a scanning electron microscope (SEM); a wide field optical microscope and a confocal microscope. We use cross-correlation techniques to recover a small area imaged with the SEM in a large area photographed with the optical microscope, which provides a possible avenue to automatic searching. We show how both structural and optical reflectivity data can be obtained from one and the same nanostructure. Since our approach does not use artificial grids or markers, it is of particular interest for samples whose structure is not known a priori, like samples created solely by self-assembly. In addition, our method is not restricted to conducting samples.

  20. Methods of analysis-Determination of pesticides in sediment using gas chromatography/mass spectrometry

    Science.gov (United States)

    Hladik, Michelle; McWayne, Megan M.

    2012-01-01

    A method for the determination of 119 pesticides in environmental sediment samples is described. The method was developed by the U.S. Geological Survey (USGS) in support of the National Water Quality Assessment (NAWQA) Program. The pesticides included in this method were chosen through prior prioritization. Herbicides, insecticides, and fungicides along with degradates are included in this method and span a variety of chemical classes including, but not limited to, chloroacetanilides, organochlorines, organophosphates, pyrethroids, triazines, and triazoles. Sediment samples are extracted by using an accelerated solvent extraction system (ASE®, and the compounds of interest are separated from co-extracted matrix interferences (including sulfur) by passing the extracts through high performance liquid chromatography (HPLC) with gel-permeation chromatography (GPC) along with the use of either stacked graphitized carbon and alumina solid-phase extraction (SPE) cartridges or packed Florisil®. Chromatographic separation, detection, and quantification of the pesticides from the sediment-sample extracts are done by using gas chromatography with mass spectrometry (GC/MS). Recoveries in test sediment samples fortified at 10 micrograms per kilogram (μg/kg) dry weight ranged from 75 to 102 percent; relative standard deviations ranged from 3 to 13 percent. Method detection limits (MDLs), calculated by using U.S. Environmental Protection Agency procedures (40 CFR 136, Appendix B), ranged from 0.6 to 3.4 μg/kg dry weight.

  1. Easy instrumental analysis

    International Nuclear Information System (INIS)

    Ko, Myeong Su; Kim, Tae Hwa; Park, Gyu Hyeon; Yang, Jong Beom; Oh, Chang Hwan; Lee, Kyoung Hye

    2010-04-01

    This textbook describes instrument analysis in easy way with twelve chapters. The contents of the book are pH measurement on principle, pH meter, pH measurement, examples of the experiments, centrifugation, Absorptiometry, Fluorescent method, Atomic absorption analysis, Gas-chromatography, Gas chromatography-mass spectrometry, High performance liquid chromatography liquid chromatograph-mass spectrometry, Electrophoresis on practical case and analysis of the result and examples, PCR on principle, device, application and examples and Enzyme-linked immunosorbent assay with indirect ELISA, sandwich ELISA and ELISA reader.

  2. Easy instrumental analysis

    Energy Technology Data Exchange (ETDEWEB)

    Ko, Myeong Su; Kim, Tae Hwa; Park, Gyu Hyeon; Yang, Jong Beom; Oh, Chang Hwan; Lee, Kyoung Hye

    2010-04-15

    This textbook describes instrument analysis in easy way with twelve chapters. The contents of the book are pH measurement on principle, pH meter, pH measurement, examples of the experiments, centrifugation, Absorptiometry, Fluorescent method, Atomic absorption analysis, Gas-chromatography, Gas chromatography-mass spectrometry, High performance liquid chromatography liquid chromatograph-mass spectrometry, Electrophoresis on practical case and analysis of the result and examples, PCR on principle, device, application and examples and Enzyme-linked immunosorbent assay with indirect ELISA, sandwich ELISA and ELISA reader.

  3. Development of a sensitive and rapid method for rifampicin impurity analysis using supercritical fluid chromatography.

    Science.gov (United States)

    Li, Wei; Wang, Jun; Yan, Zheng-Yu

    2015-10-10

    A novel simple, fast and efficient supercritical fluid chromatography (SFC) method was developed and compared with RPLC method for the separation and determination of impurities in rifampicin. The separation was performed using a packed diol column and a mobile phase B (modifier) consisting of methanol with 0.1% ammonium formate (w/v) and 2% water (v/v). Overall satisfactory resolutions and peak shapes for rifampicin quinone (RQ), rifampicin (RF), rifamycin SV (RSV), rifampicin N-oxide (RNO) and 3-formylrifamycinSV (3-FR) were obtained by optimization of the chromatography system. With gradient elution of mobile phase, all of the impurities and the active were separated within 4 min. Taking full advantage of features of SFC (such as particular selectivity, non-sloping baseline in gradient elution, and without injection solvent effects), the method was successfully used for determination of impurities in rifampicin, with more impurity peaks detected, better resolution achieved and much less analysis time needed compared with conventional reversed-phase liquid chromatography (RPLC) methods. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. A novel liquid chromatography method using diode-array detector for the determination of oleuropein in dietary supplements.

    Science.gov (United States)

    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.

  5. A simple high performance liquid chromatography method for analyzing paraquat in soil solution samples.

    Science.gov (United States)

    Ouyang, Ying; Mansell, Robert S; Nkedi-Kizza, Peter

    2004-01-01

    A high performance liquid chromatography (HPLC) method with UV detection was developed to analyze paraquat (1,1'-dimethyl-4,4'-dipyridinium dichloride) herbicide content in soil solution samples. The analytical method was compared with the liquid scintillation counting (LSC) method using 14C-paraquat. Agreement obtained between the two methods was reasonable. However, the detection limit for paraquat analysis was 0.5 mg L(-1) by the HPLC method and 0.05 mg L(-1) by the LSC method. The LSC method was, therefore, 10 times more precise than the HPLC method for solution concentrations less than 1 mg L(-1). In spite of the high detection limit, the UC (nonradioactive) HPLC method provides an inexpensive and environmentally safe means for determining paraquat concentration in soil solution compared with the 14C-LSC method.

  6. A simple method for the measurement of radioactivity of samples separated by gas chromatography

    International Nuclear Information System (INIS)

    Farkas, T.

    1981-01-01

    Gas chromatographs with flame ionization detector can be used to determine the radioactivity ( 14 C) of separated peaks. After a suitable change in the detector output the combustion product 14 CO 2 can be trapped by hyamine hydroxyde and measured by liquid scintigraphy. 90% of peak activity can be collected and measured, thus the method can be applied to determine the distribution and specific radioactivity of the components separated by gas chromatography. (author)

  7. Possibilities and limitations of the kinetic plot method in supercritical fluid chromatography.

    Science.gov (United States)

    De Pauw, Ruben; Desmet, Gert; Broeckhoven, Ken

    2013-08-30

    Although supercritical fluid chromatography (SFC) is becoming a technique of increasing importance in the field of analytical chromatography, methods to compare the performance of SFC-columns and separations in an unbiased way are not fully developed. The present study uses mathematical models to investigate the possibilities and limitations of the kinetic plot method in SFC as this easily allows to investigate a wide range of operating pressures, retention and mobile phase conditions. The variable column length (L) kinetic plot method was further investigated in this work. Since the pressure history is identical for each measurement, this method gives the true kinetic performance limit in SFC. The deviations of the traditional way of measuring the performance as a function of flow rate (fixed back pressure and column length) and the isopycnic method with respect to this variable column length method were investigated under a wide range of operational conditions. It is found that using the variable L method, extrapolations towards other pressure drops are not valid in SFC (deviation of ∼15% for extrapolation from 50 to 200bar pressure drop). The isopycnic method provides the best prediction but its use is limited when operating closer towards critical point conditions. When an organic modifier is used, the predictions are improved for both methods with respect to the variable L method (e.g. deviations decreases from 20% to 2% when 20mol% of methanol is added). Copyright © 2013 Elsevier B.V. All rights reserved.

  8. Hydroxylapatite chromatography.

    Science.gov (United States)

    Broadhurst, A V

    2001-05-01

    Hydroxylapatite (also called hydroxyapatite), a form of calcium phosphate, can be used as a matrix for the chromatography of both proteins and nucleic acids. Protocols are provided for both standard low-pressure chromatography of a protein mixture using a hydroxylapatite column prepared in the laboratory, and an HPLC method, applicable to proteins and nucleic acids, that uses a commercially available column. Alternate protocols describe column chromatography using a step gradient or batch binding and step-gradient elution.

  9. Development and validation of ultra-high performance supercritical fluid chromatography method for determination of illegal dyes and comparison to ultra-high performance liquid chromatography method.

    Science.gov (United States)

    Khalikova, Maria A; Šatínský, Dalibor; Solich, Petr; Nováková, Lucie

    2015-05-18

    A novel simple, fast and efficient ultra-high performance supercritical fluid chromatography (UHPSFC) method was developed and validated for the separation and quantitative determination of eleven illegal dyes in chili-containing spices. The method involved a simple ultrasound-assisted liquid extraction of illegal compounds with tetrahydrofuran. The separation was performed using a supercritical fluid chromatography system and CSH Fluoro-Phenyl stationary phase at 70°C. The mobile phase was carbon dioxide and the mixture of methanol:acetonitrile (1:1, v/v) with 2.5% formic acid as an additive at the flow rate 2.0 mL min(-1). The UV-vis detection was accomplished at 500 nm for seven compounds and at 420 nm for Sudan Orange G, Butter Yellow, Fast Garnet GBC and Methyl Red due to their maximum of absorbance. All eleven compounds were separated in less than 5 min. The method was successfully validated and applied using three commercial samples of chili-containing spices - Chili sauce (Indonesia), Feferony sauce (Slovakia) and Mojo sauce (Spain). The linearity range of proposed method was 0.50-9.09 mg kg(-1) (r ≥ 0.995). The detection limits were determined as signal to noise ratio of 3 and were ranged from 0.15 mg kg(-1) to 0.60 mg kg(-1) (1.80 mg kg(-1) for Fast Garnet) for standard solution and from 0.25 mg kg(-1) to 1.00 mg kg(-1) (2.50 mg kg(-1) for Fast Garnet, 1.50 mg kg(-1) for Sudan Red 7B) for chili-containing samples. The recovery values were in the range of 73.5-107.2% and relative standard deviation ranging from 0.1% to 8.2% for within-day precision and from 0.5% to 8.8% for between-day precision. The method showed potential for being used to monitor forbidden dyes in food constituents. The developed UHPSFC method was compared to the UHPLC-UV method. The orthogonality of Sudan dyes separation by these two methods was demonstrated. Benefits and drawbacks were discussed showing the reliability of both methods for monitoring of studied illegal dyes in real

  10. Recent developments in comprehensive two-dimensional gas chromatography (GC X GC) I. Introduction and instrumental set-up

    NARCIS (Netherlands)

    Adahchour, M.; Beens, J.; Vreuls, R.J.J.; Brinkman, U.A.T.

    2006-01-01

    We review the literature on comprehensive two-dimensional gas chromatography (GC × GC), emphasizing developments in the period 2003-2005. The review opens with a general introduction, the principles of the technique and the set-up of GC × GC systems. It also discusses theoretical aspects, trends in

  11. Chromatography and mass spectrometry of chemical warfare agents, toxins and related compounds: state of the art and future prospects

    NARCIS (Netherlands)

    Kientz, C.E.

    1998-01-01

    Methods for the identification of chemical warfare agents, toxins, bioregulators and related products are frequently reported in literature. These methods are often based on instrumental analysis using chromatography (gas and liquid) and mass spectrometry. Here, these instrumental techniques are

  12. Instrumental performance of an etude after three methods of practice.

    Science.gov (United States)

    Vanden Ark, S

    1997-12-01

    For 80 fifth-grade students three practice conditions (mental, mental with physical simulation, and physical with singing) produced significant mean differences in instrumental performance of an etude. No significant differences were found for traditional, physical practice.

  13. Development of an on-line mixed-mode gel liquid chromatography×reversed phase liquid chromatography method for separation of water extract from Flos Carthami.

    Science.gov (United States)

    Wang, Yu-Qing; Tang, Xu; Li, Jia-Fu; Wu, Yun-Long; Sun, Yu-Ying; Fang, Mei-Juan; Wu, Zhen; Wang, Xiu-Min; Qiu, Ying-Kun

    2017-10-13

    A novel on-line comprehensive two-dimensional liquid chromatography (2D-LC) method by coupling mixed-mode gel liquid chromatography (MMG-LC) with reversed phase liquid chromatography (RPLC) was developed. A mixture of 17 reference compounds was used to study the separation mechanism. A crude water extract of Flos Carthami was applied to evaluate the performance of the novel 2D-LC system. In the first dimension, the extract was eluted with a gradient of water/methanol over a cross-linked dextran gel Sephadex LH-20 column. Meanwhile, the advantages of size exclusion, reversed phase partition and adsorption separation mechanism were exploited before further on-line reversed phase purification on the second dimension. This novel on-line mixed-mode Sephadex LH-20×RPLC method provided higher peak resolution, sample processing ability (2.5mg) and better orthogonality (72.9%) versus RPLC×RPLC and hydrophilic interaction liquid chromatography (HILIC)×RPLC. To the best of our knowledge, this is the first report of a mixed-mode Sephadex LH-20×RPLC separation method with successful applications in on-line mode, which might be beneficial for harvesting targets from complicated medicinal plants. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Spectrometric methods used in the calibration of radiodiagnostic measuring instruments

    Energy Technology Data Exchange (ETDEWEB)

    De Vries, W [Rijksuniversiteit Utrecht (Netherlands)

    1995-12-01

    Recently a set of parameters for checking the quality of radiation for use in diagnostic radiology was established at the calibration facility of Nederlands Meetinstituut (NMI). The establishment of the radiation quality required re-evaluation of the correction factors for the primary air-kerma standards. Free-air ionisation chambers require several correction factors to measure air-kerma according to its definition. These correction factors were calculated for the NMi free-air chamber by Monte Carlo simulations for monoenergetic photons in the energy range from 10 keV to 320 keV. The actual correction factors follow from weighting these mono-energetic correction factors with the air-kerma spectrum of the photon beam. This paper describes the determination of the photon spectra of the X-ray qualities used for the calibration of dosimetric instruments used in radiodiagnostics. The detector used for these measurements is a planar HPGe-detector, placed in the direct beam of the X-ray machine. To convert the measured pulse height spectrum to the actual photon spectrum corrections must be made for fluorescent photon escape, single and multiple compton scattering inside the detector, and detector efficiency. From the calculated photon spectra a number of parameters of the X-ray beam can be calculated. The calculated first and second half value layer in aluminum and copper are compared with the measured values of these parameters to validate the method of spectrum reconstruction. Moreover the spectrum measurements offer the possibility to calibrate the X-ray generator in terms of maximum high voltage. The maximum photon energy in the spectrum is used as a standard for calibration of kVp-meters.

  15. A high pressure liquid chromatography method for separation of prolactin forms.

    Science.gov (United States)

    Bell, Damon A; Hoad, Kirsten; Leong, Lillian; Bakar, Juwaini Abu; Sheehan, Paul; Vasikaran, Samuel D

    2012-05-01

    Prolactin has multiple forms and macroprolactin, which is thought not to be bioavailable, can cause a raised serum prolactin concentration. Gel filtration chromatography (GFC) is currently the gold standard method for separating macroprolactin, but is labour-intensive. Polyethylene glycol (PEG) precipitation is suitable for routine use but may not always be accurate. We developed a high pressure liquid chromatography (HPLC) assay for macroprolactin measurement. Chromatography was carried out using an Agilent Zorbax GF-250 (9.4 × 250 mm, 4 μm) size exclusion column and 50 mmol/L Tris buffer with 0.15 mmol/L NaCl at pH 7.2 as mobile phase, with a flow rate of 1 mL/min. Serum or plasma was diluted 1:1 with mobile phase and filtered and 100 μL injected. Fractions of 155 μL were collected for prolactin measurement and elution profile plotted. The area under the curve of each prolactin peak was calculated to quantify each prolactin form, and compared with GFC. Clear separation of monomeric-, big- and macroprolactin forms was achieved. Quantification was comparable to GFC and precision was acceptable. Total time from injection to collection of the final fraction was 16 min. We have developed an HPLC method for quantification of macroprolactin, which is rapid and easy to perform and therefore can be used for routine measurement.

  16. A method for fast determination of psoralens in oral solutions of phytomedicines using liquid chromatography.

    Science.gov (United States)

    Pires, Adriana Elias; Honda, Neli Kiko; Cardoso, Cláudia Andréa Lima

    2004-10-29

    A method for sample preparation and analysis by high performance liquid chromatography with UV detection (HPLC-UV) has been developed for routine analysis of psoralen and bergapten, photosensitizing compounds, in oral solutions of phytomedicines employed in Brazil for some illnesses. The linearity, accuracy, the inter- and intra-day precision of the procedure were evaluated. Calibration curves for psoralen and bergapten were linear in the range of 1.0-600.0 microg ml(-1) and 1.0-400.0 microg ml(-1) respectively. The recoveries of the psoralens in the oral solutions analysed were 94.43-99.97%. The percentage coefficient of variation (CV) of the quantitative analysis of the psoralens in the products analysis was within 5%. In inter-equipment study was employed gas chromatography-flame ionization (CG-FID) detection.

  17. Practical method transfer from high performance liquid chromatography to ultra-high performance liquid chromatography: the importance of frictional heating.

    Science.gov (United States)

    Nováková, Lucie; Veuthey, Jean Luc; Guillarme, Davy

    2011-11-04

    In theory, with identical stationary phase chemistry, the transfer of an HPLC method to UHPLC conditions is straightforward and necessitates the calculation of new conditions based on column and instrument geometries. Occasionally, undesirable changes in selectivity, retention or efficiency have been reported and have been attributed to a frictional heating phenomenon that is due to the elevated generated pressure drop. In the present study, the frictional heating in a UHPLC system was evaluated experimentally under gradient elution conditions (acetonitrile/buffer at pH 3 and 9) with generated pressure drops in the range of 100-1000 bar on both 1.0mm and 2.1mm I.D. columns using a mixture of 10 representative basic, acidic and neutral pharmaceutical compounds. Under adiabatic conditions (i.e., still-air oven), the longitudinal temperature gradient was estimated at +4 °C, +8 °C and +16 °C at 300, 600 and 1000 bar, respectively, on a 2.1mm I.D. column using an empirical measurement procedure. With the 1.0mm I.D. column, these values were reduced to +3 °C, +6 °C and +12 °C, respectively. Finally, various approaches to eliminate or at least to reduce the effect of frictional heating are briefly discussed. Copyright © 2011 Elsevier B.V. All rights reserved.

  18. Authentication method for safeguards instruments securing data transmission

    International Nuclear Information System (INIS)

    Richter, B.; Stein, G.; Neumann, G.; Gartner, K.J.

    1986-01-01

    Because of the worldwide increase in nuclear fuel cycle activities, the need arises to reduce inspection effort by increasing the inspection efficiency per facility. Therefore, more and more advanced safeguards instruments will be designed for automatic operation. In addition, sensoring and recording devices may be well separated from each other within the facility, while the data transmission medium is a cable. The basic problem is the authenticity of the transmitted information. It has to be ensured that no potential adversary is able to falsify the transmitted safeguards data, i.e. the data transmission is secured. At present, predominantly C/S-devices are designed for automatic and remote interrogation. Also in other areas of safeguards instrumentation authentication will become a major issue, in particular, where the facility operator may offer his process instrumentation to be used also for safeguards purposes. In this paper possibilities to solve the problem of authentication are analysed

  19. Development of conjugate methods with gas chromatography for inorganic compounds analysis

    International Nuclear Information System (INIS)

    Baccan, N.

    1975-01-01

    The application of gas chromatography combined with mass spectrometry or with nuclear methods for the analysis of inorganic compounds is studied. The advantages of the use of a gas chromatograph coupled with a quadrupole mass spectrometer or with a high resolution radiation detector, are discussed. We also studied the formation and solvent extraction of metal chelates; an aliquot of the organic phase was directly injected into the gas chromatograph and the eluted compounds were detected by mass spectrometry or, when radioactive, by nuclear methods. (author)

  20. Validation of a method to determine methylmercury in fish tissues using gas chromatography

    International Nuclear Information System (INIS)

    Vega Bolannos, Luisa O.; Arias Verdes, Jose A.; Beltran Llerandi, Gilberto; Castro Diaz, Odalys; Moreno Tellez, Olga L.

    2000-01-01

    We validated a method to determine methylmercury in fish tissues using gas chromatography with an electron capture detector as described by the Association of Official Analytical Chemist (AOAC) International. The linear curve range was 0.02 to 1 g/ml and linear correlation coefficient was 0.9979. A 1 mg/kg methylmercury-contaminated fish sample was analyzed 20 times to determine repeatability of the method. The quantification limit was 0.16 mg/kg and detection limit was 0.06 ppm. Fish samples contaminated with 0.2 to 10 mg/kg methylmercury showed recovery indexes from 94.66 to 108.8%

  1. Comparison of photoacoustic radiometry to gas chromatography/mass spectrometry methods for monitoring chlorinated hydrocarbons

    International Nuclear Information System (INIS)

    Sollid, J.E.; Trujillo, V.L.; Limback, S.P.; Woloshun, K.A.

    1996-01-01

    A comparison of two methods of gas chromatography mass spectrometry (GCMS) and a nondispersive infrared technique, photoacoustic radiometry (PAR), is presented in the context of field monitoring a disposal site. First is presented an historical account describing the site and early monitoring to provide an overview. The intent and nature of the monitoring program changed when it was proposed to expand the Radiological Waste Site close to the Hazardous Waste Site. Both the sampling methods and analysis techniques were refined in the course of this exercise

  2. Efficient methods for isolating five phytochemicals from Gentiana macrophylla using high-performance countercurrent chromatography.

    Science.gov (United States)

    Rho, Taewoong; Jung, Mila; Lee, Min Won; Chin, Young-Won; Yoon, Kee Dong

    2016-12-01

    Efficient high-performance countercurrent chromatography methods were developed to isolate five typical compounds from the extracts of Gentiana macrophylla. n-Butanol-soluble extract of G. macrophylla contained three hydrophilic iridoids, loganic acid (1), swertiamarin (2) and gentiopicroside (3), and a chromene derivative, macrophylloside D (4) which were successfully isolated by flow rate gradient (1.5 mL/min in 0-60 min, 5.0 mL/min in 60-120 min), and consecutive flow rate gradient HPCCC using n-butanol/0.1% aqueous trifluoroacetic acid (1:1, v/v, normal phase mode) system. The yields of 1-4 were 22, 16, 122, and 6 mg, respectively, with purities over 97% in a flow rate gradient high-performance countercurrent chromatography, and consecutive flow rate gradient high-performance countercurrent chromatography gave 1, 2, 3 (54, 41, 348 mg, respectively, purities over 97%) and 4 (13 mg, purity at 95%) from 750 mg of sample. The main compound in methylene chloride soluble extract, 2-methoxyanofinic acid, was successfully separated by n-hexane/ethyl acetate/methanol/water (4:6:4:6, v/v/v/v, flow-rate: 4 mL/min, reversed phase mode) condition. The structures of five isolates were elucidated by 1 H, 13 C NMR and ESI-Q-TOF-MS spectroscopic data which were compared with previously reported values. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Determination of Urine Albumin by New Simple High-Performance Liquid Chromatography Method.

    Science.gov (United States)

    Klapkova, Eva; Fortova, Magdalena; Prusa, Richard; Moravcova, Libuse; Kotaska, Karel

    2016-11-01

    A simple high-performance liquid chromatography (HPLC) method was developed for the determination of albumin in patients' urine samples without coeluting proteins and was compared with the immunoturbidimetric determination of albumin. Urine albumin is important biomarker in diabetic patients, but part of it is immuno-nonreactive. Albumin was determined by high-performance liquid chromatography (HPLC), UV detection at 280 nm, Zorbax 300SB-C3 column. Immunoturbidimetric analysis was performed using commercial kit on automatic biochemistry analyzer COBAS INTEGRA ® 400, Roche Diagnostics GmbH, Manheim, Germany. The HLPC method was fully validated. No significant interference with other proteins (transferrin, α-1-acid glycoprotein, α-1-antichymotrypsin, antitrypsin, hemopexin) was found. The results from 301 urine samples were compared with immunochemical determination. We found a statistically significant difference between these methods (P = 0.0001, Mann-Whitney test). New simple HPLC method was developed for the determination of urine albumin without coeluting proteins. Our data indicate that the HPLC method is highly specific and more sensitive than immunoturbidimetry. © 2016 Wiley Periodicals, Inc.

  4. An optimized method for the measurement of acetaldehyde by high-performance liquid chromatography.

    Science.gov (United States)

    Guan, Xiangying; Rubin, Emanuel; Anni, Helen

    2012-03-01

    Acetaldehyde is produced during ethanol metabolism predominantly in the liver by alcohol dehydrogenase and rapidly eliminated by oxidation to acetate via aldehyde dehydrogenase. Assessment of circulating acetaldehyde levels in biological matrices is performed by headspace gas chromatography and reverse phase high-performance liquid chromatography (RP-HPLC). We have developed an optimized method for the measurement of acetaldehyde by RP-HPLC in hepatoma cell culture medium, blood, and plasma. After sample deproteinization, acetaldehyde was derivatized with 2,4-dinitrophenylhydrazine (DNPH). The reaction was optimized for pH, amount of derivatization reagent, time, and temperature. Extraction methods of the acetaldehyde-hydrazone (AcH-DNP) stable derivative and product stability studies were carried out. Acetaldehyde was identified by its retention time in comparison with AcH-DNP standard, using a new chromatography gradient program, and quantitated based on external reference standards and standard addition calibration curves in the presence and absence of ethanol. Derivatization of acetaldehyde was performed at pH 4.0 with an 80-fold molar excess of DNPH. The reaction was completed in 40 minutes at ambient temperature, and the product was stable for 2 days. A clear separation of AcH-DNP from DNPH was obtained with a new 11-minute chromatography program. Acetaldehyde detection was linear up to 80 μM. The recovery of acetaldehyde was >88% in culture media and >78% in plasma. We quantitatively determined the ethanol-derived acetaldehyde in hepatoma cells, rat blood and plasma with a detection limit around 3 μM. The accuracy of the method was volume (70 μl) plasma sampling. An optimized method for the quantitative determination of acetaldehyde in biological systems was developed using derivatization with DNPH, followed by a short RP-HPLC separation of AcH-DNP. The method has an extended linear range, is reproducible and applicable to small-volume sampling of culture

  5. Method transfer from high-pressure liquid chromatography to ultra-high-pressure liquid chromatography. II. Temperature and pressure effects.

    Science.gov (United States)

    Åsberg, Dennis; Samuelsson, Jörgen; Leśko, Marek; Cavazzini, Alberto; Kaczmarski, Krzysztof; Fornstedt, Torgny

    2015-07-03

    The importance of the generated temperature and pressure gradients in ultra-high-pressure liquid chromatography (UHPLC) are investigated and compared to high-pressure liquid chromatography (HPLC). The drug Omeprazole, together with three other model compounds (with different chemical characteristics, namely uncharged, positively and negatively charged) were used. Calculations of the complete temperature profile in the column at UHPLC conditions showed, in our experiments, a temperature difference between the inlet and outlet of 16 °C and a difference of 2 °C between the column center and the wall. Through van't Hoff plots, this information was used to single out the decrease in retention factor (k) solely due to the temperature gradient. The uncharged solute was least affected by temperature with a decrease in k of about 5% while for charged solutes the effect was more pronounced, with k decreases up to 14%. A pressure increase of 500 bar gave roughly 5% increase in k for the uncharged solute, while omeprazole and the other two charged solutes gave about 25, 20 and 15% increases in k, respectively. The stochastic model of chromatography was applied to estimate the dependence of the average number of adsorption/desorption events (n) and the average time spent by a molecule in the stationary phase (τs) on temperature and pressure on peak shape for the tailing, basic solute. Increasing the temperature yielded an increase in n and decrease in τs which resulted in less skew at high temperatures. With increasing pressure, the stochastic modeling gave interesting results for the basic solute showing that the skew of the peak increased with pressure. The conclusion is that pressure effects are more pronounced for both retention and peak shape than the temperature effects for the polar or charged compounds in our study. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Application of partition chromatography method for separation and analysis of actinium radionuclides

    International Nuclear Information System (INIS)

    Sinitsina, G.S.; Shestakova, I.A.; Shestakov, B.I.; Plyushcheva, N.A.; Malyshev, N.A.; Belyatskij, A.F.; Tsirlin, V.A.

    1979-01-01

    The method of partition chromatography is considered with the use of different extractants for the extraction of actinium-227, actinium-225 and actinium-228. It is advisable to extract actinium-227 from the irradiated radium with the help of D2FGFK. The use of 2DEGFK allows us to separate actinium-227 from alkaline and alkaline-earth elements. Amines have a higher radiative stability. An express-method has been developed for the identification of actinium-227 with TOA by its intrinsic α-emission in nonequilibrium preparations of irradiated radium-226 of small activity. Actinium-225 is extracted from uranium-233 with due regard for the fact that U, Th, and Ac are extracted differently by TBP from HNO 3 solutions. With the help of the given procedure one can reach the purifying coefficient of 10 4 . Actinium-228 is extracted from the radiummesothorium preparations by a deposition of decay products, including polonium-210 on the iron hydroxyde. Actinium-228 extraction from the mixture of radium radionuclides is performed by the partition chromatography method on D2EGFK. All the procedures for separation of actinium isotopes by the above methods are described

  7. Greening Reversed-Phase Liquid Chromatography Methods Using Alternative Solvents for Pharmaceutical Analysis

    Directory of Open Access Journals (Sweden)

    Moussa Yabré

    2018-05-01

    Full Text Available The greening of analytical methods has gained increasing interest in the field of pharmaceutical analysis to reduce environmental impacts and improve the health safety of analysts. Reversed-phase high-performance liquid chromatography (RP-HPLC is the most widely used analytical technique involved in pharmaceutical drug development and manufacturing, such as the quality control of bulk drugs and pharmaceutical formulations, as well as the analysis of drugs in biological samples. However, RP-HPLC methods commonly use large amounts of organic solvents and generate high quantities of waste to be disposed, leading to some issues in terms of ecological impact and operator safety. In this context, greening HPLC methods is becoming highly desirable. One strategy to reduce the impact of hazardous solvents is to replace classically used organic solvents (i.e., acetonitrile and methanol with greener ones. So far, ethanol has been the most often used alternative organic solvent. Others strategies have followed, such as the use of totally aqueous mobile phases, micellar liquid chromatography, and ionic liquids. These approaches have been well developed, as they do not require equipment investments and are rather economical. This review describes and critically discusses the recent advances in greening RP-HPLC methods dedicated to pharmaceutical analysis based on the use of alternative solvents.

  8. Chemistry and liquid chromatography methods for the analyses of primary oxidation products of triacylglycerols.

    Science.gov (United States)

    Zeb, A

    2015-05-01

    Triacylglycerols (TAGs) are one of the major components of the cells in higher biological systems, which can act as an energy reservoir in the living cells. The unsaturated fatty acid moiety is the key site of oxidation and formation of oxidation compounds. The TAG free radical generates several primary oxidation compounds. These include hydroperoxides, hydroxides, epidioxides, hydroperoxy epidioxides, hydroxyl epidioxides, and epoxides. The presence of these oxidized TAGs in the cell increases the chances of several detrimental processes. For this purpose, several liquid chromatography (LC) methods were reported in their analyses. This review is therefore focused on the chemistry, oxidation, extraction, and the LC methods reported in the analyses of oxidized TAGs. The studies on thin-layer chromatography were mostly focused on the total oxidized TAGs separation and employ hexane as major solvent. High-performance LC (HPLC) methods were discussed in details along with their merits and demerits. It was found that most of the HPLC methods employed isocratic elution with methanol and acetonitrile as major solvents with an ultraviolet detector. The coupling of HPLC with mass spectrometry (MS) highly increases the efficiency of analysis as well as enables reliable structural elucidation. The use of MS was found to be helpful in studying the oxidation chemistry of TAGs and needs to be extended to the complex biological systems.

  9. A fast isocratic liquid chromatography method for the quantification of xanthophylls and their stereoisomers.

    Science.gov (United States)

    Nimalaratne, Chamila; Lopes-Lutz, Daise; Schieber, Andreas; Wu, Jianping

    2015-12-01

    A fast isocratic liquid chromatography method was developed for the simultaneous quantification of eight xanthophylls (13-Z-lutein, 13'-Z-lutein, 13-Z-zeaxanthin, all-E-lutein, all-E-zeaxanthin, all-E-canthaxanthin, all-E-β-apo-8'-carotenoic acid ethyl ester and all-E-β-apo-8'-carotenal) within 12 min, compared to 90 min by the conventional high-performance liquid chromatography method. The separation was achieved on a YMC C30 reversed-phase column (100 mm x 2.0 mm; 3 μm) operated at 20°C using a methanol/tert-butyl methyl ether/water solvent system at a flow rate of 0.8 mL/min. The method was successfully applied to quantify lutein and zeaxanthin stereoisomers in egg yolk, raw and cooked spinach, and a dietary supplement. The method can be used for the rapid analysis of xanthophyll isomers in different food products and for quality control purposes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. New developments in radiation protection instrumentation via active electronic methods

    International Nuclear Information System (INIS)

    Umbarger, C.J.

    1981-01-01

    New developments in electronics and radiation detectors are improving on real-time data acquisition of radiation exposure and contamination conditions. Recent developments in low power circuit designs, hybrid and integrated circuits, and microcomputers have all contributed to smaller and lighter radiation detection instruments that are, at the same time, more sensitive and provide more information (e.g., radioisotope identification) than previous devices. New developments in radiation detectors, such as cadmium telluride, gas scintillation proportional counters, and imaging counters (both charged particle and photon) promise higher sensitivities and expanded uses over present instruments. These developments are being applied in such areas as health physics, waste management, environmental monitoring, in vivo measurements, and nuclear safeguards

  11. Optical Methods and Instrumentation in Brain Imaging and Therapy

    CERN Document Server

    2013-01-01

    This book provides a comprehensive up-to-date review of optical approaches used in brain imaging and therapy. It covers a variety of imaging techniques including diffuse optical imaging, laser speckle imaging, photoacoustic imaging and optical coherence tomography. A number of laser-based therapeutic approaches are reviewed, including photodynamic therapy, fluorescence guided resection and photothermal therapy. Fundamental principles and instrumentation are discussed for each imaging and therapeutic technique. Represents the first publication dedicated solely to optical diagnostics and therapeutics in the brain Provides a comprehensive review of the principles of each imaging/therapeutic modality Reviews the latest advances in instrumentation for optical diagnostics in the brain Discusses new optical-based therapeutic approaches for brain diseases

  12. Establishing the analytical procedure for acetate in water by ion chromatography method

    International Nuclear Information System (INIS)

    Nguyen Thi Hong Thinh; Ha Lan Anh; Vo Thi Anh

    2015-01-01

    In recent studies of contamination sources of arsenic, ammonium, iron, organic carbon in groundwater, acetate is measured a lot because it is the main decomposition product of organic compounds from sediment into groundwater. In order to better support for the study of the origin and mobilization mechanism of the pollutants, acetate was studied analysis method in Isotopes Hydrology Laboratory using ion chromatography technique. Project Researchers used Ion Chromatography system - DX-600 including IonPac ICE-AS1 column for separating acetate and conductivity detector CD 25 to quantify acetate in water samples. The study results showed that project team has successfully developed analytical procedures of acetate in water with acetate’s retention time is 12 minutes, limit of detection (LOD) of the method was 0.01 ppm. The accuracy of the method was established by calculating the precision and bias of 10 analysis times of a standard sample at content levels 1 ppm and 8 ppm. The results of the 10 measurements are satisfiable about precision and bias with repeated standard deviation coefficient CVR were 1.3% and 0.2% and the recoveries R were 99.92% and 101.72%. (author)

  13. DETERMINATION OF RUTIN IN LEAVES OF SALIX TRIANDRA USING THE METHOD OF PLANAR CHROMATOGRAPHY

    Directory of Open Access Journals (Sweden)

    E. G. Sannikova

    2016-01-01

    Full Text Available The aim of the study is to develop new methods of identification and quantitative determination of rutin in the leaves of Salix triandra L. with thin-layer chromatography. The digital processing of the chromatograms was performed using «Sorbfil Videodensitometer» computer program (Krasnodar. For the chromatography analysis we used plates «Sorbfil» PTSH-P-A-UV, mobile phase: n-butanol-glacial acetic acid-water (4:1:1, detecting reagent – ammonia vapors. The rutin is detected as yellow spots with Rf 0.64±0.02. The detection limit is 0.5 μg/μl. The regression equation has the form: S=4.75×103 m. With the use of this method we found that the composition of rutin in leaves of Salix triandra was in the range 1.81±0.06% on the air-dry raw material (relative standard deviation RSD%=2.5%; the measurement error E=3.12%. The method is sensitive, linear, has a small error, and does not require expensive equipment.

  14. Study of atmospheric aerosols in Zaire by instrumental neutron activation analysis, atomic absorption spectrophotometry and ion-exchange chromatography

    International Nuclear Information System (INIS)

    Tshiashala, M.D.; Lumu, B.M.; Matamba, K.; Ronneau, C.

    1992-01-01

    Instrumental neutron activation analysis and atomic absorption spectroscopy were applied to the determination of trace element abundances in airborne particulate matter collected throughout Kinshasa, Zaire. Statistical treatment of the resulting data was used to assess the variations between sites and to identify the sources of the pollutants. 10 refs, 5 tabs

  15. Guide on Economic Instruments & Non-market Valuation Methods

    DEFF Research Database (Denmark)

    Zandersen, Marianne; Bartczak, Anna; Czajkowski, Mikołaj

    The aim of this guidance document is to provide forest practitioners, decision makers and forest owners insights into the various economic instruments available to enhance the non-market ecosystem provision of forests such as a high quality biodiversity; enhanced carbon sequestration; improved...... with ecosystem degradation and iii) by recognising the substantial economic and welfare benefits of better management of ecosystems in forests. Ecosystem services contribute to economic welfare in two ways: • by contributing to the generation of income and wellbeing; and • by preventing damages that inflict...... initiatives it is therefore essential to consider trade offs and synergies between the complex interplay between ecosystem goods and services within an ecosystem,...

  16. Determination of thyroid hormones in mouse tissues by isotope-dilution microflow liquid chromatography-mass spectrometry method.

    Science.gov (United States)

    De Angelis, Meri; Giesert, Florian; Finan, Brian; Clemmensen, Christoffer; Müller, Timo D; Vogt-Weisenhorn, Daniela; Tschöp, Matthias H; Schramm, Karl-Werner

    2016-10-15

    Thyroid hormones (THs) play a critical role in the regulation of many biological processes such as growth, metabolism and development both in humans and wildlife. In general, TH levels are measured by immunoassay (IA) methods but the specificity of the antibodies used in these assays limits selectivity. In the last decade, several analytical methods using liquid chromatography-mass spectrometry (LC-MS) and tandem mass spectrometry (LC-MS/MS) have been developed to measure THs. These new techniques proved to be more accurate than the IA analysis and they were widely used for the determination of TH level in different human and animal tissues. A large part of LC-MS/MS methods described in literature employed between 200 and 500mg of sample, however this quantity can be considered too high especially when preclinical studies are conducted using mice as test subjects. Thus an analytical method that reduces the amount of tissue is essential. In this study, we developed a procedure for the analysis of six THs; L-thyroxine (T4), 3,3',5-triiodo-l-thyronine (T3), 3,3',5'-triiodo-l-thyronine (rT3), 3,5-diiodo-l-thyronine (rT2), 3,3'-diiodo-l-thyronine (T2), 3-iodo-l-thyronine (T1) using isotope ((13)C6-T4, (13)C6-T3, (13)C6-rT3, (13)C6-T2) dilution liquid chromatography-mass spectrometry. The major difference with previously described methods lies in the utilization of a nano-UPLC (Ultra Performance Liquid Chromatography) system in micro configuration. This approach leads to a reduction compared to the published methods, of column internal diameter, flow rate, and injected volume. The result of all these improvements is a decrease in the amount of sample necessary for the analysis. The method was tested on six different mouse tissues: liver, heart, kidney, muscle, lung and brown adipose tissue (BAT). The nano-UPLC system was interfaced with a quadrupole time-of-flight mass spectrometer (Q-TOF2-MS) using the positive ion mode electrospray ionization. In our analytical method

  17. A Geometrical Method for Sound-Hole Size and Location Enhancement in Lute Family Musical Instruments: The Golden Method

    Directory of Open Access Journals (Sweden)

    Soheil Jafari

    2017-11-01

    Full Text Available This paper presents a new analytical approach, the Golden Method, to enhance sound-hole size and location in musical instruments of the lute family in order to obtain better sound damping characteristics based on the concept of the golden ratio and the instrument geometry. The main objective of the paper is to increase the capability of lute family musical instruments in keeping a note for a certain time at a certain level to enhance the instruments’ orchestral characteristics. For this purpose, a geometry-based analytical method, the Golden Method is first described in detail in an itemized feature. A new musical instrument is then developed and tested to confirm the ability of the Golden Method in optimizing the acoustical characteristics of musical instruments from a damping point of view by designing the modified sound-hole. Finally, the new-developed instrument is tested, and the obtained results are compared with those of two well-known instruments to confirm the effectiveness of the proposed method. The experimental results show that the suggested method is able to increase the sound damping time by at least 2.4% without affecting the frequency response function and other acoustic characteristics of the instrument. This methodology could be used as the first step in future studies on design, optimization and evaluation of musical instruments of the lute family (e.g., lute, oud, barbat, mandolin, setar, and etc..

  18. Development of high performance liquid chromatography method for miconazole analysis in powder sample

    Science.gov (United States)

    Hermawan, D.; Suwandri; Sulaeman, U.; Istiqomah, A.; Aboul-Enein, H. Y.

    2017-02-01

    A simple high performance liquid chromatography (HPLC) method has been developed in this study for the analysis of miconazole, an antifungal drug, in powder sample. The optimized HPLC system using C8 column was achieved using mobile phase composition containing methanol:water (85:15, v/v), a flow rate of 0.8 mL/min, and UV detection at 220 nm. The calibration graph was linear in the range from 10 to 50 mg/L with r 2 of 0.9983. The limit of detection (LOD) and limit of quantitation (LOQ) obtained were 2.24 mg/L and 7.47 mg/L, respectively. The present HPLC method is applicable for the determination of miconazole in the powder sample with a recovery of 101.28 % (RSD = 0.96%, n = 3). The developed HPLC method provides short analysis time, high reproducibility and high sensitivity.

  19. Application of the Instrumental Neutron Activation Analysis and High Performance Liquid Chromatography (HPLC) in the rare earth elements determination in reference geological materials

    International Nuclear Information System (INIS)

    Figueiredo, Ana M.G.; Moraes, Noemia M.P. de; Shihomatsu, Helena M.

    1997-01-01

    Instrumental Neutron Activation Analysis (INAA) and High Performance Liquid Chromatography (HPLC) were applied to the determination of rare earth elements (REE) in the geological reference materials AGV-1, G-2 and GSP-1 (USGS). Results obtained by both techniques showed good agreement with certified values, giving relative errors less than 10%. The La, Ce, Nd, Sm, Eu, Tb, Yb and Lu REE elements were determined. All the REE except Dy and Y were determined by HPLC. The reference material G94, employed in the International Proficiency Test for Analytical Geochemistry Laboratories (GeoTP1) was analysed. The results obtained are a contribution to REE contents in this sample. The INAA and HPLC application to the determination of REE in this kind of matrix is also discussed. (author). 10 refs., 1 fig., 5 tabs

  20. A validated high performance thin layer chromatography method for determination of yohimbine hydrochloride in pharmaceutical preparations.

    Science.gov (United States)

    Badr, Jihan M

    2013-01-01

    Yohimbine is an indole alkaloid used as a promising therapy for erectile dysfunction. A number of methods were reported for the analysis of yohimbine in the bark or in pharmaceutical preparations. In the present work, a simple and sensitive high performance thin layer chromatographic method is developed for determination of yohimbine (occurring as yohimbine hydrochloride) in pharmaceutical preparations and validated according to International Conference of Harmonization (ICH) guidelines. The method employed thin layer chromatography aluminum sheets precoated with silica gel as the stationary phase and the mobile phase consisted of chloroform:methanol:ammonia (97:3:0.2), which gave compact bands of yohimbine hydrochloride. Linear regression data for the calibration curves of standard yohimbine hydrochloride showed a good linear relationship over a concentration range of 80-1000 ng/spot with respect to the area and correlation coefficient (R(2)) was 0.9965. The method was evaluated regarding accuracy, precision, selectivity, and robustness. Limits of detection and quantitation were recorded as 5 and 40 ng/spot, respectively. The proposed method efficiently separated yohimbine hydrochloride from other components even in complex mixture containing powdered plants. The amount of yohimbine hydrochloride ranged from 2.3 to 5.2 mg/tablet or capsule in preparations containing the pure alkaloid, while it varied from zero (0) to 1.5-1.8 mg/capsule in dietary supplements containing powdered yohimbe bark. We concluded that this method employing high performance thin layer chromatography (HPTLC) in quantitative determination of yohimbine hydrochloride in pharmaceutical preparations is efficient, simple, accurate, and validated.

  1. Fluidos supercríticos em química analítica. II. Cromatografia com fluido supercrítico: instrumentação Supercritical fluid in analytical chemistry. II. Supercritical fluid chromatography: instrumentation

    Directory of Open Access Journals (Sweden)

    Emanuel Carrilho

    2003-10-01

    Full Text Available The first paper in this series discussed the basic theory involved in supercritical fluid chromatography (SFC and how the technique progressed from gas and liquid chromatography. The first SFC instruments were simple adaptations of the commercially available liquid chromatographs with packed columns followed by modifications in gas chromatographs using open tubular capillary columns. In this paper, the most important aspects regarding instrumentation are covered, including practical, simple, and the most important, inexpensive solutions to build a home-made SFC system.

  2. Validation of a confirmatory method for the determination of melamine in egg by gas chromatography-mass spectrometry and ultra-performance liquid chromatography-tandem mass spectrometry

    International Nuclear Information System (INIS)

    Xia Xi; Ding Shuangyang; Li Xiaowei; Gong Xiao; Zhang Suxia; Jiang Haiyang; Li Jiancheng; Shen Jianzhong

    2009-01-01

    A sensitive and reliable method was developed and validated for detection and confirmation of melamine in egg based on gas chromatography-mass spectrometry (GC-MS) and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Trichloroacetic acid solution was used for sample extraction and precipitation of proteins. The aqueous extracts were subjected to solid-phase extraction by mixed-mode reversed-phase/strong cation-exchange cartridges. Using ultra-performance liquid chromatography and electrospray ionization in the positive ion mode, melamine was determined by LC-MS/MS, which was completed in 5 min for each injection. For the GC-MS analysis, extracted melamine was derivatized with N,O-bis(trimethylsilyl)trifluoracetamide prior to selected ion monitoring detection in electron impact mode. The average recovery of melamine from fortified samples ranged from 85.2% to 103.2%, with coefficients of variation lower than 12%. The limit of detection obtained by GC-MS and UPLC-MS/MS was 10 and 5 μg kg -1 , respectively. This validated method was successfully applied to the determination of melamine in real samples from market.

  3. Screening of inorganic gases released from firework-rockets by a gas chromatography/whistle-accelerometer method.

    Science.gov (United States)

    Chen, Kuan-Fu; Wu, Hui-Hsin; Lin, Chien-Hung; Lin, Cheng-Huang

    2013-08-30

    The use of an accelerometer for detecting inorganic gases in gas chromatography (GC) is described. A milli-whistle was connected to the outlet of the GC capillary and was used instead of a classical GC detector. When the GC carrier gases and the sample gases pass through the milli-whistle, a sound is produced, leading to vibrational changes, which can be recorded using an accelerometer. Inorganic gases, including SO2, N2 and CO2, which are released from traditional Chinese firework-rockets at relatively high levels as the result of burning the propellant and explosive material inside could be rapidly determined using the GC/whistle-accelerometer system. The method described herein is safe, the instrumentation is compact and has potential to be modified so as to be portable for use in the field. It also can be used in conjunction with FID (flame ionization detector) or TCD (thermal conductivity detector), in which either no response for FID (CO2, N2, NO2, SO2, etc.) or helium gas is needed for TCD, respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. Purification of human albumin by the combination of the method of Cohn with liquid chromatography

    Directory of Open Access Journals (Sweden)

    Tanaka K.

    1998-01-01

    Full Text Available Large volumes of plasma can be fractionated by the method of Cohn at low cost. However, liquid chromatography is superior in terms of the quality of the product obtained. In order to combine the advantages of each method, we developed an integrated method for the production of human albumin and immunoglobulin G (IgG. The cryoprecipitate was first removed from plasma for the production of factor VIII and the supernatant of the cryoprecipitate was fractionated by the method of Cohn. The first precipitate, containing fractions (F-I + II + III, was used for the production of IgG by the chromatographic method (see Tanaka K et al. (1998 Brazilian Journal of Medical and Biological Research, 31: 1375-1381. The supernatant of F-I + II + III was submitted to a second precipitation and F-IV was obtained and discarded. Albumin was obtained from the supernatant of the precipitate F-IV by liquid chromatography, ion-exchange on DEAE-Sepharose FF, filtration through Sephacryl S-200 HR and introduction of heat treatment for fatty acid precipitation. Viral inactivation was performed by pasteurization at 60ºC for 10 h. The albumin product obtained by the proposed procedure was more than 99% pure for the 15 lots of albumin produced, with a mean yield of 25.0 ± 0.5 g/l plasma, containing 99.0 to 99.3% monomer, 0.7 to 1.0% dimers, and no polymers. Prekallikrein activator levels were <=5 IU/ml. This product satisfies the requirements of the 1997 Pharmacopée Européenne.

  5. Development of the H-point standard additions method for coupled liquid-chromatography and UV-visible spectrophotometry

    Energy Technology Data Exchange (ETDEWEB)

    Campins-Falco, Pilar; Bosch-Reig, Francisco; Herraez-Hernandez, Rosa; Sevillano-Cabeza, Adela (Universidad de Valencia (Spain). Facultad de Quimica, Departamento de Quimica Analitica)

    1992-02-10

    This work establishes the fundamentals of the H-point standard additions method for liquid chromatography for the simultaneous analysis of binary mixtures with overlapped chromatographic peaks. The method was compared with the deconvolution method of peak suppression and the second derivative of elution profiles. Different mixtures of diuretics were satisfactorily resolved. (author). 21 refs.; 9 figs.; 2 tabs.

  6. Method for 236U Determination in Seawater Using Flow Injection Extraction Chromatography and Accelerator Mass Spectrometry

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Steier, Peter

    2015-01-01

    An automated analytical method implemented in a flow injection (FI) system was developed for rapid determination of 236U in 10 L seawater samples. 238U was used as a chemical yield tracer for the whole procedure, in which extraction chromatography (UTEVA) was exploited to purify uranium, after...... experimental parameters affecting the analytical effectiveness were investigated and optimized in order to achieve high chemical yields and simple and rapid analysis as well as low procedure background. Besides, the operational conditions for the target preparation prior to the AMS measurement were optimized......, on the basis of studying the coprecipitation behavior of uranium with iron hydroxide. The analytical results indicate that the developed method is simple and robust, providing satisfactory chemical yields (80−100%) and high analysis speed (4 h/sample), which could be an appealing alternative to conventional...

  7. A high performance liquid chromatography method for determination of furfural in crude palm oil.

    Science.gov (United States)

    Loi, Chia Chun; Boo, Huey Chern; Mohammed, Abdulkarim Sabo; Ariffin, Abdul Azis

    2011-09-01

    A modified steam distillation method was developed to extract furfural from crude palm oil (CPO). The collected distillates were analysed using high performance liquid chromatography (HPLC) coupled with an ultraviolet diode detector at 284nm. The HPLC method allowed identification and quantification of furfural in CPO. The unique thermal extraction of CPO whereby the fresh fruit bunches (FFB) are first subjected to steam treatment, distinguishes itself from other solvent-extracted or cold-pressed vegetable oils. The presence of furfural was also determined in the fresh palm oil from FFB (without undergoing the normal extraction process), palm olein, palm stearin, olive oil, coconut oil, sunflower oil, soya oil and corn oil. The chromatograms of the extracts were compared to that of standard furfural. Furfural was only detected in CPO. The CPO consignments obtained from four mills were shown to contain 7.54 to 20.60mg/kg furfural. Copyright © 2011 Elsevier Ltd. All rights reserved.

  8. High performance liquid chromatography method for the determination of cinnamyl alcohol dehydrogenase activity in soybean roots.

    Science.gov (United States)

    dos Santos, W D; Ferrarese, Maria de Lourdes Lucio; Ferrarese-Filho, O

    2006-01-01

    This study proposes a simple, quick and reliable method for determining the cinnamyl alcohol dehydrogenase (CAD; EC 1.1.1.195) activity in soybean (Glycine max L. Merr.) roots using reversed-phase high performance liquid chromatography (RP-HPLC). The method includes a single extraction of the tissue and conduction of the enzymatic reaction at 30 degrees C with cinnamaldehydes (coniferyl or sinapyl), substrates of CAD. Disappearance of the substrates in the reaction mixture is monitored at 340 nm (for coniferaldehyde) or 345 nm (for sinapaldehyde) by isocratic elution with methanol/acetic acid through a GLC-ODS (M) column. This HPLC technique furnishes a rapid and reliable measure of cinnamaldehyde substrates, and may be used as an alternative tool to analyze CAD activity in enzyme preparation without previous purification.

  9. Ion-Exchange Membrane Chromatography as an Alternative Method of Separation of Potato y Virus

    Directory of Open Access Journals (Sweden)

    Treder Krzysztof

    2015-12-01

    Full Text Available Procedures of separation of virus particles from a plant material are multistage. Furthermore often they are difficult in terms of methodology and require use of expensive, highly specialist equipment and yield of separation is often low. The antigen obtained is often degraded and contains admixtures of other proteins. Therefore, generation of high quality and specificity antibodies based on such antigen is very difficult and quality of the antibodies has impact on reliability, sensitivity and unambiguity of results of immunodiagnostic tests (e.g. ELISA that are currently conventionally used to detect vegetable viruses. In this study three conventionally-performed methods of separation of potato virus Y (PVY were compared and a method of separation based on membrane chromatography, as an alternative separation technique, has been presented. It has been demonstrated that in proper process conditions good quality virus preparation can be obtained.

  10. Analysis of residual toluene in food packaging via headspace extraction method using gas chromatography

    International Nuclear Information System (INIS)

    Lim, Ying Chin; Mohd Marsin Sanagi

    2008-01-01

    Polymeric materials are used in many food contact applications as packaging material. The presence of residual toluene in this food packaging material can migrate into food and thus affect the quality of food. In this study, a manual headspace analysis was successfully designed and developed. The determination of residual toluene was carried out with standard addition method and multiple headspace extraction, MHE) method using gas chromatography-flame ionization detector, GC-FID). Identification of toluene was performed by comparison of its retention time with standard toluene and GC-MS. It was found that the suitable heating temperature was 180 degree Celsius with an optimum heating time of 10 minutes. The study also found that the concentration of residual toluene in multicolored sample was higher compared to mono colored sample whereas residual toluene in sample analyzed using standard addition method was higher compared to MHE method. However, comparison with the results obtained from De Paris laboratory, France found that MHE method gave higher accuracy for sample with low analyte concentration. On the other hand, lower accuracy was obtained for sample with high concentration of residual toluene due to systematic errors. Comparison between determination methods showed that MHE method is more precise compared to standard addition method. (author)

  11. Sample displacement chromatography as a method for purification of proteins and peptides from complex mixtures

    Science.gov (United States)

    Gajdosik, Martina Srajer; Clifton, James; Josic, Djuro

    2012-01-01

    Sample displacement chromatography (SDC) in reversed-phase and ion-exchange modes was introduced approximately twenty years ago. This method takes advantage of relative binding affinities of components in a sample mixture. During loading, there is a competition among different sample components for the sorption on the surface of the stationary phase. SDC was first used for the preparative purification of proteins. Later, it was demonstrated that this kind of chromatography can also be performed in ion-exchange, affinity and hydrophobic-interaction mode. It has also been shown that SDC can be performed on monoliths and membrane-based supports in both analytical and preparative scale. Recently, SDC in ion-exchange and hydrophobic interaction mode was also employed successfully for the removal of trace proteins from monoclonal antibody preparations and for the enrichment of low abundance proteins from human plasma. In this review, the principals of SDC are introduced, and the potential for separation of proteins and peptides in micro-analytical, analytical and preparative scale is discussed. PMID:22520159

  12. Instrumental methods for analysis of some elements in flour

    International Nuclear Information System (INIS)

    Zagrodzki, P.; Dutkiewicz, E.M.; Malec, P.; Krosniak, M.; Knap, W.

    1993-10-01

    For ten various brands of flour contents of chosen (heavy) elements were determined by means of ICP, GF-AAS, PIXE and ASV/CSV methods. General performance of participating laboratories as well as pros and cons of different analytical methods were compared and discussed. (author). 6 refs, 6 figs, 7 tabs

  13. Validation of method in instrumental NAA for food products sample

    International Nuclear Information System (INIS)

    Alfian; Siti Suprapti; Setyo Purwanto

    2010-01-01

    NAA is a method of testing that has not been standardized. To affirm and confirm that this method is valid. it must be done validation of the method with various sample standard reference materials. In this work. the validation is carried for food product samples using NIST SRM 1567a (wheat flour) and NIST SRM 1568a (rice flour). The results show that the validation method for testing nine elements (Al, K, Mg, Mn, Na, Ca, Fe, Se and Zn) in SRM 1567a and eight elements (Al, K, Mg, Mn, Na, Ca, Se and Zn ) in SRM 1568a pass the test of accuracy and precision. It can be conclude that this method has power to give valid result in determination element of the food products samples. (author)

  14. A simplified method for rapid quantification of intracellular nucleoside triphosphates by one-dimensional thin-layer chromatography

    DEFF Research Database (Denmark)

    Jendresen, Christian Bille; Kilstrup, Mogens; Martinussen, Jan

    2011-01-01

    -pyrophosphate (PRPP), and inorganic pyrophosphate (PPi) in cell extracts. The method uses one-dimensional thin-layer chromatography (TLC) and radiolabeled biological samples. Nucleotides are resolved at the level of ionic charge in an optimized acidic ammonium formate and chloride solvent, permitting...... quantification of NTPs. The method is significantly simpler and faster than both current two-dimensional methods and high-performance liquid chromatography (HPLC)-based procedures, allowing a higher throughput while common sources of inaccuracies and technical problems are avoided. For determination of PPi...

  15. Validation of ascorbic acid tablets of national production by igh-performance liquid chromatography method

    International Nuclear Information System (INIS)

    Rodriguez Hernandez, Yaslenis; Suarez Perez, Yania; Izquierdo Castro, Idalberto

    2009-01-01

    We validate an analytical method by high-performance liquid chromatography to determine ascorbic acid proportion in vitamin C tablets, which was designed as an alternative method to quality control and to follow-up of active principle chemical stability, since official techniques to quality control of ascorbic acid in tablets are not selective with degradation products. Method was modified according to that reported in USP 28, 2005 for analysis of injectable product. We used a RP-18 column of 250 x 4.6 mm 5 μm with a UV detector to 245 nm. Its validation was necessary for both objectives, considering parameters required for methods of I and II categories. This method was enough linear, exact, and precise in the rank of 100-300 μg/mL. Also, it was selective with remaining components of matrix and with the possible degradation products achieved in stressing conditions. Detection and quantification limits were estimated. When method was validated it was applied to ascorbic acid quantification in two batches of expired tablets and we detected a marked influence of container in active degradation principle after 12 months at room temperature. (Author)

  16. Isotope-dilution gas chromatography-mass spectrometry method for the analysis of hydroxyurea.

    Science.gov (United States)

    Garg, Uttam; Scott, David; Frazee, Clint; Kearns, Gregory; Neville, Kathleen

    2015-06-01

    Hydroxyurea is used in the treatment of various malignancies and sickle cell disease. There are limited studies on the pharmacokinetics of hydroxyurea, particularly in pediatric patients. An accurate, precise, and sensitive method is needed to support such studies and to monitor therapeutic adherence. We describe a novel gas chromatography-mass spectrometry (GC-MS) method for the determination of hydroxyurea concentration in plasma using stable labeled hydroxyurea C N2 as an internal standard. The method involved an organic extraction followed by the preparation of trimethylsilyl (TMS) derivatives of hydroxyurea for GC-MS selected ion-monitoring analysis. The following mass-to-charge (m/z) ratio ions for silated hydroxyurea and hydroxyurea C N2 were monitored: hydroxyurea-quantitative ion 277, qualifier ions 292 and 249; hydroxyurea C N2-quantitative ion 280, qualifier ion 295. This method was evaluated for reportable range, accuracy, within-run and between-run imprecisions, and limits of quantification. The reportable range for the method was 0.1-100 mcg/mL. All results were accurate within an allowable error of 15%. Within-run and between-run imprecisions were hydroxyurea described here is accurate, sensitive, precise, and robust. Its characteristics make the method suitable for supporting pharmacokinetic studies and/or clinical therapeutic monitoring.

  17. High-performance liquid chromatography method validation for determination of tetracycline residues in poultry meat

    Directory of Open Access Journals (Sweden)

    Vikas Gupta

    2014-01-01

    Full Text Available Background: In this study, a method for determination of tetracycline (TC residues in poultry with the help of high-performance liquid chromatography technique was validated. Materials and Methods: The principle step involved in ultrasonic-assisted extraction of TCs from poultry samples by 2 ml of 20% trichloroacetic acid and phosphate buffer (pH 4, which gave a clearer supernatant and high recovery, followed by centrifugation and purification by using 0.22 μm filter paper. Results: Validity study of the method revealed that all obtained calibration curves showed good linearity (r2 > 0.999 over the range of 40-4500 ng. Sensitivity was found to be 1.54 and 1.80 ng for oxytetracycline (OTC and TC. Accuracy was in the range of 87.94-96.20% and 72.40-79.84% for meat. Precision was lower than 10% in all cases indicating that the method can be used as a validated method. Limit of detection was found to be 4.8 and 5.10 ng for OTC and TC, respectively. The corresponding values of limit of quantitation were 11 and 12 ng. Conclusion: The method reliably identifies and quantifies the selected TC and OTC in the reconstituted poultry meat in the low and sub-nanogram range and can be applied in any laboratory.

  18. A Workshop on Methods for Neutron Scattering Instrument Design. Introduction and Summary

    International Nuclear Information System (INIS)

    Hjelm, Rex P.

    1996-09-01

    The future of neutron and x-ray scattering instrument development and international cooperation was the focus of the workshop on ''Methods for Neutron Scattering Instrument Design'' September 23-25 at the E.O. Lawrence Berkeley National Laboratory. These proceedings are a collection of a portion of the invited and contributed presentations

  19. Instrumentation and quantitative methods of evaluation. Progress report, January 15-September 14, 1986

    International Nuclear Information System (INIS)

    Beck, R.N.

    1986-09-01

    This document reports progress under grant entitled ''Instrumentation and Quantitative Methods of Evaluation.'' Individual reports are presented on projects entitled the physical aspects of radionuclide imaging, image reconstruction and quantitative evaluation, PET-related instrumentation for improved quantitation, improvements in the FMI cyclotron for increased utilization, and methodology for quantitative evaluation of diagnostic performance

  20. THE REGULATION OF MONEY CIRCULATION ON THE BASIS OF USING METHODS AND INSTRUMENTS OF MONETARY POLICY

    OpenAIRE

    S. Mishchenko; S. Naumenkova

    2013-01-01

    In the article it was researched the instruments and mechanism of safeguarding stability of money market on the basis of implementing the optimal monetary policy regime. It was determined the main directions of appliance the monetary policy methods and instruments to guiding money market stability and it was also investigated the influence of transmission mechanism on providing the soundness of money circulations.

  1. Ultrasonic partial discharge monitoring method on instrument transformers

    Directory of Open Access Journals (Sweden)

    Kartalović Nenad

    2012-01-01

    Full Text Available Sonic and ultrasonic partial discharge monitoring have been applied since the early days of these phenomena monitoring. Modern measurement and partial discharge acoustic (ultrasonic and sonic monitoring method has been rapidly evolving as a result of new electronic component design, information technology and updated software solutions as well as the development of knowledge in the partial discharge diagnosis. Electrical discharges in the insulation system generate voltage-current pulses in the network and ultrasonic waves that propagate through the insulation system and structure. Amplitude-phase-frequency analysis of these signals reveals information about the intensity, type and location of partial discharges. The paper discusses the possibility of ultrasonic method selectivity improvement and the increase of diagnosis reliability in the field. Measurements were performed in the laboratory and in the field while a number of transformers were analysed for dissolved gases in the oil. A comparative review of methods for the partial discharge detection is also presented in this paper.

  2. Radon/radon-daughter measurement methods and instrumentation

    International Nuclear Information System (INIS)

    Rock, R.L.

    1977-01-01

    Radon-daughter measurement equipment and techniques have been continuously improved over the last 25 years. Improvements have been in the areas of accuracy, time and convenience. We now have miniaturized scalers and detectors available for measuring the alpha particle count rates from aerosol samples collected on filter papers. We also have small lightweight efficient pumps for conveniently collecting samples and we have various counting methods which allow us to choose between making very precise measurements or nominal measurements. Radon-daughter measurement methods used in uranium mines and mills are discussed including a personal radon-daughter-exposure integrating device which can be worn by miners

  3. Laboratory and field based evaluation of chromatography ...

    Science.gov (United States)

    The Monitor for AeRosols and GAses in ambient air (MARGA) is an on-line ion-chromatography-based instrument designed for speciation of the inorganic gas and aerosol ammonium-nitrate-sulfate system. Previous work to characterize the performance of the MARGA has been primarily based on field comparison to other measurement methods to evaluate accuracy. While such studies are useful, the underlying reasons for disagreement among methods are not always clear. This study examines aspects of MARGA accuracy and precision specifically related to automated chromatography analysis. Using laboratory standards, analytical accuracy, precision, and method detection limits derived from the MARGA chromatography software are compared to an alternative software package (Chromeleon, Thermo Scientific Dionex). Field measurements are used to further evaluate instrument performance, including the MARGA’s use of an internal LiBr standard to control accuracy. Using gas/aerosol ratios and aerosol neutralization state as a case study, the impact of chromatography on measurement error is assessed. The new generation of on-line chromatography-based gas and particle measurement systems have many advantages, including simultaneous analysis of multiple pollutants. The Monitor for Aerosols and Gases in Ambient Air (MARGA) is such an instrument that is used in North America, Europe, and Asia for atmospheric process studies as well as routine monitoring. While the instrument has been evaluat

  4. Comprehensive measurement of total nondigestible carbohydrates in foods by enzymatic-gravimetric method and liquid chromatography.

    Science.gov (United States)

    Nishibata, Toyohide; Tashiro, Kouichi; Kanahori, Sumiko; Hashizume, Chieko; Kitagawa, Machiko; Okuma, Kazuhiro; Gordon, Dennis T

    2009-09-09

    Total nondigestible carbohydrate (NDC) in foods was determined by combining, not modifications, AOAC Official Methods 991.43, 2001.03, and 2002.02. Total NDC included insoluble dietary fiber (IDF) + high-molecular-weight soluble dietary fiber (HMWSDF), nondigestible oligosaccharides (NDO) not precipitated in ethanol solution, and resistant starch (RS). Eight sources of NDC (cellulose, wheat bran, gum arabic, resistant maltodextrin, polydextrose, fructooligosaccharide, galactooligosaccharides, and RS) were incorporated in different combinations into standard formula bread samples. All of the NDC sources and bread samples were analyzed for their (1) IDF + HMWSDF content with corrections for residual RS amount using AOAC Official Method 991.43, (2) NDO by liquid chromatography (LC) in AOAC Official Method 2001.03, and (3) RS by AOAC Official Method 2002.02. The correlation coefficient (R(2)) comparing calculated amounts versus measured amounts of total NDC in 11 bread samples was 0.92. Analysis of commercial food samples was also well matched with the DF + NDO value on their nutritional label. Consequently, we confirmed a single measurement of LC can determine all NDO in foods, and total NDC in foods can be determined by unifying existing AOAC Official Methods.

  5. Magnetic characterisation of recording materials: design, instrumentation and experimental methods

    NARCIS (Netherlands)

    Samwel, E.O.

    1995-01-01

    The progress being made in the field of magnetic recording is extremely fast. The need to keep this progress going, leads to new types of recording materials which require advanced measurement systems and measurement procedures. Furthermore, the existing measurement methods need to be reviewed as

  6. A high-performance liquid chromatography method for the serotonin release assay is equivalent to the radioactive method.

    Science.gov (United States)

    Sono-Koree, N K; Crist, R A; Frank, E L; Rodgers, G M; Smock, K J

    2016-02-01

    The serotonin release assay (SRA) is considered the gold standard laboratory test for heparin-induced thrombocytopenia (HIT). The historic SRA method uses platelets loaded with radiolabeled serotonin to evaluate platelet activation by HIT immune complexes. However, a nonradioactive method is desirable. We report the performance characteristics of a high-performance liquid chromatography (HPLC) SRA method. We validated the performance characteristics of an HPLC-SRA method, including correlation with a reference laboratory using the radioactive method. Serotonin released from reagent platelets was quantified by HPLC using fluorescent detection. Results were expressed as % release and classified as positive, negative, or indeterminate based on previously published cutoffs. Serum samples from 250 subjects with suspected HIT were tested in the HPLC-SRA and with the radioactive method. Concordant classifications were observed in 230 samples (92%). Sera from 41 healthy individuals tested negative. Between-run imprecision studies showed standard deviation of performance characteristics, equivalent to the historic radioactive method, but avoids the complexities of working with radioactivity. © 2015 John Wiley & Sons Ltd.

  7. Development and validation of high-performance liquid chromatography and high-performance thin-layer chromatography methods for the quantification of khellin in Ammi visnaga seed

    Science.gov (United States)

    Kamal, Abid; Khan, Washim; Ahmad, Sayeed; Ahmad, F. J.; Saleem, Kishwar

    2015-01-01

    Objective: The present study was used to design simple, accurate and sensitive reversed phase-high-performance liquid chromatography RP-HPLC and high-performance thin-layer chromatography (HPTLC) methods for the development of quantification of khellin present in the seeds of Ammi visnaga. Materials and Methods: RP-HPLC analysis was performed on a C18 column with methanol: Water (75: 25, v/v) as a mobile phase. The HPTLC method involved densitometric evaluation of khellin after resolving it on silica gel plate using ethyl acetate: Toluene: Formic acid (5.5:4.0:0.5, v/v/v) as a mobile phase. Results: The developed HPLC and HPTLC methods were validated for precision (interday, intraday and intersystem), robustness and accuracy, limit of detection and limit of quantification. The relationship between the concentration of standard solutions and the peak response was linear in both HPLC and HPTLC methods with the concentration range of 10–80 μg/mL in HPLC and 25–1,000 ng/spot in HPTLC for khellin. The % relative standard deviation values for method precision was found to be 0.63–1.97%, 0.62–2.05% in HPLC and HPTLC for khellin respectively. Accuracy of the method was checked by recovery studies conducted at three different concentration levels and the average percentage recovery was found to be 100.53% in HPLC and 100.08% in HPTLC for khellin. Conclusions: The developed HPLC and HPTLC methods for the quantification of khellin were found simple, precise, specific, sensitive and accurate which can be used for routine analysis and quality control of A. visnaga and several formulations containing it as an ingredient. PMID:26681890

  8. Q Sepharose micro-column chromatography: A simple screening method for identifying beta thalassemia traits and hemoglobin E carriers.

    Science.gov (United States)

    Wong, Peerapon; Sritippayawan, Suchila; Suwannakhon, Narutchala; Tapprom, Akamon; Deoisares, Rawisut; Sanguansermsri, Torpong

    2016-11-01

    For beta thalassemia control program in pregnancy, mass screening of the carrier state by determination of the hemoglobin (Hb) A 2 and Hb E proportions and mutation analysis is a preferred method for making prenatal diagnoses. Q Sepharose micro-column chromatography, developed for the determination of Hb A 2 and Hb E for screening purposes, was compared with high performance liquid chromatography (HPLC) to ascertain its relative accuracy and reliability. Results using Q Sepharose micro-column chromatography in 350 blood specimens, including 50 samples genetically proven to be beta thalassemia heterozygotes, were compared to HPLC for validation. An additional study was conducted to test a clinical application on a large-scale survey for beta thalassemia in 1581 pregnant women and their spouses. The mean (±SD) Hb A 2 proportions in the normal and genetically proven beta thalassemia heterozygotes were 2.70±0.40% and 6.30±1.23%, respectively, as determined by Q-Sepharose micro-column chromatography, and 2.65±0.31% and 5.37±0.96%, respectively, as determined by HPLC. The mean Hb E proportions in the Hb E heterozygotes were 23.25±4.13% and 24.72±3.5% as determined by Q Sepharose micro-column chromatography and HPLC, respectively. In the large-scale survey for beta thalassemia, 23 at risk couples were detected. Seven affected fetuses were identified by prenatal diagnosis. Q Sepharose micro-column chromatography was found to be reliable, reproducible and well-suited for large-scale surveys. Additionally, by being reusable and convenient, this simple and economical chromatography method may be an alternative means to screen for beta thalassemia and Hb E carriers in the mass population. Copyright © 2016 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

  9. Binding kinetics of five drugs to beta2-adrenoceptor using peak profiling method and nonlinear chromatography.

    Science.gov (United States)

    Liang, Yuan; Wang, Jing; Fei, Fuhuan; Sun, Huanmei; Liu, Ting; Li, Qian; Zhao, Xinfeng; Zheng, Xiaohui

    2018-02-23

    Investigations of drug-protein interactions have advanced our knowledge of ways to design more rational drugs. In addition to extensive thermodynamic studies, ongoing works are needed to enhance the exploration of drug-protein binding kinetics. In this work, the beta2-adrenoceptor (β 2 -AR) was immobilized on N, N'-carbonyldiimidazole activated amino polystyrene microspheres to prepare an affinity column (4.6 mm × 5.0 cm, 8 μm). The β 2 -AR column was utilized to determine the binding kinetics of five drugs to the receptor. Introducing peak profiling method into this receptor chromatographic analysis, we determined the dissociation rate constants (k d ) of salbutamol, terbutaline, methoxyphenamine, isoprenaline hydrochloride and ephedrine hydrochloride to β 2 -AR to be 15 (±1), 22 (±1), 3.3 (±0.2), 2.3 (±0.2) and 2.1 (±0.1) s -1 , respectively. The employment of nonlinear chromatography (NLC) in this case exhibited the same rank order of k d values for the five drugs bound to β 2 -AR. We confirmed that both the peak profiling method and NLC were capable of routine measurement of receptor-drug binding kinetics. Compared with the peak profiling method, NLC was advantageous in the simultaneous assessment of the kinetic and apparent thermodynamic parameters. It will become a powerful method for high throughput drug-receptor interaction analysis. Copyright © 2018 Elsevier B.V. All rights reserved.

  10. Liquid chromatography method development and optimization for valsartan: pharmacokinetics of oral hydrogels in rabbits

    International Nuclear Information System (INIS)

    Sohail, M.; Minhas, M.U.

    2017-01-01

    A simple, rapid, precise, accurate high performance liquid chromatography method has been developed and subsequently validated for determination of valsartan in rabbit plasma. The method was developed employing mixture of mobile phase consisting of 0.02 M potassium dihydrogen phosphate buffer and acetonitrile (45:55), pH was adjusted to 2.7 using 50% orthophosphoric acid and pumped thorough chromatographic system at a flow rate of 1 ml/min. An isocratic elution mode was carried out at HPLC system (Agilent Technologies, 1200 series, USA) fitted with variable wavelength detector and data processing software ChemStation. For sample analysis, 20 mul sample was injected and eluate was monitored at 225nm wavelength. Pharmacokinetic evaluation was performed in rabbits after the oral administration of valsartan loaded PVA-co-poly(AA) hydrogels. The mean Cmax of valsartan was 408.439ng/ml, Tmax was 12h and half life (t1/2) was 8.812h. The extraction procedure was simple with good response even at very low drug concentration, thereby making this method suitable for pharmacokinetic application. It is concluded that developed method is simple, fast, cost effective, and reproducible for the analysis of pharmacokinetic parameters in the rabbit plasma. (author)

  11. Development and validation of a thin-layer chromatography method for stability studies of naproxen

    International Nuclear Information System (INIS)

    Rodriguez Hernandez, Yaslenis; Suarez Perez, Yania; Garcia Pulpeiro, Oscar; Rodriguez Borges, Tania

    2011-01-01

    The validation of an analytical method was carried out to be applied to the stability studies of the future formulations of naproxen suppositories for infant and adult use. The factors which mostly influenced in the naproxen stability were determined, the major degradation occurred in oxidizing acid medium and by action of light. The possible formation of esters between the free carboxyl group present in naproxen and the glyceryl monoestereate present in the base was identified as one of the degradation paths in the new formulation. The results were satisfactory. A thin-layer chromatography-based method was developed as well as the best chromatographic conditions were selected. GF 254 silica gel plates and ultraviolet developer at 254 nm were employed. Three solvent systems were evaluated of which A made up of glacial acetic: tetrahydrofurane:toluene (3:9:90 v/v/v)allowed adequate resolution between the analyte and the possible degradation products, with detection limit of 1 μg. The use of the suggested method was restricted to the identification of possible degradation products just for qualitative purposes and not as final test. The method proved to be sensitive and selective enough to be applied for the stated objective, according to the validation results

  12. Analytical method by high resolution liquid chromatography for the determination of carbamazepine in human plasma

    International Nuclear Information System (INIS)

    Jimenez Aleman, Narda M; Calero Carbonell, Jorge E; Padron Yaquis, Alejandro S; Izquierdo Lozano, Julio C

    2007-01-01

    One of the requirements to develop the studies of bioavailability and bioequivalence is to have analytic methodologies validated for the work with samples in biological fluids. A method was developed by high resolution liquid chromatography for the determination of carbamazepine in human plasma. A mixture of hydrogen phosphate of sodium: acetonitrile (65:35) adjusted to pH= 3.3 with phosphoric acid, flow of 1.2 mL/min and ultraviolet detection at 210 nm, was used as mobile phase. Propylparabene was used as an internal standard. According to the established regulations for the validation of the methods in biological fluids, the following parameters were studied: stability of the samples, lineality, specificity, precision, accuracy and limit of detection and quantification. The method proved to be specific and sensitive with a detection and quantification limit of 0.9 and 1.0 ng, respectively. The method was lineal, precise and exact in the range of concentrations of 1. 07 at 12.67 μg/mL. The mean recovery was not statistically different from 100.0 %. The analito in the proposed biological matrix remained in the studied period. The methodology described in this work is applied in our case to the study that evaluates the bioavailability and bioequivalence of a Cuban formulation of carbamazepine in healthy volunteers. (Author)

  13. Determination of nucleosides in Cordyceps sinensis and Ganoderma lucidum by high performance liquid chromatography method

    Directory of Open Access Journals (Sweden)

    Masood Shah Khan

    2015-01-01

    Full Text Available Background: Nucleosides are supportive in the regulation and modulation of various physiological processes in body, they acts as precursors in nucleic acid synthesis, enhance immune response, help in absorption of iron and influence the metabolism of fatty acids. Cordyceps sinensis and Ganoderma lucidum are well-known for its use in traditional medicine of China, Nepal and India. They are rich in nucleosides such as adenine, adenosine, cordycepin, etc. Hence, a simple, economic and accurate high-performance liquid chromatography (HPLC analytical method was proposed for determination of adenine and adenosine for the quality control of plants. Materials and Methods: Chromatographic experiments were conducted on YL9100 HPLC system (South Korea. Reversed-phase chromatography was performed on a C18 column with methanol and dihydrogen phosphate as the mobile phase in isocratic elution method at a flow rate of 1.0 mL/min. Detection was carried out at 254 nm, which gives a sharp peak of adenine and adenosine at a retention time of 6.53 ± 0.02 min and 12.41 ± 0.02, respectively. Results and Discussion: Linear regression analysis data for the calibration plot showed a good linear relationship between response and concentration in the range of 25–200 µg/mL for adenosine and 100–800 µg/mL for adenine with regression coefficient of 0.999 and 0.996, respectively. The adenine was found 0.16% and 0.71% w/w in G. lucidum and in C. sinensis, respectively, and adenosine was found to be 0.14% w/w in G. lucidum whereas absent in C. sinensis. Conclusion: The developed HPLC method for the quantification of adenosine and adenine can be used for the quality control and standardization of crude drug and for the different herbal formulations, in which adenine and adenosine are present as major constituents. The wide linearity range, sensitivity, accuracy, and simple mobile phase imply the method is suitable for routine quantification of adenosine and adenine with

  14. High Performance Thin Layer Chromatography method for analysis of 3,4-methylenedioxymethamphetamine in seized tablets

    Directory of Open Access Journals (Sweden)

    Boris E. Duffau

    2015-12-01

    Full Text Available Context: Consumption of synthetic drugs had increased in recent years, used as a recreational drug by young people who presume that consumption of this drug is harmless for health; however clinical studies have shown that this stimulant and its metabolites are toxic. Due to these reasons, chemical analysis of this illicit drug is crucial from the points of view of occupational medicine, toxicology, and law enforcement with the aim of pursuit the traffic of illegal drug. Aims: Implement and fully validate a rapid and simple method for detection and quantitation of MDMA by High-Performance Thin Layer Chromatography in seized samples. Methods: With the implemented method was analyzed 12 positive samples seized by Chilean police, to found the concentration of MDMA in ecstasy tablets. Results: The method was fully validated, the linearity of the method was evaluated by the calibration curve between 51.0 – 510.0 µg/band (R2 0.9977; limit of detection was 12.1 µg per band, and limit of quantitation was 36.8 µg per band. The precision of the method (RSD was lower than 5.0%. Accuracy was evaluated by determination of the percentage of MDMA recovered by the assay (99.13%, and relative Uncertainty was 6.66%. With this method, it was analyzed real seized samples of MDMA, results showed that all samples contained MDMA and concentration was between 18.15 – 59.84 % w/w. Conclusions: The method is selective, sensitive, and specific, with possible application in forensic analysis. To the best of our knowledge, this is the first report about concentration of MDMA in ecstasy pills in Chile.

  15. A simplified but effective method for the quality control of medicinal plants by planar chromatography.

    Science.gov (United States)

    Eloff, J N; Ntloedibe, D T; van Brummelen, R

    2011-01-01

    Three of the factors limiting the rational use of herbal medicine are uncertainty on effectivity, uncertainty on safety and variation in quality of the product. Because many herbal medicines have been used over centuries by indigenous peoples, the safety and effectivity is frequently not such a big concern. With more people collecting and distributing herbal medicine, the offered product is however, frequently not what the label indicates either through a genuine mistake, but also through fraud especially where expensive herbal medicine is concerned. Some wrong identifications have already led to serious side effects and deaths. Planar chromatography or thin layer chromatography [TLC] is widely used to verify the identity of plant extracts by determining the chemical fingerprint of the extracts. In a leading publication 17 different extractants, 41 solvent systems and 44 spray reagents have been used to verify the identity of important herbal preparations. We investigated whether a simplified system could not be developed to aid small laboratories in identifying different herbal medicines. We compared the efficacy of different extractants, identified and developed three TLC solvent systems that would separate compounds with low, medium and high polarity and then also investigated the use of several spray reagents. With acetone as extractant and benzene:ethanol:ammonia [9:1:0.1], chloroform:ethylacetate:formic acid [5:4:1] and ethylacetate:methanol:water [10:1.35:1] as TLC solvent system and vanillin-sulphuric acid as spray reagent the identity of 81 samples of more than 50 herbal preparations could be verified on the basis of the chromatograms. The same product from different suppliers usually gave similar chromatograms. More importantly in several cases it was clear that products with the same label were so different that a mistake must have occurred in the labelling. This method has found application in the quality control of the most important African medicinal

  16. The analysis of carbohydrates in milk powder by a new "heart-cutting" two-dimensional liquid chromatography method.

    Science.gov (United States)

    Ma, Jing; Hou, Xiaofang; Zhang, Bing; Wang, Yunan; He, Langchong

    2014-03-01

    In this study, a new"heart-cutting" two-dimensional liquid chromatography method for the simultaneous determination of carbohydrate contents in milk powder was presented. In this two dimensional liquid chromatography system, a Venusil XBP-C4 analysis column was used in the first dimension ((1)D) as a pre-separation column, a ZORBAX carbohydrates analysis column was used in the second dimension ((2)D) as a final-analysis column. The whole process was completed in less than 35min without a particular sample preparation procedure. The capability of the new two dimensional HPLC method was demonstrated in the determination of carbohydrates in various brands of milk powder samples. A conventional one dimensional chromatography method was also proposed. The two proposed methods were both validated in terms of linearity, limits of detection, accuracy and precision. The comparison between the results obtained with the two methods showed that the new and completely automated two dimensional liquid chromatography method is more suitable for milk powder sample because of its online cleanup effect involved. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

  17. Method of charging instruments into liquid metal coolant

    International Nuclear Information System (INIS)

    Yamazaki, Hiroshi

    1980-01-01

    Purpose: To alleviate the thermal shock of a reactor charging machine when charging the machine into liquid metal coolant after the machine is preheated in cover gas. Method: When a reactor fueling machine reaches at the lowermost portion the position immediately above liquid metal coolant surface level, the machine is stopped moving down. The reactor fueling machine is heated at the lowermost portion by thermal radiation from the surface of the liquid metal coolant. After the machine is thus preheated in cover gas, it is again steadily moved down by a winch and charged into the liquid metal coolant. Therefore, the thermal shock of the machine becomes low when charging the machine into the liquid metal coolant to eliminate the damage and deformation at the machine. (Yoshihara, H.)

  18. Fatigue resistance of engine-driven rotary nickel-titanium instruments produced by new manufacturing methods.

    Science.gov (United States)

    Gambarini, Gianluca; Grande, Nicola Maria; Plotino, Gianluca; Somma, Francesco; Garala, Manish; De Luca, Massimo; Testarelli, Luca

    2008-08-01

    The aim of the present study was to investigate whether cyclic fatigue resistance is increased for nickel-titanium instruments manufactured by using new processes. This was evaluated by comparing instruments produced by using the twisted method (TF; SybronEndo, Orange, CA) and those using the M-wire alloy (GTX; Dentsply Tulsa-Dental Specialties, Tulsa, OK) with instruments produced by a traditional NiTi grinding process (K3, SybronEndo). Tests were performed with a specific cyclic fatigue device that evaluated cycles to failure of rotary instruments inside curved artificial canals. Results indicated that size 06-25 TF instruments showed a significant increase (p 0.05) in the mean number of cycles to failure when compared with size 06-20 GT series X instruments. The new manufacturing process produced nickel-titanium rotary files (TF) significantly more resistant to fatigue than instruments produced with the traditional NiTi grinding process. Instruments produced with M-wire (GTX) were not found to be more resistant to fatigue than instruments produced with the traditional NiTi grinding process.

  19. A rapid method for the separation and estimation of uranium in geological materials using ion chromatography

    International Nuclear Information System (INIS)

    Prakash, Satya; Bangroo, P.N.

    2013-01-01

    Ion Chromatography is an elegant analytical technique which was primarily developed for the analysis of anionic species and over the years it has been used successfully to analyse various elements in different matrices. In this work the potential of Ion Chromatography has been used for the rapid separation and estimation of uranium in hydrogeochemical and other geological materials

  20. A novel fast gas chromatography method for higher time resolution measurements of speciated monoterpenes in air

    Science.gov (United States)

    Jones, C. E.; Kato, S.; Nakashima, Y.; Kajii, Y.

    2014-05-01

    Biogenic emissions supply the largest fraction of non-methane volatile organic compounds (VOC) from the biosphere to the atmospheric boundary layer, and typically comprise a complex mixture of reactive terpenes. Due to this chemical complexity, achieving comprehensive measurements of biogenic VOC (BVOC) in air within a satisfactory time resolution is analytically challenging. To address this, we have developed a novel, fully automated Fast Gas Chromatography (Fast-GC) based technique to provide higher time resolution monitoring of monoterpenes (and selected other C9-C15 terpenes) during plant emission studies and in ambient air. To our knowledge, this is the first study to apply a Fast-GC based separation technique to achieve quantification of terpenes in ambient air. Three chromatography methods have been developed for atmospheric terpene analysis under different sampling scenarios. Each method facilitates chromatographic separation of selected BVOC within a significantly reduced analysis time compared to conventional GC methods, whilst maintaining the ability to quantify individual monoterpene structural isomers. Using this approach, the C9-C15 BVOC composition of single plant emissions may be characterised within a 14.5 min analysis time. Moreover, in-situ quantification of 12 monoterpenes in unpolluted ambient air may be achieved within an 11.7 min chromatographic separation time (increasing to 19.7 min when simultaneous quantification of multiple oxygenated C9-C10 terpenoids is required, and/or when concentrations of anthropogenic VOC are significant). These analysis times potentially allow for a twofold to fivefold increase in measurement frequency compared to conventional GC methods. Here we outline the technical details and analytical capability of this chromatographic approach, and present the first in-situ Fast-GC observations of 6 monoterpenes and the oxygenated BVOC (OBVOC) linalool in ambient air. During this field deployment within a suburban forest

  1. Development of a method to extract and purify target compounds from medicinal plants in a single step: online hyphenation of expanded bed adsorption chromatography and countercurrent chromatography.

    Science.gov (United States)

    Li, Yang; Wang, Nan; Zhang, Min; Ito, Yoichiro; Zhang, Hongyang; Wang, Yuerong; Guo, Xin; Hu, Ping

    2014-04-01

    Pure compounds extracted and purified from natural sources are crucial to lead discovery and drug screening. This study presents a novel two-dimensional hyphenation of expanded bed adsorption chromatography (EBAC) and high-speed countercurrent chromatography (HSCCC) for extraction and purification of target compounds from medicinal plants in a single step. The EBAC and HSCCC were hyphenated via a six-port injection valve as an interface. Fractionation of ingredients of Salvia miltiorrhiza and Rhizoma coptidis was performed on the hyphenated system to verify its efficacy. Two compounds were harvested from Salvia miltiorrhiza, one was 52.9 mg of salvianolic acid B with an over 95% purity and the other was 2.1 mg of rosmarinic acid with a 74% purity. Another two components were purified from Rhizoma coptidis, one was 4.6 mg of coptisine with a 98% purity and one was 4.1 mg of berberine with a 82% purity. The processing time was nearly 50% that of the multistep method. The results indicate that the present method is a rapid and green way to harvest targets from medicinal plants in a single step.

  2. Evaluation of surface characteristics of rotary nickel-titanium instruments produced by different manufacturing methods.

    Science.gov (United States)

    Inan, U; Gurel, M

    2017-02-01

    Instrument fracture is a serious concern in endodontic practice. The aim of this study was to investigate the surface quality of new and used rotary nickel-titanium (NiTi) instruments manufactured by the traditional grinding process and twisting methods. Total 16 instruments of two rotary NiTi systems were used in this study. Eight Twisted Files (TF) (SybronEndo, Orange, CA, USA) and 8 Mtwo (VDW, Munich, Germany) instruments were evaluated. New and used of 4 experimental groups were evaluated using an atomic force microscopy (AFM). New and used instruments were analyzed on 3 points along a 3 mm. section at the tip of the instrument. Quantitative measurements according to the topographical deviations were recorded. The data were statistically analyzed with paired samples t-test and independent samples t-test. Mean root mean square (RMS) values for new and used TF 25.06 files were 10.70 ± 2.80 nm and 21.58 ± 6.42 nm, respectively, and the difference between them was statistically significant (P instruments produced by twisting method (TF 25.06) had better surface quality than the instruments produced by traditional grinding process (Mtwo 25.06 files).

  3. Interlaboratory study of a liquid chromatography method for erythromycin: determination of uncertainty.

    Science.gov (United States)

    Dehouck, P; Vander Heyden, Y; Smeyers-Verbeke, J; Massart, D L; Marini, R D; Chiap, P; Hubert, Ph; Crommen, J; Van de Wauw, W; De Beer, J; Cox, R; Mathieu, G; Reepmeyer, J C; Voigt, B; Estevenon, O; Nicolas, A; Van Schepdael, A; Adams, E; Hoogmartens, J

    2003-08-22

    Erythromycin is a mixture of macrolide antibiotics produced by Saccharopolyspora erythreas during fermentation. A new method for the analysis of erythromycin by liquid chromatography has previously been developed. It makes use of an Astec C18 polymeric column. After validation in one laboratory, the method was now validated in an interlaboratory study. Validation studies are commonly used to test the fitness of the analytical method prior to its use for routine quality testing. The data derived in the interlaboratory study can be used to make an uncertainty statement as well. The relationship between validation and uncertainty statement is not clear for many analysts and there is a need to show how the existing data, derived during validation, can be used in practice. Eight laboratories participated in this interlaboratory study. The set-up allowed the determination of the repeatability variance, s(2)r and the between-laboratory variance, s(2)L. Combination of s(2)r and s(2)L results in the reproducibility variance s(2)R. It has been shown how these data can be used in future by a single laboratory that wants to make an uncertainty statement concerning the same analysis.

  4. A high-throughput method for liquid chromatography-tandem mass spectrometry determination of plasma alkylresorcinols, biomarkers of whole grain wheat and rye intake

    DEFF Research Database (Denmark)

    Ross, Alastair B; Svelander, Cecilia; Savolainen, Otto I

    2016-01-01

    supported extraction methods for extracting alkylresorcinols from plasma and improved a normal-phase liquid chromatography coupled to a tandem mass spectrometer method to reduce sample analysis time. The method was validated and compared with gas chromatography-mass spectrometry analysis. Sample preparation...

  5. Validation of the Mass-Extraction-Window for Quantitative Methods Using Liquid Chromatography High Resolution Mass Spectrometry.

    Science.gov (United States)

    Glauser, Gaétan; Grund, Baptiste; Gassner, Anne-Laure; Menin, Laure; Henry, Hugues; Bromirski, Maciej; Schütz, Frédéric; McMullen, Justin; Rochat, Bertrand

    2016-03-15

    A paradigm shift is underway in the field of quantitative liquid chromatography-mass spectrometry (LC-MS) analysis thanks to the arrival of recent high-resolution mass spectrometers (HRMS). The capability of HRMS to perform sensitive and reliable quantifications of a large variety of analytes in HR-full scan mode is showing that it is now realistic to perform quantitative and qualitative analysis with the same instrument. Moreover, HR-full scan acquisition offers a global view of sample extracts and allows retrospective investigations as virtually all ionized compounds are detected with a high sensitivity. In time, the versatility of HRMS together with the increasing need for relative quantification of hundreds of endogenous metabolites should promote a shift from triple-quadrupole MS to HRMS. However, a current "pitfall" in quantitative LC-HRMS analysis is the lack of HRMS-specific guidance for validated quantitative analyses. Indeed, false positive and false negative HRMS detections are rare, albeit possible, if inadequate parameters are used. Here, we investigated two key parameters for the validation of LC-HRMS quantitative analyses: the mass accuracy (MA) and the mass-extraction-window (MEW) that is used to construct the extracted-ion-chromatograms. We propose MA-parameters, graphs, and equations to calculate rational MEW width for the validation of quantitative LC-HRMS methods. MA measurements were performed on four different LC-HRMS platforms. Experimentally determined MEW values ranged between 5.6 and 16.5 ppm and depended on the HRMS platform, its working environment, the calibration procedure, and the analyte considered. The proposed procedure provides a fit-for-purpose MEW determination and prevents false detections.

  6. Nuclear medicine and imaging research (instrumentation and quantitative methods of evaluation)

    International Nuclear Information System (INIS)

    Beck, R.N.; Cooper, M.; Chen, C.T.

    1992-07-01

    This document is the annual progress report for project entitled ''Instrumentation and Quantitative Methods of Evaluation.'' Progress is reported in separate sections individually abstracted and indexed for the database. Subject areas reported include theoretical studies of imaging systems and methods, hardware developments, quantitative methods of evaluation, and knowledge transfer: education in quantitative nuclear medicine imaging

  7. Method Development for Pesticide Residue Analysis in Farmland Soil using High Perfomance Liquid Chromatography

    Science.gov (United States)

    Theresia Djue Tea, Marselina; Sabarudin, Akhmad; Sulistyarti, Hermin

    2018-01-01

    A method for the determination of diazinon and chlorantraniliprole in soil samples has been developed. The analyte was extracted with acetonitrile from farmland soil sample. Determination and quantification of diazinon and chlorantraniliprole were perfomed by high perfomance liquid chromatography (HPLC) with an UV detector. Several parameters of HPLC method were optimized with respect to sensitivity, high resolution of separation, and accurate determination of diazinon and chlorantraniliprole. Optimum conditions for the separation of two pesticides were eluent composition of acetonitrile:water ratio of 60:40, 0.4 mL/min of flow rate, and 220 nm of wavelength. Under the optimum conditions, diazinon linearity was in the range from 1-25 ppm with R2 of 0.9976, 1.19 mgL-1 LOD, and 3.98 mgL-1 LOQ; while the linearity of chlorantraniliprole was in the range from 0.2-5 mgL-1 with R2 of 0.9972, 0.39 mgL-1 LOD, and 1.29 mgL-1 LOQ. When the method was applied to the soil sample, both pesticides showed acceptable recoveries for real sample of more than 85%: thus, the developed method meets the validation requirement. Under this developed method, the concentrations of both pesticides in the soil samples were below the LOD and LOQ (0.577 mgL-1 for diazinon and 0.007 mgL-1 for chlorantraniliprole). Therefore, it can be concluded that the soil samples used in this study have neither diazinon nor chlorantraniliprole.

  8. Hydrophilic interaction liquid chromatography method for measuring the composition of aquatic humic substances

    KAUST Repository

    Wang, Renqi; Gutié rrez, Leonardo A.; Ng, Siuchoon; Croue, Jean-Philippe

    2015-01-01

    A hydrophilic interaction liquid chromatography (HILIC) method was developed to measure the composition of humic substances from river, reservoir, and treated wastewater based on their physicochemical properties. The current method fractionates the humic substances into four well-defined groups based on parallel analyses with a neutral and a cationic HILIC column, using mobile phases of varied compositions and pH. The results indicate that: (i) the proportion of carboxylic acids in the humic substances from terrestrial origins is less than half of that from treated wastewater (Jeddah, KSA), (ii) a higher content of basic compounds was observed in the humic substances from treated wastewater and Ribou Reservoir (Cholet, France) than in the sample from Loire River (France), (iii) a higher percentage of hydrophobic macromolecules were found in the humic substances from Loire River than in the other samples, and (iv) humic substances of treated wastewater contained less ionic neutral compounds (i.e., pKa 5-9) than the waters from terrestrial origins. The physicochemical property disparity amongst the compounds in each humic substances sample was also evaluated. The humic substances from the lightly humic Loire river displayed the highest disparity, whereas the highly humic Suwannee river (Georgia, USA) showed the most homogeneous humic substances.

  9. Sensitive liquid chromatography-tandem mass spectrometry method for quantification of hydrochlorothiazide in human plasma.

    Science.gov (United States)

    Ramakrishna, N V S; Vishwottam, K N; Manoj, S; Koteshwara, M; Wishu, S; Varma, D P

    2005-12-01

    A simple, rapid, sensitive and specific liquid chromatography-tandem mass spectrometry method was developed and validated for quantification of hydrochlorothiazide (I), a common diuretic and anti-hypertensive agent. The analyte and internal standard, tamsulosin (II) were extracted by liquid-liquid extraction with diethyl ether-dichloromethane (70:30, v/v) using a Glas-Col Multi-Pulse Vortexer. The chromatographic separation was performed on a reversed-phase column (Waters symmetry C18) with a mobile phase of 10 mm ammonium acetate-methanol (15:85, v/v). The protonated analyte was quantitated in negative ionization by multiple reaction monitoring with a mass spectrometer. The mass transitions m/z 296.1 solidus in circle 205.0 and m/z 407.2 solidus in circle 184.9 were used to measure I and II, respectively. The assay exhibited a linear dynamic range of 0.5-200 ng/mL for hydrochlorothiazide in human plasma. The lower limit of quantitation was 500 pg/mL, with a relative standard deviation of less than 9%. Acceptable precision and accuracy were obtained for concentrations over the standard curve ranges. A run time of 2.5 min for each sample made it possible to analyze a throughput of more than 400 human plasma samples per day. The validated method has been successfully used to analyze human plasma samples for application in pharmacokinetic, bioavailability or bioequivalence studies. (c) 2005 John Wiley & Sons, Ltd.

  10. Quality Evaluation of Potentilla fruticosa L. by High Performance Liquid Chromatography Fingerprinting Associated with Chemometric Methods.

    Science.gov (United States)

    Liu, Wei; Wang, Dongmei; Liu, Jianjun; Li, Dengwu; Yin, Dongxue

    2016-01-01

    The present study was performed to assess the quality of Potentilla fruticosa L. sampled from distinct regions of China using high performance liquid chromatography (HPLC) fingerprinting coupled with a suite of chemometric methods. For this quantitative analysis, the main active phytochemical compositions and the antioxidant activity in P. fruticosa were also investigated. Considering the high percentages and antioxidant activities of phytochemicals, P. fruticosa samples from Kangding, Sichuan were selected as the most valuable raw materials. Similarity analysis (SA) of HPLC fingerprints, hierarchical cluster analysis (HCA), principle component analysis (PCA), and discriminant analysis (DA) were further employed to provide accurate classification and quality estimates of P. fruticosa. Two principal components (PCs) were collected by PCA. PC1 separated samples from Kangding, Sichuan, capturing 57.64% of the variance, whereas PC2 contributed to further separation, capturing 18.97% of the variance. Two kinds of discriminant functions with a 100% discrimination ratio were constructed. The results strongly supported the conclusion that the eight samples from different regions were clustered into three major groups, corresponding with their morphological classification, for which HPLC analysis confirmed the considerable variation in phytochemical compositions and that P. fruticosa samples from Kangding, Sichuan were of high quality. The results of SA, HCA, PCA, and DA were in agreement and performed well for the quality assessment of P. fruticosa. Consequently, HPLC fingerprinting coupled with chemometric techniques provides a highly flexible and reliable method for the quality evaluation of traditional Chinese medicines.

  11. Alternative sorptive extraction method for gas chromatography determination of halogenated anisoles in water and wine samples

    International Nuclear Information System (INIS)

    Montes, R.; Rodriguez, I.; Rubi, E.; Bollain, M.H.; Cela, R.

    2007-01-01

    An alternative sorptive microextraction method for the determination of five halogenated anisoles in water and wine matrices is proposed. Analytes were concentrated in an inexpensive and disposable piece of bulk polydimethylsiloxane (PDMS), desorbed with a small volume of organic solvent, and determined by gas chromatography with electron-capture detection (GC-ECD) or tandem mass spectrometry (GC-MS/MS). The influence of several factors on the efficiency of extraction and desorption steps was investigated in detail and the observed behaviour justified on the basis of thermodynamics and kinetics of the solid-phase microextraction technique. Under optimised conditions, analytes were first extracted in the headspace (HS) mode, at room temperature, for 2.5 h and then desorbed with 1 mL of n-pentane. This extract was further evaporated to 50 μL. The overall extraction yield of the procedure ranged from 40 to 55% and the limits of quantification remained between 0.5 and 20 ng L -1 , depending on the compound considered and the detection technique. Precision and linearity of the method were excellent for all species with both GC-ECD and GC-MS/MS detection. Matrix effects were evaluated with different water and wine samples; moreover, the suitability of the PDMS sorbent for storage of analytes, under different conditions, was demonstrated

  12. Analysis of Fluconazole in Human Urine Sample by High Performance Liquid Chromatography Method

    International Nuclear Information System (INIS)

    Hermawan, D; Ali, N A Md; Ibrahim, W A Wan; Sanagi, M M

    2013-01-01

    A method for determination of fluconazole, antifungal drug in human urine by using reversed-phased high performance liquid chromatography (RP-HPLC) with ultraviolet (UV) detector was developed. Optimization HPLC conditions were carried out by changing the flow rate and composition of mobile phase. The optimum separation conditions at a flow rate 0.85 mL/min with a composition of mobile phase containing methanol:water (70:30, v/v) with UV detection at a wavelength 254 nm was able to analyze fluconazole within 3 min. The excellent linearity was obtained in the range of concentration 1 to 10 μg/mL with r 2 = 0.998. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.39 μg/mL and 1.28 μg/mL, respectively. Solid phase extraction (SPE) method using octadecylsilane (C18) as a sorbent was used to clean-up and pre-concentrated of the urine sample prior to HPLC analysis. The average recoveries of fluconazole in spiked urine sample was 72.4% with RSD of 3.21% (n=3).

  13. Quality Evaluation of Potentilla fruticosa L. by High Performance Liquid Chromatography Fingerprinting Associated with Chemometric Methods

    Science.gov (United States)

    Liu, Wei; Wang, Dongmei; Liu, Jianjun; Li, Dengwu; Yin, Dongxue

    2016-01-01

    The present study was performed to assess the quality of Potentilla fruticosa L. sampled from distinct regions of China using high performance liquid chromatography (HPLC) fingerprinting coupled with a suite of chemometric methods. For this quantitative analysis, the main active phytochemical compositions and the antioxidant activity in P. fruticosa were also investigated. Considering the high percentages and antioxidant activities of phytochemicals, P. fruticosa samples from Kangding, Sichuan were selected as the most valuable raw materials. Similarity analysis (SA) of HPLC fingerprints, hierarchical cluster analysis (HCA), principle component analysis (PCA), and discriminant analysis (DA) were further employed to provide accurate classification and quality estimates of P. fruticosa. Two principal components (PCs) were collected by PCA. PC1 separated samples from Kangding, Sichuan, capturing 57.64% of the variance, whereas PC2 contributed to further separation, capturing 18.97% of the variance. Two kinds of discriminant functions with a 100% discrimination ratio were constructed. The results strongly supported the conclusion that the eight samples from different regions were clustered into three major groups, corresponding with their morphological classification, for which HPLC analysis confirmed the considerable variation in phytochemical compositions and that P. fruticosa samples from Kangding, Sichuan were of high quality. The results of SA, HCA, PCA, and DA were in agreement and performed well for the quality assessment of P. fruticosa. Consequently, HPLC fingerprinting coupled with chemometric techniques provides a highly flexible and reliable method for the quality evaluation of traditional Chinese medicines. PMID:26890416

  14. Alternative sorptive extraction method for gas chromatography determination of halogenated anisoles in water and wine samples

    Energy Technology Data Exchange (ETDEWEB)

    Montes, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain); Rodriguez, I. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain)], E-mail: qnisaac@usc.es; Rubi, E.; Bollain, M.H.; Cela, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain)

    2007-09-05

    An alternative sorptive microextraction method for the determination of five halogenated anisoles in water and wine matrices is proposed. Analytes were concentrated in an inexpensive and disposable piece of bulk polydimethylsiloxane (PDMS), desorbed with a small volume of organic solvent, and determined by gas chromatography with electron-capture detection (GC-ECD) or tandem mass spectrometry (GC-MS/MS). The influence of several factors on the efficiency of extraction and desorption steps was investigated in detail and the observed behaviour justified on the basis of thermodynamics and kinetics of the solid-phase microextraction technique. Under optimised conditions, analytes were first extracted in the headspace (HS) mode, at room temperature, for 2.5 h and then desorbed with 1 mL of n-pentane. This extract was further evaporated to 50 {mu}L. The overall extraction yield of the procedure ranged from 40 to 55% and the limits of quantification remained between 0.5 and 20 ng L{sup -1}, depending on the compound considered and the detection technique. Precision and linearity of the method were excellent for all species with both GC-ECD and GC-MS/MS detection. Matrix effects were evaluated with different water and wine samples; moreover, the suitability of the PDMS sorbent for storage of analytes, under different conditions, was demonstrated.

  15. Current role of liquid chromatography coupled to mass spectrometry in clinical toxicology screening methods.

    Science.gov (United States)

    Viette, Véronique; Fathi, Marc; Rudaz, Serge; Hochstrasser, Denis; Veuthey, Jean-Luc

    2011-07-01

    Abstract Toxicological screening is the analysis of a biological specimen to detect and identify compounds in patients admitted to the hospital with acute intoxication of unknown origin. The screening of a wide range of toxicologically relevant compounds in biological samples is a serious challenge for clinical laboratories. The high selectivity and sensitivity of liquid chromatography coupled to mass spectrometry or tandem mass spectrometry technology provides an attractive alternative to the current methods. For these reasons, an increasing number of applications for multi-target screening or general screening of unknown compounds in biological matrices are being published. This paper is an overview of sample clean-up, chromatographic separation and mass spectrometry detection procedures which can be combined to obtain screening methods adapted to the constraints and needs of various laboratories, and none specifically in clinical toxicology. Currently the techniques are in the hands of specialists, principally in academic institutes. However, the evolution in technology should allow application of the techniques as a tool in toxicology laboratories and thus more widespread exploitation of their potential.

  16. New EDTA determination method based on ion chromatography with suppressed conductimetric detection

    International Nuclear Information System (INIS)

    Gyoergy Patzay; Yahya Ramadan; Csilla Tonko

    2014-01-01

    A novel direct method for the determination of EDTA in alkaline radioactive evaporator residue solution was developed and validated based on ion chromatography with suppressed conductimetric detection and anion exchange columns (A Supp 4, 4 mm × 250 mm and A Supp 5, 4 mm × 150 mm). The yttrium-EDTA complex resulted one single chromatographic peak in the eluent and allowed the correct determination of EDTA in an alkaline, high concentration radioactive waste water. Depending on coexisting substances, suitable eluent is 10.0 mM carbonate buffer/pH 10.6 or 10.75 (t R ,Y-EDTA = 7.01 and 6.4 min, respectively). For 10.0 mM carbonate buffer/pH 10.6 and isocratic flow rate of 1.0 cm 3 /min, a linear calibration curve was obtained from 5 to 40 mg/dm 3 (r > 0.999) EDTA. Good resolution was achieved from commonly coexisting anions (chloride, nitrite, nitrate, sulphate, phosphate, bromide and citrate). The developed simple ion chromatographic method was applied for the assay of EDTA in various radioactive alkaline solutions. (author)

  17. Amphenicols stability in medicated feed – development and validation of liquid chromatography method

    Directory of Open Access Journals (Sweden)

    Pietro Wojciech Jerzy

    2014-12-01

    Full Text Available A liquid chromatography-ultraviolet detection method for the determination of florfenicol (FF and thiamphenicol (TAP in feeds is presented. The method comprises the extraction of analytes from the matrix with a mixture of methanol and acetonitrile, drying of the extract, and its dissolution in phosphate buffer. The analysis was performed with a gradient programme of the mobile phase composed of acetonitrile and buffer (pH = 7.3 on a Zorbax Eclipse Plus C18 (150 × 4.6 mm, 5 μm analytical column with UV (λ = 220 nm detection. The analytical procedure has been successfully adopted and validated for quantitative determination of florfenicol and thiamphenicol in feed samples. Sensitivity, specificity, linearity, repeatability, and intralaboratory reproducibility were included in the validation. The mean recovery of amphenicols was 93.5% within the working range of 50-4000 mg/kg. Simultaneous determination of chloramphenicol, which is banned in the feed, was also included within the same procedure of FF and TAP stability studies. Storing the medicated feed at room temperature for up to one month decreased concentration in the investigated drugs even by 45%. These findings are relevant to successful provision of therapy to animals.

  18. Improved method for the determination of the cortisol production rate using high-performance liquid chromatography and liquid scintillation counting

    NARCIS (Netherlands)

    van Ingen, H. E.; Endert, E.

    1988-01-01

    Two new methods for the determination of the cortisol production rate using reversed-phase high-performance liquid chromatography are described. One uses ultraviolet detection at 205 nm, the other on-line post-column derivatization with benzamidine, followed by fluorimetric detection. The specific

  19. Novel method for measurement of glutathione kinetics in neonates using liquid chromatography coupled to isotope ratio mass spectrometry

    NARCIS (Netherlands)

    Schierbeek, Henk; te Braake, Frans; Godin, Jean-Philippe; Fay, Laurent-Bernard; van Goudoever, Johannes B.

    2007-01-01

    A novel analytical method using liquid chromatography coupled to isotope ratio mass spectrometry (LC/IRMS) was developed for measuring the fractional synthesis rate (FSR) of glutathione (GSH) in neonates after infusion of [1-(13)C]-glycine as a tracer. After transformation of GSH into GSSG, its

  20. Calibration of shahid's analytical method for adulterated Zn-edta fertilizers by ion chromatography and atomic absorption spectroscopy

    International Nuclear Information System (INIS)

    Khan, M.S.A.; Akram, M.; Qazi, M.A.

    2010-01-01

    Chelated zinc fertilizers are usually recommended in calcareous alkaline soils to provide Zn nutrition in order to prevent possible Zn precipitation. In Punjab (Pakistan), Zn EDTA products are being manufactured, and marketed to meet the zinc requirement of various crops grown in Zn deficient soils. Under fertilizer control order, 1973 (amended), their quality has to be monitored by the Agriculture Department, Government of the Punjab. None of the traditional method was found suitable which can separate the mineral fraction from that of chelated adulterated fertilizer except for those methods based on ion chromatography. Calibration of ion chromatography method was carried out by determining the mineral Zn fraction leading to estimate remaining Zn EDTA fraction in fertilizer samples of adulterated nature i.e. mixture of chelated and mineral fraction. In order to achieve the objective atomic absorption spectroscopy was coupled with ion chromatography. The method offers a specific, reliable technique for determination of chelated zinc in fertilizers. In the first step chelation was broken down with concentrated sulphuric acid treatment and total zinc contents were determined by atomic absorption spectroscopy. In second step, non-chelated (mineral) portion of zinc was determined by ion chromatography using cation column and conductivity detector. Chelated zinc was calculated by subtracting non-chelated (mineral) fraction from total zinc contents. (author)

  1. Simple, rapid, and sensitive liquid chromatography-fluorescence method for the quantification of tranexamic acid in blood

    NARCIS (Netherlands)

    Huertas-Pérez, José Fernando; Heger, Michal; Dekker, Henk; Krabbe, Hans; Lankelma, Jan; Ariese, Freek

    2007-01-01

    Tranexamic acid (TA) is a synthetic antifibrinolytic agent that is being considered as a candidate adjuvant drug for site-specific pharmaco-laser therapy of port wine stains. For drug utility studies, a high-performance liquid chromatography (HPLC)-fluorescence method was developed for the

  2. Determination of methyldibromoglutaronitrile in cosmetic products by high-performance liquid chromatography with electrochemical detection. Method validation

    DEFF Research Database (Denmark)

    Rastogi, Suresh Chandra; Zachariae, Claus; Johansen, Jeanne D

    2004-01-01

    An increased frequency of contact allergy to methyldibromoglutaronitrile (MDBGN), a commonly used preservative in cosmetics and other consumer products, has been reported in recent years. A high-performance liquid chromatography (HPLC) method for the determination of MDBGN in cosmetic products ha...

  3. High-performance liquid chromatography method with radiochemical detection for measurement of nitric oxide synthase, arginase, and arginine decarboxylase activities

    DEFF Research Database (Denmark)

    Volke, A; Wegener, Gregers; Vasar, E

    2006-01-01

    regulate NOS activity. We aimed to develop a HPLC-based method to measure simultaneously the products of these three enzymes. Traditionally, the separation of amino acids and related compounds with HPLC has been carried out with precolumn derivatization and reverse phase chromatography. We describe here...

  4. Determination of methyldibromoglutaronitrile in cosmetic products by high-performance liquid chromatography with electrochemical detection. Method validation

    DEFF Research Database (Denmark)

    Rastogi, Suresh Chandra; Zachariae, Claus; Johansen, Jeanne D

    2004-01-01

    An increased frequency of contact allergy to methyldibromoglutaronitrile (MDBGN), a commonly used preservative in cosmetics and other consumer products, has been reported in recent years. A high-performance liquid chromatography (HPLC) method for the determination of MDBGN in cosmetic products has...

  5. Method of determining of polybrominated diphenyl ethers in fish and fish products by the method of liquid chromatography

    Directory of Open Access Journals (Sweden)

    O.N. Timofeeva

    2016-09-01

    Full Text Available The aim of the work was to develop a methodology for determining of polybrominated diphenyl ethers (PBDE in fish and fish products for the control of impurities content in the food and environmental objects in general. The conditions of chromatography (temperature conditions, the impact of the speed and magnitude of dividing of the gas-carrier stream using a HP-1 capillary columns, the DB-5, HP-50 +, DB-1; and lipids destructive and non-destructive cleaning methods of extract during the determination of PBDEs. The method of determination of 2,2,4,4-Tetrabromodiphenyl ether (BDE-47, 2,2,4,4,5-pentabromodiphenyl ether (BDE-99 and decabromodiphenyl ether (BDE-209 in fish and fish products by the liquid chromatography with electron detector was suggested. The method of PBDE is based on the extraction of samples with hexane-acetone (3:1, purification of the extract with concentrated sulfuric acid (phase ratio hexane-sulfuric acid – 5:1. The second purification step is carried out by using solid phase extraction cartridges «SiOH-H2SO4/SA» and hexane as the eluent. Gas chromatographic analysis of the determination of BDE-47 and BDE-99 is carried out on low-polar capillary column DB-5 (30 m x0.25 mm x0.25 mum with the programming of the column temperature. In determining the BDE-209 a DB-1 nonpolar capillary column was used (15 m x 0.25 mm x 0.1 mum with the column temperature programming. Calculation of the content of BDE-47 and BDE-99 is carried out with the internal standard (2,2, 3,4,4-pentabromodiphenyl ether (BDE-85, BDE-209 by absolute calibration. In determining the BDE-209 the calibration matrix was used. The range of concentrations of the calibration solutions for the determination of BDE-47 and BDE-99 is 0.005–0.05 g/cm 3 , for BDE-209 0.05–0.3 g/cm 3 . The technique allows the measurement of BDE-47 and BDE-99 in the range of 0.0002–0.05 mg/kg of the product concerned; BDE-209 – in the range of 0.002–0.3 mg/kg. The metrological

  6. A method for the deliberate and deliberative selection of policy instrument mixes for climate change adaptation

    Directory of Open Access Journals (Sweden)

    Heleen L. P. Mees

    2014-06-01

    Full Text Available Policy instruments can help put climate adaptation plans into action. Here, we propose a method for the systematic assessment and selection of policy instruments for stimulating adaptation action. The multi-disciplinary set of six assessment criteria is derived from economics, policy, and legal studies. These criteria are specified for the purpose of climate adaptation by taking into account four challenges to the governance of climate adaptation: uncertainty, spatial diversity, controversy, and social complexity. The six criteria and four challenges are integrated into a step-wise method that enables the selection of instruments starting from a generic assessment and ending with a specific assessment of policy instrument mixes for the stimulation of a specific adaptation measure. We then apply the method to three examples of adaptation measures. The method's merits lie in enabling deliberate choices through a holistic and comprehensive set of adaptation specific criteria, as well as deliberative choices by offering a stepwise method that structures an informed dialog on instrument selection. Although the method was created and applied by scientific experts, policy-makers can also use the method.

  7. Column Liquid Chromatography.

    Science.gov (United States)

    Majors, Ronald E.; And Others

    1984-01-01

    Reviews literature covering developments of column liquid chromatography during 1982-83. Areas considered include: books and reviews; general theory; columns; instrumentation; detectors; automation and data handling; multidimensional chromatographic and column switching techniques; liquid-solid chromatography; normal bonded-phase, reversed-phase,…

  8. New radiochemical methods for determination of 237Np a 241Pu using extraction chromatography (Presentation)

    International Nuclear Information System (INIS)

    Strisovska, J.

    2013-01-01

    Thesis was focused on the development of a new methodology for the separation of anthropogenic transuranium radionuclides 237 Np a 241 Pu from different kinds of matrices. The analytical methods used in this study were based on extraction chromatography and were optimized according to the sample type. The proposed radiochemical procedure is a combination of two algorithms, which represent the separation of radionuclides by using extraction chromatographic sorbents TEVA resin and TRU resin supplied by Eichrom Technologies LLC. 239 Np a 237 Np were selectively captured on sorbent TEVA resin in oxidation state 4+. TRU resin was used for purification of plutonium fraction from interfering americium radionuclide. 242 Pu and 239 Np radionuclides as tracers have been used to monitor the radiochemical yields of separation. Before every radiochemical separation tracer radionuclide 239 Np was obtained by separation from the parent radionuclide 2 43 Am, which is in radioactive equilibrium to 239 Np. The average yield of chemical separation was 69,3% for 239 Np at 277 keV energy line and 65,9% at 228 keV energy line. The NPL AH-B08069 (2008) samples which consist of the mixture of alpha-radionuclides were used for the modification and optimization of separation method used for separation of Np and Pu in model samples. This method provided high radiochemical yields of 239,240 Pu (95,0 ± 3,5)% and 237 Np (87,9 ± 3,0)%.. Reliability of the method was verified by applying our modified separation procedures on reference materials IAEA-375 and IAEA-414 supplied by International Atomic Energy Agency. A good agreement between the results is obtained by this procedure and the certified values were found. Samples of contaminated soils from the area of Nuclear power plant A-1 Jaslovske Bohunice which is stored temporarily before disposal were analyzed using developed separation procedure. Specific activity of investigated radionuclides was determined in these samples. (author)

  9. Methods in endogenous steroid profiling - A comparison of gas chromatography mass spectrometry (GC-MS) with supercritical fluid chromatography tandem mass spectrometry (SFC-MS/MS).

    Science.gov (United States)

    Teubel, Juliane; Wüst, Bernhard; Schipke, Carola G; Peters, Oliver; Parr, Maria Kristina

    2018-06-15

    In various fields of endocrinology, the determination of steroid hormones synthesised by the human body plays an important role. Research on central neurosteroids has been intensified within the last years, as they are discussed as biomarkers for various cognitive disorders. Their concentrations in cerebrospinal fluid (CSF) are considered to be regulated independently from peripheral fluids. For that reason, the challenging matrix CSF becomes a very interesting specimen for analysis. Concentrations are expected to be very low and available amount of CSF is limited. Thus, a comprehensive method for very sensitive quantification of a set of analytes as large as possible in one analytical aliquot is desired. However, high structural similarities of the selected panel of 51 steroids and steroid sulfates, including numerous isomers, challenges achievement of chromatographic selectivity. Since decades the analysis of endogenous steroids in various body fluids is mainly performed by gas chromatography (GC) coupled to (tandem) mass spectrometry (MS(/MS)). Due to the structure of the steroids of interest, derivatisation is performed to meet the analytical requirements for GC-MS(/MS). Most of the laboratories use a two-step derivatisation in multi-analyte assays that was already published in the 1980s. However, for some steroids this elaborate procedure yields multiple isomeric derivatives. Thus, some laboratories utilize (ultra) high performance liquid chromatography ((U)HPLC)-MS/MS as alternative but, even UHPLC is not able to separate some of the isomeric pairs. Supercritical fluid chromatography (SFC) as an orthogonal separation technique to GC and (U)HPLC may help to overcome these issues. Within this project the two most promising methods for endogenous steroid profiling were investigated and compared: the "gold standard" GC-MS and the orthogonal separation technique SFC-MS/MS. Different derivatisation procedures for gas chromatographic detection were explored and the

  10. Tundish Cover Flux Thickness Measurement Method and Instrumentation Based on Computer Vision in Continuous Casting Tundish

    Directory of Open Access Journals (Sweden)

    Meng Lu

    2013-01-01

    Full Text Available Thickness of tundish cover flux (TCF plays an important role in continuous casting (CC steelmaking process. Traditional measurement method of TCF thickness is single/double wire methods, which have several problems such as personal security, easily affected by operators, and poor repeatability. To solve all these problems, in this paper, we specifically designed and built an instrumentation and presented a novel method to measure the TCF thickness. The instrumentation was composed of a measurement bar, a mechanical device, a high-definition industrial camera, a Siemens S7-200 programmable logic controller (PLC, and a computer. Our measurement method was based on the computer vision algorithms, including image denoising method, monocular range measurement method, scale invariant feature transform (SIFT, and image gray gradient detection method. Using the present instrumentation and method, images in the CC tundish can be collected by camera and transferred to computer to do imaging processing. Experiments showed that our instrumentation and method worked well at scene of steel plants, can accurately measure the thickness of TCF, and overcome the disadvantages of traditional measurement methods, or even replace the traditional ones.

  11. High-performance liquid chromatography ultraviolet-photodiode array detection method for aflatoxin B1 in cattle feed supplements

    Science.gov (United States)

    Mochamad, Lazuardi; Hermanto, Bambang

    2017-01-01

    Aim: The objective of the current study is to determine the concentration of aflatoxin B1 using high-performance liquid chromatography (HPLC) with a photodiode array (PDA) detector. Materials and Methods: Aflatoxin B1 certified reference grade from Trilogy Analytical Laboratory dissolved acetonitrile (ACN) at 10 µg/mL was using standard assessment. HPLC instruments such as ultraviolet-PDA detector used a Shimadzu LC-6AD pump with DGU-20A5 degasser, communication module-20A, and PDA detector SPD-M20A with FRC-10A fraction collector. The HPLC was set isocratic method at 354 nm with a reverse-phase ODS C18 column (LiChrospher® 100 RP-18; diameter, 5 µm) under a 20°C controlled column chamber. Rheodyne® sample loops were performed in 20 µL capacities. The mobile phase was performed at fraction 63:26:11 H2O: methanol:ACN at pH 6.8. A total of 1 kg of feed contained 10% bread crumbs and 30% concentrated, 40% forage, and 20% soybean dregs were using commercials samples. Samples were extracted by ACN and separated with solid phase extraction ODS 1 mL than elution with mobile phase to collect at drying samples performed. The samples were ready to use after added 1 mL mobile phase than injected into the system of HPLC. Results: We found that the retention time of aflatoxin B1 was approximately 10.858 min. Linearity of 0.01-0.08 µg/mL aflatoxin B1 dissolved in mobile phase was obtained at R2=0.9. These results demonstrate that these methods can be used to analyze aflatoxin B1 and gain 89-99% recovery. The limit of detection of this assay was obtained at 3.5 × 10−6 µg/mL. Conclusion: This method was easy to apply and suitable to analyzing at small concentrations of aflatoxin B1 in formulated product of feed cattle. PMID:28919686

  12. Report: Affinity Chromatography.

    Science.gov (United States)

    Walters, Rodney R.

    1985-01-01

    Supports, affinity ligands, immobilization, elution methods, and a number of applications are among the topics considered in this discussion of affinity chromatography. An outline of the basic principles of affinity chromatography is included. (JN)

  13. THE REGULATION OF MONEY CIRCULATION ON THE BASIS OF USING METHODS AND INSTRUMENTS OF MONETARY POLICY

    Directory of Open Access Journals (Sweden)

    S. Mishchenko

    2013-05-01

    Full Text Available In the article it was researched the instruments and mechanism of safeguarding stability of money market on the basis of implementing the optimal monetary policy regime. It was determined the main directions of appliance the monetary policy methods and instruments to guiding money market stability and it was also investigated the influence of transmission mechanism on providing the soundness of money circulations.

  14. Inverse gas chromatography as a method for determination of surface properties of binding materials

    Science.gov (United States)

    Yu, Jihai; Lu, Xiaolei; Yang, Chunxia; Du, Baoli; Wang, Shuxian; Ye, Zhengmao

    2017-09-01

    Inverse gas chromatography (IGC) is a promising measurement technique for investigating the surface properties of binding materials, which are the major influence element for the adsorption performance of superplasticizer. In this work, using the IGC method, blast furnace slag (BFS), sulphoaluminate cement (SAC) and portland cement (P·O) are employed to systematically evaluate the corresponding dispersive component (γsd), specific surface free energy (γsab), and acid-base properties. The obtained results show that γsd contributes to a major section of the surface free energy in the three binding materials, suggesting they are of a relatively low polarity. Compared to the two kinds of cements, the BFS possesses the highest dispersive and specific surface free energies (the values are 45.01 mJ/m2 and 11.68 mJ/m2, respectively), and also exhibits a wider distribution range of γsd, indicating their surfaces are heterogeneous. For acid-base properties, the results indicate the surfaces of three samples are basic in nature. In addition, the adsorption investigation shows that per unit surface of BFS adsorbs the most superplasticizer molecules, which indicates the higher surface free energies is beneficial to the superplasticizer adsorption.

  15. Liquid chromatography-high resolution mass spectrometric methods for the surveillance monitoring of cyanotoxins in freshwaters.

    Science.gov (United States)

    Bogialli, Sara; Bortolini, Claudio; Di Gangi, Iole Maria; Di Gregorio, Federica Nigro; Lucentini, Luca; Favaro, Gabriella; Pastore, Paolo

    2017-08-01

    A comprehensive risk management on human exposure to cyanotoxins, whose production is actually unpredictable, is limited by reliable analytical tools for monitoring as many toxic algal metabolites as possible. Two analytical approaches based on a LC-QTOF system for target analysis and suspect screening of cyanotoxins in freshwater were presented. A database with 369 compounds belonging to cyanobacterial metabolites was developed and used for a retrospective data analysis based on high resolution mass spectrometry (HRMS). HRMS fragmentation of the suspect cyanotoxin precursor ions was subsequently performed for correctly identifying the specific variants. Alternatively, an automatic tandem HRMS analysis tailored for cyanotoxins was performed in a single chromatographic run, using the developed database as a preferred precursor ions list. Twenty-five extracts of surface and drinking waters contaminated by cyanobacteria were processed. The identification of seven uncommon microcystins (M(O)R, MC-FR, MSer 7 -YR, D-Asp 3 MSer 7 -LR, MSer 7 -LR, dmAdda-LR and dmAdda-YR) and 6 anabaenopeptins (A, B, F, MM850, MM864, oscyllamide Y) was reported. Several isobaric variants, fully separated by chromatography, were pointed out. The developed methods are proposed to be used by environmental and health agencies for strengthening the surveillance monitoring of cyanotoxins in water. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. A gas chromatography-mass spectrometry method for the quantitation of clobenzorex.

    Science.gov (United States)

    Cody, J T; Valtier, S

    1999-01-01

    Drugs metabolized to amphetamine or methamphetamine are potentially significant concerns in the interpretation of amphetamine-positive urine drug-testing results. One of these compounds, clobenzorex, is an anorectic drug that is available in many countries. Clobenzorex (2-chlorobenzylamphetamine) is metabolized to amphetamine by the body and excreted in the urine. Following administration, the parent compound was detectable for a shorter time than the metabolite amphetamine, which could be detected for days. Because of the potential complication posed to the interpretation of amphetamin-positive drug tests following administration of this drug, the viability of a current amphetamine procedure using liquid-liquid extraction and conversion to the heptafluorobutyryl derivative followed by gas chromatography-mass spectrometry (GC-MS) analysis was evaluated for identification and quantitation of clobenzorex. Qualitative identification of the drug was relatively straightforward. Quantitative analysis proved to be a far more challenging process. Several compounds were evaluated for use as the internal standard in this method, including methamphetamine-d11, fenfluramine, benzphetamine, and diphenylamine. Results using these compounds proved to be less than satisfactory because of poor reproducibility of the quantitative values. Because of its similar chromatographic properties to the parent drug, the compound 3-chlorobenzylamphetamine (3-Cl-clobenzorex) was evaluated in this study as the internal standard for the quantitation of clobenzorex. Precision studies showed 3-Cl-clobenzorex to produce accurate and reliable quantitative results (within-run relative standard deviations [RSDs] clobenzorex.

  17. Simple micellar electrokinetic chromatography method for the determination of hydrogen sulfide in hen tissues.

    Science.gov (United States)

    Kubalczyk, Paweł; Borowczyk, Kamila; Chwatko, Grażyna; Głowacki, Rafał

    2015-04-01

    A new method for the determination of hydrogen sulfide in hen tissues has been developed and validated. For estimation of hydrogen sulfide content, a sample (0.1 g) of hen tissue was treated according to the procedure consisted of some essential steps: simultaneous homogenization of a tissue and derivatization of hydrogen sulfide to its S-quinolinium derivative with 2-chloro-1-methylquinolinium tetrafluoroborate, separation of so-formed derivative by micellar electrokinetic chromatography with sweeping, and detection and quantitation with the use of UV detector set to measure analytical signals at 375 nm. Effective electrophoretic separation was achieved using fused silica capillary (effective length 41.5 cm, 75 μm id) and 0.05 mol/L, pH 8 phosphate buffer with the addition of 0.04 mol/L SDS and 26% ACN. The lower limit of quantification was 0.12 μmol hydrogen sulfide in 1 g of tissue. The calibration curve prepared in tissue homogenate for hydrogen sulfide showed linearity in the range from 0.15 to 2.0 μmol/g, with the coefficient of correlation 0.9978. The relative standard deviation of the points of the calibration curve varied from 8.3 to 3.2% RSD. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. A Straightforward Method for Glucosinolate Extraction and Analysis with High-pressure Liquid Chromatography (HPLC).

    Science.gov (United States)

    Grosser, Katharina; van Dam, Nicole M

    2017-03-15

    Glucosinolates are a well-studied and highly diverse class of natural plant compounds. They play important roles in plant resistance, rapeseed oil quality, food flavoring, and human health. The biological activity of glucosinolates is released upon tissue damage, when they are mixed with the enzyme myrosinase. This results in the formation of pungent and toxic breakdown products, such as isothiocyanates and nitriles. Currently, more than 130 structurally different glucosinolates have been identified. The chemical structure of the glucosinolate is an important determinant of the product that is formed, which in turn determines its biological activity. The latter may range from detrimental (e.g., progoitrin) to beneficial (e.g., glucoraphanin). Each glucosinolate-containing plant species has its own specific glucosinolate profile. For this reason, it is important to correctly identify and reliably quantify the different glucosinolates present in brassicaceous leaf, seed, and root crops or, for ecological studies, in their wild relatives. Here, we present a well-validated, targeted, and robust method to analyze glucosinolate profiles in a wide range of plant species and plant organs. Intact glucosinolates are extracted from ground plant materials with a methanol-water mixture at high temperatures to disable myrosinase activity. Thereafter, the resulting extract is brought onto an ion-exchange column for purification. After sulfatase treatment, the desulfoglucosinolates are eluted with water and the eluate is freeze-dried. The residue is taken up in an exact volume of water, which is analyzed by high-pressure liquid chromatography (HPLC) with a photodiode array (PDA) or ultraviolet (UV) detector. Detection and quantification are achieved by conducting comparisons of the retention times and UV spectra of commercial reference standards. The concentrations are calculated based on a sinigrin reference curve and well-established response factors. The advantages and

  19. Methods for separating boron from borated paraffin wax and its determination by ion chromatography

    International Nuclear Information System (INIS)

    Jeyakumar, S.

    2015-01-01

    Boron compounds are found to be useful in shielding against high-energy neutrons. In radiotherapy treatments, in order to protect occupational workers and patients from the undesirable neutron and gamma doses, paraffin wax containing B 4 C/boric acid is used. Low-level borate wastes generated from the nuclear power plants have been immobilized with paraffin wax using a concentrate waste drying system (CWDS). Borated paraffin waxes are prepared by mixing calculated amounts of either boric acid or boron carbide with the molten wax. This necessitates the determination of boron at different locations in order to check the homogeneous distribution of B over the borated wax. The determination of boron in nuclear materials is inevitable due to its high neutron absorption cross section. For the determination of boron in borated waxes, not many methods have been reported. A method based on the pyrohydrolysis extraction of boron and its quantification with ion chromatography was proposed for paraffin waxes borated with H 3 BO 3 and B 4 C. The B 4 C optimum pyrohydrolysis conditions were identified. Wax samples were mixed with U 3 O 8 , which prevents the sample from flare up, and also accelerates the extraction of boron. Pyrohydrolysis was carried out with moist O 2 at 950℃ for 60 and 90 min for wax with H 3 BO 3 and wax with B 4 C, respectively. Two simple methods of separation based on alkali extraction and melting wax in alkali were also developed exclusively for wax with H 3 BO 3 . In all the separations, the recovery of B was above 98%. During IC separation, B was separated as boron-mannitol anion complex. Linear calibration was obtained between 0.1 and 50 ppm of B, and LOD was calculated as 5 ppb (S/N=3). The reproducibility was better than 5% (RSD)

  20. A Method for Modeling the Virtual Instrument Automatic Test System Based on the Petri Net

    Institute of Scientific and Technical Information of China (English)

    MA Min; CHEN Guang-ju

    2005-01-01

    Virtual instrument is playing the important role in automatic test system. This paper introduces a composition of a virtual instrument automatic test system and takes the VXIbus based a test software platform which is developed by CAT lab of the UESTC as an example. Then a method to model this system based on Petri net is proposed. Through this method, we can analyze the test task scheduling to prevent the deadlock or resources conflict. At last, this paper analyzes the feasibility of this method.

  1. Gas chromatography

    International Nuclear Information System (INIS)

    Cram, S.P.; Risby, T.H.; Field, L.R.; Yu, W.L.

    1980-01-01

    In addition to the published literature for the years 1978 - 79, this review of developments in the field of gas chromatography includes earlier articles of particular significance appearing in foreign journals and the patent literature which was not available at the time of the previous review. The articles cited were selected as presenting the most fundamental developments in theory, methodology, and instrumentation. Some applications are cited if they reflect an advance in the state-of-the-art or have particular relevance to new developments. 1149 references are cited

  2. Effect of kinetic properties of extraction systems on separation of some elements by liquid chromatography method with free fixed phase

    International Nuclear Information System (INIS)

    Fedotov, P.S.; Maryutina, T.A.; Pichugin, A.A.; Spivakov, B.Ya.

    1993-01-01

    Effect of kinetic properties of a series of extraction systems on the separation of certain elements by the method of liquid chromatography with free fixed phase is considered. Chromatographic behaviour of europium 3 and iron 3 ions when using systems based on di-2-ethylhexylphosphovers acid and tetraphenylmethylenediphosphine dioxide is investigated. Kinetic properties of the extraction systems used are studied by diffusion cell method with mixing, europium 3 and iron 3 mass transfer coefficients are determined

  3. Sensitive method for the analysis of carbohydrates by gas chromatography of 3H-labeled alditol acetates

    International Nuclear Information System (INIS)

    Prehm, P.; Scheid, A.

    1978-01-01

    A highly sensitive method has been developed for the analysis of carbohydrates from glycoproteins or lipopolysaccharides. The method is based on labeling the carbohydrates with [ 3 H] sodium borohydride, acetylating the resulting alditols and separating them by gas chromatography. The gas effluent is fractionated by trapping on silicone-coated glass beads and the amount of radioactivity is determined. This permits the quantitation of as little as 0.2 nmoles monosaccharide with an accuracy of 10 to 15%. (Auth)

  4. 30 CFR 75.1719-3 - Methods of measurement; light measuring instruments.

    Science.gov (United States)

    2010-07-01

    ... being measured and a sufficient distance from the surface to allow the light sensing element in the... 30 Mineral Resources 1 2010-07-01 2010-07-01 false Methods of measurement; light measuring... § 75.1719-3 Methods of measurement; light measuring instruments. (a) Compliance with § 75.1719-1(d...

  5. Method of case hardening depth testing by using multifunctional ultrasonic testing instrument

    International Nuclear Information System (INIS)

    Salchak, Y A; Sednev, D A; Ardashkin, I B; Kroening, M

    2015-01-01

    The paper describes usability of ultrasonic case hardening depth control applying standard instrument of ultrasonic inspections. The ultrasonic method of measuring the depth of the hardened layer is proposed. Experimental series within the specified and multifunctional ultrasonic equipment are performed. The obtained results are compared with the results of a referent method of analysis. (paper)

  6. Comparison of the BioRad Variant and Primus Ultra2 high-pressure liquid chromatography (HPLC) instruments for the detection of variant hemoglobins.

    Science.gov (United States)

    Gosselin, R C; Carlin, A C; Dwyre, D M

    2011-04-01

    Hemoglobin variants are a result of genetic changes resulting in abnormal or dys-synchronous hemoglobin chain production (thalassemia) or the generation of hemoglobin chain variants such as hemoglobin S. Automated high-pressure liquid chromatography (HPLC) systems have become the method of choice for the evaluation of patients suspected with hemoglobinopathies. In this study, we evaluated the performance of two HPLC methods used in the detection of common hemoglobin variants: Variant and Ultra2. There were 377 samples tested, 26% (99/377) with HbS, 8.5% (32/377) with HbC, 20.7% (78/377) with other hemoglobin variant or thalassemia, and 2.9% with increased hemoglobin A(1) c. The interpretations of each chromatograph were compared. There were no differences noted for hemoglobins A(0), S, or C. There were significant differences between HPLC methods for hemoglobins F, A(2), and A(1) c. However, there was good concordance between normal and abnormal interpretations (97.9% and 96.2%, respectively). Both Variant and Ultra2 HPLC methods were able to detect most common hemoglobin variants. There was better discrimination for fast hemoglobins, between hemoglobins E and A(2), and between hemoglobins S and F using the Ultra2 HPLC method. © 2010 Blackwell Publishing Ltd.

  7. High-performance liquid chromatography electrospray mass spectrometry as a method in proteomic research

    International Nuclear Information System (INIS)

    Walcher, W.

    2003-06-01

    During the sequencing of the human genome it became clear, that a lot of human diseases and/or malfunctions don't base on genomic information, but on differences at the protein level. Therefore biochemistry, biology and medicine are faced to various novel problems where new and authentic analysis methods are needed. Miniaturized chromatographic separation methods are frequently the methods of choice for the separation of peptides and proteins, when the amount of sample is limited. Monolithic capillary columns were prepared by copolymerization of styrene and divinylbenzene in the presence of a suitable porogen mixture of 1-decanol and tetrahydrofuran. The synthesized columns enabled the highly efficient separation of peptides and proteins by reversed-phase high-performance liquid chromatography (RP-HPLC) with peak capacities of 80 and more in 10 minutes. By the hyphenation of RP-HPLC to electrospray mass spectrometry (ESI-MS) the potential of the analysis method was even extended. The monolithic column technology was further miniaturized from 200 μm to 100 and 50 μm inner diameters to improve detection limits by RP-HPLC-ESI-MS. After the optimization of the RP-HPLC-ESI-MS method, the ion source and the ion transfer optics of an ion trap mass spectrometer (LCQ classic, Thermofinnigan) have been advanced for protein and peptide analysis. The improved RP-HPLC-ESI-MS system was subsequently applied to the detection of posttranslational protein modifications at the example of the nitration of bovine serum albumin (BSA). The results of the RP-HPLC-ESI-MS analysis were found to be highly reproducible, which enabled the determination of nitration degrees for different tyrosine residues in the protein sequence. Y 1 60, Y 4 96 and Y 3 52 or Y369 were found to be the predominant positions of protein nitration in BSA. At last light harvesting proteins from the photosystem II (PSII) of higher plants have been analyzed by RP-HPLC-ESI-MS and RP-HPLC-ESI-MSMS. Beside the

  8. Instrumental analysis

    International Nuclear Information System (INIS)

    Jae, Myeong Gi; Lee, Won Seong; Kim, Ha Hyeok

    1989-02-01

    This book give description of electronic engineering such as circuit element and device, circuit analysis and logic digital circuit, the method of electrochemistry like conductometry, potentiometry and current measuring, spectro chemical analysis with electromagnetic radiant rays, optical components, absorption spectroscopy, X-ray analysis, atomic absorption spectrometry and reference, chromatography like gas-chromatography and liquid-chromatography and automated analysis on control system evaluation of automated analysis and automated analysis system and reference.

  9. Instrumental analysis

    Energy Technology Data Exchange (ETDEWEB)

    Jae, Myeong Gi; Lee, Won Seong; Kim, Ha Hyeok

    1989-02-15

    This book give description of electronic engineering such as circuit element and device, circuit analysis and logic digital circuit, the method of electrochemistry like conductometry, potentiometry and current measuring, spectro chemical analysis with electromagnetic radiant rays, optical components, absorption spectroscopy, X-ray analysis, atomic absorption spectrometry and reference, chromatography like gas-chromatography and liquid-chromatography and automated analysis on control system evaluation of automated analysis and automated analysis system and reference.

  10. Method developments approaches in supercritical fluid chromatography applied to the analysis of cosmetics.

    Science.gov (United States)

    Lesellier, E; Mith, D; Dubrulle, I

    2015-12-04

    Analyses of complex samples of cosmetics, such as creams or lotions, are generally achieved by HPLC. These analyses are often multistep gradients, due to the presence of compounds with a large range of polarity. For instance, the bioactive compounds may be polar, while the matrix contains lipid components that are rather non-polar, thus cosmetic formulations are usually oil-water emulsions. Supercritical fluid chromatography (SFC) uses mobile phases composed of carbon dioxide and organic co-solvents, allowing for good solubility of both the active compounds and the matrix excipients. Moreover, the classical and well-known properties of these mobile phases yield fast analyses and ensure rapid method development. However, due to the large number of stationary phases available for SFC and to the varied additional parameters acting both on retention and separation factors (co-solvent nature and percentage, temperature, backpressure, flow rate, column dimensions and particle size), a simplified approach can be followed to ensure a fast method development. First, suited stationary phases should be carefully selected for an initial screening, and then the other operating parameters can be limited to the co-solvent nature and percentage, maintaining the oven temperature and back-pressure constant. To describe simple method development guidelines in SFC, three sample applications are discussed in this paper: UV-filters (sunscreens) in sunscreen cream, glyceryl caprylate in eye liner and caffeine in eye serum. Firstly, five stationary phases (ACQUITY UPC(2)) are screened with isocratic elution conditions (10% methanol in carbon dioxide). Complementary of the stationary phases is assessed based on our spider diagram classification which compares a large number of stationary phases based on five molecular interactions. Secondly, the one or two best stationary phases are retained for further optimization of mobile phase composition, with isocratic elution conditions or, when

  11. Determination of 2-naphthylamine in urine by a novel reversed-phase high-performance liquid chromatography method

    DEFF Research Database (Denmark)

    Hansen, Åse Marie; Poulsen, O M; Christensen, J M

    1992-01-01

    A high-performance liquid chromatographic method for the determination of 2-naphthylamine in urine using fluorescence detection was developed. The method validation analysis showed the method to be in analytical control, i.e. the distribution of the difference between the observed and true values...... of the method evaluation samples did not deviate significantly from the normal distribution. The recovery of the method was 85%. The entire run time of chromatography was 10 min using isocratic elution (acetonitrile-water, 35:65), and the retention time for 2-naphthylamine was 5.8 min. The relative short time...

  12. Application of high-performance liquid chromatography-tandem mass spectrometry with a quadrupole/linear ion trap instrument for the analysis of pesticide residues in olive oil.

    Science.gov (United States)

    Hernando, M D; Ferrer, C; Ulaszewska, M; García-Reyes, J F; Molina-Díaz, A; Fernández-Alba, A R

    2007-11-01

    This article describes the development of an enhanced liquid chromatography-mass spectrometry (LC-MS) method for the analysis of pesticides in olive oil. One hundred pesticides belonging to different classes and that are currently used in agriculture have been included in this method. The LC-MS method was developed using a hybrid quadrupole/linear ion trap (QqQ(LIT)) analyzer. Key features of this technique are the rapid scan acquisition times, high specificity and high sensitivity it enables when the multiple reaction monitoring (MRM) mode or the linear ion-trap operational mode is employed. The application of 5 ms dwell times using a linearly accelerating (LINAC) high-pressure collision cell enabled the analysis of a high number of pesticides, with enough data points acquired for optimal peak definition in MRM operation mode and for satisfactory quantitative determinations to be made. The method quantifies over a linear dynamic range of LOQs (0.03-10 microg kg(-1)) up to 500 microg kg(-1). Matrix effects were evaluated by comparing the slopes of matrix-matched and solvent-based calibration curves. Weak suppression or enhancement of signals was observed (ion (EPI) and MS3 were developed.

  13. Validating a High Performance Liquid Chromatography-Ion Chromatography (HPLC-IC) Method with Conductivity Detection After Chemical Suppression for Water Fluoride Estimation.

    Science.gov (United States)

    Bondu, Joseph Dian; Selvakumar, R; Fleming, Jude Joseph

    2018-01-01

    A variety of methods, including the Ion Selective Electrode (ISE), have been used for estimation of fluoride levels in drinking water. But as these methods suffer many drawbacks, the newer method of IC has replaced many of these methods. The study aimed at (1) validating IC for estimation of fluoride levels in drinking water and (2) to assess drinking water fluoride levels of villages in and around Vellore district using IC. Forty nine paired drinking water samples were measured using ISE and IC method (Metrohm). Water samples from 165 randomly selected villages in and around Vellore district were collected for fluoride estimation over 1 year. Standardization of IC method showed good within run precision, linearity and coefficient of variance with correlation coefficient R 2  = 0.998. The limit of detection was 0.027 ppm and limit of quantification was 0.083 ppm. Among 165 villages, 46.1% of the villages recorded water fluoride levels >1.00 ppm from which 19.4% had levels ranging from 1 to 1.5 ppm, 10.9% had recorded levels 1.5-2 ppm and about 12.7% had levels of 2.0-3.0 ppm. Three percent of villages had more than 3.0 ppm fluoride in the water tested. Most (44.42%) of these villages belonged to Jolarpet taluk with moderate to high (0.86-3.56 ppm) water fluoride levels. Ion Chromatography method has been validated and is therefore a reliable method in assessment of fluoride levels in the drinking water. While the residents of Jolarpet taluk (Vellore distict) are found to be at a high risk of developing dental and skeletal fluorosis.

  14. Instrumental analysis

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Seung Jae; Seo, Seong Gyu

    1995-03-15

    This textbook deals with instrumental analysis, which consists of nine chapters. It has Introduction of analysis chemistry, the process of analysis and types and form of the analysis, Electrochemistry on basic theory, potentiometry and conductometry, electromagnetic radiant rays and optical components on introduction and application, Ultraviolet rays and Visible spectrophotometry, Atomic absorption spectrophotometry on introduction, flame emission spectrometry and plasma emission spectrometry. The others like infrared spectrophotometry, X-rays spectrophotometry and mass spectrometry, chromatography and the other instrumental analysis like radiochemistry.

  15. Instrumental analysis

    International Nuclear Information System (INIS)

    Kim, Seung Jae; Seo, Seong Gyu

    1995-03-01

    This textbook deals with instrumental analysis, which consists of nine chapters. It has Introduction of analysis chemistry, the process of analysis and types and form of the analysis, Electrochemistry on basic theory, potentiometry and conductometry, electromagnetic radiant rays and optical components on introduction and application, Ultraviolet rays and Visible spectrophotometry, Atomic absorption spectrophotometry on introduction, flame emission spectrometry and plasma emission spectrometry. The others like infrared spectrophotometry, X-rays spectrophotometry and mass spectrometry, chromatography and the other instrumental analysis like radiochemistry.

  16. A Simple Thin Layer Chromatography Method for Separation of Selected Natural Steroid Hormones

    International Nuclear Information System (INIS)

    Nowakowska, J.; Rudnicka-Litka, K.; Ciura, K.; Pikul, P.; Piotrowicz, J.

    2015-01-01

    Chromatographic properties of seven steroids: estrogens (β-estradiol and estrone), androgens (testosterone, methyltestosterone, trans-androsterone), progesterone and cholesterol have been studied by planar chromatography with usage of High Performance Thin Layer Chromatography (HPTLC) and Thin Layer Chromatography (TLC) plates. Normal, reversed and cyano-bonded silica stationary phases were tested with five binary mobile phases (acetonitrile-water, acetonitrile-DMSO, acetonitrile-methanol, acetone-petroleum ether, acetone-water) in which the concentration of organic modifier varied from 0 to 100 % (v/v). This study reports the optimization of steroid hormones separation. Principal Component Analysis (PCA) based on calculated molecular descriptors quantitatively differentiating solutes was performed in order to investigate the similarity and dissimilarity between tested compounds. The separation abilities of mobile and stationary phases were compared based on separation factor α. Chromatographic retention data and possible retention mechanisms also were discussed. (author)

  17. Method development and validation for the determination of pesticides in green coffee by gas chromatography

    International Nuclear Information System (INIS)

    Dallos Corredor, David; Guerrero Dallos, Jairo Arturo

    2005-01-01

    This study describes the implementation and validation of a multiresidue methodology for the determination of organochlorine, organophosphorus and pyrethroids pesticides in green coffee. Pesticides residues were extracted from green samples with an acetone-water (2:1) mixture followed by ethyl acetate cyclohexane (1:1) partitioning. The clean up steps include gel permeation chromatography and mini column chromatography using silica gel. Final determination was carried out by high-resolution gas chromatography with a pulsed split less injection mode and simultaneous detection by μ-ECD and NPD coupled in parallel. The methodology is specific, selective precise and accurate. Recoveries of majority of pesticides from spiked samples range from 70 to 110% at fortification levels of 0.038 mg/kg-1.536 mg/kg with limit of quantitation between 0.011 mg/kg and 0.100 mg/kg

  18. Calibration method based on direct radioactivity measurement for radioactive gas monitoring instruments

    International Nuclear Information System (INIS)

    Yoshida, Makoto; Ohi, Yoshihiro; Chida, Tohru; Wu, Youyang.

    1993-01-01

    A calibration method for radioactive gas monitoring instruments was studied. In the method, gaseous radioactivity standards were provided on the basis of the direct radioactivity measurement by the diffusion-in long proportional counter method (DLPC method). The radioactivity concentration of the gas mixture through a monitoring instrument was determined by sampling the known volume of the gas mixture into the proportional counter used for the DLPC method. Since oxygen in the gas mixture decreased the counting efficiency in a proportional counter, the influence on calibration was experimentally estimated. It was not serious and able to be easily corrected. By the present method, the relation between radioactivity concentration and ionization current was determined for a gas-flow ionization chamber with 1.5 l effective volume. It showed good agreement with the results in other works. (author)

  19. Pre-validation methods for developing a patient reported outcome instrument

    Directory of Open Access Journals (Sweden)

    Castillo Mayret M

    2011-08-01

    Full Text Available Abstract Background Measures that reflect patients' assessment of their health are of increasing importance as outcome measures in randomised controlled trials. The methodological approach used in the pre-validation development of new instruments (item generation, item reduction and question formatting should be robust and transparent. The totality of the content of existing PRO instruments for a specific condition provides a valuable resource (pool of items that can be utilised to develop new instruments. Such 'top down' approaches are common, but the explicit pre-validation methods are often poorly reported. This paper presents a systematic and generalisable 5-step pre-validation PRO instrument methodology. Methods The method is illustrated using the example of the Aberdeen Glaucoma Questionnaire (AGQ. The five steps are: 1 Generation of a pool of items; 2 Item de-duplication (three phases; 3 Item reduction (two phases; 4 Assessment of the remaining items' content coverage against a pre-existing theoretical framework appropriate to the objectives of the instrument and the target population (e.g. ICF; and 5 qualitative exploration of the target populations' views of the new instrument and the items it contains. Results The AGQ 'item pool' contained 725 items. Three de-duplication phases resulted in reduction of 91, 225 and 48 items respectively. The item reduction phases discarded 70 items and 208 items respectively. The draft AGQ contained 83 items with good content coverage. The qualitative exploration ('think aloud' study resulted in removal of a further 15 items and refinement to the wording of others. The resultant draft AGQ contained 68 items. Conclusions This study presents a novel methodology for developing a PRO instrument, based on three sources: literature reporting what is important to patient; theoretically coherent framework; and patients' experience of completing the instrument. By systematically accounting for all items dropped

  20. Comparison of extraction chromatography and a procedure based on the molecular recognition method as separation methods in the determination of neptunium and plutonium radionuclides

    International Nuclear Information System (INIS)

    Strisovska, Jana; Galanda, Dusan; Drabova, Veronika; Kuruc, Jozef

    2012-01-01

    The potential of various types of sorbents for separation of radionuclides of plutonium and neptunium were examined. Extraction chromatography and a procedure based on the molecular recognition method were used for the separation. The suitability of the various sorbent types and brands for this purpose was determined. (orig.)

  1. A simple, sensitive and rapid isocratic reversed-phase high-performance liquid chromatography method for determination and stability study of curcumin in pharmaceutical samples

    Science.gov (United States)

    Amanolahi, Farjad; Mohammadi, Ali; Kazemi Oskuee, Reza; Nassirli, Hooriyeh; Malaekeh-Nikouei, Bizhan

    2017-01-01

    Objective: This study was designed to develop and validate a new reversed-phase high-performance liquid chromatography (RP-HPLC) method based on Q2 (R1) International Conference on Harmonization (ICH) guideline for determination of curcumin in pharmaceutical samples. Materials and Methods: The HPLC instrument method was optimized with isocratic elution with acetonitrile: ammonium acetate (45:55, v/v, pH 3.5), C18 column (150 mm×4.6 mm×5 µm particle size) and a flow rate of 1 ml/min in ambient condition and total retention time of 17 min. The volume of injection was set at 20 µl and detection was recorded at 425 nm. The robustness of the method was examined by changing the mobile phase composition, mobile phase pH, and flow rate. Results: The method was validated with respect to precision, accuracy and linearity in a concentration range of 2-100 µg/ml. The limit of detection (LOD) and limit of quantification (LOQ) were 0.25 and 0.5 µg/ml, respectively. The percentage of recovery was 98.9 to 100.5 with relative standard deviation (RSD) < 0.638%. Conclusion: The method was found to be simple, sensitive and rapid for determination of curcumin in pharmaceutical samples and had enough sensitivity to detect degradation product of curcumin produced under photolysis and hydrolysis stress condition. PMID:29062806

  2. A new method for the radiation representation of musical instruments in auralizations

    DEFF Research Database (Denmark)

    Rindel, Jens Holger; Otondo, Felipe

    2005-01-01

    A new method for the representation of sound sources that vary their directivity in time in auralizations is introduced. A recording method with multi-channel anechoic recordings is proposed in connection with the use of a multiple virtual source reproduction system in auralizations. Listening ex...... to be significant. Further applications of the method are considered for ensembles within room auralizations as well as in the field of studio recording techniques for large instruments....

  3. A fast, comprehensive screening method for doping agents in urine by gas chromatography-triple quadrupole mass spectrometry.

    Science.gov (United States)

    Van Eenoo, Peter; Van Gansbeke, Wim; De Brabanter, Nik; Deventer, Koen; Delbeke, Frans T

    2011-05-27

    The use of performance enhancing drugs in sports is prohibited. For the detection of misuse of such substances gas chromatography or liquid chromatography coupled to mass spectrometry are the most frequently used detection techniques. In this work the development and validation of a fast gas chromatography tandem mass spectrometric method for the detection of a wide range of doping agents is described. The method can determine 13 endogenous steroids (the steroid profile), 19-norandrosterone, salbutamol and 11-nor-Δ9-tetrahydrocannabinol.9carboxylic acid in the applicable ranges and to detect qualitatively over 140 substances in accordance with the minimum required performance levels of the World Anti-Doping Agency in 1ml of urine. The classes of substances included in the method are anabolic steroids, β2-agonists, stimulants, narcotics, hormone antagonists and modulators and beta-blockers. Moreover, using a short capillary column and hydrogen as a carrier gas the run time of the method is less than 8min. Copyright © 2010 Elsevier B.V. All rights reserved.

  4. FJ-2207 measuring instrument detection pipe surface a level of pollution method

    International Nuclear Information System (INIS)

    Wang Jiangong

    2010-01-01

    On the pipe surface contamination were detected α level of pollution is a frequently encountered dose-detection work. Because the pipeline surface arc, while the measuring probe for the plane, which for accurate measurement difficult. In this paper, on the FJ-2207-type pipe surface contamination measuring instrument measuring pollution levels in the α method was studied. Introduced the FJ-2207 measuring instrument detection pipe surface α pollution levels. Studied this measuring instrument on the same sources of surface, plane α level of radioactivity measured differences in the results obtained control of the apparatus when the direct measurement of the surface correction factor, and gives 32-216 specifications commonly used pipe direct measurement of the amendment factor. Convenient method, test results are reliable for the accurate measurement of pipe pollution levels in the surface of α as a reference and learning. (authors)

  5. USAGE OF PICTOGRAMS TO INTRODUCE MUSICAL INSTRUMENTS TO EDUCABLE MENTALLY RETARDED CHILDREN AS AN ALTERNATIVE METHOD

    Directory of Open Access Journals (Sweden)

    Gunsu YILMA

    2014-01-01

    Full Text Available The purpose of this research is to examine and investigate the perception ability of musical instruments of educable mentally retarded children with the support of visual elements. The research is conducted for every children individually in a special education and rehabilitation centre. The problematic of this research is the level of perception ability of musical instruments with visual support on mild mentally retarded children. In this research, perception ability of defining pictograms by music is introduced as an alternative method. It is researched that how educable mentally retarded children perceive pictograms by music tools. In this case, it is aimed to introduce musical instruments to educable mentally retarded children by pictograms with music. The research is applied with a qualitative approach. Data were obtained with the recorder, then they were turned into texts and analyzed with content analysis method.

  6. Cross validation of gas chromatography-flame photometric detection and gas chromatography-mass spectrometry methods for measuring dialkylphosphate metabolites of organophosphate pesticides in human urine.

    Science.gov (United States)

    Prapamontol, Tippawan; Sutan, Kunrunya; Laoyang, Sompong; Hongsibsong, Surat; Lee, Grace; Yano, Yukiko; Hunter, Ronald Elton; Ryan, P Barry; Barr, Dana Boyd; Panuwet, Parinya

    2014-01-01

    We report two analytical methods for the measurement of dialkylphosphate (DAP) metabolites of organophosphate pesticides in human urine. These methods were independently developed/modified and implemented in two separate laboratories and cross validated. The aim was to develop simple, cost effective, and reliable methods that could use available resources and sample matrices in Thailand and the United States. While several methods already exist, we found that direct application of these methods required modification of sample preparation and chromatographic conditions to render accurate, reliable data. The problems encountered with existing methods were attributable to urinary matrix interferences, and differences in the pH of urine samples and reagents used during the extraction and derivatization processes. Thus, we provide information on key parameters that require attention during method modification and execution that affect the ruggedness of the methods. The methods presented here employ gas chromatography (GC) coupled with either flame photometric detection (FPD) or electron impact ionization-mass spectrometry (EI-MS) with isotopic dilution quantification. The limits of detection were reported from 0.10ng/mL urine to 2.5ng/mL urine (for GC-FPD), while the limits of quantification were reported from 0.25ng/mL urine to 2.5ng/mL urine (for GC-MS), for all six common DAP metabolites (i.e., dimethylphosphate, dimethylthiophosphate, dimethyldithiophosphate, diethylphosphate, diethylthiophosphate, and diethyldithiophosphate). Each method showed a relative recovery range of 94-119% (for GC-FPD) and 92-103% (for GC-MS), and relative standard deviations (RSD) of less than 20%. Cross-validation was performed on the same set of urine samples (n=46) collected from pregnant women residing in the agricultural areas of northern Thailand. The results from split sample analysis from both laboratories agreed well for each metabolite, suggesting that each method can produce

  7. A new method for the assessment of the surface topography of NiTi rotary instruments.

    Science.gov (United States)

    Ferreira, F; Barbosa, I; Scelza, P; Russano, D; Neff, J; Montagnana, M; Zaccaro Scelza, M

    2017-09-01

    To describe a new method for the assessment of nanoscale alterations in the surface topography of nickel-titanium endodontic instruments using a high-resolution optical method and to verify the accuracy of the technique. Noncontact three-dimensional optical profilometry was used to evaluate defects on a size 25, .08 taper reciprocating instrument (WaveOne ® ), which was subjected to a cyclic fatigue test in a simulated root canal in a clear resin block. For the investigation, an original procedure was established for the analysis of similar areas located 3 mm from the tip of the instrument before and after canal preparation to enable the repeatability and reproducibility of the measurements with precision. All observations and analysis were taken in areas measuring 210 × 210 μm provided by the software of the equipment. The three-dimensional high-resolution image analysis showed clear alterations in the surface topography of the examined cutting blade and flute of the instrument, before and after use, with the presence of surface irregularities such as deformations, debris, grooves, cracks, steps and microcavities. Optical profilometry provided accurate qualitative nanoscale evaluation of similar surfaces before and after the fatigue test. The stability and repeatability of the technique enables a more comprehensive understanding of the effects of wear on the surface of endodontic instruments. © 2016 International Endodontic Journal. Published by John Wiley & Sons Ltd.

  8. Atmospheric pressure photoionisation : An ionization method for liquid chromatography-mass spectrometry

    NARCIS (Netherlands)

    Robb, DB; Covey, TR; Bruins, AP

    2000-01-01

    Atmospheric pressure photoionization (APPI) has been successfully demonstrated to provide high sensitivity to LC-MS analysis. A vacuum-ultraviolet lamp designed for photoionization detection in gas chromatography is used as a source of 10-eV photons. The mixture of samples and solvent eluting from

  9. Applying the Mixed Methods Instrument Development and Construct Validation Process: the Transformative Experience Questionnaire

    Science.gov (United States)

    Koskey, Kristin L. K.; Sondergeld, Toni A.; Stewart, Victoria C.; Pugh, Kevin J.

    2018-01-01

    Onwuegbuzie and colleagues proposed the Instrument Development and Construct Validation (IDCV) process as a mixed methods framework for creating and validating measures. Examples applying IDCV are lacking. We provide an illustrative case integrating the Rasch model and cognitive interviews applied to the development of the Transformative…

  10. Bayesian methods for meta-analysis of causal relationships estimated using genetic instrumental variables

    DEFF Research Database (Denmark)

    Burgess, Stephen; Thompson, Simon G; Thompson, Grahame

    2010-01-01

    Genetic markers can be used as instrumental variables, in an analogous way to randomization in a clinical trial, to estimate the causal relationship between a phenotype and an outcome variable. Our purpose is to extend the existing methods for such Mendelian randomization studies to the context o...

  11. Field astrobiology research instruments and methods in moon-mars analogue site.

    NARCIS (Netherlands)

    Foing, B.H.; Stoker, C.; Zavaleta, J.; Ehrenfreund, P.; Sarrazin, P.; Blake, D.; Page, J.; Pletser, V.; Hendrikse, J.; Oliveira Lebre Direito, M.S.; Kotler, M.; Martins, Z.; Orzechowska, G.; Thiel, C.S.; Clarke, J.; Gross, J.; Wendt, L.; Borst, A.; Peters, S.; Wilhelm, M.-B.; Davies, G.R.; EuroGeoMars 2009 Team, ILEWG

    2011-01-01

    We describe the field demonstration of astrobiology instruments and research methods conducted in and from the Mars Desert Research Station (MDRS) in Utah during the EuroGeoMars campaign 2009 coordinated by ILEWG, ESA/ESTEC and NASA Ames, with the contribution of academic partners. We discuss the

  12. New highly sensitive method of simultaneous instrumental neutron activation determination of 12 microelements in vine

    International Nuclear Information System (INIS)

    Shoniya, N.I.

    1977-01-01

    The main principles and methods of simultaneous multi-element instrumental neutron activation determination of microelements in vine seeds are presented. The methods permit to carry out quantitative evaluation for every single corn of the seeds. It is shown that the method of instrumental neutron activation analysis with the utilization of a semiconductor spectrometer of high resolution and mini electronic computer permit to carry out serial determinations of 12 microelements in the individual corns of vine seeds of different sorts. This method will permit to determine the missing or excess content of this or that biologically important microelement in soils, plants, fruit and genetic material - seeds, and so to determine the optimum conditions of growing plants by applying microelement fertilizers as extra nutrient means

  13. Design and operation of dust measuring instrumentation based on the beta-radiation method

    International Nuclear Information System (INIS)

    Lilienfeld, P.

    1975-01-01

    The theory, instrument design aspects and applications of beta-radiation attenuation for the measurement of the mass concentration of airborne particulates are reviewed. Applicable methods of particle collection, beta sensing configurations, source ( 63 Ni, 14 C, 147 Pr, 85 Kr) and detector design criteria, electronic signal processing, digital control and instrument programming techniques are treated. Advantages, limitations and error sources of beta-attenuation instrumentation are analyzed. Applications to industrial dust measurements, source testing, ambient monitoring, and particle size analysis are the major areas of practical utilization of this technique, and its inherent capability for automated and unattended operation provides compatibility with process control synchronization and alarm, telemetry, and incorporation into pollution monitoring network sensing stations. (orig.) [de

  14. Experimental innovations in surface science a guide to practical laboratory methods and instruments

    CERN Document Server

    Yates, John T

    2015-01-01

    This book is a new edition of a classic text on experimental methods and instruments in surface science. It offers practical insight useful to chemists, physicists, and materials scientists working in experimental surface science. This enlarged second edition contains almost 300 descriptions of experimental methods. The more than 50 active areas with individual scientific and measurement concepts and activities relevant to each area are presented in this book. The key areas covered are: Vacuum System Technology, Mechanical Fabrication Techniques, Measurement Methods, Thermal Control, Delivery of Adsorbates to Surfaces, UHV Windows, Surface Preparation Methods, High Area Solids, Safety. The book is written for researchers and graduate students.

  15. Rare earths analysis of rock samples by instrumental neutron activation analysis, internal standard method

    International Nuclear Information System (INIS)

    Silachyov, I.

    2016-01-01

    The application of instrumental neutron activation analysis for the determination of long-lived rare earth elements (REE) in rock samples is considered in this work. Two different methods are statistically compared: the well established external standard method carried out using standard reference materials, and the internal standard method (ISM), using Fe, determined through X-ray fluorescence analysis, as an element-comparator. The ISM proved to be the more precise method for a wide range of REE contents and can be recommended for routine practice. (author)

  16. Simultaneous separation of antihyperlipidemic drugs by green ultrahigh-performance liquid chromatography-diode array detector method: Improving the health of liquid chromatography.

    Science.gov (United States)

    Alghazi, Mansoor; Alanazi, Fars; Mohsin, Kazi; Siddiqui, Nasir Ali; Shakeel, Faiyaz; Haq, Nazrul

    2017-04-01

    Statins in combination with fibrates show beneficial effects on the lipoprotein profile of patients because they have positive complimentary effects on lipid profile. A new green ultrahigh-performance liquid chromatography-diode array detector method for simultaneous analysis of simvastatin (SMV) and fenofibrate (FNF) in standard form, marketed formulations, and self-emulsifying drug delivery system formulations was developed and validated in the present investigation. The method utilized C 18 as stationary phase and a combination of methanol:water (8:2) as an eluent. It was found that selected eluent provided short run time (2.5 minutes), better peak symmetry and satisfactory values of other chromatographic parameters such as resolution (Rs=2.325), capacity factor (k, 3.0 and 4.2 for SMV and FNF, respectively), selectivity (α =1.4), and number of theoretical plates (N, 4265 and 5285 for SMV and FNF, respectively). An excellent linear relationship (r 2 0.998 and 0.997 for SMV and FNF, respectively) was observed for linear regression data for the calibration plots. The developed system was validated for accuracy, precision, robustness (˃ 2% for both drugs) and recovery (98-102% for both drugs). Results obtained from the statistical treatment of the values obtained for different parameters proved that the method is suitable, reproducible, and selective for the simultaneous analysis of SMV and FNF in bulk, marketed, and self-emulsifying drug delivery system formulations. The replacement of commonly applied toxic solvents with innocuous and environmentally benign solvents provides a better option than the more toxic processes in drug analysis. Copyright © 2016. Published by Elsevier B.V.

  17. Determine equilibrium dissociation constant of drug-membrane receptor affinity using the cell membrane chromatography relative standard method.

    Science.gov (United States)

    Ma, Weina; Yang, Liu; Lv, Yanni; Fu, Jia; Zhang, Yanmin; He, Langchong

    2017-06-23

    The equilibrium dissociation constant (K D ) of drug-membrane receptor affinity is the basic parameter that reflects the strength of interaction. The cell membrane chromatography (CMC) method is an effective technique to study the characteristics of drug-membrane receptor affinity. In this study, the K D value of CMC relative standard method for the determination of drug-membrane receptor affinity was established to analyze the relative K D values of drugs binding to the membrane receptors (Epidermal growth factor receptor and angiotensin II receptor). The K D values obtained by the CMC relative standard method had a strong correlation with those obtained by the frontal analysis method. Additionally, the K D values obtained by CMC relative standard method correlated with pharmacological activity of the drug being evaluated. The CMC relative standard method is a convenient and effective method to evaluate drug-membrane receptor affinity. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Evaluation of two disinfection/sterilization methods on silicon rubber-based composite finishing instruments.

    Science.gov (United States)

    Lacerda, Vánia A; Pereira, Leandro O; Hirata JUNIOR, Raphael; Perez, Cesar R

    2015-12-01

    To evaluate the effectiveness of disinfection/sterilization methods and their effects on polishing capacity, micomorphology, and composition of two different composite fiishing and polishing instruments. Two brands of finishing and polishing instruments (Jiffy and Optimize), were analyzed. For the antimicrobial test, 60 points (30 of each brand) were used for polishing composite restorations and submitted to three different groups of disinfection/sterilization methods: none (control), autoclaving, and immersion in peracetic acid for 60 minutes. The in vitro tests were performed to evaluate the polishing performance on resin composite disks (Amelogen) using a 3D scanner (Talyscan) and to evaluate the effects on the points' surface composition (XRF) and micromorphology (MEV) after completing a polishing and sterilizing routine five times. Both sterilization/disinfection methods were efficient against oral cultivable organisms and no deleterious modification was observed to point surface.

  19. An ergonomics based design research method for the arrangement of helicopter flight instrument panels.

    Science.gov (United States)

    Alppay, Cem; Bayazit, Nigan

    2015-11-01

    In this paper, we study the arrangement of displays in flight instrument panels of multi-purpose civil helicopters following a user-centered design method based on ergonomics principles. Our methodology can also be described as a user-interface arrangement methodology based on user opinions and preferences. This study can be outlined as gathering user-centered data using two different research methods and then analyzing and integrating the collected data to come up with an optimal instrument panel design. An interview with helicopter pilots formed the first step of our research. In that interview, pilots were asked to provide a quantitative evaluation of basic interface arrangement principles. In the second phase of the research, a paper prototyping study was conducted with same pilots. The final phase of the study entailed synthesizing the findings from interviews and observational studies to formulate an optimal flight instrument arrangement methodology. The primary results that we present in our paper are the methodology that we developed and three new interface arrangement concepts, namely relationship of inseparability, integrated value and locational value. An optimum instrument panel arrangement is also proposed by the researchers. Copyright © 2015 Elsevier Ltd and The Ergonomics Society. All rights reserved.

  20. High-performance liquid chromatography analysis methods developed for quantifying enzymatic esterification of flavonoids in ionic liquids

    DEFF Research Database (Denmark)

    Lue, Bena-Marie; Guo, Zheng; Xu, X.B.

    2008-01-01

    Methods using reversed-phase high-performance liquid chromatography (RP-HPLC) with ELSD were investigated to quantify enzymatic reactions of flavonoids with fatty acids in the presence of diverse room temperature ionic liquids (RTILs). A buffered salt (preferably triethylamine-acetate) was found...... essential for separation of flavonoids from strongly polar RTILs, whereby RTILs were generally visible as two major peaks identified based on an ion-pairing/exchanging hypothesis. C8 and C12 stationary phases were optimal while mobile phase pH (3-7) had only a minor influence on separation. The method...

  1. Intercomparison of two comparative reactivity method instruments inf the Mediterranean basin during summer 2013

    Science.gov (United States)

    Zannoni, N.; Dusanter, S.; Gros, V.; Sarda Esteve, R.; Michoud, V.; Sinha, V.; Locoge, N.; Bonsang, B.

    2015-09-01

    The hydroxyl radical (OH) plays a key role in the atmosphere, as it initiates most of the oxidation processes of volatile organic compounds (VOCs), and can ultimately lead to the formation of ozone and secondary organic aerosols (SOAs). There are still uncertainties associated with the OH budget assessed using current models of atmospheric chemistry and direct measurements of OH sources and sinks have proved to be valuable tools to improve our understanding of the OH chemistry. The total first order loss rate of OH, or total OH reactivity, can be directly measured using three different methods, such as the following: total OH loss rate measurement, laser-induced pump and probe technique and comparative reactivity method. Observations of total OH reactivity are usually coupled to individual measurements of reactive compounds in the gas phase, which are used to calculate the OH reactivity. Studies using the three methods have highlighted that a significant fraction of OH reactivity is often not explained by individually measured reactive compounds and could be associated to unmeasured or unknown chemical species. Therefore accurate and reproducible measurements of OH reactivity are required. The comparative reactivity method (CRM) has demonstrated to be an advantageous technique with an extensive range of applications, and for this reason it has been adopted by several research groups since its development. However, this method also requires careful corrections to derive ambient OH reactivity. Herein we present an intercomparison exercise of two CRM instruments, CRM-LSCE (Laboratoire des Sciences du Climat et de l'Environnement) and CRM-MD (Mines Douai), conducted during July 2013 at the Mediterranean site of Ersa, Cape Corsica, France. The intercomparison exercise included tests to assess the corrections needed by the two instruments to process the raw data sets as well as OH reactivity observations. The observation was divided in three parts: 2 days of plant

  2. Development of a high performance liquid chromatography method and a liquid chromatography-tandem mass spectrometry method with pressurized liquid extraction for simultaneous quantification and confirmation of cyromazine, melamine and its metabolites in foods of animal origin

    International Nuclear Information System (INIS)

    Yu Huan; Tao Yanfei; Chen Dongmei; Wang Yulian; Liu Zhaoying; Pan Yuanhu; Huang Lingli; Peng Dapeng; Dai Menghong; Liu Zhenli; Yuan Zonghui

    2010-01-01

    Simple and sensitive methods have been developed for simultaneous detection of cyromazine, melamine and their metabolites (ammeline, ammelide and cyanuric acid) in samples of animal origins. These include a high performance liquid chromatography (HPLC) method and a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method and are useful in regular monitoring and in toxicity studies of these molecules. Representative samples used in this study include muscles and livers of swine, bovine, sheep and chicken, kidneys of swine, bovine and sheep, and milk powder. A new sample preparation procedure with pressurized liquid extraction (PLE) at 1400 psi and 70 deg. C was investigated. Quantification of these five compounds by HPLC was achieved using an APS-2 column with UV detection at 230 nm. Limit of detection (LOD) was at 10 μg kg -1 , and limit of quantification (LOQ) was at 40 μg kg -1 . Recoveries of the five analytes in spiked samples ranged from 72.2% to 115.4% with RSD less than 12%. Confirmatory analysis of the analytes was performed using LC-MS/MS in selected reaction monitoring (SRM) mode. The LOD and LOQ were 5 μg kg -1 and 15 μg kg -1 , respectively. This is the first simultaneous analysis of cyromazine, melamine, ammeline, ammelide and cyanuric acid residues in complex tissue samples using PLE and HPLC. It is expected that these methods will find many practical applications in evaluating the safety of cyromazine, melamine and their metabolites.

  3. Compound-Specific Chlorine Isotope Analysis of Tetrachloromethane and Trichloromethane by Gas Chromatography-Isotope Ratio Mass Spectrometry vs Gas Chromatography-Quadrupole Mass Spectrometry: Method Development and Evaluation of Precision and Trueness.

    Science.gov (United States)

    Heckel, Benjamin; Rodríguez-Fernández, Diana; Torrentó, Clara; Meyer, Armin; Palau, Jordi; Domènech, Cristina; Rosell, Mònica; Soler, Albert; Hunkeler, Daniel; Elsner, Martin

    2017-03-21

    Compound-specific chlorine isotope analysis of tetrachloromethane (CCl 4 ) and trichloromethane (CHCl 3 ) was explored by both, gas chromatography-isotope ratio mass spectrometry (GC-IRMS) and GC-quadrupole MS (GC-qMS), where GC-qMS was validated in an interlaboratory comparison between Munich and Neuchâtel with the same type of commercial GC-qMS instrument. GC-IRMS measurements analyzed CCl isotopologue ions, whereas GC-qMS analyzed the isotopologue ions CCl 3 , CCl 2 , CCl (of CCl 4 ) and CHCl 3 , CHCl 2 , CHCl (of CHCl 3 ), respectively. Lowest amount dependence (good linearity) was obtained (i) in H-containing fragment ions where interference of 35 Cl- to 37 Cl-containing ions was avoided; (ii) with tuning parameters favoring one predominant rather than multiple fragment ions in the mass spectra. Optimized GC-qMS parameters (dwell time 70 ms, 2 most abundant ions) resulted in standard deviations of 0.2‰ (CHCl 3 ) and 0.4‰ (CCl 4 ), which are only about twice as large as 0.1‰ and 0.2‰ for GC-IRMS. To compare also the trueness of both methods and laboratories, samples from CCl 4 and CHCl 3 degradation experiments were analyzed and calibrated against isotopically different reference standards for both CCl 4 and CHCl 3 (two of each). Excellent agreement confirms that true results can be obtained by both methods provided that a consistent set of isotopically characterized reference materials is used.

  4. A multi-criteria evaluation method for climate change mitigation policy instruments

    International Nuclear Information System (INIS)

    Konidari, Popi; Mavrakis, Dimitrios

    2007-01-01

    This paper presents an integrated multi-criteria analysis method for the quantitative evaluation of climate change mitigation policy instruments. The method consists of: (i) a set of criteria supported by sub-criteria, all of which describe the complex framework under which these instruments are selected by policy makers and implemented, (ii) an Analytical Hierarchy Process (AHP) process for defining weight coefficients for criteria and sub-criteria according to the preferences of three stakeholders groups and (iii) a Multi-Attribute Theory (MAUT)/Simple Multi-Attribute Ranking Technique (SMART) process for assigning grades to each instrument that is evaluated for its performance under a specific sub-criterion. Arguments for the selected combination of these standard methods and definitions for criteria/sub-criteria are quoted. Consistency and robustness tests are performed. The functionality of the proposed method is tested by assessing the aggregate performances of the EU emission trading scheme at Denmark, Germany, Greece, Italy, Netherlands, Portugal, Sweden and United Kingdom. Conclusions are discussed

  5. Sparse feature learning for instrument identification: Effects of sampling and pooling methods.

    Science.gov (United States)

    Han, Yoonchang; Lee, Subin; Nam, Juhan; Lee, Kyogu

    2016-05-01

    Feature learning for music applications has recently received considerable attention from many researchers. This paper reports on the sparse feature learning algorithm for musical instrument identification, and in particular, focuses on the effects of the frame sampling techniques for dictionary learning and the pooling methods for feature aggregation. To this end, two frame sampling techniques are examined that are fixed and proportional random sampling. Furthermore, the effect of using onset frame was analyzed for both of proposed sampling methods. Regarding summarization of the feature activation, a standard deviation pooling method is used and compared with the commonly used max- and average-pooling techniques. Using more than 47 000 recordings of 24 instruments from various performers, playing styles, and dynamics, a number of tuning parameters are experimented including the analysis frame size, the dictionary size, and the type of frequency scaling as well as the different sampling and pooling methods. The results show that the combination of proportional sampling and standard deviation pooling achieve the best overall performance of 95.62% while the optimal parameter set varies among the instrument classes.

  6. Ultra-high-pressure liquid chromatography tandem mass spectrometry method for the determination of 9 organophosphate flame retardants in water samples

    NARCIS (Netherlands)

    Lorenzo, M.; Campo, J.; Picó, Y.

    2016-01-01

    Few methods are available for comprehensive organophosphate flame retardants (PFRs) detection in water and wastewater. Gas chromatography has been employed previously, but this approach is less selective, not amenable for use with deuterated standards and can suffer unfavorable fragmentation.

  7. COMPUTER-ASSISTED HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT WITH APPLICATIONS TO THE ISOLATION AND ANALYSIS OF PHYTOPLANKTON PIGMENTS. (R826944)

    Science.gov (United States)

    We used chromatography modeling software to assist in HPLC method development, with the goalof enhancing separations through the exclusive use of gradient time and column temperature. Wesurveyed nine stationary phases for their utility in pigment purification and natur...

  8. METHOD 332.0: DETERMINATION OF PERCHLORATE IN DRINKING WATER BY ION CHROMATOGRAPHY WITH SUPPRESSED CONDUCTIVITY AND ELECTROSPRAY IONIZATION MASS SPECTROMETRY

    Science.gov (United States)

    This method is applicable to the identification and quantitation of perchlorate in raw and finished drinking waters. The approach used is ion chromatography with suppressed conductivity and electrospray ionization mass spectrometry (IC-ESI/MS)

  9. EPA Method 8321B (SW-846): Solvent-Extractable Nonvolatile Compounds by High Performance Liquid Chromatography-Thermospray-Mass Spectrometry (HPLC-TS-MS) or Ultraviolet (UV) Detection

    Science.gov (United States)

    Method 8321B describes procedures for preparation and analysis of solid, aqueous liquid, drinking water and wipe samples using high performance liquid chromatography and mass spectrometry for extractable non-volatile compounds.

  10. Validation parameters of instrumental method for determination of total bacterial count in milk

    Directory of Open Access Journals (Sweden)

    Nataša Mikulec

    2004-10-01

    Full Text Available The method of flow citometry as rapid, instrumental and routine microbiological method is used for determination of total bacterial count in milk. The results of flow citometry are expressed as individual bacterial cells count. Problems regarding the interpretation of the results of total bacterial count can be avoided by transformation of the results of flow citometry method onto the scale of reference method (HRN ISO 6610:2001.. The method of flow citometry, like any analitycal method, according to the HRN EN ISO/IEC 17025:2000 standard, requires validation and verification. This paper describes parameters of validation: accuracy, precision, specificity, range, robustness and measuring uncertainty for the method of flow citometry.

  11. Reference Proteome Extracts for Mass Spec Instrument Performance Validation and Method Development

    Science.gov (United States)

    Rosenblatt, Mike; Urh, Marjeta; Saveliev, Sergei

    2014-01-01

    Biological samples of high complexity are required to test protein mass spec sample preparation procedures and validate mass spec instrument performance. Total cell protein extracts provide the needed sample complexity. However, to be compatible with mass spec applications, such extracts should meet a number of design requirements: compatibility with LC/MS (free of detergents, etc.)high protein integrity (minimal level of protein degradation and non-biological PTMs)compatibility with common sample preparation methods such as proteolysis, PTM enrichment and mass-tag labelingLot-to-lot reproducibility Here we describe total protein extracts from yeast and human cells that meet the above criteria. Two extract formats have been developed: Intact protein extracts with primary use for sample preparation method development and optimizationPre-digested extracts (peptides) with primary use for instrument validation and performance monitoring

  12. Gas chromatography in space

    Science.gov (United States)

    Akapo, S. O.; Dimandja, J. M.; Kojiro, D. R.; Valentin, J. R.; Carle, G. C.

    1999-01-01

    Gas chromatography has proven to be a very useful analytical technique for in situ analysis of extraterrestrial environments as demonstrated by its successful operation on spacecraft missions to Mars and Venus. The technique is also one of the six scientific instruments aboard the Huygens probe to explore Titan's atmosphere and surface. A review of gas chromatography in previous space missions and some recent developments in the current environment of fiscal constraints and payload size limitations are presented.

  13. Method Development and Validation for the Determination of Caffeine: An Alkaloid from Coffea arabica by High-performance Liquid Chromatography Method.

    Science.gov (United States)

    Naveen, P; Lingaraju, H B; Deepak, M; Medhini, B; Prasad, K Shyam

    2018-01-01

    The present study was investigated to develop and validate a reversed phase high performance liquid chromatography method for the determination of caffeine from bean material of Coffee arabica. The separation was achieved on a reversed-phase C18 column using a mobile phase composed of water: methanol (50:50) at a flow rate of 1.0 mlmin-1. The detection was carried out on a UV detector at 272 nm. The developed method was validated according to the requirements for International Conference on Harmonisation (ICH) guidelines, which includes specificity, linearity, precision, accuracy, limit of detection and limit of quantitation. The developed method validates good linearity with excellent correlation coefficient (R2 > 0.999). In repeatability and intermediate precision, the percentage relative standard deviation (% RSD) of peak area was less than 1% shows high precision of the method. The recovery rate for caffeine was within 98.78% - 101.28% indicates high accuracy of the method. The low limit of detection and limit of quantitation of caffeine enable the detection and quantitation of caffeine from C. arabica at low concentrations. The developed HPLC method is a simple, rapid, precisely, accurately and widely accepted and it is recommended for efficient assays in routine work. A simple, accurate, and sensitive high-performance liquid chromatography (HPLC) method for caffeine from Coffea arabica has been developed and validated. The developed HPLC method was validated for linearity, specificity, precision, recovery, limits of detection, and limits of quantification by the International Conference on Harmonization guidelines. The results revealed that the proposed method is highly reliable. This method could be successfully applied for routine quality work analysis. Abbreviation Used: C. arabica : Coffee arabica, ICH: International Conference on Harmonisation, % RSD: Percentage Relative Standard Deviation, R2: Correlation Coefficient, ppm: Parts per million, LOD: Limits

  14. Precision of GNSS instruments by static method comparing in real time

    Directory of Open Access Journals (Sweden)

    Slavomír Labant

    2009-09-01

    Full Text Available Tablet paper describes comparison of measuring accuracy two apparatus from the firm Leica. One of them recieve signals onlyfrom GPS satelites and another instrument is working with GPS and also with GLONASS satelites. Measuring is carry out by RTK staticmethod with 2 minutes observations. Measurement processing is separated to X, Y (position and h (heigh. Adjustment of directobservations is used as a adjusting method.

  15. Instruments and methods of scintillation spectra processing for radiation control tasks

    International Nuclear Information System (INIS)

    Antropov, S.Yu.; Ermilov, A.P.; Ermilov, S.A.; Komarov, N.A.; Krokhin, I.I.

    2005-01-01

    On gamma-spectrometer the response function could be calculated on the base of sensitivity data, energy resolution and form of Compton spectrum part. On the scintillation gamma-spectrometer with Na-I(Tl) crystal 63x63 mm the method allows to divide the 5-10 components mixtures, and on the beta-spectrometer of 2-3 component mixtures. The approach is realized in the 'Progress' program-instrumental complexes

  16. Developments in FT-ICR MS instrumentation, ionization techniques, and data interpretation methods for petroleomics.

    Science.gov (United States)

    Cho, Yunju; Ahmed, Arif; Islam, Annana; Kim, Sunghwan

    2015-01-01

    Because of the increasing importance of heavy and unconventional crude oil as an energy source, there is a growing need for petroleomics: the pursuit of more complete and detailed knowledge of the chemical compositions of crude oil. Crude oil has an extremely complex nature; hence, techniques with ultra-high resolving capabilities, such as Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS), are necessary. FT-ICR MS has been successfully applied to the study of heavy and unconventional crude oils such as bitumen and shale oil. However, the analysis of crude oil with FT-ICR MS is not trivial, and it has pushed analysis to the limits of instrumental and methodological capabilities. For example, high-resolution mass spectra of crude oils may contain over 100,000 peaks that require interpretation. To visualize large data sets more effectively, data processing methods such as Kendrick mass defect analysis and statistical analyses have been developed. The successful application of FT-ICR MS to the study of crude oil has been critically dependent on key developments in FT-ICR MS instrumentation and data processing methods. This review offers an introduction to the basic principles, FT-ICR MS instrumentation development, ionization techniques, and data interpretation methods for petroleomics and is intended for readers having no prior experience in this field of study. © 2014 Wiley Periodicals, Inc.

  17. A novel liquid chromatography/mass spectrometry method for determination of neurotransmitters in brain tissue: Application to human tauopathies.

    Science.gov (United States)

    Forgacsova, Andrea; Galba, Jaroslav; Garruto, Ralph M; Majerova, Petra; Katina, Stanislav; Kovac, Andrej

    2018-01-15

    Neurotransmitters, small molecules widely distributed in the central nervous system are essential in transmitting electrical signals across neurons via chemical communication. Dysregulation of these chemical signaling molecules is linked to numerous neurological diseases including tauopathies. In this study, a precise and reliable liquid chromatography method was established with tandem mass spectrometry detection for the simultaneous determination of aspartic acid, asparagine, glutamic acid, glutamine, γ-aminobutyric acid, N-acetyl-l-aspartic acid, pyroglutamic acid, acetylcholine and choline in human brain tissue. The method was successfully applied to the analysis of human brain tissues from three different tauopathies; corticobasal degeneration, progressive supranuclear palsy and parkinsonism-dementia complex of Guam. Neurotransmitters were analyzed on ultra-high performance chromatography (UHPLC) using an ethylene bridged hybrid amide column coupled with tandem mass spectrometry (MS/MS). Identification and quantification of neurotransmitters was carried out by ESI+ mass spectrometry detection. We optimized sample preparation to achieve simple and fast extraction of all nine analytes. Our method exhibited an excellent linearity for all analytes (all coefficients of determination >0.99), with inter-day and intra-day precision yielding relative standard deviations 3.2%-11.2% and an accuracy was in range of 92.6%-104.3%. The present study, using the above method, is the first to demonstrate significant alterations of brain neurotransmitters caused by pathological processes in the brain tissues of patient with three different tauopathies. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Analysis of Trace Pharmaceuticals and Related Compounds in Municipal Wastewaters by Preconcentration, Chromatography, Derivatization, and Separation Methods

    Directory of Open Access Journals (Sweden)

    Petra Camilla Lindholm

    2014-05-01

    Full Text Available A significant portion of pharmaceuticals and other organic chemicals consumed by people and animals are released into municipal wastewater treatment plants. Most of them are degraded during the wastewater treatment processes, but some of them degrade only partially and may be widely transported and dispersed into the aquatic environment. This is why efficient and fast analytical methods are needed for detection of organic compounds in wastewaters at trace levels. Because wastewaters often consist of complex matrices and high-molecular mass materials, e.g., lignocellulosic biomass, which may bring challenges to the sample preparation procedures, efficient pre-concentration methods such as solid phase extraction (SPE solid phase microextraction (SPME, or single drop microextraction (SDME are needed. The most common analysis methods are gas chromatography (GC and liquid chromatography (LC coupled with tandem mass spectrometry (MS/MS. The aim of this review is to give an overview of chromatographic and spectroscopic methods when characterizing low- and medium-molecular weight organic pollutants, mainly focusing on pharmaceuticals, biocides, and personal care products in environmental matrices.

  19. Liquid chromatography/tandem mass spectrometry method for quantitative estimation of solutol HS15 and its applications

    OpenAIRE

    Bhaskar, V. Vijaya; Middha, Anil; Srivastava, Pratima; Rajagopal, Sriram

    2015-01-01

    A rapid, sensitive and selective pseudoMRM (pMRM)-based method for the determination of solutol HS15 (SHS15) in rat plasma was developed using liquid chromatography/tandem mass spectrometry (LCâMS/MS). The most abundant ions corresponding to SHS15 free polyethyleneglycol (PEG) oligomers at m/z 481, 525, 569, 613, 657, 701, 745, 789, 833, 877, 921 and 965 were selected for pMRM in electrospray mode of ionization. Purity of the lipophilic and hydrophilic components of SHS15 was estimated using ...

  20. Unexpected but Most Welcome: Mixed Methods for the Validation and Revision of the Participatory Evaluation Measurement Instrument

    Science.gov (United States)

    Daigneault, Pierre-Marc; Jacob, Steve

    2014-01-01

    Although combining methods is nothing new, more contributions about why and how to mix methods for validation purposes are needed. This article presents a case of validating the inferences drawn from the Participatory Evaluation Measurement Instrument, an instrument that purports to measure stakeholder participation in evaluation. Although the…

  1. Lipidomics by Supercritical Fluid Chromatography

    Directory of Open Access Journals (Sweden)

    Laurent Laboureur

    2015-06-01

    Full Text Available This review enlightens the role of supercritical fluid chromatography (SFC in the field of lipid analysis. SFC has been popular in the late 1980s and 1990s before almost disappearing due to the commercial success of liquid chromatography (LC. It is only 20 years later that a regain of interest appeared when new commercial instruments were introduced. As SFC is fully compatible with the injection of extracts in pure organic solvent, this technique is perfectly suitable for lipid analysis and can be coupled with either highly universal (UV or evaporative light scattering or highly specific (mass spectrometry detection methods. A short history of the use of supercritical fluids as mobile phase for the separation oflipids will be introduced first. Then, the advantages and drawbacks of SFC are discussed for each class of lipids (fatty acyls, glycerolipids, glycerophospholipids, sphingolipids, sterols, prenols, polyketides defined by the LIPID MAPS consortium.

  2. Lipidomics by Supercritical Fluid Chromatography

    Science.gov (United States)

    Laboureur, Laurent; Ollero, Mario; Touboul, David

    2015-01-01

    This review enlightens the role of supercritical fluid chromatography (SFC) in the field of lipid analysis. SFC has been popular in the late 1980s and 1990s before almost disappearing due to the commercial success of liquid chromatography (LC). It is only 20 years later that a regain of interest appeared when new commercial instruments were introduced. As SFC is fully compatible with the injection of extracts in pure organic solvent, this technique is perfectly suitable for lipid analysis and can be coupled with either highly universal (UV or evaporative light scattering) or highly specific (mass spectrometry) detection methods. A short history of the use of supercritical fluids as mobile phase for the separation oflipids will be introduced first. Then, the advantages and drawbacks of SFC are discussed for each class of lipids (fatty acyls, glycerolipids, glycerophospholipids, sphingolipids, sterols, prenols, polyketides) defined by the LIPID MAPS consortium. PMID:26090714

  3. Instrumentation to Measure the Capacitance of Biosensors by Sinusoidal Wave Method

    Directory of Open Access Journals (Sweden)

    Pavan Kumar KATHUROJU

    2009-09-01

    Full Text Available Micro Controller based instrumentation to measure the capacitance of biosensors is developed. It is based on frequency domain technique with sinusoidal wave input. Changes in the capacitance of biosensor because of the analyte specific reaction are calculated by knowing the current flowing through the sample. A dedicated 8-bit microcontroller (AT89C52 and its associated peripherals are employed for the hardware and application specific software is developed in ‘C’ language. The paper describes the methodology, instrumentation details along with a specific application to glucose sensing. The measurements are conducted with glucose oxidase based capacitance biosensor and the obtained results are compared with the conventional method of sugar measurements using the UV-Visible spectroscopy (Phenol-Sulphuric acid assay method. Measurement accuracy of the instrument is found to be ± 5 %. Experiments are conducted on glucose sensor with different bias voltages. It is found that for bias voltages varying from 0.5 to 0.7 Volt, the measurements are good for this application.

  4. A single-run liquid chromatography mass spectrometry method to quantify neuroactive kynurenine pathway metabolites in rat plasma.

    Science.gov (United States)

    Orsatti, Laura; Speziale, Roberto; Orsale, Maria Vittoria; Caretti, Fulvia; Veneziano, Maria; Zini, Matteo; Monteagudo, Edith; Lyons, Kathryn; Beconi, Maria; Chan, Kelvin; Herbst, Todd; Toledo-Sherman, Leticia; Munoz-Sanjuan, Ignacio; Bonelli, Fabio; Dominguez, Celia

    2015-03-25

    Neuroactive metabolites in the kynurenine pathway of tryptophan catabolism are associated with neurodegenerative disorders. Tryptophan is transported across the blood-brain barrier and converted via the kynurenine pathway to N-formyl-L-kynurenine, which is further degraded to L-kynurenine. This metabolite can then generate a group of metabolites called kynurenines, most of which have neuroactive properties. The association of tryptophan catabolic pathway alterations with various central nervous system (CNS) pathologies has raised interest in analytical methods to accurately quantify kynurenines in body fluids. We here describe a rapid and sensitive reverse-phase HPLC-MS/MS method to quantify L-kynurenine (KYN), kynurenic acid (KYNA), 3-hydroxy-L-kynurenine (3HK) and anthranilic acid (AA) in rat plasma. Our goal was to quantify these metabolites in a single run; given their different physico-chemical properties, major efforts were devoted to develop a chromatography suitable for all metabolites that involves plasma protein precipitation with acetonitrile followed by chromatographic separation by C18 RP chromatography, detected by electrospray mass spectrometry. Quantitation range was 0.098-100 ng/ml for 3HK, 9.8-20,000 ng/ml for KYN, 0.49-1000 ng/ml for KYNA and AA. The method was linear (r>0.9963) and validation parameters were within acceptance range (calibration standards and QC accuracy within ±30%). Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Hydrophilic Interaction Liquid Chromatography/Mass Spectrometry: An Attractive and Prospective Method for the Quantitative Bioanalysis in Drug Metabolism.

    Science.gov (United States)

    Li, Zheng; Han, Jie; Sun, Shi-an; Chen, Kai; Tang, Dao-quan

    2016-01-01

    During the development, dosage optimization and safety evaluation of a drug, rapid and precise monitoring of administered drug and/or its metabolites in biological samples including blood, plasma, serum, tissues and saliva are vital. As drug biotransformation produces more hydrophilic metabolites for the enhancement of drug elimination, which is often a challenge for traditional reversed-phase liquid chromatography (RPLC) separation. Because hydrophilic interaction liquid chromatography (HILIC) is capable of retaining polar compounds and readily compatible with mass spectrometry (MS), HILIC has been used as a complementary separation technique to RPLC for analysis of polar metabolites, especially polar drugs and their metabolites. This review covers core aspects of HILIC-MS/MS method and overall profile of its application in analysis of drug and/or its metabolites. The emphasis of this paper has been placed on the applications of HILIC-MS/MS method in quantitative bioanalysis of drugs alone or along with their metabolites in drug metabolism studies in recent years. As a fundamental and critical step of bioanalytical method, conventional sample preparation techniques of biological matrices for the HILIC-MS/MS analysis of drugs and/or their metabolites are also briefly featured.

  6. Development of a Method for Rapid Determination of Morpholine in Juices and Drugs by Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Mengsi Cao

    2018-01-01

    Full Text Available A reliable derivatization method has been developed to detect and quantify morpholine in apple juices and ibuprofen with gas chromatography-mass spectrometry. Morpholine can react with sodium nitrite under acidic condition to produce stable and volatile N-nitrosomorpholine derivative. In this experiment, various factors affecting the derivatization and extraction process were optimized, including volume and concentration of hydrochloric acid, quantity of sodium nitrite, derivatization temperature, derivatization time, extraction reagents, and extraction time. The derivative was extracted with dichloromethane and determined by gas chromatography-mass spectrometry. The linearity range of morpholine was 10–500 μg·L−1 with good correlation, and limits of detection (LOD and limits of quantification (LOQ were 7.3 μg·L−1 and 24.4 μg·L−1, respectively. Low, medium, and high concentrations of morpholine were added in apple juices and ibuprofen samples to evaluate standard recovery rate and relative standard deviation. The spiked recovery rate ranged from 94.3% to 109.0%, and the intraday repeatability and interday reproducibility were 2.0%–4.4% and 3.3%–7.0%, respectively. The developed method has good accuracy and precision. This quantitative method for morpholine is simple, sensitive, rapid, and low cost and can successfully be applied to analyze the residual morpholine in apple juices and drug samples.

  7. Studies on the instrumental neutron activation analysis by cadmium ratio method and pair comparator method

    Energy Technology Data Exchange (ETDEWEB)

    Chao, H E; Lu, W D; Wu, S C

    1977-12-01

    The cadmium ratio method and pair comparator method provide a solution for the effects on the effective activation factors resulting from the variation of neutron spectrum at different irradiation positions as usually encountered in the single comparator method. The relations between the activation factors and neutron spectrum in terms of cadmium ratio of the comparator Au or of the activation factor of Co-Au pair for the elements, Sc, Cr, Mn, Co, La, Ce, Sm, and Th have been determined. The activation factors of the elements at any irradiation position can then be obtained from the cadmium ratio of the comparator and/or the activation factor of the comparator pair. The relations determined should be able to apply to different reactors and/or different positions of a reactor. It is shown that, for the isotopes /sup 46/Sc, /sup 51/Cr, /sup 56/Mn, /sup 60/Co, /sup 140/La, /sup 141/Ce, /sup 153/Sm and /sup 233/Pa, the thermal neutron activation factors determined by these two methods were generally in agreement with theoretical values. Their I/sub 0//sigma/sub th/ values appeared to agree with literature values also. The methods were applied to determine the contents of elements Sc, Cr, Mn, La, Ce, Sm, and Th in U.S.G.S. Standard Rock G-2, and the results were also in agreement with literature values. The cadmium ratio method and pair comparator method improved the single comparator method, and they are more suitable to analysis for multi-elements of a large number of samples.

  8. A method for automating calibration and records management for instrumentation and dosimetry

    International Nuclear Information System (INIS)

    O'Brien, J.M. Jr.; Rushton, R.O.; Burns, R.E. Jr.

    1993-01-01

    Current industry requirements are becoming more stringent on quality assurance records and documentation for calibration of instruments and dosimetry. A novel method is presented here that will allow a progressive automation scheme to be used in pursuit of that goal. This concept is based on computer-controlled irradiators that can act as stand-alone devices or be interfaced to other components via a computer local area network. In this way, complete systems can be built with modules to create a records management system to meet the needs of small laboratories or large multi-building calibration groups. Different database engines or formats can be used simply by replacing a module. Modules for temperature and pressure monitoring or shipping and receiving can be added, as well as equipment modules for direct IEEE-488 interface to electrometers and other instrumentation

  9. A method for automating calibration and records management for instrumentation and dosimetry

    Energy Technology Data Exchange (ETDEWEB)

    O`Brien, J.M. Jr.; Rushton, R.O.; Burns, R.E. Jr. [Atlan-Tech, Inc., Roswell, GA (United States)

    1993-12-31

    Current industry requirements are becoming more stringent on quality assurance records and documentation for calibration of instruments and dosimetry. A novel method is presented here that will allow a progressive automation scheme to be used in pursuit of that goal. This concept is based on computer-controlled irradiators that can act as stand-alone devices or be interfaced to other components via a computer local area network. In this way, complete systems can be built with modules to create a records management system to meet the needs of small laboratories or large multi-building calibration groups. Different database engines or formats can be used simply by replacing a module. Modules for temperature and pressure monitoring or shipping and receiving can be added, as well as equipment modules for direct IEEE-488 interface to electrometers and other instrumentation.

  10. Determination of thyroid hormones in mouse tissues by isotope-dilution microflow liquid chromatography-mass spectrometry method

    DEFF Research Database (Denmark)

    De Angelis, Meri; Giesert, Florian; Finan, Brian

    2016-01-01

    ). The nano-UPLC system was interfaced with a quadrupole time-of-flight mass spectrometer (Q-TOF2-MS) using the positive ion mode electrospray ionization. In our analytical method the instrumental calibration curves were constructed from 0 to 100pgμL(-1) and all of them showed good linearity (r(2)>0.99...

  11. Novel materials and methods for solid-phase extraction and liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Ambrose, Diana [Iowa State Univ., Ames, IA (United States)

    1997-06-24

    This report contains a general introduction which discusses solid-phase extraction and solid-phase micro-extraction as sample preparation techniques for high-performance liquid chromatography, which is also evaluated in the study. This report also contains the Conclusions section. Four sections have been removed and processed separately: silicalite as a sorbent for solid-phase extraction; a new, high-capacity carboxylic acid functionalized resin for solid-phase extraction; semi-micro solid-phase extraction of organic compounds from aqueous and biological samples; and the high-performance liquid chromatographic determination of drugs and metabolites in human serum and urine using direct injection and a unique molecular sieve.

  12. Quality by Design in the development of hydrophilic interaction liquid chromatography method with gradient elution for the analysis of olanzapine.

    Science.gov (United States)

    Tumpa, Anja; Stajić, Ana; Jančić-Stojanović, Biljana; Medenica, Mirjana

    2017-02-05

    This paper deals with the development of hydrophilic interaction liquid chromatography (HILIC) method with gradient elution, in accordance with Analytical Quality by Design (AQbD) methodology, for the first time. The method is developed for olanzapine and its seven related substances. Following step by step AQbD methodology, firstly as critical process parameters (CPPs) temperature, starting content of aqueous phase and duration of linear gradient are recognized, and as critical quality attributes (CQAs) separation criterion S of critical pairs of substances are investigated. Rechtschaffen design is used for the creation of models that describe the dependence between CPPs and CQAs. The design space that is obtained at the end is used for choosing the optimal conditions (set point). The method is fully validated at the end to verify the adequacy of the chosen optimal conditions and applied to real samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Validation of high-performance liquid chromatography (HPLC method for quantitative analysis of histamine in fish and fishery products

    Directory of Open Access Journals (Sweden)

    B.K.K.K. Jinadasa

    2016-12-01

    Full Text Available A high-performance liquid chromatography method is described for quantitative determination and validation of histamine in fish and fishery product samples. Histamine is extracted from fish/fishery products by homogenizing with tri-chloro acetic acid, separated with Amberlite CG-50 resin and C18-ODS Hypersil reversed phase column at ambient temperature (25°C. Linear standard curves with high correlation coefficients were obtained. An isocratic elution program was used; the total elution time was 10 min. The method was validated by assessing the following aspects; specificity, repeatability, reproducibility, linearity, recovery, limits of detection, limit of quantification and uncertainty. The validated parameters are in good agreement with method and it is a useful tool for determining histamine in fish and fishery products.

  14. Reliability of the input admittance of bowed-string instruments measured by the hammer method.

    Science.gov (United States)

    Zhang, Ailin; Woodhouse, Jim

    2014-12-01

    The input admittance at the bridge, measured by hammer testing, is often regarded as the most useful and convenient measurement of the vibrational behavior of a bowed string instrument. However, this method has been questioned, due especially to differences between human bowing and hammer impact. The goal of the research presented here is to investigate the reliability and accuracy of this classic hammer method. Experimental studies were carried out on cellos, with three different driving conditions and three different boundary conditions. Results suggest that there is nothing fundamentally different about the hammer method, compared to other kinds of excitation. The third series of experiments offers an opportunity to explore the difference between the input admittance measuring from one bridge corner to another and that of single strings. The classic measurement is found to give a reasonable approximation to that of all four strings. Some possible differences between the hammer method and normal bowing and implications of the acoustical results are also discussed.

  15. Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticals

    Directory of Open Access Journals (Sweden)

    Carla M. Teglia

    2015-10-01

    Full Text Available An efficient generic static headspace gas chromatography (HSGC method was developed, optimized and validated for the routine determination of several residual solvents (RS in drug substance, using a strategy with two sets of calibration. Dimethylsulfoxide (DMSO was selected as the sample diluent and internal standards were used to minimize signal variations due to the preparative step. A gas chromatograph from Agilent Model 6890 equipped with flame ionization detector (FID and a DB-624 (30 m×0.53 mm i.d., 3.00 µm film thickness column was used. The inlet split ratio was 5:1. The influencing factors in the chromatographic separation of the analytes were determined through a fractional factorial experimental design. Significant variables: the initial temperature (IT, the final temperature (FT of the oven and the carrier gas flow rate (F were optimized using a central composite design. Response transformation and desirability function were applied to find out the optimal combination of the chromatographic variables to achieve an adequate resolution of the analytes and short analysis time. These conditions were 30 °C for IT, 158 °C for FT and 1.90 mL/min for F. The method was proven to be accurate, linear in a wide range and very sensitive for the analyzed solvents through a comprehensive validation according to the ICH guidelines. Keywords: Headspace gas chromatography, Residual solvents, Pharmaceuticals, Surface response methodology, Desirability function

  16. A sediment extraction and cleanup method for wide-scope multitarget screening by liquid chromatography-high-resolution mass spectrometry.

    Science.gov (United States)

    Massei, Riccardo; Byers, Harry; Beckers, Liza-Marie; Prothmann, Jens; Brack, Werner; Schulze, Tobias; Krauss, Martin

    2018-01-01

    Previous studies on organic sediment contaminants focused mainly on a limited number of highly hydrophobic micropollutants accessible to gas chromatography using nonpolar, aprotic extraction solvents. The development of liquid chromatography-high-resolution mass spectrometry (LC-HRMS) permits the spectrum of analysis to be expanded to a wider range of more polar and ionic compounds present in sediments and allows target, suspect, and nontarget screening to be conducted with high sensitivity and selectivity. In this study, we propose a comprehensive multitarget extraction and sample preparation method for characterization of sediment pollution covering a broad range of physicochemical properties that is suitable for LC-HRMS screening analysis. We optimized pressurized liquid extraction, cleanup, and sample dilution for a target list of 310 compounds. Finally, the method was tested on sediment samples from a small river and its tributaries. The results show that the combination of 100 °C for ethyl acetate-acetone (50:50, neutral extract) followed by 80 °C for acetone-formic acid (100:1, acidic extract) and methanol-10 mM sodium tetraborate in water (90:10, basic extract) offered the best extraction recoveries for 287 of 310 compounds. At a spiking level of 1 μg mL -1 , we obtained satisfactory cleanup recoveries for the neutral extract-(93 ± 23)%-and for the combined acidic/basic extracts-(42 ± 16)%-after solvent exchange. Among the 69 compounds detected in environmental samples, we successfully quantified several pharmaceuticals and polar pesticides.

  17. Comparative investigation of the gel chromatography column scanning method for quality control of /sup 99/sup(m)Tc-methylenediphosphonate

    Energy Technology Data Exchange (ETDEWEB)

    Darte, L

    1981-04-01

    Gel chromatography column scanning (GCS) is the method of choice for quality control of sup(99m)Tc-MDP preparations. Using this method all the labelled components are obtained rapidly in one simple test procedure. The influence of various parameters such as gel type, column size, prehistory of column, equilibration, eluent, elution volume and flow rate upon the results have been investigated. Test results for sup(99 m)Tc-MDP have been compared for several different GCS systems, a few TLC systems and column chromatography with fraction collection. The GCS technique, optimized for testing sup(99m)Tc-MDP preparations has been applied in a few experiments in which very good reproducibility is required: Labelling kinetics and stability when stored at room temperature or in a refrigerator and influence of the sup(99m)Te/(sup(99m)Tc + /sup 99/Tc) atomic ratio and of the amount of radioactivity on the sup(99m)Tc-MDP labelling yield, covering parameter ranges of clinical interest, have been studied.

  18. A postprocessing method in the HMC framework for predicting gene function based on biological instrumental data

    Science.gov (United States)

    Feng, Shou; Fu, Ping; Zheng, Wenbin

    2018-03-01

    Predicting gene function based on biological instrumental data is a complicated and challenging hierarchical multi-label classification (HMC) problem. When using local approach methods to solve this problem, a preliminary results processing method is usually needed. This paper proposed a novel preliminary results processing method called the nodes interaction method. The nodes interaction method revises the preliminary results and guarantees that the predictions are consistent with the hierarchy constraint. This method exploits the label dependency and considers the hierarchical interaction between nodes when making decisions based on the Bayesian network in its first phase. In the second phase, this method further adjusts the results according to the hierarchy constraint. Implementing the nodes interaction method in the HMC framework also enhances the HMC performance for solving the gene function prediction problem based on the Gene Ontology (GO), the hierarchy of which is a directed acyclic graph that is more difficult to tackle. The experimental results validate the promising performance of the proposed method compared to state-of-the-art methods on eight benchmark yeast data sets annotated by the GO.

  19. Analytical Method Validation of High-Performance Liquid Chromatography and Stability-Indicating Study of Medroxyprogesterone Acetate Intravaginal Sponges

    Directory of Open Access Journals (Sweden)

    Nidal Batrawi

    2017-02-01

    Full Text Available Medroxyprogesterone acetate is widely used in veterinary medicine as intravaginal dosage for the synchronization of breeding cycle in ewes and goats. The main goal of this study was to develop reverse-phase high-performance liquid chromatography method for the quantification of medroxyprogesterone acetate in veterinary vaginal sponges. A single high-performance liquid chromatography/UV isocratic run was used for the analytical assay of the active ingredient medroxyprogesterone. The chromatographic system consisted of a reverse-phase C18 column as the stationary phase and a mixture of 60% acetonitrile and 40% potassium dihydrogen phosphate buffer as the mobile phase; the pH was adjusted to 5.6. The method was validated according to the International Council for Harmonisation (ICH guidelines. Forced degradation studies were also performed to evaluate the stability-indicating properties and specificity of the method. Medroxyprogesterone was eluted at 5.9 minutes. The linearity of the method was confirmed in the range of 0.0576 to 0.1134 mg/mL ( R 2 > 0.999. The limit of quantification was shown to be 3.9 µg/mL. Precision and accuracy ranges were found to be %RSD <0.2 and 98% to 102%, respectively. Medroxyprogesterone capacity factor value of 2.1, tailing factor value of 1.03, and resolution value of 3.9 were obtained in accordance with ICH guidelines. Based on the obtained results, a rapid, precise, accurate, sensitive, and cost-effective analysis procedure was proposed for quantitative determination of medroxyprogesterone in vaginal sponges. This analytical method is the only available method to analyse medroxyprogesterone in veterinary intravaginal dosage form.

  20. Improved retrieval of cloud base heights from ceilometer using a non-standard instrument method

    Science.gov (United States)

    Wang, Yang; Zhao, Chuanfeng; Dong, Zipeng; Li, Zhanqing; Hu, Shuzhen; Chen, Tianmeng; Tao, Fa; Wang, Yuzhao

    2018-04-01

    Cloud-base height (CBH) is a basic cloud parameter but has not been measured accurately, especially under polluted conditions due to the interference of aerosol. Taking advantage of a comprehensive field experiment in northern China in which a variety of advanced cloud probing instruments were operated, different methods of detecting CBH are assessed. The Micro-Pulse Lidar (MPL) and the Vaisala ceilometer (CL51) provided two types of backscattered profiles. The latter has been employed widely as a standard means of measuring CBH using the manufacturer's operational algorithm to generate standard CBH products (CL51 MAN) whose quality is rigorously assessed here, in comparison with a research algorithm that we developed named value distribution equalization (VDE) algorithm. It was applied to both the profiles of lidar backscattering data from the two instruments. The VDE algorithm is found to produce more accurate estimates of CBH for both instruments and can cope with heavy aerosol loading conditions well. By contrast, CL51 MAN overestimates CBH by 400 m and misses many low level clouds under such conditions. These findings are important given that CL51 has been adopted operationally by many meteorological stations in China.

  1. The influence of different referencing methods on the accuracy of δ(13) C value measurement of ethanol fuel by gas chromatography/combustion/isotope ratio mass spectrometry.

    Science.gov (United States)

    Neves, Laura A; Rodrigues, Janaína M; Daroda, Romeu J; Silva, Paulo R M; Ferreira, Alexandre A; Aranda, Donato A G; Eberlin, Marcos N; Fasciotti, Maíra

    2015-11-15

    Brazil is the largest producer of sugar cane bioethanol in the world. Isotope ratio mass spectrometry (IRMS) is the technique of choice to certify the origin/raw materials for ethanol production, but the lack of certified reference materials (CRMs) for accurate measurements of δ(13) C values traceable to Vienna Pee Dee Belemnite (VPDB), the international zero point for (13) C/(12) C measurements, certified and compatible with gas chromatography (GC)/IRMS instruments may compromise the accuracy of δ(13) C determinations. We evaluated the influence of methods for the calibration and normalization of raw δ(13) C values of ethanol samples. Samples were analyzed by GC/C/IRMS using two different GC columns. Different substances were used as isotopic standards for the working gas calibration. The δ(13) C values obtained with the three methods of normalization were statistically compared with those obtained with elemental analyzer (EA)/IRMS, since the δ(13) C results obtained using EA are traceable to VPDB via the NBS 22 reference material. It was observed that both the isotopic reference material for CO2 calibration and the GC column have a major effect on the δ(13) C measurements, leading to a bias of almost 2-3 ‰ in the δ(13) C values. All three methods of normalization were equivalent in performance, enabling an improvement in the GC/C/IRMS accuracy, compared with the EA/IRMS reference values for the samples. All the methods of CO2 calibration, chromatography and normalization presented in this work demonstrated several sources of traceability and accuracy loss for the determination of δ(13) C values in ethanol fuel samples by GC/C/IRMS. This work has also shown the importance of using proper CRMs traceable to VPBD that should be compatible and certified using GC/C/IRMS, ideally in a wide range of δ(13) C values. This is important not only for bioethanol fuel samples, but also for many analytes commonly analyzed by IRMS. Copyright © 2015 John Wiley & Sons

  2. Effect of freezing method and frozen storage duration on instrumental quality of lamb throughout display.

    Science.gov (United States)

    Muela, E; Sañudo, C; Campo, M M; Medel, I; Beltrán, J A

    2010-04-01

    This study evaluated the effect of freezing method (FM) (air blast freezer, freezing tunnel, or nitrogen chamber) and frozen storage duration (FSD) (1, 3, or 6 months) on the instrumental measurements of quality of thawed lamb, aged for a total of 72 h, throughout a 10-d display period, compared to the quality of fresh meat. pH, colour, lipid oxidation, thawing, and cooking losses in Longissimus thoracis and lumborum muscle, were determined following standard methods. FM affected yellowness, FSD redness and thawing losses, and both affected oxidation (increased as freezing rate decreased and/or as storage duration increased). When compared with fresh meat, the main differences appeared on oxidation (where a significant interaction between treatment (3FM x 3FSD + fresh meat) with display duration was detected), and on total losses (thaw + cook losses). Oxidation was lower in fresh meat, but values were not significantly different from those stored frozen for 1 month. Fresh meat had smaller total losses than did thawed meat, but losses were not significantly different from meat frozen in the freezing tunnel and stored frozen for 1 month. Display duration had a greater effect on instrumental quality parameters than did FM or FSD. pH, b*, and oxidation increased, and L* and a* decreased with an increase in the number of days on display. In conclusion, neither freezing method nor frozen storage up to 6 months influenced extensively the properties of lamb when instrumental measurements of quality were measured in meat that had been displayed for 1d after thawing. The small deterioration shown in this study should not give consumers concerns about frozen meat. 2009 Elsevier Ltd. All rights reserved.

  3. Comparison of Dorris-Gray and Schultz methods for the calculation of surface dispersive free energy by inverse gas chromatography.

    Science.gov (United States)

    Shi, Baoli; Wang, Yue; Jia, Lina

    2011-02-11

    Inverse gas chromatography (IGC) is an important technique for the characterization of surface properties of solid materials. A standard method of surface characterization is that the surface dispersive free energy of the solid stationary phase is firstly determined by using a series of linear alkane liquids as molecular probes, and then the acid-base parameters are calculated from the dispersive parameters. However, for the calculation of surface dispersive free energy, generally, two different methods are used, which are Dorris-Gray method and Schultz method. In this paper, the results calculated from Dorris-Gray method and Schultz method are compared through calculating their ratio with their basic equations and parameters. It can be concluded that the dispersive parameters calculated with Dorris-Gray method will always be larger than the data calculated with Schultz method. When the measuring temperature increases, the ratio increases large. Compared with the parameters in solvents handbook, it seems that the traditional surface free energy parameters of n-alkanes listed in the papers using Schultz method are not enough accurate, which can be proved with a published IGC experimental result. © 2010 Elsevier B.V. All rights reserved.

  4. Development of a sample preparation method for the analysis of current-use pesticides in sediment using gas chromatography.

    Science.gov (United States)

    Wang, Dongli; Weston, Donald P; Ding, Yuping; Lydy, Michael J

    2010-02-01

    Pyrethroid insecticides have been implicated as the cause of sediment toxicity to Hyalella azteca in both agricultural and urban areas of California; however, for a subset of these toxic sediments (approximately 30%), the cause of toxicity remains unidentified. This article describes the analytical method development for seven additional pesticides that are being examined to determine if they might play a role in the unexplained toxicity. A pressurized liquid extraction method was optimized to simultaneously extract diazinon, methyl parathion, oxyfluorfen, dicofol, fenpropathrin, pyraclostrobin, and indoxacarb from sediment, and the extracts were cleaned using a two-step solid-phase extraction procedure. The final extract was analyzed for the target pesticides by gas chromatography/nitrogen-phosphorus detector (GC/NPD), and gas chromatography/electron capture detector (GC/ECD), after sulfur was removed by shaking with copper and cold crystallization. Three sediments were used as reference matrices to assess method accuracy and precision. Method detection limits were 0.23-1.8 ng/g dry sediment using seven replicates of sediment spiked at 1.0 ng/g dry sediment. Recoveries ranged from 61.6 to 118% with relative standard deviations of 2.1-17% when spiked at 5.0 and 50 ng/g dry sediment. The three reference sediments, spiked with 50 ng/g dry weight of the pesticide mixture, were aged for 0.25, 1, 4, 7, and 14 days. Recoveries of the pesticides in the sediments generally decreased with increased aging time, but the magnitude of the decline was pesticide and sediment dependent. The developed method was applied to field-collected sediments from the Central Valley of California.

  5. Collaborative trial validation study of two methods, one based on high performance liquid chromatography-tandem mass spectrometry and on gas chromatography-mass spectrometry for the determination of acrylamide in bakery and potato products.

    Science.gov (United States)

    Wenzl, Thomas; Karasek, Lubomir; Rosen, Johan; Hellenaes, Karl-Erik; Crews, Colin; Castle, Laurence; Anklam, Elke

    2006-11-03

    A European inter-laboratory study was conducted to validate two analytical procedures for the determination of acrylamide in bakery ware (crispbreads, biscuits) and potato products (chips), within a concentration range from about 20 microg/kg to about 9000 microgg/kg. The methods are based on gas chromatography-mass spectrometry (GC-MS) of the derivatised analyte and on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) of native acrylamide. Isotope dilution with isotopically labelled acrylamide was an integral part of both methods. The study was evaluated according to internationally accepted guidelines. The performance of the HPLC-MS/MS method was found to be superior to that of the GC-MS method and to be fit-for-the-purpose.

  6. A novel single-step, multipoint calibration method for instrumented Lab-on-Chip systems

    DEFF Research Database (Denmark)

    Pfreundt, Andrea; Patou, François; Zulfiqar, Azeem

    2014-01-01

    for instrument-based PoC blood biomarker analysis systems. Motivated by the complexity of associating high-accuracy biosensing using silicon nanowire field effect transistors with ease of use for the PoC system user, we propose a novel one-step, multipoint calibration method for LoC-based systems. Our approach...... specifically addresses the important interfaces between a novel microfluidic unit to integrate the sensor array and a mobile-device hardware accessory. A multi-point calibration curve is obtained by generating a defined set of reference concentrations from a single input. By consecutively splitting the flow...

  7. Application of instrumental neutron activation analysis and multivariate statistical methods to archaeological Syrian ceramics

    International Nuclear Information System (INIS)

    Bakraji, E. H.; Othman, I.; Sarhil, A.; Al-Somel, N.

    2002-01-01

    Instrumental neutron activation analysis (INAA) has been utilized in the analysis of thirty-seven archaeological ceramics fragment samples collected from Tal AI-Wardiate site, Missiaf town, Hamma city, Syria. 36 chemical elements were determined. These elemental concentrations have been processed using two multivariate statistical methods, cluster and factor analysis in order to determine similarities and correlation between the various samples. Factor analysis confirms that samples were correctly classified by cluster analysis. The results showed that samples can be considered to be manufactured using three different sources of raw material. (author)

  8. Trace elements in cigarette tobacco by a method of instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Noordin Ibrahim

    1986-01-01

    A total of ten cigarette brands were investigated for determining the trace elemental concentrations in tobacco so as to assess their role in the induction of related diseases through smoking. A method instrumental Neutron Activation analysis was employed due to high sensitivity, speed and ability to analyse sample for a wide spectrum of elements simultaneously. A total of 18 elements were detected of which the majority are toxic elements. A full result and conclusion will be reported in the forthcoming paper. (A.J.)

  9. A Method of Separation Assurance for Instrument Flight Procedures at Non-Radar Airports

    Science.gov (United States)

    Conway, Sheila R.; Consiglio, Maria

    2002-01-01

    A method to provide automated air traffic separation assurance services during approach to or departure from a non-radar, non-towered airport environment is described. The method is constrained by provision of these services without radical changes or ambitious investments in current ground-based technologies. The proposed procedures are designed to grant access to a large number of airfields that currently have no or very limited access under Instrument Flight Rules (IFR), thus increasing mobility with minimal infrastructure investment. This paper primarily addresses a low-cost option for airport and instrument approach infrastructure, but is designed to be an architecture from which a more efficient, albeit more complex, system may be developed. A functional description of the capabilities in the current NAS infrastructure is provided. Automated terminal operations and procedures are introduced. Rules of engagement and the operations are defined. Results of preliminary simulation testing are presented. Finally, application of the method to more terminal-like operations, and major research areas, including necessary piloted studies, are discussed.

  10. Comparison of extraction methods for the analysis of natural dyes in historical textiles by high-performance liquid chromatography.

    Science.gov (United States)

    Valianou, Lemonia; Karapanagiotis, Ioannis; Chryssoulakis, Yannis

    2009-12-01

    Different methods for the extraction of Dactylopius coccus Costa, Rubia tinctorum L., Isatis tinctoria L., Reseda luteola L., Curcuma longa L. and Cotinus coggygria Scop. from wool fibres are investigated using high-performance liquid chromatography with diode array detector (HPLC-DAD). The efficiencies of five extraction methods which include the use of HCl (widely used extraction method), citric acid, oxalic acid, TFA and a combination of HCOOH and EDTA are compared on the basis of the (a) number, (b) relative quantities, measured as HPLC peak areas and (c) signal-to-noise ratios (S/N) of the compounds extracted from the wool substrates. Flavonoid glycosides and curcuminoids contained in R. luteola L. and C. longa L., respectively, according to liquid chromatography with mass spectrometry (LC-MS) identifications, are not detected after treating the fibres with HCl. All the other milder methods are successful in extracting these compounds. Experiments are performed using HPLC-DAD to compare the HPLC peak areas and the S/N of the following extracted compounds: indigotin, indirubin, curcumin, demethoxycurcumin, bisdemethoxycurcumin, fisetin, sulfuretin, luteolin, luteolin-7-O-glucoside, apigenin, carminic acid, alizarin, puruprin and rubiadin. It is shown that the TFA method provides overall the best results as it gives elevated extraction yields except for fisetin, luteolin, apigenin and luteolin-7-O-glucoside and highest S/N except for fisetin and luteolin-7-O-glucoside. It is noteworthy that treatment of the fibres with the typical HCl extraction method results overall in very low S/N. The TFA method is selected for further studies, as follows. First, it is applied on silk dyed samples and compared with the HCl method. The same relative differences of the TFA and HCl methods observed for the wool dyed samples are reported for the silk dyed samples too, except for rubiadin, luteolin and apigenin. Thus, in most cases, the nature of the substrate (wool or silk

  11. Instrumental neutron activation analysis as a routine method for rock analysis

    International Nuclear Information System (INIS)

    Rosenberg, R.J.

    1977-06-01

    Instrumental neutron activation methods for the analysis of geological samples have been developed. Special emphasis has been laid on the improvement of sensitivity and accuracy in order to maximize tha quality of the analyses. Furthermore, the procedures have been automated as far as possible in order to minimize the cost of the analysis. A short review of the basic literature is given followed by a description of the principles of the method. All aspects concerning the sensitivity are discussed thoroughly in view of the analyst's possibility of influencing them. Experimentally determined detection limits for Na, Al, K, Ca, Sc, Cr, Ti, V, Mn, Fe, Ni, Co, Rb, Zr, Sb, Cs, Ba, La, Ce, Nd, Sm, Eu, Gd, Tb, Dy, Yb, Lu, Hf, Ta, Th and U are given. The errors of the method are discussed followed by actions taken to avoid them. The most significant error was caused by flux deviation, but this was avoided by building a rotating sample holder for rotating the samples during irradiation. A scheme for the INAA of 32 elements is proposed. The method has been automated as far as possible and an automatic γ-spectrometer and a computer program for the automatic calculation of the results are described. Furthermore, a completely automated uranium analyzer based on delayed neutron counting is described. The methods are discussed in view of their applicability to rock analysis. It is stated that the sensitivity varies considerably from element to element and instrumental activation analysis is an excellent method for the analysis of some specific elements like lanthanides, thorium and uranium but less so for many other elements. The accuracy is good varying from 2% to 10% for most elements. Instrumental activation analysis for most elements is rather an expensive method there being, however, a few exceptions. The most important of these is uranium. The analysis of uranium by delayed neutron counting is an inexpensive means for the analysis of large numbers of samples needed for

  12. Sensitive method for the quantitative determination of bromocriptine in human plasma by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Salvador, Arnaud; Dubreuil, Didier; Denouel, Jannick; Millerioux, L

    2005-06-25

    A sensitive LC-MS-MS assay for the quantitative determination of bromocriptine has been developed and validated and is described in this work. The assay involved the extraction of the analyte from 1 ml of human plasma using a solid phase extraction on Oasis MCX cartridges. Chromatography was performed on a Symmetry C18 (2.1 mm x 100 mm, 3.5 microm) column using a mobile phase consisting of 25:75:01 acetonitrile-water-formic acid with a flow rate of 250 microl/min. The linearity was within the concentration range of 2-500 pg/ml. The lower limit of quantification was 2 pg/ml. This method has been demonstrated to be an improvement over existing methods due to its greater sensitivity and specificity.

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

    Science.gov (United States)

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

    2011-01-01

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

  14. Liquid chromatography tandem mass spectrometry method for simultaneous determination of metoprolol tartrate and ramipril in human plasma.

    Science.gov (United States)

    Gowda, K Veeran; Mandal, Uttam; Senthamil Selvan, P; Sam Solomon, W D; Ghosh, Animesh; Sarkar, Amlan Kanti; Agarwal, Sangita; Nageswar Rao, T; Pal, Tapan Kumar

    2007-10-15

    A simple, rapid, sensitive and specific liquid chromatography-tandem mass spectrometry method was developed and validated for quantification of metoprolol tartrate (MT) and ramipril, in human plasma. Both the drugs were extracted by liquid-liquid extraction with diethyl ether-dichloromethane (70:30, v/v). The chromatographic separation was performed on a reversed-phase C8 column with a mobile phase of 10 mM ammonium formate-methanol (3:97, v/v). The protonated analyte was quantitated in positive ionization by multiple reaction monitoring with a mass spectrometer. The method was validated over the concentration range of 5-500 ng/ml for metoprolol and ramipril in human plasma. The precursor to product ion transitions of m/z 268.0-103.10 and m/z 417.20-117.20 were used to measure metoprolol and ramipril, respectively.

  15. High-performance liquid chromatography analysis methods developed for quantifying enzymatic esterification of flavonoids in ionic liquids.

    Science.gov (United States)

    Lue, Bena-Marie; Guo, Zheng; Xu, Xuebing

    2008-07-11

    Methods using reversed-phase high-performance liquid chromatography (RP-HPLC) with ELSD were investigated to quantify enzymatic reactions of flavonoids with fatty acids in the presence of diverse room temperature ionic liquids (RTILs). A buffered salt (preferably triethylamine-acetate) was found essential for separation of flavonoids from strongly polar RTILs, whereby RTILs were generally visible as two major peaks identified based on an ion-pairing/exchanging hypothesis. C8 and C12 stationary phases were optimal while mobile phase pH (3-7) had only a minor influence on separation. The method developed was successfully applied for primary screening of RTILs (>20), with in depth evaluation of substrates in 10 RTILs, for their evaluation as reaction media.

  16. Analytical method by high resolution liquid chromatography for the stability study of cloratidine syrup 0.1 %

    International Nuclear Information System (INIS)

    Torres Amaro, Leonid; Garcia Penna, Caridad M; Pardo Ruiz, Zenia

    2007-01-01

    A high resolution liquid chromatography method was validated to study the stability of cloratidine syrup 0.1 %. The calibration curve in the range from 13.6 to 3.36 μg/mL was lineal, with a coefficient of correlation equal to 0.99975. The intercept and slope statistical test was not significant. The recovery obtained was 100.2 % in the concentration range studied, and the Cochran and Student (t) tests results were not important. The variation coefficient in the repeatability study was equal to 0.41 % for 10 replications assayed, whereas in the reproducibility Fischer and Student tests were not remarkable. The method proved to be specific, lineal, accurate, and exact. (Author)

  17. Assessing Mucoadhesion in Polymer Gels: The Effect of Method Type and Instrument Variables

    Directory of Open Access Journals (Sweden)

    Jéssica Bassi da Silva

    2018-03-01

    Full Text Available The process of mucoadhesion has been widely studied using a wide variety of methods, which are influenced by instrumental variables and experiment design, making the comparison between the results of different studies difficult. The aim of this work was to standardize the conditions of the detachment test and the rheological methods of mucoadhesion assessment for semisolids, and introduce a texture profile analysis (TPA method. A factorial design was developed to suggest standard conditions for performing the detachment force method. To evaluate the method, binary polymeric systems were prepared containing poloxamer 407 and Carbopol 971P®, Carbopol 974P®, or Noveon® Polycarbophil. The mucoadhesion of systems was evaluated, and the reproducibility of these measurements investigated. This detachment force method was demonstrated to be reproduceable, and gave different adhesion when mucin disk or ex vivo oral mucosa was used. The factorial design demonstrated that all evaluated parameters had an effect on measurements of mucoadhesive force, but the same was not observed for the work of adhesion. It was suggested that the work of adhesion is a more appropriate metric for evaluating mucoadhesion. Oscillatory rheology was more capable of investigating adhesive interactions than flow rheology. TPA method was demonstrated to be reproducible and can evaluate the adhesiveness interaction parameter. This investigation demonstrates the need for standardized methods to evaluate mucoadhesion and makes suggestions for a standard study design.

  18. Peg Precipitation Coupled with Chromatography is a New and Sufficient Method for the Purification of Botulinum Neurotoxin Type B

    Science.gov (United States)

    Zhao, Yao; Kang, Lin; Gao, Shan; Gao, Xing; Xin, Wenwen; Wang, Jinglin

    2012-01-01

    Clostridium botulinum neurotoxins are used to treat a variety of neuro-muscular disorders, as well as in cosmetology. The increased demand requires efficient methods for the production and purification of these toxins. In this study, a new purification process was developed for purifying type B neurotoxin. The kinetics of C.botulinum strain growth and neurotoxin production were determined for maximum yield of toxin. The neurotoxin was purified by polyethylene glycol (PEG) precipitation and chromatography. Based on design of full factorial experiment, 20% (w/v) PEG-6000, 4°C, pH 5.0 and 0.3 M NaCl were optimal conditions to obtain a high recovery rate of 87% for the type B neurotoxin complex, as indicated by a purification factor of 61.5 fold. Furthermore, residual bacterial cells, impurity proteins and some nucleic acids were removed by PEG precipitation. The following purification of neurotoxin was accomplished by two chromatography techniques using Sephacryl™ S-100 and phenyl HP columns. The neurotoxin was recovered with an overall yield of 21.5% and the purification factor increased to 216.7 fold. In addition, a mouse bioassay determined the purified neurotoxin complex possessed a specific toxicity (LD50) of 4.095 ng/kg. PMID:22761863

  19. Validation of a liquid chromatography method for the simultaneous determination of sulfadimethoxine and trimethoprim and application to a stability study.

    Science.gov (United States)

    Louati, K; Mistiri, F; Kallel, M; Safta, F

    2010-03-01

    A liquid chromatography method is described for the simultaneous determination of sulfadimetoxine and trimethoprim from a veterinary formulation at the proportion of 187 mg and 40 mg respectively in presence of some excipient. The solution was subjected to different International Conference On Harmonisation prescribed stress conditions (hydrolysis, oxidation and photolysis). A stability-indicating high-performance liquid chromatography method was developed for the analysis of active substances in presence of their major degradation products. It involved a Knauer Eurospher C18 thermostated column at 25 degrees C, and 9.57 mM phosphate buffer (pH adjusted to 2.0 with orthophosphoric acid)-acetonitrile (70:30 v/v) as mobile phase. The mobile phase flow rate and sample volume injected were 1.2 mL/min and 20 microL, respectively. The selected wavelength for the determination was 248 nm. The method was validated for linearity, precision, accuracy and specificity, and then applied to a stability study of sulfadimetoxine and trimethoprim in the veterinary solution packaged in high density polyethylene plastic bottles of 1 L and 100 mL thermosealed and no thermosealed and corked by a white cap, at both accelerated and long-term conditions required by the International Conference On Harmonisation. The method developed, which separates all of the most degradation products formed under variety of conditions, proved to be simple, accurate, precise and specific. The results of the stress degradation show that the solution is more sensitive to hydrolysis. The stability studies carried out on three batches of each presentation show that the finished product remains stable for six months. Copyright 2010 Elsevier Masson SAS. All rights reserved.

  20. Determination of parabens using two microextraction methods coupled with capillary liquid chromatography-UV detection.

    Science.gov (United States)

    Chen, Chen-Wen; Hsu, Wen-Chan; Lu, Ya-Chen; Weng, Jing-Ru; Feng, Chia-Hsien

    2018-02-15

    Parabens are common preservatives and environmental hormones. As such, possible detrimental health effects could be amplified through their widespread use in foods, cosmetics, and pharmaceutical products. Thus, the determination of parabens in such products is of particular importance. This study explored vortex-assisted dispersive liquid-liquid microextraction techniques based on the solidification of a floating organic drop (VA-DLLME-SFO) and salt-assisted cloud point extraction (SA-CPE) for paraben extraction. Microanalysis was performed using a capillary liquid chromatography-ultraviolet detection system. These techniques were modified successfully to determine four parabens in 19 commercial products. The regression equations of these parabens exhibited good linearity (r 2 =0.998, 0.1-10μg/mL), good precision (RSD<5%) and accuracy (RE<5%), reduced reagent consumption and reaction times (<6min), and excellent sample versatility. VA-DLLME-SFO was also particularly convenient due to the use of a solidified extract. Thus, the VA-DLLME-SFO technique was better suited to the extraction of parabens from complex matrices. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. A method for retrieving endodontic or atypical nonendodontic separated instruments from the root canal: a report of two cases.

    Science.gov (United States)

    Monteiro, Jardel Camilo do Carmo; Kuga, Milton Carlos; Dantas, Andrea Abi Rached; Jordão-Basso, Keren Cristina Fagundes; Keine, Katia Cristina; Ruchaya, Prashant Jay; Faria, Gisele; Leonardo, Renato de Toledo

    2014-11-01

    This clinical report presents a new method for retrieving separated instruments from the root canal with minimally invasive procedures. The presence of separated instrument in root canal may interfere in the endodontic treatment prognosis. There are several recommended methods to retrieve separated instruments, but some are difficult in clinically practice. This study describes two cases of separated instrument removal from the root canal using a stainless-steel prepared needle associated with a K-file. Case 1 presented a fractured gutta-percha condenser within the mandibular second premolar, it was separated during incorrect intracanal medication calcium hydroxide placement. Case 2 had a fractured sewing needle within the upper central incisor that the patient used to remove food debris from the root canal. After cervical preparation, the fractured instruments were fitted inside a prepared needle and then an endodontic instrument (#25 K-file) was adapted with clockwise turning motion between the needle inner wall and the fragment. The endodontic or atypical nonendodontic separated instrument may be easily pull on of the root canal using a single and low cost device. The methods for retrieving separated instruments from root canal are difficult and destructive procedures. The present case describes a simple method to solve this problem.

  2. Main Achievements 2003-2004 - Interdisciplinary Research - Radiation detection methods for health, earth and environmental sciences - Detection methods in gas chromatography

    International Nuclear Information System (INIS)

    2005-01-01

    Detection methods in gas chromatography are under development, especially ultra-sensitive gas chromatography detection methods to monitor the atmosphere (with respect to gases active in the destruction of the Earth ozone layer). A new chromatographic method has been elaborated for Ne determination, and technique for determination of Ar and N 2 in groundwater has been significantly improved. Measurements of neon are performed by means of a chromatographic system equipped with a helium ionization detector (PD-HID) doped with neon pulse discharge, working with a modified sample introduction system. The Ar and N 2 contents are determined by a thermal-conductivity detector (TCD). The problem of separation of Ar from O 2 has been solved by catalytic removal of the latter from the sample. The measurement reproducibility is 1%, 2% and 0.5% for Ar, Ne and N 2 , respectively. Both methods were successfully applied in measurements of groundwaters in the Cracow area. The excess air contents are in the range of about 1 to 3 cm 3 STP L-1. The values of recharge temperatures for Holocen water agree reasonably well with the yearly mean long-term surface air temperature (8.2 o C)

  3. Chromatography resin support

    Science.gov (United States)

    Dobos, James G.

    2002-01-01

    An apparatus and method of using an improved chromatography resin support is disclosed. The chromatography support platform is provided by a stainless steel hollow cylinder adapted for being inserted into a chromatography column. An exterior wall of the stainless steel cylinder defines a groove for carrying therein an "O"-ring. The upper surface of the stainless steel column is covered by a fine stainless steel mesh welded to the edges of the stainless steel cylinder. When placed upon a receiving ledge defined within a chromatography column, the "O"-ring provides a fluid tight seal with the inner edge wall of the chromatography cylinder. The stainless steel mesh supports the chromatography matrix and provides a back flushable support which is economical and simple to construct.

  4. Separation techniques: Chromatography

    Science.gov (United States)

    Coskun, Ozlem

    2016-01-01

    Chromatography is an important biophysical technique that enables the separation, identification, and purification of the components of a mixture for qualitative and quantitative analysis. Proteins can be purified based on characteristics such as size and shape, total charge, hydrophobic groups present on the surface, and binding capacity with the stationary phase. Four separation techniques based on molecular characteristics and interaction type use mechanisms of ion exchange, surface adsorption, partition, and size exclusion. Other chromatography techniques are based on the stationary bed, including column, thin layer, and paper chromatography. Column chromatography is one of the most common methods of protein purification. PMID:28058406

  5. Chromatography of phosphorus oxoacids

    International Nuclear Information System (INIS)

    Ohashi, S.

    1975-01-01

    The present state of studies on the chromatographic separation of phosphorus oxoacids is surveyed. In this paper, chromatographic techniques are divided into four groups, i.e. paper and thin-layer chromatography, paper electrophoresis, ion-exchange chromatography, and gel chromatography. The separation mechanisms and characteristics for these chromatographic methods are discussed and some examples for the separation of phosphorus oxoacids are described. As examples of the application of ion-exchange and gel chromatography, studies on the hot atom chemistry of 32 P in solid inorganic phosphates and those on the substitution reactions between diphosphonate (diphosphite) and polyphosphates are reported. (author)

  6. A method of estimating GPS instrumental biases with a convolution algorithm

    Science.gov (United States)

    Li, Qi; Ma, Guanyi; Lu, Weijun; Wan, Qingtao; Fan, Jiangtao; Wang, Xiaolan; Li, Jinghua; Li, Changhua

    2018-03-01

    This paper presents a method of deriving the instrumental differential code biases (DCBs) of GPS satellites and dual frequency receivers. Considering that the total electron content (TEC) varies smoothly over a small area, one ionospheric pierce point (IPP) and four more nearby IPPs were selected to build an equation with a convolution algorithm. In addition, unknown DCB parameters were arranged into a set of equations with GPS observations in a day unit by assuming that DCBs do not vary within a day. Then, the DCBs of satellites and receivers were determined by solving the equation set with the least-squares fitting technique. The performance of this method is examined by applying it to 361 days in 2014 using the observation data from 1311 GPS Earth Observation Network (GEONET) receivers. The result was crosswise-compared with the DCB estimated by the mesh method and the IONEX products from the Center for Orbit Determination in Europe (CODE). The DCB values derived by this method agree with those of the mesh method and the CODE products, with biases of 0.091 ns and 0.321 ns, respectively. The convolution method's accuracy and stability were quite good and showed improvements over the mesh method.

  7. Two-step Purification Method for Aging Pigments A2E and Iso-A2E Using Medium Pressure Liquid Chromatography

    International Nuclear Information System (INIS)

    Park, Sang Il; Park, Sang Cheol; Kim, So Ra; Jang, Young Pyo

    2016-01-01

    A newly modified method for the efficient purification of A2E and iso-A2E using reverse phase silica gel resin with medium pressure liquid chromatography (MPLC) was suggested. MPLC is one of the various preparative column chromatography techniques and separation under pressure renders the use of smaller particle size resins possible and increases the diversity of available stationary phases. A simplified two-step purification method was developed for the purification of aging pigments in eye, A2E and iso-A2E. With simple two-step elution of mobile phase in reverse phase MPLC, A2E and iso-A2E were successfully purified with great efficiency compare with previous column chromatography and HPLC method. This method provides more simple, convenient, cost-effective, and less time-consuming procedure for mass purification of aging pigments A2E and iso-A2E

  8. Two-step Purification Method for Aging Pigments A2E and Iso-A2E Using Medium Pressure Liquid Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Park, Sang Il; Park, Sang Cheol [Kyunghee Univ., Seoul (Korea, Republic of); Kim, So Ra; Jang, Young Pyo [Seoul National Univ., Seoul (Korea, Republic of)

    2016-09-15

    A newly modified method for the efficient purification of A2E and iso-A2E using reverse phase silica gel resin with medium pressure liquid chromatography (MPLC) was suggested. MPLC is one of the various preparative column chromatography techniques and separation under pressure renders the use of smaller particle size resins possible and increases the diversity of available stationary phases. A simplified two-step purification method was developed for the purification of aging pigments in eye, A2E and iso-A2E. With simple two-step elution of mobile phase in reverse phase MPLC, A2E and iso-A2E were successfully purified with great efficiency compare with previous column chromatography and HPLC method. This method provides more simple, convenient, cost-effective, and less time-consuming procedure for mass purification of aging pigments A2E and iso-A2E.

  9. Automatic Recognition Method for Optical Measuring Instruments Based on Machine Vision

    Institute of Scientific and Technical Information of China (English)

    SONG Le; LIN Yuchi; HAO Liguo

    2008-01-01

    Based on a comprehensive study of various algorithms, the automatic recognition of traditional ocular optical measuring instruments is realized. Taking a universal tools microscope (UTM) lens view image as an example, a 2-layer automatic recognition model for data reading is established after adopting a series of pre-processing algorithms. This model is an optimal combination of the correlation-based template matching method and a concurrent back propagation (BP) neural network. Multiple complementary feature extraction is used in generating the eigenvectors of the concurrent network. In order to improve fault-tolerance capacity, rotation invariant features based on Zernike moments are extracted from digit characters and a 4-dimensional group of the outline features is also obtained. Moreover, the operating time and reading accuracy can be adjusted dynamically by setting the threshold value. The experimental result indicates that the newly developed algorithm has optimal recognition precision and working speed. The average reading ratio can achieve 97.23%. The recognition method can automatically obtain the results of optical measuring instruments rapidly and stably without modifying their original structure, which meets the application requirements.

  10. Simplified and rapid method for extraction of ergosterol from natural samples and detection with quantitative and semi-quantitative methods using thin-layer chromatography

    OpenAIRE

    Larsen, Cand.scient Thomas; Ravn, Senior scientist Helle; Axelsen, Senior Scientist Jørgen

    2004-01-01

    A new and simplified method for extraction of ergosterol (ergoste-5,7,22-trien-3-beta-ol) from fungi in soil and litter was developed using pre-soaking extraction and paraffin oil for recovery. Recoveries of ergosterol were in the range of 94 - 100% depending on the solvent to oil ratio. Extraction efficiencies equal to heat-assisted extraction treatments were obtained with pre-soaked extraction. Ergosterol was detected with thin-layer chromatography (TLC) using fluorodensitometry with a quan...

  11. The potential of soft computing methods in NPP instrumentation and control

    International Nuclear Information System (INIS)

    Hampel, R.; Chaker, N.; Kaestner, W.; Traichel, A.; Wagenknecht, M.; Gocht, U.

    2002-01-01

    The method of signal processing by soft computing include the application of fuzzy logic, synthetic neural networks, and evolutionary algorithms. The article contains an outline of the objectives and results of the application of fuzzy logic and methods of synthetic neural networks in nuclear measurement and control. The special requirements to be met by the software in safety-related areas with respect to reliability, evaluation, and validation are described. Possible uses may be in off-line applications in modeling, simulation, and reliability analysis as well as in on-line applications (real-time systems) for instrumentation and control. Safety-related aspects of signal processing are described and analyzed for the fuzzy logic and synthetic neural network concepts. Application are covered in selected examples. (orig.)

  12. Comparison of methods and instruments for 222Rn/220Rn progeny measurement

    International Nuclear Information System (INIS)

    Liu Yanyang; Shang Bing; Wu Yunyun; Zhou Qingzhi

    2012-01-01

    In this paper, comparisons were made among three methods of measurement (grab measurement, continuous measurement and integrating measurement) and also measurement of different instruments for a radon/thoron mixed chamber. Taking the optimized five-segment method as a comparison criterion, for the equilibrium-equivalent concentration of 222 Rn, measured results of Balm and 24 h integrating detectors are 31% and 29% higher than the criterion, the results of Wl x, however, is 20% lower; and for 220 Rn progeny, the results of Fiji-142, Kf-602D, BWLM and 24 h integrating detector are 86%, 18%, 28% and 36% higher than the criterion respectively, except that of WLx, which is 5% lower. For the differences shown, further research is needed. (authors)

  13. A method of sample preparation for N15 determination in amino acids separated by paper chromatography

    International Nuclear Information System (INIS)

    Secer, M.

    1988-01-01

    The amino acids separated with two dimensional paper chromatography were isolated in two ways which make their 15 N determination possible 1) After developing the spots of chromatograms with ninhydrin they were cut out and shaken 30' with 2 ml dist. H 2 O. To destroy the ninhydrin-NH 3 colour complex, the extraction solution was heated in boiling waterbath for 10' and then 0.5 ml 2 N HCl was added to the solution and continued to heat for further 10'. For the 15 N determination of amino acids by emissionspectrometer this colour complex must be destroyed completely. It was reached with adding 2 ml 30% H 2 O 2 to the solution and heating it 5' in 100 0 C waterbath. After the evaporation of colourless solution under IR-lamp at 70 0 C, the white powder was dissolved with 50 ul dist. H 2 O and centrifuged 10'. The clear supernatant was used to gain N 2 gas by the CuO/CaO combustion. N 2 gas is necessary for the 15 N/ 14 N ratio determination by emissionsspectrometer. 2) In the second way, the destroying of ninhydrin-NH 3 colour complex was easier and quicker this way the spots were eluted (extracted) with 50% alcohol and 30% H 2O2 with 1:1 ratio. After shaking the solution 30', it turns quite colourless. It means that the ninhydrin-NH 3 colour complex was completely destroyed. Further works have been done as described in the first way. We have found out that one amino acid should have 10-20 ug N in it to assess the 15 N enrichment. In order to attain this quantity of N for certain amino acids, the spots of three separately run chromatograms were combined

  14. Analytical Chemistry Laboratory (ACL) procedure compendium. Volume 3, Inorganic instrumental methods

    Energy Technology Data Exchange (ETDEWEB)

    1993-08-01

    The methods cover: C in solutions, F (electrode), elements by atomic emission spectrometry, inorganic anions by ion chromatography, Hg in water/solids/sludges, As, Se, Bi, Pb, data calculations for SST (single shell tank?) samples, Sb, Tl, Ag, Pu, O/M ratio, ignition weight loss, pH value, ammonia (N), Cr(VI), alkalinity, U, C sepn. from soil/sediment/sludge, Pu purif., total N, water, C and S, surface Cl/F, leachable Cl/F, outgassing of Ge detector dewars, gas mixing, gas isotopic analysis, XRF of metals/alloys/compounds, H in Zircaloy, H/O in metals, inpurity extraction, reduced/total Fe in glass, free acid in U/Pu solns, density of solns, Kr/Xe isotopes in FFTF cover gas, H by combustion, MS of Li and Cs isotopes, MS of lanthanide isotopes, GC operation, total Na on filters, XRF spectroscopy QC, multichannel analyzer operation, total cyanide in water/solid/sludge, free cyanide in water/leachate, hydrazine conc., ICP-MS, {sup 99}Tc, U conc./isotopes, microprobe analysis of solids, gas analysis, total cyanide, H/N{sub 2}O in air, and pH in soil.

  15. Comparison of neutron activation analysis with other instrumental methods for elemental analysis of airborne particulate matter

    International Nuclear Information System (INIS)

    Regge, P. de; Lievens, F.; Delespaul, I.; Monsecour, M.

    1976-01-01

    A comparison of instrumental methods, including neutron activation analysis, X-ray fluorescence spectrometry, atomic absorption spectrometry and emission spectrometry, for the analysis of heavy metals in airborne particulate matter is described. The merits and drawbacks of each method for the routine analysis of a large number of samples are discussed. The sample preparation technique, calibration and statistical data relevant to each method are given. Concordant results are obtained by the different methods for Co, Cu, Ni, Pb and Zn. Less good agreement is obtained for Fe, Mn and V. The results are not in agreement for the elements Cd and Cr. Using data obtained on the dust sample distributed by Euratom-ISPRA within the framework of an interlaboratory comparison, the accuracy of each method for the various elements is estimated. Neutron activation analysis was found to be the most sensitive and accurate of the non-destructive analysis methods. Only atomic absorption spectrometry has a comparable sensitivity, but requires considerable preparation work. X-ray fluorescence spectrometry is less sensitive and shows biases for Cr and V. Automatic emission spectrometry with simultaneous measurement of the beam intensities by photomultipliers is the fastest and most economical technique, though at the expense of some precision and sensitivity. (author)

  16. Separation of metals in the form of ion associates by the method of thin-layer chromatography

    International Nuclear Information System (INIS)

    Shapovalova, E.N.; Timerbaev, A.R.; Bol'shova, T.A.; Mel'nik, S.V.; Kordejro, E.

    1990-01-01

    Behaviour of pyridylazo resorcinates of certain metals (Ga, In, Fe, Co) in the form of ionic pairs with tri-n-octylamine (TOA) under conditions of thin-layer chromatography (TLC) has been studied. For all eluents investigated Ga and In complexes possess the highest mobility. Selectivity of ionic associate separation decreases with an increase in mobile phase polarity. Mixtures with 10-15 % content of isopropanol in eluating solution are the optimal ones. Separation of Ga and In from Fe 3+ and Co takes place with separation criterion 3.1 and 4.1 respectively. An attempt to separate ionic associates of In and Ga failed owing to similar stability of their pyridylazoresorcinates. Solution of the problem of In and Ga determination in the presence of iron can contribute to concrete application of the method

  17. Analytical method by high resolution-liquid chromatography for assay of 2 g Clonazepam tablets disolution without lactose

    International Nuclear Information System (INIS)

    Garcia Penna, Caridad M; Diego Leon, Rafael; Castinneira Diaz, Mirta; Hernandez Cervera, Mirna; Martinez Espinosa, Vivian

    2007-01-01

    A valid method was developed to assess 2 mg Clonazepam tablets disolution without lactose by high-performance liquid chromatography by UV detection to 254 nm. Establishment of Clonazepam in dissolution medium was confirmed, and parameters of specificity, linearity, and accuracy were assessed, as well as influence of filtration and stability or active principle. Linearity curve was drawed in rank of 1, 2-2,6 μg/mL, with a correlation coefficient similar to 0,99418; statistical test wasn't statistically significant for interceptor and slope. In study, it was possible to demonstrate that stability or active principle in dissolution was maintained in more than double of duration of dissolution assay. (Author)

  18. [Study on the analytical methods of catechins in tea and green tea polyphenol samples by high performance liquid chromatography].

    Science.gov (United States)

    Dai, J; Wang, H X; Chen, S W; Tang, J

    2001-09-01

    Hypersil BDS C18 and Zorbax SB C18, suitable to separate simultaneously seven kinds of catechins and caffeine, were screened out from seven brands of reversed-phase columns. Mobile phase was a solution of methanol-water-acetic acid (or trifluoro acetic acid). Seven kinds of catechins in tea samples from six places in China and three green tea polyphenol(GTP) samples from different producers were separated and determined in 30 min by isocratic and gradient elutions. The effects of mobile phase components and temperature of column on retention parameters of catechins and caffeine are reviewed. Chromatographic conditions and pretreatment methods of samples were optimized. Gallocatechin gallate(GCG) and (-)-catechin gallate(CG) were identified by electrospray ionization mass spectrometry(ESI-MS) and prepared by high performance liquid chromatography for quantitative analysis. The other catechins, (-)-epigallocatechin (EGC), (+)-catechin (D-C), (-)-epicatechin(EC), (-)-epigallocatechin gallate(EGCG), (-)-epicatechin gallate(ECG) were identified with standards.

  19. Development of a high-performance liquid chromatography method for the determination of florfenicol in animal feedstuffs.

    Science.gov (United States)

    Yang, JinJing; Sun, GuiZhi; Qian, MingRong; Huang, LingLi; Ke, XianBing; Yang, Bo

    2017-11-15

    An effective thin layer chromatography (TLC) purification procedure coupled to high-performance liquid chromatography (HPLC) method was developed for the determination of florfenicol (FF) in pig, chicken and fish feedstuffs. The feedstuff samples were extracted with ethyl acetate, defatted with n-hexane saturated with acetonitrile, and further purified by TLC. The chromatographic separation was performed on a Waters Symmetry C 18 column using an isocratic procedure with acetonitrile-water (35:65, v/v) at 0.6mL/min. The ultraviolet (UV) detector was set at a wavelength of 225nm. The FF concentrations in feedstuff samples were quantified using a standard curve. Good linear correlations (y=159075x-15054, r>0.9999) were achieved within the concentration range of 0.05-200μg/mL. The recoveries of FF spiked at levels of 1, 100 and 1000μg/g ranged from 80.6% to 105.3% with the intra-day and inter-day relative standard deviation (RSD) less than 9.3%. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.02 and 0.06mg/kg for pig feedstuffs, 0.02 and 0.07mg/kg for chicken feedstuffs, and 0.02 and 0.05mg/kg for fish feedstuffs, respectively. This reliable, simple and cost-effective method could be applied to the routine monitoring of FF in animal feedstuffs. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. New ultra-performance liquid chromatography-tandem mass spectrometry method for the determination of irbesartan in human plasma

    Directory of Open Access Journals (Sweden)

    Tanveer A. Wani

    2015-09-01

    Full Text Available With the objective of reducing analysis time and maintaining good efficiency, there has been substantial focus on high-speed chromatographic separations and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS is a preeminent analytical tool for rapid biomedical analysis. In this study a simple, rapid, sensitive, and specific ultra-performance liquid chromatography-MS/MS method was developed and validated for quantification of the angiotensin II receptor antagonist, irbesartan (IRB, in human plasma. After a simple protein precipitation using methanol and acetonitrile, IRB and internal standard (IS telmisartan were separated on Acquity UPLC BEH C18 column (50 mm × 2.1 mm, i.d. 1.7 μm, Waters, Milford, MA, USA using a mobile phase consisted of acetonitrile: methanol: 10 mM ammonium acetate (70: 15: 15 v/v/v with a flow rate of 0.4 mL/min and detected MS/MS in negative ion mode. The ion transitions recorded in multiple reaction monitoring mode were m/z 427.2→193.08 for IRB and m/z 513.2→469.3 for IS. The assay exhibited a linear dynamic range of 2–500 ng/mL for IRB in human plasma with good correlation coefficient of (0.995 and with a lower limit of quantitation of 2 ng/mL. The intra- and interassay precisions were satisfactory; the relative standard deviations did not exceed 9.91%. The proposed UPLC-MS/MS method is simple, rapid, and highly sensitive, and hence it could be reliable for pharmacokinetic and toxicokinetic study in both animals and humans.

  1. Method for the direct determination of available carbohydrates in low-carbohydrate products using high-performance anion exchange chromatography.

    Science.gov (United States)

    Ellingson, David; Potts, Brian; Anderson, Phillip; Burkhardt, Greg; Ellefson, Wayne; Sullivan, Darryl; Jacobs, Wesley; Ragan, Robert

    2010-01-01

    An improved method for direct determination of available carbohydrates in low-level products has been developed and validated for a low-carbohydrate soy infant formula. The method involves modification of an existing direct determination method to improve specificity, accuracy, detection levels, and run times through a more extensive enzymatic digestion to capture all available (or potentially available) carbohydrates. The digestion hydrolyzes all common sugars, starch, and starch derivatives down to their monosaccharide components, glucose, fructose, and galactose, which are then quantitated by high-performance anion-exchange chromatography with photodiode array detection. Method validation consisted of specificity testing and 10 days of analyzing various spike levels of mixed sugars, maltodextrin, and corn starch. The overall RSD was 4.0% across all sample types, which contained within-day and day-to-day components of 3.6 and 3.4%, respectively. Overall average recovery was 99.4% (n = 10). Average recovery for individual spiked samples ranged from 94.1 to 106% (n = 10). It is expected that the method could be applied to a variety of low-carbohydrate foods and beverages.

  2. Detailed characterizations of a Comparative Reactivity Method (CRM) instrument: experiments vs. modelling

    Science.gov (United States)

    Michoud, V.; Hansen, R. F.; Locoge, N.; Stevens, P. S.; Dusanter, S.

    2015-04-01

    The Hydroxyl radical (OH) is an important oxidant in the daytime troposphere that controls the lifetime of most trace gases, whose oxidation leads to the formation of harmful secondary pollutants such as ozone (O3) and Secondary Organic Aerosols (SOA). In spite of the importance of OH, uncertainties remain concerning its atmospheric budget and integrated measurements of the total sink of OH can help reducing these uncertainties. In this context, several methods have been developed to measure the first-order loss rate of ambient OH, called total OH reactivity. Among these techniques, the Comparative Reactivity Method (CRM) is promising and has already been widely used in the field and in atmospheric simulation chambers. This technique relies on monitoring competitive OH reactions between a reference molecule (pyrrole) and compounds present in ambient air inside a sampling reactor. However, artefacts and interferences exist for this method and a thorough characterization of the CRM technique is needed. In this study, we present a detailed characterization of a CRM instrument, assessing the corrections that need to be applied on ambient measurements. The main corrections are, in the order of their integration in the data processing: (1) a correction for a change in relative humidity between zero air and ambient air, (2) a correction for the formation of spurious OH when artificially produced HO2 react with NO in the sampling reactor, and (3) a correction for a deviation from pseudo first-order kinetics. The dependences of these artefacts to various measurable parameters, such as the pyrrole-to-OH ratio or the bimolecular reaction rate constants of ambient trace gases with OH are also studied. From these dependences, parameterizations are proposed to correct the OH reactivity measurements from the abovementioned artefacts. A comparison of experimental and simulation results is then discussed. The simulations were performed using a 0-D box model including either (1) a

  3. A reversed-phase high-performance liquid chromatography method for the determination of cotrimoxazole (trimethoprim/ sulphamethoxazole) in children treated for malaria

    DEFF Research Database (Denmark)

    Rønn, A M; Mutabingwa, T K; Kreisby, S

    1999-01-01

    A high-performance liquid chromatography (HPLC) method was developed for the simultaneous analysis of trimethoprim (TMP), sulphamethoxazole (SMX), and acetylsulphamethoxazole (AcSMX) in small amounts of blood. The method involved precipitation with 50 microL trichloracetic acid (1M) to 125 micro...

  4. METHOD 544. DETERMINATION OF MICROCYSTINS AND NODULARIN IN DRINKING WATER BY SOLID PHASE EXTRACTION AND LIQUID CHROMATOGRAPHY/TANDEM MASS SPECTROMETRY (LC/MS/MS)

    Science.gov (United States)

    Method 544 is an accurate and precise analytical method to determine six microcystins (including MC-LR) and nodularin in drinking water using solid phase extraction and liquid chromatography tandem mass spectrometry (SPE-LC/MS/MS). The advantage of this SPE-LC/MS/MS is its sensi...

  5. Using method triangulation to validate a new instrument (CPWQ-com) assessing cancer patients' satisfaction with communication

    DEFF Research Database (Denmark)

    Ross, Lone; Lundstrøm, Louise Hyldborg; Petersen, Morten Aagaard

    2012-01-01

    Patients' perceptions of care including the communication with health care staff is recognized as an important aspect of the quality of cancer care. Using mixed methods, we developed and validated a short instrument assessing this communication.......Patients' perceptions of care including the communication with health care staff is recognized as an important aspect of the quality of cancer care. Using mixed methods, we developed and validated a short instrument assessing this communication....

  6. Methods and instrumentation for investigating Hall sensors during their irradiation in nuclear research reactors

    International Nuclear Information System (INIS)

    Bolshakova, I.; Holyaka, R.; Makido, E.; Marusenkov, A.; Shurygin, F.; Yerashok, V.; Moreau, P. J.; Vayakis, G.; Duran, I.; Stockel, J.; Chekanov, V.; Konopleva, R.; Nazarkin, I.; Kulikov, S.; Leroy, C.

    2009-01-01

    Present work discusses the issues of creating the instrumentation for testing the semiconductor magnetic field sensors during their irradiation with neutrons in nuclear reactors up to fluences similar to neutron fluences in steady-state sensor locations in ITER. The novelty of the work consists in Hall sensor parameters being investigated: first, directly during the irradiation (in real time), and, second, at high irradiation levels (fast neutron fluence > 10 18 n/cm 2 ). Developed instrumentation has been successfully tested and applied in the research experiments on radiation stability of magnetic sensors in IBR-2 (JINR, Dubna) and VVR-M (PNPI, Saint-Petersburg) reactors. The 'Remote-Rad' bench consists of 2 heads (head 1 and head 2) bearing investigated sensors put in a ceramic setting, of electronic unit, of personal computer and of signal lines. Each head contains 6 Hall sensors and a coil for generating test magnetic field. Moreover head 1 contains thermocouples for temperature measurement while the temperature of head 2 is measured by thermo-resistive method. The heads are placed in the reactor channel

  7. A fully Bayesian method for jointly fitting instrumental calibration and X-ray spectral models

    International Nuclear Information System (INIS)

    Xu, Jin; Yu, Yaming; Van Dyk, David A.; Kashyap, Vinay L.; Siemiginowska, Aneta; Drake, Jeremy; Ratzlaff, Pete; Connors, Alanna; Meng, Xiao-Li

    2014-01-01

    Owing to a lack of robust principled methods, systematic instrumental uncertainties have generally been ignored in astrophysical data analysis despite wide recognition of the importance of including them. Ignoring calibration uncertainty can cause bias in the estimation of source model parameters and can lead to underestimation of the variance of these estimates. We previously introduced a pragmatic Bayesian method to address this problem. The method is 'pragmatic' in that it introduced an ad hoc technique that simplified computation by neglecting the potential information in the data for narrowing the uncertainty for the calibration product. Following that work, we use a principal component analysis to efficiently represent the uncertainty of the effective area of an X-ray (or γ-ray) telescope. Here, however, we leverage this representation to enable a principled, fully Bayesian method that coherently accounts for the calibration uncertainty in high-energy spectral analysis. In this setting, the method is compared with standard analysis techniques and the pragmatic Bayesian method. The advantage of the fully Bayesian method is that it allows the data to provide information not only for estimation of the source parameters but also for the calibration product—here the effective area, conditional on the adopted spectral model. In this way, it can yield more accurate and efficient estimates of the source parameters along with valid estimates of their uncertainty. Provided that the source spectrum can be accurately described by a parameterized model, this method allows rigorous inference about the effective area by quantifying which possible curves are most consistent with the data.

  8. MODERN INSTRUMENTAL METHODS TO CONTROL THE SEED QUALITY IN ROOT VEGETABLES

    Directory of Open Access Journals (Sweden)

    F. B. Musaev

    2017-01-01

    Full Text Available The standard methods of analysis don’t meet all modern requirements to determine the seed a quality. These methods can’t unveil inner deficiencies that are very important to control seed viability. The capabilities of new instrumental method to analyze the seed quality of root vegetables were regarded in the article. The method of micro-focus radiography is distinguished from other existing methods by more sensitivity, rapidity and easiness to be performed. Based on practical importance the visualization of inner seed structure, it allows determining far before seed germination the degree of endosperm development and embryo; the presence of inner damages and infections, occupation and damage caused by pests. The use of micro-focus radiography enables to detect the degree of seed quality difference for some traits such as monogermity and self-fertilization that are economically valuable for breeding program in red beet. With the aid of the method the level of seed development, damage and inner deficiencies in carrot and parsnip can be revealed. In X-ray projection seeds of inbred lines of radish significantly differed from variety population ones for their underdevelopment in the inner structure. The advantage of the method is that seeds rest undamaged after quality analyzing and both can be used for further examination with the use of other methods or be sown; that is quite important for breeders, when handling with small quantity or collectable plant breeding material. The results radiography analyses can be saved and archived that enables to watch for seed qualities in dynamic; this data can be also used at possible arbitration cases. 

  9. A validated high performance thin layer chromatography method for determination of yohimbine hydrochloride in pharmaceutical preparations

    OpenAIRE

    Jihan M Badr

    2013-01-01

    Background: Yohimbine is an indole alkaloid used as a promising therapy for erectile dysfunction. A number of methods were reported for the analysis of yohimbine in the bark or in pharmaceutical preparations. Materials and Method: In the present work, a simple and sensitive high performance thin layer chromatographic method is developed for determination of yohimbine (occurring as yohimbine hydrochloride) in pharmaceutical preparations and validated according to International Conference of Ha...

  10. Development of a liquid chromatography-electrospray chemical ionization tandem mass spectrometry analytical method for analysis of eleven hydroxylated polybrominated diphenyl ethers.

    Science.gov (United States)

    Feo, Maria Luisa; Barón, Enrique; Aga, Diana S; Eljarrat, Ethel; Barceló, Damià

    2013-08-02

    Recently, hydroxylated polybrominated diphenyl ethers (OH-PBDEs) have emerged as environmentally relevant pollutants due to recent reports of their natural production and metabolism. Recent mechanistic studies in human and rats have shown that some OH-PBDEs are more potent than parent compounds (PBDEs) and may contribute substantially to neurodevelopmental disorders by direct neurotoxicity, or indirectly through altered thyroid disruption. However, analytical methodologies for determination of OH-PBDEs are currently limited. In this study a robust liquid chromatography-electrospray tandem triple quadrupole-linear ion trap mass spectrometer (LC-ESI-QqLIT-MS-MS) in negative mode method was developed for the determination of eleven OH-tri- to OH-hexa-PBDEs. Two different columns were tested and compared for chromatographic separation: a C18 BetaBasic and a Purospher STAR RP 18, working at pH 8 and 10, respectively. Mobile phase (acetonitrile:water) was optimized by changing the pH of the aqueous phase and the concentration of the organic modifier (methanol). The MS-MS parameters (declustering potential (DP), collision energy (CE) and cell exit potential (CXP)) were optimized. Selected reaction monitoring (SRM) was used in order to increase sensitivity. Two SRM transitions ([M-H](-)>[Br](-)) were selected for each OH-PBDE, one for quantification and the second one for confirmation. Under the optimized conditions, the instrumental limits of detection were between 0.17 and 0.72injectedpg. The method provided good linearity (r>0.99 for a concentration range of 0.30-100ng/mL), accuracy and precision (%Dev and %RSD≤20% for intra- and inter-assays). Copyright © 2013 Elsevier B.V. All rights reserved.

  11. Quality evaluation of fish and other seafood by traditional and nondestructive instrumental methods: Advantages and limitations.

    Science.gov (United States)

    Hassoun, Abdo; Karoui, Romdhane

    2017-06-13

    Although being one of the most vulnerable and perishable products, fish and other seafoods provide a wide range of health-promoting compounds. Recently, the growing interest of consumers in food quality and safety issues has contributed to the increasing demand for sensitive and rapid analytical technologies. Several traditional physicochemical, textural, sensory, and electrical methods have been used to evaluate freshness and authentication of fish and other seafood products. Despite the importance of these standard methods, they are expensive and time-consuming, and often susceptible to large sources of variation. Recently, spectroscopic methods and other emerging techniques have shown great potential due to speed of analysis, minimal sample preparation, high repeatability, low cost, and, most of all, the fact that these techniques are noninvasive and nondestructive and, therefore, could be applied to any online monitoring system. This review describes firstly and briefly the basic principles of multivariate data analysis, followed by the most commonly traditional methods used for the determination of the freshness and authenticity of fish and other seafood products. A special focus is put on the use of rapid and nondestructive techniques (spectroscopic techniques and instrumental sensors) to address several issues related to the quality of these products. Moreover, the advantages and limitations of each technique are reviewed and some perspectives are also given.

  12. New method for determination of epichlorohydrin in epoxy-coated cans by oxolane derivatization and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Sung, Jun Hyun; Lee, Young Ja; Park, Hyun Jin

    2008-08-01

    A new method was developed for the determination of epichlorohydrin (ECH) in food contact surface of epoxy-coated cans. The oxolane derivative, which produced by reaction of epoxy moiety in ECH with cyclopentanone in the presence of borontrifluoride-diethyletherate, was analyzed by gas chromatography (GC)/mass spectrometry (MS). 1,2-Epoxyhexane was used as internal standard (IS), which produced an oxolane derivative under the same reaction mechanism as ECH. The developed method was validated with 1 ng ml(-1) of limit of detection (LOD, surface area related 20 ng dm(-2)), >0.999 of linearity. Good precision, which was tested both in terms of intra-day repeatability and inter-day reproducibility, and 97.3-102.7% of good recoveries were obtained on three spiked levels of 5.2, 40.3 and 149.1 ng ml(-1). The excellent validation data suggests that this method is more simple, quick and effective than the official method in European Committee for Standardization (CEN) to determine the residual amount of ECH in food contact materials for food law compliance test. The residual amount of ECH for 13 epoxy-coated can samples was analyzed, and none of the samples was found to be detectable levels of ECH in epoxy-coated cans.

  13. Toxic Cyanobacteria in Svalbard: Chemical Diversity of Microcystins Detected Using a Liquid Chromatography Mass Spectrometry Precursor Ion Screening Method

    Directory of Open Access Journals (Sweden)

    Julia Kleinteich

    2018-04-01

    Full Text Available Cyanobacteria synthesize a large variety of secondary metabolites including toxins. Microcystins (MCs with hepato- and neurotoxic potential are well studied in bloom-forming planktonic species of temperate and tropical regions. Cyanobacterial biofilms thriving in the polar regions have recently emerged as a rich source for cyanobacterial secondary metabolites including previously undescribed congeners of microcystin. However, detection and detailed identification of these compounds is difficult due to unusual sample matrices and structural congeners produced. We here report a time-efficient liquid chromatography-mass spectrometry (LC-MS precursor ion screening method that facilitates microcystin detection and identification. We applied this method to detect six different MC congeners in 8 out of 26 microbial mat samples of the Svalbard Archipelago in the Arctic. The congeners, of which [Asp3, ADMAdda5, Dhb7] MC-LR was most abundant, were similar to those reported in other polar habitats. Microcystins were also determined using an Adda-specific enzyme-linked immunosorbent assay (Adda-ELISA. Nostoc sp. was identified as a putative toxin producer using molecular methods that targeted 16S rRNA genes and genes involved in microcystin production. The mcy genes detected showed highest similarities to other Arctic or Antarctic sequences. The LC-MS precursor ion screening method could be useful for microcystin detection in unusual matrices such as benthic biofilms or lichen.

  14. Validation of a liquid chromatography ultraviolet method for determination of herbicide diuron and its metabolites in soil samples

    Directory of Open Access Journals (Sweden)

    ANA LUCIA S.M. FELICIO

    2016-01-01

    Full Text Available ABSTRACT Diuron is one of the most widely herbicide used worldwide, which can undergo degradation producing three primary metabolites: 3,4-dichlorophenylurea, 3-(3,4-dichlorophenyl-1-methylurea, and 3,4-dichloroaniline. Since the persistence of diuron and its by-products in ecosystems involves risk of toxicity to environment and human health, a reliable quantitative method for simultaneous monitoring of these compounds is required. Hence, a simple method without preconcentration step was validated for quantitation of diuron and its main metabolites by high performance liquid chromatography with ultraviolet detection. Separation was achieved in less than 11 minutes using a C18 column, mobile phase composed of acetonitrile and water (45:55 v/v at 0.86 mL min-1 and detection at 254 nm. The validated method using solid-liquid extraction followed by an isocratic chromatographic elution proved to be specific, precise and linear (R2 ˃ 0.99, presenting more than 90% of recovery. The method was successfully applied to quantify diuron and their by-products in soil samples collected in a sugarcane cultivation area, focusing on the environmental control.

  15. A quantification method for peroxyacetyl nitrate (PAN) using gas chromatography (GC) with a non-radioactive pulsed discharge detector (PDD)

    Science.gov (United States)

    Zhang, Lei; Jaffe, Daniel A.; Gao, Xin; McClure, Crystal D.

    2018-04-01

    In this study, we developed a method for continuous PAN measurements by gas chromatography (GC) with a non-radioactive pulsed discharge detector (PDD). Operational parameters were optimized based on the ratio of peak height over baseline noise (P/N ratio). The GC/PDD system was compared with a traditional radioactive electron-capture detector (ECD). In the lab, the method detection limit (MDL) of the new GC/PDD method (9 pptv) was lower than the radioactive GC/ECD method (15 pptv), demonstrating its excellent potential. The MDL of GC/PDD in the field campaign at the Mt. Bachelor Observatory (MBO) was 23 pptv, higher than in the lab. This was caused in part by the decreased slope of the calibration curve resulting from the low air pressure level at MBO. However, the MDL level of GC/PDD at MBO is still low enough for accurate PAN measurements, although special attention should be paid to its application at high-elevation sites. Observations of PAN were conducted at MBO in the summer of 2016 with the GC/PDD system, and provided more evidence of the performance of the system. PAN was found to be highly correlated with CO. The promising performance of GC/PDD which does not require a radioactive source makes it a useful approach for accurate PAN measurements in the field.

  16. Multiclass methods for the analysis of antibiotic residues in milk by liquid chromatography coupled to mass spectrometry: A review.

    Science.gov (United States)

    Rossi, Rosanna; Saluti, Giorgio; Moretti, Simone; Diamanti, Irene; Giusepponi, Danilo; Galarini, Roberta

    2018-02-01

    Milk is an important and beneficial food from a nutritional point of view, being an indispensable source of high quality proteins. Furthermore, it is a raw material for many dairy products, such as yoghurt, cheese, cream etc. Before reaching consumers, milk goes through production, processing and circulation. Each step involves potentially unsafe factors, such as chemical contamination that can affect milk quality. Antibiotics are widely used in veterinary medicine for dry cow therapy and mastitis treatment in lactating cows, which can cause the presence of antimicrobial residues in milk. In order to ensure consumers' safety, milk is analyzed to make sure that the fixed Maximum Residue Limits (MRLs) for antibiotics are not exceeded. Multiclass methods can monitor more drug classes through a single analysis, so they are faster, less time-consuming and cheaper than traditional methods (single-class); this aspect is particularly important for milk, which is a highly perishable food. Nevertheless, multiclass methods for veterinary drug residues in foodstuffs are real analytical challenges. This article reviews the major multiclass methods published for the determination of antibiotic residues in milk by liquid chromatography coupled to mass spectrometry, with a special focus on sample preparation approaches.

  17. A novel high-performance thin layer chromatography method for quantification of long chain aliphatic hydrocarbons from Cissus quadrangularis

    Directory of Open Access Journals (Sweden)

    Vandana Jain

    2016-08-01

    Full Text Available Context: A high-performance thin layer chromatography (HPTLC is an analytical technique, which can be used for the determination of constituents or marker components in various parts of the plants. Earlier studies have estimated phytoconstituents from the stem and other aerial plant parts of Cissus quadrangularis Linn. Estimation of hydrocarbons can also be successfully done using HPTLC technique using suitable derivatization. Aims: To develop and validate a simple and rapid method for the estimation of long chain aliphatic hydrocarbons from the leaves of C. quadrangularis using HPTLC technique. Methods: Precoated silica gel 60 F254 plates were used as stationary phase. The mobile phase used was hexane (100 %. The detection of spots was carried out using berberine sulphate as detecting reagent. Results: The method was validated in terms of linearity, sensitivity, accuracy, and precision. Linearity range was found to be 2-10 µg/mL, limit of detection 0.127 µg/mL, and limit of quantification 0.384 µg/mL. Conclusions: A novel, simple, accurate, precise and sensitive HPTLC method has been developed and validated for the estimation of long chain aliphatic hydrocarbons obtained from the leaves of C. quadrangularis Linn.

  18. [Multi-residue method for screening of pesticides in crops by liquid chromatography with tandem mass spectrometry].

    Science.gov (United States)

    Tanizawa, Haruna; Shima, Mikie; Ikehara, Chieko; Kobata, Masakazu; Sato, Motoaki

    2005-10-01

    A simple and rapid method was developed for the screening of 82 pesticides/metabolites in a wide variety of crops, using solid-phase extraction and liquid chromatography with tandem mass spectrometry (LC/MS/MS). After extraction with methanol, the filtered extracts were made up to 100 mL and a 2 mL aliquot was subjected to solid-phase extraction. Co-extractives were removed with a C18 mini-column, while pesticides were retained on 3 kinds of mini-columns (HLB, SAX, activated carbon), and then eluted with acetonitrile. Analysis was performed by LC/MS/MS, and MS acquisition parameters were established in positive and negative ESI modes. The utility of the method was demonstrated by the analysis of 6 crops (carrot, cabbage, onion, spinach, lemon, brown rice) and one mixed vegetable juice. Of 82 compounds tested, 75 in carrot and 62 in lemon were obtained with recoveries ranging from 70-120%. For all samples tested, 75 compounds could be obtained with recoveries of over 50%, and the detection limits of most compounds were lower than 0.01 microg/g. This method provides acceptable performance for analysis of these 75 compounds. Further, by using aliquots of the extracts with small-scale mini-columns, purified samples could be obtained. This proposed method with small matrix effects, is effective and suitable for screening of multiple residual pesticides by using LC/MS/MS.

  19. Screening of extraction methods for glycoproteins from jellyfish ( Rhopilema esculentum) oral-arms by high performance liquid chromatography

    Science.gov (United States)

    Ren, Guoyan; Li, Bafang; Zhao, Xue; Zhuang, Yongliang; Yan, Mingyan; Hou, Hu; Zhang, Xiukun; Chen, Li

    2009-03-01

    In order to select an optimum extraction method for the target glycoprotein (TGP) from jellyfish ( Rhopilema esculentum) oral-arms, a high performance liquid chromatography (HPLC)-assay for the determination of the TGP was developed. Purified target glycoprotein was taken as a standard glycoprotein. The results showed that the calibration curves for peak area plotted against concentration for TGP were linear ( r = 0.9984, y = 4.5895 x+47.601) over concentrations ranging from 50 to 400 mgL-1. The mean extraction recovery was 97.84% (CV2.60%). The fractions containing TGP were isolated from jellyfish ( R. esculentum) oral-arms by four extraction methods: 1) water extraction (WE), 2) phosphate buffer solution (PBS) extraction (PE), 3) ultrasound-assisted water extraction (UA-WE), 4) ultrasound-assisted PBS extraction (UA-PE). The lyophilized extract was dissolved in Milli-Q water and analyzed directly on a short TSK-GEL G4000PWXL (7.8 mm×300 mm) column. Our results indicated that the UA-PE method was the optimum extraction method selected by HPLC.

  20. Air and Surface Sampling Method for Assessing Exposures to Quaternary Ammonium Compounds Using Liquid Chromatography Tandem Mass Spectrometry.

    Science.gov (United States)

    LeBouf, Ryan F; Virji, Mohammed Abbas; Ranpara, Anand; Stefaniak, Aleksandr B

    2017-07-01

    This method was designed for sampling select quaternary ammonium (quat) compounds in air or on surfaces followed by analysis using ultraperformance liquid chromatography tandem mass spectrometry. Target quats were benzethonium chloride, didecyldimethylammonium bromide, benzyldimethyldodecylammonium chloride, benzyldimethyltetradecylammonium chloride, and benzyldimethylhexadecylammonium chloride. For air sampling, polytetrafluoroethylene (PTFE) filters are recommended for 15-min to 24-hour sampling. For surface sampling, Pro-wipe® 880 (PW) media was chosen. Samples were extracted in 60:40 acetonitrile:0.1% formic acid for 1 hour on an orbital shaker. Method detection limits range from 0.3 to 2 ng/ml depending on media and analyte. Matrix effects of media are minimized through the use of multiple reaction monitoring versus selected ion recording. Upper confidence limits on accuracy meet the National Institute for Occupational Safety and Health 25% criterion for PTFE and PW media for all analytes. Using PTFE and PW analyzed with multiple reaction monitoring, the method quantifies levels among the different quats compounds with high precision (detection limits to capture quats on air sampling filters with only a 15-min sample duration with a maximum assessed storage time of 103 days before sample extraction. This method will support future exposure assessment and quantitative epidemiologic studies to explore exposure-response relationships and establish levels of quats exposures associated with adverse health effects. © The Author 2017. Published by Oxford University Press on behalf of the British Occupational Hygiene Society.

  1. Rapid method for determination of glyphosate in groundwater using high performance liquid chromatography and solid-phase extraction after derivatization

    Directory of Open Access Journals (Sweden)

    Valdir Eduardo Olivo

    2015-04-01

    Full Text Available The intensive use of pesticides in agriculture has prompted researchers to develop new methods for identifying these pollutants in water. This study sought to validate a high performance liquid chromatography (HPLC method to determine the concentration of the pesticide glyphosate in groundwater samples by using solid-phase extraction (SPE filters after derivatization with chloroformate 9-fluorenylmethoxycarbonyl (FMOC-Cl. For the HPLC method, we evaluated the following main validation parameters: linearity, specificity, precision, accuracy, robustness, and limits of detection and quantification. After validation of the method, we determined the concentration of glyphosate in samples from thirteen deep, tubular wells distributed in urban and rural areas in Chapecó, SC, Brazil. The solvent used in the extraction of excess FMOC-Cl was dichloromethane and subsequently filtration was performed on C18 SPE, and injected into the chromatograph column in amino polymer with fluorescence detection. The analytical curve made in ultrapure water was linear, with a correlation coefficient of 0.99. The limits of detection and quantification were 0.24 and 0.07 µg L-1, respectively. Recovery tests in natural waters ranged from 90.37 to 101.70%. Glyphosate was detected in 5 of the thirteen wells evaluated. The highest concentration of glyphosate (6.80 µg L-1 was detected in a countryside well, near the municipal water supply. Despite the low levels of glyphosate detected in our study, any amount present in groundwater samples is worrisome, as these molecules have low ground mobility.

  2. Formic acid hydrolysis/liquid chromatography isotope dilution mass spectrometry: An accurate method for large DNA quantification.

    Science.gov (United States)

    Shibayama, Sachie; Fujii, Shin-Ichiro; Inagaki, Kazumi; Yamazaki, Taichi; Takatsu, Akiko

    2016-10-14

    Liquid chromatography-isotope dilution mass spectrometry (LC-IDMS) with formic acid hydrolysis was established for the accurate quantification of λDNA. The over-decomposition of nucleobases in formic acid hydrolysis was restricted by optimizing the reaction temperature and the reaction time, and accurately corrected by using deoxynucleotides (dNMPs) and isotope-labeled dNMPs as the calibrator and the internal standard, respectively. The present method could quantify λDNA with an expanded uncertainty of 4.6% using 10fmol of λDNA. The analytical results obtained with the present method were validated by comparing with the results of phosphate-base quantification by inductively coupled plasma-mass spectrometry (ICP-MS). The results showed good agreement with each other. We conclude that the formic acid hydrolysis/LC-IDMS method can quantify λDNA accurately and is promising as the primary method for the certification of DNA as reference material. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Trace Level Determination of Mesityl Oxide and Diacetone Alcohol in Atazanavir Sulfate Drug Substance by a Gas Chromatography Method.

    Science.gov (United States)

    Raju, K V S N; Pavan Kumar, K S R; Siva Krishna, N; Madhava Reddy, P; Sreenivas, N; Kumar Sharma, Hemant; Himabindu, G; Annapurna, N

    2016-01-01

    A capillary gas chromatography method with a short run time, using a flame ionization detector, has been developed for the quantitative determination of trace level analysis of mesityl oxide and diacetone alcohol in the atazanavir sulfate drug substance. The chromatographic method was achieved on a fused silica capillary column coated with 5% diphenyl and 95% dimethyl polysiloxane stationary phase (Rtx-5, 30 m x 0.53 mm x 5.0 µm). The run time was 20 min employing programmed temperature with a split mode (1:5) and was validated for specificity, sensitivity, precision, linearity, and accuracy. The detection and quantitation limits obtained for mesityl oxide and diacetone alcohol were 5 µg/g and 10 µg/g, respectively, for both of the analytes. The method was found to be linear in the range between 10 µg/g and 150 µg/g with a correlation coefficient greater than 0.999, and the average recoveries obtained in atazanavir sulfate were between 102.0% and 103.7%, respectively, for mesityl oxide and diacetone alcohol. The developed method was found to be robust and rugged. The detailed experimental results are discussed in this research paper.

  4. Optimization and validation of high-performance liquid chromatography method for analyzing 25-desacetyl rifampicin in human urine

    Science.gov (United States)

    Lily; Laila, L.; Prasetyo, B. E.

    2018-03-01

    A selective, reproducibility, effective, sensitive, simple and fast High-Performance Liquid Chromatography (HPLC) was developed, optimized and validated to analyze 25-Desacetyl Rifampicin (25-DR) in human urine which is from tuberculosis patient. The separation was performed by HPLC Agilent Technologies with column Agilent Eclipse XDB- Ci8 and amobile phase of 65:35 v/v methanol: 0.01 M sodium phosphate buffer pH 5.2, at 254 nm and flow rate of 0.8ml/min. The mean retention time was 3.016minutes. The method was linear from 2–10μg/ml 25-DR with a correlation coefficient of 0.9978. Standard deviation, relative standard deviation and coefficient variation of 2, 6, 10μg/ml 25-DR were 0-0.0829, 03.1752, 0-0.0317%, respectively. The recovery of 5, 7, 9μg/ml25-DR was 80.8661, 91.3480 and 111.1457%, respectively. Limits of detection (LoD) and quantification (LoQ) were 0.51 and 1.7μg/ml, respectively. The method has fulfilled the validity guidelines of the International Conference on Harmonization (ICH) bioanalytical method which includes parameters of specificity, linearity, precision, accuracy, LoD, and LoQ. The developed method is suitable for pharmacokinetic analysis of various concentrations of 25-DR in human urine.

  5. Microwave measurement of electrical fields in different media – principles, methods and instrumentation

    International Nuclear Information System (INIS)

    St. Kliment Ohridski, Faculty of Physics, James Bourchier blvd., Sofia 1164 (Bulgaria))" data-affiliation=" (Sofia University St. Kliment Ohridski, Faculty of Physics, James Bourchier blvd., Sofia 1164 (Bulgaria))" >Dankov, Plamen I

    2014-01-01

    This paper, presented in the frame of 4th International Workshop and Summer School on Plasma Physics (IWSSPP'2010, Kiten, Bulgaria), is a brief review of the principles, methods and instrumentation of the microwave measurements of electrical fields in different media. The main part of the paper is connected with the description of the basic features of many field sensors and antennas – narrow-, broadband and ultra-wide band, miniaturized, reconfigurable and active sensors, etc. The main features and applicability of these sensors for determination of electric fields in different media is discussed. The last part of the paper presents the basic principles for utilization of electromagnetic 3-D simulators for E-field measurement purposes. Two illustrative examples have been given – the determination of the dielectric anisotropy of multi-layer materials and discussion of the selectivity of hairpin-probe for determination of the electron density in dense gaseous plasmas.

  6. [Research on fractal tones generating method for tinnitus rehabilitation based on musical instrument digital interface technology].

    Science.gov (United States)

    Wang, Lu; He, Peiyu; Pan, Fan

    2014-08-01

    Tinnitus is a subjective sensation of sound without external stimulation. It has become ubiquitous and has therefore aroused much attention in recent years. According to the survey, ameliorating tinnitus based on special music and reducing pressure have good effects on the treatment of it. Meantime, vicious cycle chains between tinnitus and bad feelings have been broken. However, tinnitus therapy has been restricted by using looping music. Therefore, a method of generating fractal tones based on musical instrument digital interface (MIDI) technology and pink noise has been proposed in this paper. The experimental results showed that the fractal fragments were self-similar, incompletely reduplicate, and no sudden changes in pitches and would have a referential significance for tinnitus therapy.

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

    Science.gov (United States)

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

    2012-02-23

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

  8. Annotation of the human serum metabolome by coupling three liquid chromatography methods to high-resolution mass spectrometry.

    Science.gov (United States)

    Boudah, Samia; Olivier, Marie-Françoise; Aros-Calt, Sandrine; Oliveira, Lydie; Fenaille, François; Tabet, Jean-Claude; Junot, Christophe

    2014-09-01

    This work aims at evaluating the relevance and versatility of liquid chromatography coupled to high resolution mass spectrometry (LC/HRMS) for performing a qualitative and comprehensive study of the human serum metabolome. To this end, three different chromatographic systems based on a reversed phase (RP), hydrophilic interaction chromatography (HILIC) and a pentafluorophenylpropyl (PFPP) stationary phase were used, with detection in both positive and negative electrospray modes. LC/HRMS platforms were first assessed for their ability to detect, retain and separate 657 metabolite standards representative of the chemical families occurring in biological fluids. More than 75% were efficiently retained in either one LC-condition and less than 5% were exclusively retained by the RP column. These three LC/HRMS systems were then evaluated for their coverage of serum metabolome. The combination of RP, HILIC and PFPP based LC/HRMS methods resulted in the annotation of about 1328 features in the negative ionization mode, and 1358 in the positive ionization mode on the basis of their accurate mass and precise retention time in at least one chromatographic condition. Less than 12% of these annotations were shared by the three LC systems, which highlights their complementarity. HILIC column ensured the greatest metabolome coverage in the negative ionization mode, whereas PFPP column was the most effective in the positive ionization mode. Altogether, 192 annotations were confirmed using our spectral database and 74 others by performing MS/MS experiments. This resulted in the formal or putative identification of 266 metabolites, among which 59 are reported for the first time in human serum. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Comparison of sample preparation methods for reliable plutonium and neptunium urinalysis using automatic extraction chromatography

    DEFF Research Database (Denmark)

    Qiao, Jixin; Xu, Yihong; Hou, Xiaolin

    2014-01-01

    This paper describes improvement and comparison of analytical methods for simultaneous determination of trace-level plutonium and neptunium in urine samples by inductively coupled plasma mass spectrometry (ICP-MS). Four sample pre-concentration techniques, including calcium phosphate, iron......), it endows urinalysis methods with better reliability and repeatability compared with co-precipitation techniques. In view of the applicability of different pre-concentration techniques proposed previously in the literature, the main challenge behind relevant method development is pointed to be the release...

  10. Validation of a high-performance liquid chromatography/fluorescence detection method for the simultaneous quantification of fifteen polycyclic aromatic hydrocarbons

    DEFF Research Database (Denmark)

    Hansen, Åse Marie; Olsen, I L; Holst, E

    1991-01-01

    A high-performance liquid chromatography/fluorescence method using multiple wavelength shift for simultaneous quantification of different PAH compounds was developed. The new method was superior to the methods of DONG and GREENBERG [J. Liquid Chromatogr. 11, 1887-1905 (1988)] and WISE et al...... that no systematic errors, and only small unsystematic errors, could be demonstrated. Furthermore, the method had a good reproducibility and a high sensitivity....

  11. Comparison of fine particle measurements from a direct-reading instrument and a gravimetric sampling method.

    Science.gov (United States)

    Kim, Jee Young; Magari, Shannon R; Herrick, Robert F; Smith, Thomas J; Christiani, David C

    2004-11-01

    Particulate air pollution, specifically the fine particle fraction (PM2.5), has been associated with increased cardiopulmonary morbidity and mortality in general population studies. Occupational exposure to fine particulate matter can exceed ambient levels by a large factor. Due to increased interest in the health effects of particulate matter, many particle sampling methods have been developed In this study, two such measurement methods were used simultaneously and compared. PM2.5 was sampled using a filter-based gravimetric sampling method and a direct-reading instrument, the TSI Inc. model 8520 DUSTTRAK aerosol monitor. Both sampling methods were used to determine the PM2.5 exposure in a group of boilermakers exposed to welding fumes and residual fuel oil ash. The geometric mean PM2.5 concentration was 0.30 mg/m3 (GSD 3.25) and 0.31 mg/m3 (GSD 2.90)from the DUSTTRAK and gravimetric method, respectively. The Spearman rank correlation coefficient for the gravimetric and DUSTTRAK PM2.5 concentrations was 0.68. Linear regression models indicated that log, DUSTTRAK PM2.5 concentrations significantly predicted loge gravimetric PM2.5 concentrations (p gravimetric PM2.5 concentrations was found to be modified by surrogate measures for seasonal variation and type of aerosol. PM2.5 measurements from the DUSTTRAK are well correlated and highly predictive of measurements from the gravimetric sampling method for the aerosols in these work environments. However, results from this study suggest that aerosol particle characteristics may affect the relationship between the gravimetric and DUSTTRAK PM2.5 measurements. Recalibration of the DUSTTRAK for the specific aerosol, as recommended by the manufacturer, may be necessary to produce valid measures of airborne particulate matter.

  12. Eddy Covariance Method for CO2 Emission Measurements: CCS Applications, Principles, Instrumentation and Software

    Science.gov (United States)

    Burba, George; Madsen, Rod; Feese, Kristin

    2013-04-01

    The Eddy Covariance method is a micrometeorological technique for direct high-speed measurements of the transport of gases, heat, and momentum between the earth's surface and the atmosphere. Gas fluxes, emission and exchange rates are carefully characterized from single-point in-situ measurements using permanent or mobile towers, or moving platforms such as automobiles, helicopters, airplanes, etc. Since the early 1990s, this technique has been widely used by micrometeorologists across the globe for quantifying CO2 emission rates from various natural, urban and agricultural ecosystems [1,2], including areas of agricultural carbon sequestration. Presently, over 600 eddy covariance stations are in operation in over 120 countries. In the last 3-5 years, advancements in instrumentation and software have reached the point when they can be effectively used outside the area of micrometeorology, and can prove valuable for geological carbon capture and sequestration, landfill emission measurements, high-precision agriculture and other non-micrometeorological industrial and regulatory applications. In the field of geological carbon capture and sequestration, the magnitude of CO2 seepage fluxes depends on a variety of factors. Emerging projects utilize eddy covariance measurement to monitor large areas where CO2 may escape from the subsurface, to detect and quantify CO2 leakage, and to assure the efficiency of CO2 geological storage [3,4,5,6,7,8]. Although Eddy Covariance is one of the most direct and defensible ways to measure and calculate turbulent fluxes, the method is mathematically complex, and requires careful setup, execution and data processing tailor-fit to a specific site and a project. With this in mind, step-by-step instructions were created to introduce a novice to the conventional Eddy Covariance technique [9], and to assist in further understanding the method through more advanced references such as graduate-level textbooks, flux networks guidelines, journals

  13. Benefits and Limitations of Lab-on-a-Chip Method over Reversed-Phase High-Performance Liquid Chromatography Method in Gluten Proteins Evaluation

    Directory of Open Access Journals (Sweden)

    Dragan Živančev

    2015-01-01

    Full Text Available RP-HPLC (reversed-phase high-performance liquid chromatography is widely used to determine the amounts of the different gluten protein types. However, this method is time-consuming, especially at early stages of wheat breeding, when large number of samples needs to be analyzed. On the other hand, LoaC (Lab-on-a-Chip technique has the potential for a fast, reliable, and automatable analysis of proteins. In the present study, benefits and limitations of Lab-on-a-Chip method over RP-HPLC method in gluten proteins evaluation were explored in order to determine in which way LoaC method should be improved in order to make its results more compliant with the results of RP-HPLC method. Strong correlation (P≤0.001 was found between numbers of HMW glutenin peaks determined by LoaC and RP-HPLC methods. Significant correlations (P≤0.05 were obtained between percentages of HMW and LMW glutenin subunits calculated with regard to total HMW + LMW area. Even more significant correlation (P≤0.001 was found when percentages of individual HMW areas were calculated with regard to total HMW. RP-HPLC method showed superiority in determination of gliadins since larger number and better resolution of gliadin peaks were obtained by this method.

  14. Instrumentation and methods evaluations for shallow land burial of waste materials: water erosion

    International Nuclear Information System (INIS)

    Hostetler, D.D.; Murphy, E.M.; Childs, S.W.

    1981-08-01

    The erosion of geologic materials by water at shallow-land hazardous waste disposal sites can compromise waste containment. Erosion of protective soil from these sites may enhance waste transport to the biosphere through water, air, and biologic pathways. The purpose of this study was to review current methods of evaluating soil erosion and to recommend methods for use at shallow-land, hazardous waste burial sites. The basic principles of erosion control are: minimize raindrop impact on the soil surface; minimize runoff quantity; minimize runoff velocity; and maximize the soil's resistance to erosion. Generally soil erosion can be controlled when these principles are successfully applied at waste disposal sites. However, these erosion control practices may jeopardize waste containment. Typical erosion control practices may enhance waste transport by increasing subsurface moisture movement and biologic uptake of hazardous wastes. A two part monitoring program is recommended for US Department of Energy (DOE) hazardous waste disposal sites. The monitoring programs and associated measurement methods are designed to provide baseline data permitting analysis and prediction of long term erosion hazards at disposal sites. These two monitoring programs are: (1) site reconnaissance and tracking; and (2) site instrumentation. Some potential waste transport problems arising from erosion control practices are identified. This report summarizes current literature regarding water erosion prediction and control

  15. Validation of Analysis Method of pesticides in fresh tomatoes by Gas Chromatography associated to a liquid scintillation counting

    International Nuclear Information System (INIS)

    Dhib, Ahlem

    2011-01-01

    Pesticides are nowadays considered as toxic for human health. The maximum residues levels (MRL) in foodstuff are more and more strict. Therefore, selective analytical techniques are necessary for their identification and their quantification. The aim of this study is to set up a multi residue method for the determination of pesticides in tomatoes by gas chromatography with μECD detector (GC/μECD) associated to liquid scintillation counting. A global analytical protocol consisting of a QuECHERS version of the extraction step followed by purification step of the resulting extract on a polymeric sorbent was set up. The 14 C-chloropyrifos used as an internal standard proved excellent to control the different steps needed for the sample preparation. The method optimized is specific, selective with a recovery averaged more than 70 pour cent, repetitive and reproducible. Although some others criteria need to be checked regarding validation before its use in routine analysis, the potential of the method has been demonstrated.

  16. Quantification of the level of fat-soluble vitamins in feed based on the novel microemulsion electrokinetic chromatography (MEEKC) method.

    Science.gov (United States)

    Olędzka, Ilona; Kowalski, Piotr; Bałuch, Alicja; Bączek, Tomasz; Paradziej-Łukowicz, Jolanta; Taciak, Marcin; Pastuszewska, Barbara

    2014-02-01

    Simultaneous quantification of liposoluble vitamins is not a new area of interest, since these compounds co-determine the nutritional quality of food and feed, a field widely explored in the human and animal diet. However, the development of appropriate methods is still a matter of concern, especially when the vitamin composition is highly complex, as is the case with feed designated for laboratory animals, representing a higher health and microbiological status. A method combining microemulsion electrokinetic chromatography (MEEKC) with liquid-liquid extraction was developed for the determination of four fat-soluble vitamins in animal feed. A separation medium consisting of 25 mmol L⁻¹ phosphate buffer (pH 2.5), 2-propanol, 1-butanol, sodium dodecyl sulfate and octane allowed the simultaneous determination of vitamins A, D, E and K within a reasonable time of 25 min. The polarity of the separation voltage was reversed in view of the strongly suppressed electro-osmotic flow, and the applied voltage was set at 12 kV. The fat-soluble vitamins were separated in the order of decreasing hydrophobicity. It was proved that the proposed MEEKC method was sufficiently specific and sensitive for screening fat-soluble vitamins in animal feed samples after their sterilization. © 2013 Society of Chemical Industry.

  17. Development of an analytical method to quantify total isoflavones in phytotherapic capsules using high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Liliane C. C. Auwerter

    2012-12-01

    Full Text Available Isoflavones can be found in grains and leaves of soybean. Currently, these are sold in pharmacies as phytotherapic capsules. Isoflavones have been recommended by doctors, especially for women, due to their ability to relieve menopause symptoms, among other benefits. However, no method exists for the official control of isoflavone content in capsules sold in the Brazilian market. This study aims to develop an appropriate analytical method to determine the total isoflavone content (daidzin, glycitin, and genistin, and their respective aglycone forms in phytotherapic capsules purchased in pharmacies in Curitiba, Parana State, Brazil, using the technique of high-performance liquid chromatography with UV detection (UV-HPLC. The HPLC system consisted of a quaternary pump, an autosampler, and Waters reversed-phase C18 column (5 μm × 300 mm. Analyses were carried out at 40 °C, using a flow rate of 1.0 mL/min (acetonitrile and acetic acid 0.1%, and detection was performed at 254 nm. The method was validated as required by ANVISA and showed to be reliable for the following parameters: linearity (r² >0.99, selectivity (correlation between 0.99 and 1.00, precision (relative standard derivation <1.59%, accuracy (from 80% to 111.63% intraday and from 80% to 117.88% interday recovery, and robustness.

  18. Development of an analytical method to quantify total isoflavones in phytotherapic capsules using high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Liliane C. C. Auwerter

    2012-10-01

    Full Text Available Isoflavones can be found in grains and leaves of soybean. Currently, these are sold in pharmacies as phytotherapic capsules. Isoflavones have been recommended by doctors, especially for women, due to their ability to relieve menopause symptoms, among other benefits. However, no method exists for the official control of isoflavone content in capsules sold in the Brazilian market. This study aims to develop an appropriate analytical method to determine the total isoflavone content (daidzin, glycitin, and genistin, and their respective aglycone forms in phytotherapic capsules purchased in pharmacies in Curitiba, Parana State, Brazil, using the technique of high-performance liquid chromatography with UV detection (UV-HPLC. The HPLC system consisted of a quaternary pump, an autosampler, and Waters reversed-phase C18 column (5 μm × 300 mm. Analyses were carried out at 40 °C, using a flow rate of 1.0 mL/min (acetonitrile and acetic acid 0.1%, and detection was performed at 254 nm. The method was validated as required by ANVISA and showed to be reliable for the following parameters: linearity (r² >0.99, selectivity (correlation between 0.99 and 1.00, precision (relative standard derivation <1.59%, accuracy (from 80% to 111.63% intraday and from 80% to 117.88% interday recovery, and robustness.

  19. Determining the Levels of Volatile Organic Pollutants in Urban Air Using a Gas Chromatography-Mass Spectrometry Method

    Science.gov (United States)

    Nicoara, Simona; Tonidandel, Loris; Traldi, Pietro; Watson, Jonathan; Morgan, Geraint; Popa, Ovidiu

    2009-01-01

    The paper presents the application of a method based on coupled gas chromatography-mass spectrometry, using an isotopically labelled internal standard for the quantitative analysis of benzene (B), toluene (T), ethyl benzene (E), and o-, m-, p-xylenes (X). Their atmospheric concentrations were determined based on short-term sampling, in different sites of Cluj-Napoca, a highly populated urban centre in N-W Romania, with numerous and diversified road vehicles with internal combustion engines. The method is relatively inexpensive and simple and shows good precision and linearity in the ranges of 7–60 μg/m3 (B), 13–90 μg/m3 (T), 7–50 μg/m3 (E), 10–70 μg/m3 (X-m,p), and 20–130 μg/m3 (X-o). The limits of quantitation/detection of the method LOQ/LOD are of 10/5 μg/m3 (Xo), 5/3 μg/m3 (B, E, X-m,p), and of 3/1 μg/m3 (T), respectively. PMID:20168976

  20. Determining the Levels of Volatile Organic Pollutants in Urban Air Using a Gas Chromatography-Mass Spectrometry Method

    Directory of Open Access Journals (Sweden)

    Simona Nicoara

    2009-01-01

    Full Text Available The paper presents the application of a method based on coupled gas chromatography-mass spectrometry, using an isotopically labelled internal standard for the quantitative analysis of benzene (B, toluene (T, ethyl benzene (E, and o-, m-, p-xylenes (X. Their atmospheric concentrations were determined based on short-term sampling, in different sites of Cluj-Napoca, a highly populated urban centre in N-W Romania, with numerous and diversified road vehicles with internal combustion engines. The method is relatively inexpensive and simple and shows good precision and linearity in the ranges of 7–60 μg/m3 (B, 13–90 μg/m3 (T, 7–50 μg/m3 (E, 10–70 μg/m3 (X-m,p, and 20–130 μg/m3 (X-o. The limits of quantitation/detection of the method LOQ/LOD are of 10/5 μg/m3 (Xo, 5/3 μg/m3 (B, E, X-m,p, and of 3/1 μg/m3 (T, respectively.

  1. A simple method for purification of lipopolysaccharides from E. coli 55:B5 using size exclusion chromatography

    International Nuclear Information System (INIS)

    Perdomo, Rolando; Montero, Vivian

    2006-01-01

    Several methods for the extraction of endotoxin or lipopolysaccharide from Gram negative bacteria have been described. However, the product is often contaminated with nucleic acids or proteins in a proportion depending on the extraction method used. Molecular and immunological studies require further purification of the raw LPS. We present here, a simple method for the purification of raw LPS obtained by the standard hot phenol-water procedure using size exclusion chromatography in Sepharose CL-6B. We demonstrated that the using of DNAse and RNAse treatment of the sample before the chromatographic step is necessary to abrogate the nucleic acid contamination in the LPS fraction. The spectrophotometric properties of the pure LPS were verified, supporting the immediate online detection of the LPS and oligonucleotides fractions spectrophotometrically at 206 nm. The mobile phase used (NaCl 0.2 M) do not absorb at 206 nm while maintains the LPS aggregates and therefore, allows the separation of the LPS fraction from the oligoribonucleotide and desoxioligoribonucleotide fractions. The yield of pure LPS was around 98%. Chemical and biological characterizations were conducted in order to assess the feasibility of the procedure developed. (Author)

  2. Validation of a chiral liquid chromatography-tandem mass spectrometry method for the determination of pantoprazole in dog plasma.

    Science.gov (United States)

    Chen, Meixia; Xia, Yu; Ma, Zhiyu; Li, Liang; Zhong, Dafang; Chen, Xiaoyan

    2012-10-01

    Pantoprazole (PAN), a selective proton pump inhibitor, is used clinically as a racemic mixture for the treatment of acid-related gastrointestinal disorders. To investigate its stereoselective pharmacokinetics, a chiral liquid chromatography-tandem mass spectrometry method was developed and validated to determine the pantoprazole enantiomers in dog plasma. After liquid-liquid extraction, a baseline resolution of enantiomers was achieved on an ovomucoid column using the mobile phase of methanol:acetonitrile:10mM ammonium formate (pH 7) (10.4:2.6:87, v/v/v) at 30°C within 10min. Stable isotopically labeled (+)-d(3)-pantoprazole and (-)-d(3)-pantoprazole were used as internal standards. Acquisition of mass spectrometric data was performed in multiple reaction monitoring mode via positive atmospheric pressure chemical ionization. The method was linear in the concentration range of 20.0-10,000ng/mL for each enantiomer using 25μL of dog plasma. The lower limit of quantification (LLOQ) for each enantiomer was 20.0ng/mL. Intra- and inter-day precision ranged from 3.2% to 10.3% for (+)-pantoprazole and 3.7-10.0% for (-)-pantoprazole. Accuracy varied from -1.4% to -0.2% for (+)-pantoprazole and -1.6% to 0.8% for (-)-pantoprazole. The validated method was applied successfully for stereoselective pharmacokinetic studies of racemic pantoprazole. Copyright © 2012 Elsevier B.V. All rights reserved.

  3. A liquid chromatography with tandem mass spectrometry method for quantitating total and unbound ceritinib in patient plasma and brain tumor

    Directory of Open Access Journals (Sweden)

    Xun Bao

    2018-02-01

    Full Text Available A rapid, sensitive, and robust reversed-phase liquid chromatography with tandem mass spectrometry method was developed and validated for the determination of total and unbound ceritinib, a second-generation ALK inhibitor, in patient plasma and brain tumor tissue samples. Sample preparation involved simple protein precipitation with acetonitrile. Chromatographic separation was achieved on a Waters ACQUITY UPLC BEH C18 column using a 4-min gradient elution consisting of mobile phase A (0.1% formic acid in water and mobile phase B (0.1% formic acid in acetonitrile, at a flow rate of 0.4 mL/min. Ceritinib and the internal standard ([13C6]ceritinib were monitored using multiple reaction monitoring mode under positive electrospray ionization. The lower limit of quantitation (LLOQ was 1 nM of ceritinib in plasma. The calibration curve was linear over ceritinib concentration range of 1–2000 nM in plasma. The intra- and inter-day precision and accuracy were within the generally accepted criteria for bioanalytical method (<15%. The method was successfully applied to assess ceritinib brain tumor penetration, as assessed by the unbound drug brain concentration to unbound drug plasma concentration ratio, in patients with brain tumors.

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

    Science.gov (United States)

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

    2016-03-01

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

  5. A High-Performance Thin Layer Chromatography (HPTLC) Method for Simultaneous Determination of Diphenhydramine Hydrochloride and Naproxen Sodium in Tablets.

    Science.gov (United States)

    Bhole, R P; Shinde, S S; Chitlange, S S; Wankhede, S B

    2015-01-01

    A rapid and simple high-performance thin layer chromatography (HPTLC) method with densitometry at 230 nm was developed and validated for simultaneous determination of diphenhydramine hydrochloride (DPH) and naproxen sodium (NPS) from pharmaceutical preparation. The separation was carried out on aluminum plates precoated with silica gel 60 F254 using mobile phase toluene:methanol:glacial acetic acid (7.5:1:0.2, v/v/v). The linearity range lies between 200 and 1200 ng/band for DPH and 1760 and 10,560 ng/band for NPS with correlation coefficients of 0.994 and 0.995, respectively. The R f value for DPH is 0.20 ± 0.05 and for NPS is 0.61 ± 0.06. % Recoveries of DPH and NPS was in the range of 99.70%-99.95% and 99.63%-99.95%, respectively. Limit of detection value for DPH was 13.21 ng/band and for NPS was 8.03 ng/band. Limit of quantitation value for DPH was 40.06 ng/band and for NPS was 24.34 ng/band. The developed method was validated as per ICH guidelines. In stability testing, DPH was found unstable to acid and alkaline hydrolysis, and DPH and NPS were found unstable to oxidation, whereas both the drugs were stable to neutral and photodegradation. The proposed method was successfully applied for the routine quantitative analysis of dosage form containing DPH and NPS.

  6. Optimized and validated high-performance liquid chromatography method for the determination of deoxynivalenol and aflatoxins in cereals.

    Science.gov (United States)

    Skendi, Adriana; Irakli, Maria N; Papageorgiou, Maria D

    2016-04-01

    A simple, sensitive and accurate analytical method was optimized and developed for the determination of deoxynivalenol and aflatoxins in cereals intended for human consumption using high-performance liquid chromatography with diode array and fluorescence detection and a photochemical reactor for enhanced detection. A response surface methodology, using a fractional central composite design, was carried out for optimization of the water percentage at the beginning of the run (X1, 80-90%), the level of acetonitrile at the end of gradient system (X2, 10-20%) with the water percentage fixed at 60%, and the flow rate (X3, 0.8-1.2 mL/min). The studied responses were the chromatographic peak area, the resolution factor and the time of analysis. Optimal chromatographic conditions were: X1 = 80%, X2 = 10%, and X3 = 1 mL/min. Following a double sample extraction with water and a mixture of methanol/water, mycotoxins were rapidly purified by an optimized solid-phase extraction protocol. The optimized method was further validated with respect to linearity (R(2) >0.9991), sensitivity, precision, and recovery (90-112%). The application to 23 commercial cereal samples from Greece showed contamination levels below the legally set limits, except for one maize sample. The main advantages of the developed method are the simplicity of operation and the low cost. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Magnetic solid phase extraction and static headspace gas chromatography-mass spectrometry method for the analysis of polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Cai, Ying; Yan, Zhihong; Wang, Lijia; NguyenVan, Manh; Cai, Qingyun

    2016-01-15

    A magnetic solid phase extraction (MSPE) protocol combining a static headspace gas chromatography coupled to mass spectrometry (HS-GC-MS) method has been developed for extraction, and determination of 16 polycyclic aromatic hydrocarbons (PAHs) in drinking water samples. Magnetic nanoparticles (MNPs) were coated with 3-aminopropyltriethoxysilane and modified by cholesterol chloroformate. Transmission electron microscope, vibrating sample magnetometer, Fourier transform infrared spectrometry and X-ray photoelectron spectroscopy were used to characterize the cholesterol-functionalized sorbents, and the main parameters affecting the extraction as well as HS sampling, such as sorbent amount, extraction time, oven temperature and equilibration time have been investigated and established. Combination with HS sampling, the MSPE procedure was simple, fast and environmentally friendly, without need of any organic solvent. Method validation proved the feasibility of the developed sorbents for the quantitation of the investigated analytes at trace levels obtaining the limit of detection (S/N=3) ranging from 0.20 to 7.8 ng/L. Good values for intra and inter-day precision were obtained (RSDs ≤ 9.9%). The proposed method was successfully applied to drinking water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. A microanalytical method for ammonium and short-chain primary aliphatic amines using precolumn derivatization and capillary liquid chromatography.

    Science.gov (United States)

    Moliner-Martínez, Y; Herráez-Hernández, R; Campíns-Falcó, P

    2007-09-14

    A new microscale method is presented for the determination of ammonium and primary short-chain aliphatic amines (methylamine, ethylamine, propylamine, n-butylamine and n-pentylamine) in water. The assay uses precolumn derivatization with the reagent o-phthaldialdehyde (OPA) in combination with the thiol N-acetyl-L-cysteine (NAC), and capillary liquid chromatography with UV detection at 330 nm. The described method is very simple and rapid as no preconcentration of the analytes is necessary, and the volume of sample required is only 0.1 mL. Under the proposed conditions good linearity has been obtained up to a concentration of the analytes of 10.0 mgL(-1), the limits of detection being of 8-50 microgL(-1). No matrix effect was found, and recoveries between 97 and 110% were obtained. The precision of the method was good, and the achieved variation coefficients were below 12%. The reliability of the proposed approach has been tested by analyzing a microsample of fogwater collected from leaf surfaces.

  9. Validation of histamine determination Method in yoghurt using High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    M Jahedinia

    2014-02-01

    Full Text Available Biogenic amines are organic, basic nitrogenous compounds of low molecular weight that are mainly generated by the enzymatic decarboxylation of amino acids by microorganisms. Dairy products are among the foods with the highest amine content. A wide variety of methods and procedures for determination of histamine and biogenic amines have been established. Amongst, HPLC method is considered as reference method. The aim of this study was to validate Reversed Phase HPLC method determination of histamine in yoghurt. The mobile phase consisted of acetonitrile/water (18:88 v/v and the flow rate was set at 0.5 ml/min using isocratic HPLC. Detection was carried out at 254 nm using UV-detector. Calibration curve that was constructed using peak area of standards was linear and value of correlation coefficient (r2 was estimated at 0.998. Good recoveries were observed for histamine under investigation at all spiking levels and average of recoveries was 84%. The RSD% value from repeatability test was found to be %4.4. Limit of detection and limit of quantitation were 0.14 and 0.42 µ/ml, respectively. The results of validation tests showed that the method is reliable and rapid for quantification of histamine in yoghurt.

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

    Science.gov (United States)

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

    2010-05-21

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

  11. A novel method for selective separation of {sup 111}In from impurities by ion exchange chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Yavari, R.; Khanachi, A.R.; Ghannad Maragheh, M.; Bagheri, G. [Jaber Ibn-e Hayan Research Laboratories, A.E.O.I., Tehran (Iran)

    2004-07-01

    {sup 111}In is one of the most important cyclotron-produced radionuclides that is prepared from nuclear reactions like Cd (p,xn){sup 111}In and Cd (d,xn) {sup 111}In. It is used in various branches of medicine such as lymphoscintigraphy and cisternography. Several methods have been reported in the literature for the separation of carrier-free {sup 111}In from irradiated cadmium matrix. But there has not been a sufficiently fast method for this purpose until recently. In this work, a new method has been developed for the separation of {sup 111}In from a cadmium target by using Dowex 50W-X8 as an ion exchanger. (orig.)

  12. Direct liquid chromatography method for the simultaneous quantification of hydroxytyrosol and tyrosol in red wines.

    Science.gov (United States)

    Piñeiro, Zulema; Cantos-Villar, Emma; Palma, Miguel; Puertas, Belen

    2011-11-09

    A validated HPLC method with fluorescence detection for the simultaneous quantification of hydroxytyrosol and tyrosol in red wines is described. Detection conditions for both compounds were optimized (excitation at 279 and 278 and emission at 631 and 598 nm for hydroxytyrosol and tyrosol, respectively). The validation of the analytical method was based on selectivity, linearity, robustness, detection and quantification limits, repeatability, and recovery. The detection and quantification limits in red wines were set at 0.023 and 0.076 mg L(-1) for hydroxytyrosol and at 0.007 and 0.024 mg L(-1) for tyrosol determination, respectively. Precision values, both within-day and between-day (n = 5), remained below 3% for both compounds. In addition, a fractional factorial experimental design was developed to analyze the influence of six different conditions on analysis. The final optimized HPLC-fluorescence method allowed the analysis of 30 nonpretreated Spanish red wines to evaluate their hydroxytyrosol and tyrosol contents.

  13. Method development for Lawsone estimation in Trichup herbal hair powder by high-performance thin layer chromatography

    Directory of Open Access Journals (Sweden)

    Maunang M Patel

    2013-01-01

    Full Text Available A simple, specific, accurate, precise and robust high-performance thin-layer chromatographic method has been developed and validated for estimation of Lawsone in Trichup herbal hair powder (coded as a THHP, polyherbal formulation. The chromatographic development was carried out on aluminum plates pre-coated with silica gel 60F 254 and good resolution was achieved with Toluene: Ethyl acetate: Glacial acetic acid (8:1:1 v/v/v as mobile phase. Lawsone detection was carried out densitometrically at 277 nm and obtained retardation factor value was 0.46 ± 0.02. The method was validated with respect to specificity, linearity, accuracy, precision and robustness. The calibration curve was achieved to be linear over a range of 5-60 μg/ml and regression coefficient was obtained 0.998. Accuracy of chromatographic method was evaluated by standard addition method; recovery was obtained 99.25 ± 0.61% . The peak purity of Lawsone was achieved 0.999 r. Relative standard deviation for intraday and inter-day precision was 0.37-0.56% and 0.42-0.55%, respectively. The limit of detection and limit of quantification of the Lawsone were found to be 1.08 μg/m land 3.28 μg/ml, respectively. This result shows that the method was well validated. In the present study, the Lawsone content was found 0.322 ± 0.014% in THHP. This study reveals that the proposed high performance thin layer chromatography method is accurate, fast and cost- effective for routine estimation of Lawsone in polyherbal formulation.

  14. Method Development for the Determination of Fluorotelomer Alcohols in Soils by Gas Chromatography Mass Spectrometry

    Science.gov (United States)

    Fluorotelomer alcohols (FTOHs) have been widely studied as precursors to perfluorocarboxylates, e.g. 8:2 FTOH degrades to perfluorooctanoic acid (PFOA). This presentation describes an analytical method for the extraction and analysis of 6:2, 8:2, and 10:2 FTOHs. Gas chromatograph...

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

    NARCIS (Netherlands)

    Dias, M.G.; Oliveira, L.; Camoes, M.F.G.F.C.; Nunes, B.; Versloot, P.; Hulshof, P.J.M.

    2010-01-01

    Three sets of extraction/saponification/HPLC conditions for food carotenoid quantification were technically and economically compared. Samples were analysed for carotenoids a-carotene, ß-carotene, ß-cryptoxanthin, lutein, lycopene, and zeaxanthin. All methods demonstrated good performance in the

  16. Development and Validation of High Performance Liquid Chromatography Method for Determination Atorvastatin in Tablet

    Science.gov (United States)

    Yugatama, A.; Rohmani, S.; Dewangga, A.

    2018-03-01

    Atorvastatin is the primary choice for dyslipidemia treatment. Due to patent expiration of atorvastatin, the pharmaceutical industry makes copy of the drug. Therefore, the development methods for tablet quality tests involving atorvastatin concentration on tablets needs to be performed. The purpose of this research was to develop and validate the simple atorvastatin tablet analytical method by HPLC. HPLC system used in this experiment consisted of column Cosmosil C18 (150 x 4,6 mm, 5 µm) as the stationary reverse phase chomatography, a mixture of methanol-water at pH 3 (80:20 v/v) as the mobile phase, flow rate of 1 mL/min, and UV detector at wavelength of 245 nm. Validation methods were including: selectivity, linearity, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ). The results of this study indicate that the developed method had good validation including selectivity, linearity, accuracy, precision, LOD, and LOQ for analysis of atorvastatin tablet content. LOD and LOQ were 0.2 and 0.7 ng/mL, and the linearity range were 20 - 120 ng/mL.

  17. Influence of drying method on the surface energy of cellulose nanofibrils determined by inverse gas chromatography

    Science.gov (United States)

    Yucheng Peng; Douglas J. Gardner; Yousoo Han; Zhiyong Cai; Mandla A. Tshabalala

    2013-01-01

    Research and development of the renewable nanomaterial cellulose nanofibrils (CNFs) has received considerable attention. The effect of drying on the surface energy of CNFs was investigated. Samples of nanofibrillated cellulose (NFC) and cellulose nanocrystals (CNC) were each subjected to four separate drying methods: air-drying, freeze-drying, spray-drying, and...

  18. Molar mass determination of lignins by size-exclusion chromatography: towards standardisation of the method

    NARCIS (Netherlands)

    Baumberger, S.; Abaecherli, A.; Fasching, M.; Gellerstedt, G.; Gosselink, R.J.A.; Hortling, B.; Li, J.; Saake, B.; Jong, de E.

    2007-01-01

    The reactivity and physicochemical properties of lignins are partly governed by their molar mass distribution. The development of reliable standard methods for determination of the molar mass distribution is not only relevant for designing technical lignins for specific applications, but also for

  19. A quick and easy high performance liquid chromatography method for evaluation of cefixime in human plasma

    Directory of Open Access Journals (Sweden)

    Hossein Danafar

    2015-12-01

    Full Text Available Cefixime is essential member of orally energetic third generation cephalosporin and has tremendous activity aligned with many pathogens. The virtual bioavailability of a newly industrial dispersible tablet as compared with a recognized identified formulation.  A simple and available reversed-phase HPLC method with UV detection has been urbanized and validate for cefixime evaluate in human plasma using a C18 analytical column and a mobile phase of tetrabutylammonium hydroxide (pH 6.5-acetonitrile (3:1 v/v. The detection wavelength was 280 nm. To method observed major linear response-concentration association all through the cefixime concentration range of 15-100 ng/ml, with the average accuracy within-run and between-run values of 97.29% and 99.27%. The average drug recovery from plasma was 98.2% throughout the linear concentration range. The limits of detection (LOD and quantitation (LOQ of the method were 5 and 15 ng/ml, respectively. The method is quick, easy, very steady and precise for the partition, assignment, evaluation of cefixime in human plasma.

  20. Emission quantification using the tracer gas dispersion method: The influence of instrument, tracer gas species and source simulation

    DEFF Research Database (Denmark)

    Delre, Antonio; Mønster, Jacob; Samuelsson, Jerker

    2018-01-01

    The tracer gas dispersion method (TDM) is a remote sensing method used for quantifying fugitive emissions by relying on the controlled release of a tracer gas at the source, combined with concentration measurements of the tracer and target gas plumes. The TDM was tested at a wastewater treatment...... plant for plant-integrated methane emission quantification, using four analytical instruments simultaneously and four different tracer gases. Measurements performed using a combination of an analytical instrument and a tracer gas, with a high ratio between the tracer gas release rate and instrument...... precision (a high release-precision ratio), resulted in well-defined plumes with a high signal-to-noise ratio and a high methane-to-tracer gas correlation factor. Measured methane emission rates differed by up to 18% from the mean value when measurements were performed using seven different instrument...

  1. A sensitive and selective liquid chromatography/tandem mass spectrometry method for quantitative analysis of efavirenz in human plasma.

    Directory of Open Access Journals (Sweden)

    Praveen Srivastava

    Full Text Available A selective and a highly sensitive method for the determination of the non-nucleoside reverse transcriptase inhibitor (NNRTI, efavirenz, in human plasma has been developed and fully validated based on high performance liquid chromatography tandem mass spectrometry (LC-MS/MS. Sample preparation involved protein precipitation followed by one to one dilution with water. The analyte, efavirenz was separated by high performance liquid chromatography and detected with tandem mass spectrometry in negative ionization mode with multiple reaction monitoring. Efavirenz and ¹³C₆-efavirenz (Internal Standard, respectively, were detected via the following MRM transitions: m/z 314.20243.90 and m/z 320.20249.90. A gradient program was used to elute the analytes using 0.1% formic acid in water and 0.1% formic acid in acetonitrile as mobile phase solvents, at a flow-rate of 0.3 mL/min. The total run time was 5 min and the retention times for the internal standard (¹³C₆-efavirenz and efavirenz was approximately 2.6 min. The calibration curves showed linearity (coefficient of regression, r>0.99 over the concentration range of 1.0-2,500 ng/mL. The intraday precision based on the standard deviation of replicates of lower limit of quantification (LLOQ was 9.24% and for quality control (QC samples ranged from 2.41% to 6.42% and with accuracy from 112% and 100-111% for LLOQ and QC samples. The inter day precision was 12.3% and 3.03-9.18% for LLOQ and quality controls samples, and the accuracy was 108% and 95.2-108% for LLOQ and QC samples. Stability studies showed that efavirenz was stable during the expected conditions for sample preparation and storage. The lower limit of quantification for efavirenz was 1 ng/mL. The analytical method showed excellent sensitivity, precision, and accuracy. This method is robust and is being successfully applied for therapeutic drug monitoring and pharmacokinetic studies in HIV-infected patients.

  2. Liquid chromatography tandem mass spectrometry method for the estimation of lamotrigine in human plasma: Application to a pharmacokinetic study

    Directory of Open Access Journals (Sweden)

    Santosh Ghatol

    2013-04-01

    Full Text Available A reliable, selective and sensitive liquid chromatography tandem mass spectrometry method was developed and validated for the quantification of lamotrigine in human plasma using lamotrigine-13C3, d3 as an internal standard. Analyte and internal standard were extracted from human plasma by solid-phase extraction and detected in positive ion mode by tandem mass spectrometry with electrospray ionization (ESI interface. Chromatographic separation was performed on a Chromolith® SpeedROD; RP-18e column (50−4.6 mm i.d. using acetonitrile: 5±0.1 mM ammonium formate solution (90:10, v/v as the mobile phase at a flow rate of 0.500 mL/min. The calibration curves were linear over the range of 5.02–1226.47 ng/mL with the lower limit of quantitation validated at 5.02 ng/mL. The analytes were found stable in human plasma through three freeze (−20 °C-thaw (ice-cold water bath cycles and under storage on bench-top in ice-cold water bath for at least 6.8 h, and also in the mobile phase at 10 °C for at least 57 h. The method has shown good reproducibility, as the intra- and inter-day precisions were within 3.0%, while the accuracies were within ±6.0% of nominal values. The validated LC–MS/MS method was applied for the evaluation of pharmacokinetic and bioequivalence parameters of lamotrigine after an oral administration of 50 mg lamotrigine tablet to thirty-two healthy adult male volunteers. Keywords: Lamotrigine, Liquid chromatography/tandem mass spectrometry, Solid phase extraction, Pharmacokinetic study

  3. Optimization of determination of 126Sn by ion exchange chromatography method (presentation)

    International Nuclear Information System (INIS)

    Pasteka, L.; Dulanska, S.

    2013-01-01

    The aim of the work is to optimize the uptake of tin on anion exchange resins and application of this knowledge for the analysis of samples of radioactive waste from the device of Jaslovske Bohunice and Mochovce in determining of 126 Sn. First to be optimized a method for the separation of tin on ion exchange sorbent Anion Exchange Resin (1-X8, Chloride Form) from Eichrom Technologies. Model sample was prepared in 7 mol dm -3 HCl, because in that environment a sorbent effectively captures the tin, which is bounded complexly with chloride anions as SnCl 6 2- . The radiochemical separation yield was monitored by gamma spectrometric measurements on high purity germanium detector HPGe (E = 391 keV) by adding isotope 113 Sn to each model solution. The method of tin separation was optimized on model samples.

  4. [Simultaneous determination of eleven components in Ginkgo biloba leaves by high performance liquid chromatography method].

    Science.gov (United States)

    Lv, Jin-Li; Yang, Biao; Li, Meng-Xuan; Meng, Zhao-Qing; Ma, Shi-Ping; Wang, Zhen-Zhong; Ding, Gang; Huang, Wen-Zhe; Xiao, Wei

    2017-03-01

    To study Ginkgo biloba leaves in different producing area, we establish an HPLC method for the simultaneously determination of seven flavonoids glycosides and four biflavonoids in G. biloba leaves. The analysis was performed on an Agilent ZORBAX SB-C₁₈ column(4.6 mm×250 mm, 5 μm) wich acetonitrile, and 0.4% phosphoric acid as mobile phase at flow rate of 1 mL•min⁻¹ in a gradient edution, and the detection was carried out at 254 nm.The calibration curves of the seven flavonoids glycosides and four biflavonoids had a good linearitiy with good recoveries. The established HPLC method is simple, rapid, accurate, reliable, and sensitive, and can be applied to the identification and quality control of G. biloba leaves. Copyright© by the Chinese Pharmaceutical Association.

  5. Study on atmospheric hydrogen enrichment by cryopump method and isotope separation by gas chromatography

    International Nuclear Information System (INIS)

    Taniyama, Yuki; Momoshima, Noriyuki

    2001-01-01

    To obtain the information of source of atmospheric hydrogen tritium an analysis of tritium isotopes is thought to be effective. So an atmospheric hydrogen enrichment apparatus and a cryogenic gas chromatographic column were made. Experiments were carried out to study the performance of cryopump to enrich atmospheric hydrogen and the column to separate hydrogen isotopes that obtained by cryopump method. The cryopump was able to process about 1000 1 atmosphere and the column was able to separate hydrogen isotopes with good resolution. (author)

  6. Method Optimization for Rapid Measurement of Carbohydrates in Plasma by Liquid Chromatography Tandem Mass Spectrometry

    International Nuclear Information System (INIS)

    Nguyen, Ductoan; Yu, Jondong; Mho, Sunil; Lee, Gwang; Lee, Haelee; Paik, Manjeong; Yee, Sungtae

    2013-01-01

    In conclusion, the developed HPLC coupled with ESI-MS was a powerful technique for the separation and characterization of carbohydrates by either SIM or MRM mode. The present method will be useful for the monitoring of carbohydrate profile in biological fluids from various diseases including diabetic ketoacidosis, hypoglycemia and hyperosmolar coma. Carbohydrates are one of the most abundant classes of organic compounds in nature, which not only constitute complex biomolecules in human and animals but are also distributed in plants and bacteria

  7. Method for the Determination of Ammonia in Mainstream Cigarette Smoke Using Ion Chromatography.

    Directory of Open Access Journals (Sweden)

    Christina Vaughan Watson

    Full Text Available Ammonia in mainstream smoke is present in both the particulate and vapor phases. The presence of ammonia in the cigarette filler material and smoke is of significance because of the potential role ammonia could have in raising the "smoke pH." An increased smoke pH could shift a fraction of total nicotine to free-base nicotine, which is reportedly more rapidly absorbed by the smoker. Methods measuring ammonia in smoke typically employ acid filled impingers to trap the smoke. We developed a fast, reliable method to measure ammonia in mainstream smoke without the use of costly and time consuming impingers to examine differences in ammonia delivery. The method uses both a Cambridge filter pad and a Tedlar bag to capture particulate and vapor phases of the smoke. We quantified ammonia levels in the mainstream smoke of 50 cigarette brands from 5 manufacturers. Ammonia levels ranged from approximately 1μg to 23μg per cigarette for ISO smoking conditions and 38μg to 67μg per cigarette for Canadian intense smoking conditions and statistically significance differences were observed between brands and manufacturers. Our findings suggest that ammonia levels vary by brand and are higher under Canadian intense smoking conditions.

  8. Proceedings of a workshop on methods for neutron scattering instrumentation design

    International Nuclear Information System (INIS)

    Hjelm, R.P.

    1997-09-01

    The future of neutron and x-ray scattering instrument development and international cooperation was the focus of the workshop. The international gathering of about 50 participants representing 15 national facilities, universities and corporations featured oral presentations, posters, discussions and demonstrations. Participants looked at a number of issues concerning neutron scattering instruments and the tools used in instrument design. Objectives included: (1) determining the needs of the neutron scattering community in instrument design computer code and information sharing to aid future instrument development, (2) providing for a means of training scientists in neutron scattering and neutron instrument techniques, and (3) facilitating the involvement of other scientists in determining the characteristics of new instruments that meet future scientific objectives, and (4) fostering international cooperation in meeting these needs. The scope of the meeting included: (1) a review of x-ray scattering instrument design tools, (2) a look at the present status of neutron scattering instrument design tools and models of neutron optical elements, and (3) discussions of the present and future needs of the neutron scattering community. Selected papers were abstracted separately for inclusion to the Energy Science and Technology Database

  9. Proceedings of a workshop on methods for neutron scattering instrumentation design

    Energy Technology Data Exchange (ETDEWEB)

    Hjelm, R.P. [ed.] [Los Alamos National Lab., NM (United States)

    1997-09-01

    The future of neutron and x-ray scattering instrument development and international cooperation was the focus of the workshop. The international gathering of about 50 participants representing 15 national facilities, universities and corporations featured oral presentations, posters, discussions and demonstrations. Participants looked at a number of issues concerning neutron scattering instruments and the tools used in instrument design. Objectives included: (1) determining the needs of the neutron scattering community in instrument design computer code and information sharing to aid future instrument development, (2) providing for a means of training scientists in neutron scattering and neutron instrument techniques, and (3) facilitating the involvement of other scientists in determining the characteristics of new instruments that meet future scientific objectives, and (4) fostering international cooperation in meeting these needs. The scope of the meeting included: (1) a review of x-ray scattering instrument design tools, (2) a look at the present status of neutron scattering instrument design tools and models of neutron optical elements, and (3) discussions of the present and future needs of the neutron scattering community. Selected papers were abstracted separately for inclusion to the Energy Science and Technology Database.

  10. An optimized method for fatty acid analysis, including quantification of trans fatty acids, in human adipose tissue by gas-liquid chromatography

    DEFF Research Database (Denmark)

    Bysted, Anette; Cold, S; Hølmer, Gunhild Kofoed

    1999-01-01

    Considering the need for a quick direct method for measurement of the fatty acid composition including trans isomers ofhuman adipose tissue we have developed a procedure using gas-liquid chromatography (GLC) alone, which is thussuitable for validation of fatty acid status in epidemiological studies...... for 25 min, and finally raised at 25 degrees C/min to 225 degrees C. The trans and cis isomers of18:1 were well separated from each other, as shown by silver-ion thin-layer chromatography. Verification by standardsshowed that the trans 18:1 isomers with a double bond in position 12 or lower were...

  11. Multiclass mycotoxin analysis in edible oils using a simple solvent extraction method and liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Eom, Taeyong; Cho, Hyun-Deok; Kim, Junghyun; Park, Mihee; An, Jinyoung; Kim, Moosung; Kim, Sheen-Hee; Han, Sang Beom

    2017-11-01

    A simple and rapid method for the simultaneous determination of 11 mycotoxins - aflatoxins B 1 , B 2 , G 1 and G 2 ; fumonisins B 1 , B 2 and B 3 ; ochratoxin A; zearalenone; deoxynivalenol; and T-2 toxin - in edible oils was established using liquid chromatography tandem mass spectrometry (LC-MS/MS). In this study, QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe), QuEChERS with dispersive liquid-liquid microextraction, and solvent extraction were examined for sample preparation. Among these methods, solvent extraction with a mixture of formic acid/acetonitrile (5/95, v/v) successfully extracted all target mycotoxins. Subsequently, a defatting process using n-hexane was employed to remove the fats present in the edible oil samples. Mass spectrometry was carried out using electrospray ionisation in polarity switching mode with multiple reaction monitoring. The developed LC-MS/MS method was validated by assessing the specificity, linearity, recovery, limit of quantification (LOQ), accuracy and precision with reference to Commission Regulation (EC) 401/2006. Mycotoxin recoveries of 51.6-82.8% were achieved in addition to LOQs ranging from 0.025 ng/g to 1 ng/g. The edible oils proved to be relatively uncomplicated matrices and the developed method was applied to 9 edible oil samples, including soybean oil, corn oil and rice bran oil, to evaluate potential mycotoxin contamination. The levels of detection were significantly lower than the international regulatory standards. Therefore, we expect that our developed method, based on simple, two-step sample preparation process, will be suitable for the large-scale screening of mycotoxin contamination in edible oils.

  12. A novel method for analysing key corticosteroids in polar bear (Ursus maritimus) hair using liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Weisser, Johan J; Hansen, Martin; Björklund, Erland; Sonne, Christian; Dietz, Rune; Styrishave, Bjarne

    2016-04-01

    This paper presents the development and evaluation of a methodology for extraction, clean-up and analysis of three key corticosteroids (aldosterone, cortisol and corticosterone) in polar bear hair. Such a methodology can be used to monitor stress biomarkers in polar bears and may provide as a useful tool for long-term and retrospective information. We developed a combined pressurized liquid extraction (PLE)-solid phase extraction (SPE) procedure for corticosteroid extraction and clean-up followed by high pressure liquid chromatography tandem mass spectrometry (HPLC-MS/MS) analysis. This procedure allows for the simultaneous determination of multiple steroids, which is in contrast to previous polar bear studies based on ELISA techniques. Absolute method recoveries were 81%, 75% and 60% for cortisol, corticosterone and aldosterone, respectively. We applied the developed method on a hair sample pooled from four East Greenland polar bears. Herein cortisol and corticosterone were successfully determined in levels of 0.32±0.02ng/g hair and 0.13±0.02ng/g hair, respectively. Aldosterone was below limit of detection (LODpolar bears was consistent with cortisol levels previously determined in the Southern Hudson Bay and James Bay in Canada using ELISA kits. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Prediction of retention in micellar electrokinetic chromatography based on molecular structural descriptors by using the heuristic method

    International Nuclear Information System (INIS)

    Liu Huanxiang; Yao Xiaojun; Liu Mancang; Hu Zhide; Fan Botao

    2006-01-01

    Based on calculated molecular descriptors from the solutes' structure alone, the micelle-water partition coefficients of 103 solutes in micellar electrokinetic chromatography (MEKC) were predicted using the heuristic method (HM). At the same time, in order to show the influence of different molecular descriptors on the micelle-water partition of solute and to well understand the retention mechanism in MEKC, HM was used to build several multivariable linear models using different numbers of molecular descriptors. The best 6-parameter model gave the following results: the square of correlation coefficient R 2 was 0.958 and the mean relative error was 3.98%, which proved that the predictive values were in good agreement with the experimental results. From the built model, it can be concluded that the hydrophobic, H-bond, polar interactions of solutes with the micellar and aqueous phases are the main factors that determine their partitioning behavior. In addition, this paper provided a simple, fast and effective method for predicting the retention of the solutes in MEKC from their structures and gave some insight into structural features related to the retention of the solutes

  14. Chiral liquid chromatography-mass spectrometry (LC-MS/MS) method development for the detection of salbutamol in urine samples.

    Science.gov (United States)

    Chan, Sue Hay; Lee, Warren; Asmawi, Mohd Zaini; Tan, Soo Choon

    2016-07-01

    A sequential solid-phase extraction (SPE) method was developed and validated using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) for the detection and quantification of salbutamol enantiomers in porcine urine. Porcine urine samples were hydrolysed with β-glucuronidase/arylsulfatase from Helix pomatia and then subjected to a double solid-phase extraction (SPE) first using the Abs-Elut Nexus SPE and then followed by the Bond Elut Phenylboronic Acid (PBA) SPE. The salbutamol enantiomers were separated using the Astec CHIROBIOTIC™ T HPLC column (3.0mm×100mm; 5μm) maintained at 15°C with a 15min isocratic run at a flow rate of 0.4mL/min. The mobile phase constituted of 5mM ammonium formate in methanol. Salbutamol and salbutamol-tert-butyl-d9 (internal standard, IS) was monitored and quantified with the multiple reaction monitoring (MRM) mode. The method showed good linearity for the range of 0.1-10ng/mL with limit of quantification at 0.3ng/mL. Analysis of the QC samples showed intra- and inter-assay precisions to be less than 5.04%, and recovery ranging from 83.82 to 102.33%. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Development of Extraction Methods for the Analysis of Perfluorinated Compounds in Leather with High Performance Liquid Chromatography Tandem Mass Spectrometry

    Science.gov (United States)

    Zhang, Yan; Wang, Youchao; Tang, Chuanjiang; Nie, Jingmei; Xu, Chengtao

    2018-01-01

    Perfluorinated compounds (PFCs), used to provide water, oil, grease, heat and stain repellency to a range of textile and other products, have been found to be persistent in the environment and are associated with adverse effects on humans and wildlife. This study presents the development and validation of an analytical method to determine the simultaneous presence of eleven PFCs in leather using solid-phase extraction followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The perfluorinated compounds were primarily extracted from the samples by a liquid extraction procedure by ultrasonic, in which the parameters were optimized. Then the solid-phase extraction (SPE) is the most important advantages of the developed methodology. The sample volume and elution conditions were optimized by means of an experimental design. The proposed method was applied to determine the PFCs in leather, where the detection limits of the eleven compounds were 0.09-0.96 ng/L, and the recoveries of all compounds spiked at 5 ng/L concentration level were in the range of 65-96%, with a better RSD lower than 19% (n = 7).

  16. Optimized method for the determination of itopride in human plasma by high-performance liquid chromatography with fluorimetric detection.

    Science.gov (United States)

    Ptácek, Pavel; Klíma, Josef; Macek, Jan

    2009-03-15

    A high-performance liquid chromatographic method with fluorescence detection for the determination of itopride in human plasma is reported. The sample preparation was based on liquid-liquid extraction of itopride from plasma with t-butylmethylether and dichloromethane (70:30, v/v) mixture followed by a back extraction of the analyte to the phosphate buffer (pH 3.2). Liquid chromatography was performed on an octadecylsilica column (55 mm x 4 mm, 3 microm particles), the mobile phase consisted of acetonitrile-triethylamine-15 mM dihydrogenpotassium phosphate (14.5:0.5:85, v/v/v), pH of the mobile phase was adjusted to 4.8. The run time was 3 min. The fluorimetric detector was operated at 250/342 nm (excitation/emission wavelength). Naratriptan was used as the internal standard. The limit of quantitation was 9.5 ng/ml using 0.5 ml of plasma. The method precision and inaccuracy were less than 8%. The assay was applied to the analysis of samples from a bioequivalence study.

  17. Liquid chromatography – tandem mass spectrometry method for the determination of ten tetracycline residues in muscle samples

    Directory of Open Access Journals (Sweden)

    Gajda Anna

    2015-09-01

    Full Text Available A liquid chromatography – tandem mass spectrometry (LC-MS/MS method for the determination of oxytetracycline (OTC, 4-epi oxytetracycline (4-epi OTC, tetracycline (TC, 4-epi tetracycline (4-epi TC, chlortetracycline (CTC, 4-epi chlortetracycline (4-epi CTC, doxycycline (DC, minocycline (MINO, methacycline (META and rolitetracycline (ROLI residues in muscles was developed. The procedure consisted of an oxalic acid extraction followed by protein removal with trichloroacetic acid. Further solid phase clean-up on polymeric (Strata X reversed phase columns was performed to obtain an extract suitable for LC-MS/MS analysis. The tetracyclines were separated on a C 18 analytical column with mobile phase consisting of 0.01% formic acid in acetonitrile and 0.01% formic acid in water in gradient mode. The method was validated according to the Commission Decision 2002/657/EC. The recoveries of all target compounds were 91.8% – 103.6%. The decision limits were from 109.0 to 119.8 μg/kg and detection capability varied within the range of 122.2 to 137.6 μg/kg, depending on the analyte.

  18. Standardization method for measurement of hydroxyurea by Ultra High Efficiency Liquid Chromatography in plasma of patients with sickle cell disease

    Directory of Open Access Journals (Sweden)

    Darcielle Bruna Dias Elias

    2014-09-01

    Full Text Available Sickle cell anemia (SCA is a recessively inherited disease characterized by chronic hemolytic anemia, chronic inflammation, and acute episodes of hemolysis. Hydroxyurea (HU is widely used to increase the levels of fetal hemoglobin (HbF. The objective of this study was to standardize and validate a method for the quantification of HU in human plasma by using ultra high performance liquid chromatography (UPLC in order to determine the plasma HU levels in adult patients with SCA who had been treated with HU. We used an analytical reverse phase column (Nucleosil C18 with a mobile phase consisting of acetonitrile/water (16.7/83.3. The retention times of HU, urea, and methylurea were 6.7, 7.7, and 11.4 min, respectively. All parameters of the validation process were defined. To determine the precision and accuracy of quality controls, HU in plasma was used at concentrations of 100, 740, and 1600 µM, with methylurea as the internal standard. Linearity was assessed in the range of 50-1600 µM HU in plasma, obtaining a correlation coefficient of 0.99. The method was accurate and precise and can be used for the quantitative determination of HU for therapeutic monitoring of patients with SCA treated with HU.

  19. Improved method for the determination of serotonin in plasma by high-performance liquid chromatography using on-line sample pre-treatment

    NARCIS (Netherlands)

    Takkenberg, B.; Endert, E.; van Ingen, H. E.; Ackermans, M.

    1991-01-01

    An improved method for the determination of serotonin in platelet-rich plasma (PRP) and platelet-poor plasma (PPP), by reversed-phase high-performance liquid chromatography with electrochemical detection and direct plasma injection, is described. The chromatographic system comprises a strong

  20. A liquid chromatography-mass spectrometry method for the quantification of bioavailability and bioconversion of beta-carotene to retinol in humans

    NARCIS (Netherlands)

    Yan Wang,; Xiaoying Xu,; Lieshout, van M.; West, C.E.; Lugtenburg, J.; Verhoeven, M.A.; Creemers, A.F.L.

    2000-01-01

    A method based on high-performance liquid chromatography-atmospheric pressure chemical ionization mass spectrometry (APCI LC-MS) was developed for the quantification of the bioavailability of retinyl palmitate and -carotene and the bioconversion of -carotene to retinol in humans. Following oral

  1. A validated liquid chromatography-tandem mass spectrometry method for the quantitative determination of 4 beta-hydroxycholesterol in human plasma

    NARCIS (Netherlands)

    van de Merbel, Nico C.; Bronsema, Kees J.; van Hout, Mischa W. J.; Nilsson, Ralf; Sillen, Henrik

    2011-01-01

    A novel liquid chromatography-tandem mass spectrometry method is described for the quantitative determination of the endogenous CYP 3A4/5 marker 4 beta-hydroxycholesterol in human K(2)-EDTA plasma. It is based on alkaline hydrolysis to convert esterified to free 4 beta-hydroxycholesterol, followed

  2. Determination of telmisartan in human blood plasma: Part II: Liquid chromatography-tandem mass spectrometry method development, comparison to immunoassay and pharmacokinetic study

    NARCIS (Netherlands)

    Hempen, C.M.; Gläsle-Schwarz, Liane; Kunz, Ulrich; Karst, U.

    2006-01-01

    A new liquid chromatography/atmospheric pressure chemical ionization-tandem mass spectrometry (LC/APCI-MS/MS) method with on-line sample clean-up for the determination of telmisartan in human blood plasma is presented. This technique is compared to a previously introduced enzyme-linked immunosorbent

  3. Comparative Study of Continuous Pralidoxime Infusion versus Intermittent Dosing: Application of High-Performance Liquid Chromatography Method on Serum of Organophosphate Poisoned Patients

    Directory of Open Access Journals (Sweden)

    Girish Thunga

    2013-09-01

    How to cite this article: Thunga G, Pandey S, Nair S, Mylapuri R, Vidyasagar S, Kunhikatta V, et al. Comparative Study of Continuous Pralidoxime Infusion versus Intermittent Dosing: Application of High-Performance Liquid Chromatography Method on Serum of Organophosphate Poisoned Patients. Asia Pac J Med Toxicol 2013;2:105-10.

  4. A new liquid chromatography - tandem mass spectrometry method using atmospheric pressure photo ionization for the simultaneous determination of azaarenes and azaarones in Dutch river sediments

    NARCIS (Netherlands)

    Brulik, J.; Simek, Z.; de Voogt, P.

    2013-01-01

    A new method for the analysis of azaarenes and their degradation products (azaarones) was developed, optimized and validated using liquid chromatography coupled with atmospheric pressure photo ionization tandem mass spectrometric detection (LC-APPI/MS/MS). Seventeen compounds including 4 PAHs

  5. Validation of an analytical method for the determination of spiramycin, virginiamycin and tylosin in feeding-stuffs bij thin-layer chromatography and bio-autography

    NARCIS (Netherlands)

    Vincent, U.; Gizzi, G.; Holst, von C.; Jong, de J.; Michard, J.

    2007-01-01

    An inter-laboratory validation was carried out to determine the performance characteristics of an analytical method based on thin-layer chromatography (TLC) coupled to microbiological detection (bio-autography) for screening feed samples for the presence of spiramycin, tylosin and virginiamycin.

  6. An on-line normal-phase high performance liquid chromatography method for the rapid detection of radical scavengers in non-polar food matrixes

    NARCIS (Netherlands)

    Zhang, Q.; Klift, van der E.J.C.; Janssen, H.G.; Beek, van T.A.

    2009-01-01

    An on-line method for the rapid pinpointing of radical scavengers in non-polar mixtures like vegetable oils was developed. To avoid problems with dissolving the sample, normal-phase chromatography on bare silica gel was used with mixtures of hexane and methyl tert-butyl ether as the eluent. The high

  7. Supercritical fluid chromatography

    Science.gov (United States)

    Vigdergauz, M. S.; Lobachev, A. L.; Lobacheva, I. V.; Platonov, I. A.

    1992-03-01

    The characteristic features of supercritical fluid chromatography (SCFC) are examined and there is a brief historical note concerning the development of the method. Information concerning the use of supercritical fluid chromatography in the analysis of objects of different nature is presented in the form of a table. The roles of the mobile and stationary phases in the separation process and the characteristic features of the apparatus and of the use of the method in physicochemical research are discussed. The bibliography includes 364 references.

  8. Determination of haloacetic acids in water by ion chromatography--method development.

    Science.gov (United States)

    Lopez-Avila, V; Liu, Y; Charan, C

    1999-01-01

    The microextraction/ion chromatographic (IC) method developed in this study involves extraction of 9 haloacetic acids (HAAs) from aqueous samples (acidified with sulfuric acid to a pH of copper sulfate pentahydrate and sodium sulfate) with methyl tert-butyl ether (MTBE), back extraction into reagent water, and analysis by IC with conductivity detection. The separation column consists of an Ion Pac AG-11 (2 mm id x 50 mm length) guard column and an Ion Pac AS-11 (2 mm id x 250 mm length) analytical column, and the concentration column is a 4 mm id x 35 mm length Dionex TAC-LP column. Use of the 2 mm id Dionex AS-11 column improved detection limits especially for trichloracetic acid (TCAA), bromodichloroacetic acid (BDCAA), dibromochloroacetic acid (DBCAA), and tribromoacetic acid (TBAA). The peak interfering with BCAA elutes at the same retention time as nitrate; however, we have not confirmed the presence of nitrate. Stability studies indicate that HAAs are stable in water for at least 8 days when preserved with ammonium chloride at 100 mg/L and stored at 4 degrees C in the dark. At day 30, recoveries were still high (e.g., 92.1-106%) for dichloroacetic acid (DCAA), BCAA, dibromoacetic acid (DBAA), trichloroacetic acid (TCAA), BDCAA, and DBCAA. However, recoveries of monochloroacetic acid (MCAA), monobromoacetic acid (MBAA), and TBAA were only 54.6, 56.8, and 66.8%, respectively. Stability studies of HAAs in H2SO4-saturated MTBE indicate that all compounds except TBAA are stable for 48 h when stored at 4 degrees C in the dark. TBAA recoveries dropped to 47.1% after 6 h of storage and no TBAA was detected after 48 h of storage. The method described here is only preliminary and was tested in only one laboratory. Additional research is needed to improve method performance.

  9. Field estimation of soil water content. A practical guide to methods, instrumentation and sensor technology

    International Nuclear Information System (INIS)

    2008-01-01

    During a period of five years, an international group of soil water instrumentation experts were contracted by the International Atomic Energy Agency to carry out a range of comparative assessments of soil water sensing methods under laboratory and field conditions. The detailed results of those studies are published elsewhere. Most of the devices examined worked well some of the time, but most also performed poorly in some circumstances. The group was also aware that the choice of a water measurement technology is often made for economic, convenience and other reasons, and that there was a need to be able to obtain the best results from any device used. The choice of a technology is sometimes not made by the ultimate user, or even if it is, the main constraint may be financial rather than technical. Thus, this guide is presented in a way that allows the user to obtain the best performance from any instrument, while also providing guidance as to which instruments perform best under given circumstances. That said, this expert group of the IAEA reached several important conclusions: (1) the field calibrated neutron moisture meter (NMM) remains the most accurate and precise method for soil profile water content determination in the field, and is the only indirect method capable of providing accurate soil water balance data for studies of crop water use, water use efficiency, irrigation efficiency and irrigation water use efficiency, with a minimum number of access tubes; (2) those electromagnetic sensors known as capacitance sensors exhibit much more variability in the field than either the NMM or direct soil water measurements, and they are not recommended for soil water balance studies for this reason (impractically large numbers of access tubes and sensors are required) and because they are rendered inaccurate by changes in soil bulk electrical conductivity (including temperature effects) that often occur in irrigated soils, particularly those containing

  10. Validation of a high performance liquid chromatography method for the stabilization of epigallocatechin gallate.

    Science.gov (United States)

    Fangueiro, Joana F; Parra, Alexander; Silva, Amélia M; Egea, Maria A; Souto, Eliana B; Garcia, Maria L; Calpena, Ana C

    2014-11-20

    Epigallocatechin gallate (EGCG) is a green tea catechin with potential health benefits, such as anti-oxidant, anti-carcinogenic and anti-inflammatory effects. In general, EGCG is highly susceptible to degradation, therefore presenting stability problems. The present paper was focused on the study of EGCG stability in HEPES (N-2-hydroxyethylpiperazine-N'-2-ethanesulfonic acid) medium regarding the pH dependency, storage temperature and in the presence of ascorbic acid a reducing agent. The evaluation of EGCG in HEPES buffer has demonstrated that this molecule is not able of maintaining its physicochemical properties and potential beneficial effects, since it is partially or completely degraded, depending on the EGCG concentration. The storage temperature of EGCG most suitable to maintain its structure was shown to be the lower values (4 or -20 °C). The pH 3.5 was able to provide greater stability than pH 7.4. However, the presence of a reducing agent (i.e., ascorbic acid) was shown to provide greater protection against degradation of EGCG. A validation method based on RP-HPLC with UV-vis detection was carried out for two media: water and a biocompatible physiological medium composed of Transcutol®P, ethanol and ascorbic acid. The quantification of EGCG for purposes, using pure EGCG, requires a validated HPLC method which could be possible to apply in pharmacokinetic and pharmacodynamics studies. Copyright © 2014. Published by Elsevier B.V.

  11. Method optimization for drug impurity profiling in supercritical fluid chromatography: Application to a pharmaceutical mixture.

    Science.gov (United States)

    Muscat Galea, Charlene; Didion, David; Clicq, David; Mangelings, Debby; Vander Heyden, Yvan

    2017-12-01

    A supercritical chromatographic method for the separation of a drug and its impurities has been developed and optimized applying an experimental design approach and chromatogram simulations. Stationary phase screening was followed by optimization of the modifier and injection solvent composition. A design-of-experiment (DoE) approach was then used to optimize column temperature, back-pressure and the gradient slope simultaneously. Regression models for the retention times and peak widths of all mixture components were built. The factor levels for different grid points were then used to predict the retention times and peak widths of the mixture components using the regression models and the best separation for the worst separated peak pair in the experimental domain was identified. A plot of the minimal resolutions was used to help identifying the factor levels leading to the highest resolution between consecutive peaks. The effects of the DoE factors were visualized in a way that is familiar to the analytical chemist, i.e. by simulating the resulting chromatogram. The mixture of an active ingredient and seven impurities was separated in less than eight minutes. The approach discussed in this paper demonstrates how SFC methods can be developed and optimized efficiently using simple concepts and tools. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Cluster cosmological analysis with X ray instrumental observables: introduction and testing of AsPIX method

    International Nuclear Information System (INIS)

    Valotti, Andrea

    2016-01-01

    Cosmology is one of the fundamental pillars of astrophysics, as such it contains many unsolved puzzles. To investigate some of those puzzles, we analyze X-ray surveys of galaxy clusters. These surveys are possible thanks to the bremsstrahlung emission of the intra-cluster medium. The simultaneous fit of cluster counts as a function of mass and distance provides an independent measure of cosmological parameters such as Ω m , σ s , and the dark energy equation of state w0. A novel approach to cosmological analysis using galaxy cluster data, called top-down, was developed in N. Clerc et al. (2012). This top-down approach is based purely on instrumental observables that are considered in a two-dimensional X-ray color-magnitude diagram. The method self-consistently includes selection effects and scaling relationships. It also provides a means of bypassing the computation of individual cluster masses. My work presents an extension of the top-down method by introducing the apparent size of the cluster, creating a three-dimensional X-ray cluster diagram. The size of a cluster is sensitive to both the cluster mass and its angular diameter, so it must also be included in the assessment of selection effects. The performance of this new method is investigated using a Fisher analysis. In parallel, I have studied the effects of the intrinsic scatter in the cluster size scaling relation on the sample selection as well as on the obtained cosmological parameters. To validate the method, I estimate uncertainties of cosmological parameters with MCMC method Amoeba minimization routine and using two simulated XMM surveys that have an increasing level of complexity. The first simulated survey is a set of toy catalogues of 100 and 10000 deg 2 , whereas the second is a 1000 deg 2 catalogue that was generated using an Aardvark semi-analytical N-body simulation. This comparison corroborates the conclusions of the Fisher analysis. In conclusion, I find that a cluster diagram that accounts

  13. New separation and detection methods in capillary electrophoresis and ion chromatography for the analysis of ionic compounds

    International Nuclear Information System (INIS)

    Mayrhofer, K.

    1999-10-01

    The first part of the thesis deals with the simultaneous analysis of inorganic anions and organic acids in electrodeposition coatings with the co-electroosmotic capillary electrophoresis. The coating of workpieces, e.g. car bodies, by means of an electrodeposition process is an important methodology especially in the automotiv industries. It is usually performed by introducing the object into a basin filled with a water-based electro-dipcoat, applying a voltage of 200-400 Volts (direct current) and using the bodywork as cathode. Because the workpiece has to pass a number of preliminary treatments before the coating procedure, ionic compound may be carried into the basin. If the concentrations of these ionic impurities is too high, the electro-deposition of the binding agent fails or the thickness of the coating is not reproducible. The organic acids are used as neutralization agents in order to control and to keep the pH of the basin constant. The common method of analysing ionic impurities is ion chromatography. The organic acids have to be separated in an ion exclusion chromatography column because organic acids may coelute with the inorganic anions or elute with the dead volume. Therefore a separation method for capillary electrophoresis was developed which enables the simultaneouse analysis of inorganic anions and organic acids in less then 5 minutes. Chloride, nitrate, sulfate, fuoride, phosphate, carbonate, formic acid, acetic acid, lactic acid and butyric acid were detected with indirect UV-detection at 254 nm. For removal of the the binding agent and the pigments the lacquer was mixed with a 0.01 M sodium hydroxide solution and then filtered through a 0.45 μm filter cartridge. 5 mM trimellitic acid, titrated with sodium hydroxid to pH 10, 0.001 % hexadimethrinbromide and 20 % acetonitrile served as buffer. The analytes were separated with a satisfactory resolution. Between every analysis the fused silica capillary was purged for two minutes with buffer. So

  14. [Various methods for the determination of preservatives in food. II. Gaschromatography, high performance liquid chromatography, TAS-method (author's transl)].

    Science.gov (United States)

    Hild, J; Gertz, C

    1980-02-01

    For the quantitative determination of preservatives in food, analyses were carried out by means of GLC, HPLC, and TLC according to the TAS-method. Using the alkaline extract (sample preparation see part I) the preservatives can be analysed as free acid or appropriate ester out the same GLC-column without any interference from coextractives. A fast and accurate HPLC determination can be achieved by direct injection of the alkaline extract. All preservatives were well separated and detected at a wavelength of 225 resp. 232 nm. As a quick test for the qualitative estimation the TLC (TAS) method is suggested and a suitable solvent system is proposed.

  15. RESEARCH OF SOPHORA JAPONICA L. FLOWER BUDS VOLATILE COMPOUNDS WITH GAS-CHROMATOGRAPHY/MASS- SPECTROMETRY METHOD

    Directory of Open Access Journals (Sweden)

    Cholak I.S.

    2013-10-01

    Full Text Available This work represents the results of the research ofessential oil contained in Sophora japonica L. flowerbuds volatile compounds collected during the nextstages of their development: green flower buds, formedflower buds and the beginning of flower buds opening.Essential oil assay content in Sophora japonica L.flower buds was determined with hydrodistillationmethod. Content of essential oil in the raw material isless than 0,1%. Qualitative composition and assaycontent of Sophora japonica L. flower buds essential oilconstituents were determined with chromato-massspectrometry method. In consequence of the research 80constituents were identified in Sophora japonica L.flower buds out of which 61 substances are during thegreen flower buds and beginning of flower budsopening stages, 66 substances are during formed flowerbuds stage. Substances are represented by aliphatic andcyclic terpenoids, their alcohols and ketones. Mostvolatile substances were extracted on the stage offormed buds.

  16. Improved resins and novel materials and methods for solid phase extraction and high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Freeze, Ronald [Iowa State Univ., Ames, IA (United States)

    1997-10-08

    Solid-phase extraction (SPE) has grown to be one of the most widely used methods for isolation and preconcentration of a vast range of compounds from aqueous solutions. By modifying polymeric SPE resins with chelating functional groups, the selective uptake of metals was accomplished. The resin, along with adsorbed metals, was vaporized in the ICP and detection of the metals was then possible using either mass or emission spectroscopy. Drug analyses in biological fluids have received heightened attention as drug testing is on the increase both in sports and in the work environment. By using a direct-injection technique, biological fluids can be injected directly into the liquid chromatographic system with no pretreatment. A new surfactant, a sulfonated form of Brij-30 (Brij-S) is shown to prevent the uptake of serum proteins on commercial HPLC columns by forming a thin coating on the silica C18 surface. Excellent separations of eight or more drugs with a wide range of retention times were obtained. The separations had sharper peaks and lower retention times than similar separations performed with the surfactant sodium dodecylsulfate (SDS). Quantitative recovery of a number of drugs with limits of detection near 1 ppm with a 5 μl injection volume were obtained. Finally, a method for solid-phase extraction in a syringe is introduced. The system greatly reduced the volume of solvent required to elute adsorbed analytes from the SPE bed while providing a semi-automated setup. SPE in a syringe consists of a very small bed of resin-loaded membrane packed into a GC or HPLC syringe. After extraction, elution was performed with just a few μl of solvent. This small elution volume allowed injection of the eluent directly from the syringe into the chromatographic system, eliminating the handling problems associated with such small volumes.

  17. Determination of avermectins by the internal standard recovery correction - high performance liquid chromatography - quantitative Nuclear Magnetic Resonance method.

    Science.gov (United States)

    Zhang, Wei; Huang, Ting; Li, Hongmei; Dai, Xinhua; Quan, Can; He, Yajuan

    2017-09-01

    Quantitative Nuclear Magnetic Resonance (qNMR) is widely used to determine the purity of organic compounds. For the compounds with lower purity especially molecular weight more than 500, qNMR is at risk of error for the purity, because the impurity peaks are likely to be incompletely separated from the peak of major component. In this study, an offline ISRC-HPLC-qNMR (internal standard recovery correction - high performance liquid chromatography - qNMR) was developed to overcome this problem. It is accurate by excluding the influence of impurity; it is low-cost by using common mobile phase; and it extends the applicable scope of qNMR. In this method, a mix solution of the sample and an internal standard was separated by HPLC with common mobile phases, and only the eluents of the analyte and the internal standard were collected in the same tube. After evaporation and re-dissolution, it was determined by qNMR. A recovery correction factor was determined by comparison of the solutions before and after these procedures. After correction, the mass fraction of analyte was constant and it was accurate and precise, even though the sample loss varied during these procedures, or even in bad resolution of HPLC. Avermectin B 1 a with the purity of ~93% and the molecular weight of 873 was analyzed. Moreover, the homologues of avermectin B 1 a were determined based on the identification and quantitative analysis by tandem mass spectrometry and HPLC, and the results were consistent with the results of traditional mass balance method. The result showed that the method could be widely used for the organic compounds, and could further promote qNMR to become a primary method in the international metrological systems. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Development of a Microemulsion High Performance Liquid Chromatography (MELC Method for Determination of Salbutamol in Metered-Dose Inhalers (MDIS

    Directory of Open Access Journals (Sweden)

    J Hanaee

    2013-02-01

    Full Text Available Introduction: A sensitive and rapid oil-in-water (O/W microemulsion high performance liquid chromatography (MELC method has been developed. The water-in-oil (w/o microemulsion was used as a mobile phase in the determination of salbutamol in aqueous solutions. In addition, the influence of operating parameters on the separation performance was examined. Methods: The samples were injected into C18, (250mm×4.6mm analytical columns maintained at 25oC with a flow rate 1 ml/min. The mobile phase was 95.5% v/v aqueous orthophosphate buffer 20 mM (adjusted to pH 3 with orthophosphoric acid, 0.5% ethyl acetate, 1.5% Brij35, and 2.5% 1-butanol, all w/w. The salbutamol and internal standard peaks were detected by fluorescence detection at the excitation and emission wavelengths of 267 and 313 nm respectively. Results: The method had an accuracy of > 97.78% and the calibration curve was linear (r2 = 0.99 over salbutamol concentrations ranging from 25 to 500 ng/mL. The intra-day and inter-day precisions (CV % were <1.6 and <1.8, respectively. The limit of detection (LOD and limit of quantitation (LOQ were 9.61ng/ml and 29.13ng/ml, respectively. Conclusion: The method reported is simple, precise and accurate, and has the capacity to be used for determination of salbutamol in the pharmaceutical preparation.

  19. A Facile, Nonreactive Hydrogen Peroxide (H2O2) Detection Method Enabled by Ion Chromatography with UV Detector.

    Science.gov (United States)

    Song, Mingrui; Wang, Junli; Chen, Baiyang; Wang, Lei

    2017-11-07

    Hydrogen peroxide (H 2 O 2 ) is ubiquitous in the natural environment, and it is now widely used for pollutant control in water and wastewater treatment processes. However, current analytical methods for H 2 O 2 inevitably require reactions between H 2 O 2 and other reactants to yield signals and are thus likely subjective to the interferences of coexisting colored, oxidative, and reductive compounds. In order to overcome these barriers, we herein for the first time propose to analyze H 2 O 2 by ion chromatography (IC) using an ultraviolet (UV) detector. The proposal is based on two principles: first, that H 2 O 2 can deprotonate to hydroperoxyl ion (HO 2 - ) when eluent pH is higher than the acid-dissociation coefficient of H 2 O 2 (pK a = 11.6); and second, that after separation from other compounds via IC column, H 2 O 2 can be quantified by a UV detector. Under favorable operating conditions, this method has successfully achieved acceptable recoveries (>91%) of H 2 O 2 dosed to ultrapure and natural waters, a calibration curve with R 2 > 0.99 for a wide range of H 2 O 2 concentrations from 0.1 to 50 mg/L and a method detection limit of 0.027 mg/L. In addition, this approach was shown to be capable of distinguishing H 2 O 2 from anions (e.g., fluoride and chloride) and organics (e.g., glycolate) and monochloramine, suggesting that it is insensitive to many neighboring compounds as long as they do not react quickly with H 2 O 2 . Hence, this study proves the combination of IC and UV detector a facile and reliable method for H 2 O 2 measurement.

  20. [Improvement of the method for methylmercury determination in aquatic products using liquid chromatography online coupled with atomic fluorescence spectrometry].

    Science.gov (United States)

    Shang, Xiaohong; Zhao, Yunfeng; Zhang, Lei; Li, Xiaowei; Wu, Yongning

    2011-07-01

    The improvement method was developed for methylmercury determination using liquid chromatography online coupled with cold vapor atomic fluorescence spectrometry (LC-CV-AFS). Cysteine was used as complexing agent in mobile phase instead of mercaptoethanol. Under the optimized conditions, baseline separation of mercury species could be achieved within 8 min on a C18 column with a mobile phase of 5% (v/v) acetonitrile-1 g/L L-cysteine-50 mmol/L ammonium acetate aqueous solution. The linear range of calibration curve of methylmercury was 1-50 microg/L and the limit of detection (S/N = 3) for methylmercury was 0.3 microg/L. Ultrasonication assisted hydrochloric acid extraction was used to extract methylmercury from seafood samples. The sample extract was cleaned up by a C18 solid phase extraction (SPE) cartridge. For validation of the method, certified reference materials and spiked seafood samples were analyzed. The determined methylmercury contents of certified reference materials NIST1566b, BCR464 and GBW10029 agreed well with the certified values. The determined methylmercury values for Food Analysis Performance Assessment Scheme (FAPAS) sample 07115 were satisfied. The recoveries of methylmercury in seafood samples at three spiked levels (10, 50 and 500 microg/kg) ranged from 89% to 112%, including cooked seafood food. The precision of the method based on relative standard deviation (RSD) was not more than 7%. The present method of LC-CV-AFS is accurate, sensitive, simple, and can meet the demand of methylmercury determination in seafood.

  1. Development of liquid chromatography-tandem mass spectrometry methods for the quantitation of Anisakis simplex proteins in fish.

    Science.gov (United States)

    Fæste, Christiane Kruse; Moen, Anders; Schniedewind, Björn; Haug Anonsen, Jan; Klawitter, Jelena; Christians, Uwe

    2016-02-05

    The parasite Anisakis simplex is present in many marine fish species that are directly used as food or in processed products. The anisakid larvae infect mostly the gut and inner organs of fish but have also been shown to penetrate into the fillet. Thus, human health can be at risk, either by contracting anisakiasis through the consumption of raw or under-cooked fish, or by sensitisation to anisakid proteins in processed food. A number of different methods for the detection of A. simplex in fish and products thereof have been developed, including visual techniques and PCR for larvae tracing, and immunological assays for the determination of proteins. The recent identification of a number of anisakid proteins by mass spectrometry-based proteomics has laid the groundwork for the development of two quantitative liquid chromatography-tandem mass spectrometry methods for the detection of A. simplex in fish that are described in the present study. Both, the label-free semi-quantitative nLC-nESI-Orbitrap-MS/MS (MS1) and the heavy peptide-applying absolute-quantitative (AQUA) LC-TripleQ-MS/MS (MS2) use unique reporter peptides derived from anisakid hemoglobin and SXP/RAL-2 protein as analytes. Standard curves in buffer and in salmon matrix showed limits of detection at 1μg/mL and 10μg/mL for MS1 and 0.1μg/mL and 2μg/mL for MS2. Preliminary method validation included the assessment of sensitivity, repeatability, reproducibility, and applicability to incurred and naturally-contaminated samples for both assays. By further optimization and full validation in accordance with current recommendations the LC-MS/MS methods could be standardized and used generally as confirmative techniques for the detection of A. simplex protein in fish. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Comparative Analysis of Volatile Defensive Secretions of Three Species of Pyrrhocoridae (Insecta: Heteroptera by Gas Chromatography-Mass Spectrometric Method.

    Directory of Open Access Journals (Sweden)

    Jan Krajicek

    Full Text Available The true bugs (Hemiptera: Heteroptera have evolved a system of well-developed scent glands that produce diverse and frequently strongly odorous compounds that act mainly as chemical protection against predators. A new method of non-lethal sampling with subsequent separation using gas chromatography with mass spectrometric detection was proposed for analysis of these volatile defensive secretions. Separation was performed on Rtx-200 column containing fluorinated polysiloxane stationary phase. Various mechanical irritation methods (ultrasonics, shaking, pressing bugs with plunger of syringe were tested for secretion sampling with a special focus on non-lethal irritation. The preconcentration step was performed by sorption on solid phase microextraction (SPME fibers with different polarity. For optimization of sampling procedure, Pyrrhocoris apterus was selected. The entire multi-parameter optimization procedure of secretion sampling was performed using response surface methodology. The irritation of bugs by pressing them with a plunger of syringe was shown to be the most suitable. The developed method was applied to analysis of secretions produced by adult males and females of Pyrrhocoris apterus, Pyrrhocoris tibialis and Scantius aegyptius (all Heteroptera: Pyrrhocoridae. The chemical composition of secretion, particularly that of alcohols, aldehydes and esters, is species-specific in all three pyrrhocorid species studied. The sexual dimorphism in occurrence of particular compounds is largely limited to alcohols and suggests their epigamic intraspecific function. The phenetic overall similarities in composition of secretion do not reflect either relationship of species or similarities in antipredatory color pattern. The similarities of secretions may be linked with antipredatory strategies. The proposed method requires only a few individuals which remain alive after the procedure. Thus secretions of a number of species including even the rare

  3. Influence of different manufacturing methods on the cyclic fatigue of rotary nickel-titanium endodontic instruments.

    Science.gov (United States)

    Rodrigues, Renata C V; Lopes, Hélio P; Elias, Carlos N; Amaral, Georgiana; Vieira, Victor T L; De Martin, Alexandre S

    2011-11-01

    The aim of this study was to evaluate, by static and dynamic cyclic fatigue tests, the number of cycles to fracture (NCF) 2 types of rotary NiTi instruments: Twisted File (SybronEndo, Orange, CA), which is manufactured by a proprietary twisting process, and RaCe files (FKG Dentaire, La Chaux-de-Fonds, Switzerland), which are manufactured by grinding. Twenty Twisted Files (TFs) and 20 RaCe files #25/.006 taper instruments were allowed to rotate freely in an artificial curved canal at 310 rpm in a static or a dynamic model until fracture occurred. Measurements of the fractured fragments showed that fracture occurred at the point of maximum flexure in the midpoint of the curved segment. The NCF was significantly lower for RaCe instruments compared with TFs. The NCF was also lower for instruments subjected to the static test compared with the dynamic model in both groups. Scanning electron microscopic analysis revealed ductile morphologic characteristics on the fractured surfaces of all instruments and no plastic deformation in their helical shafts. Rotary NiTi endodontic instruments manufactured by twisting present greater resistance to cyclic fatigue compared with instruments manufactured by grinding. The fracture mode observed in all instruments was of the ductile type. Copyright © 2011 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

  4. Instrumental neutron activation analysis of river habitants by the k(0)-standardization method

    International Nuclear Information System (INIS)

    Momoshima, N.; Toyoshima, T.; Matsushita, R.; Fukuda, A.; Hibino, K.

    2005-01-01

    Analysis of metal concentrations in samples use reference materials for determination, which means elements out of the references are not possible to be determined. The instrumental neutron activation analysis (INAA) with k(O)-standardization method makes possible to determine metals without use of reference materials, which is very attractive for environmental sample analysis, River habitants would be available as a bio-indicator from which river water quality or metal contamination level could be evaluated. We analyzed river fishes and river insects by INAA with k(O)-standardization to examine the possibility of these habitants as a bio-indicator of water system. Small fishes, Oryzias latipes and Gambusia affinis were collected at 3 different rivers every month and river insects, families of Heptageniidae, Baetidae, Perlidae, Hydropsychidae, Psephenidae were collected at a fixed point of the river. The dried samples were irradiated at the research reactor, JRR-4 (3.5MW), JAERI for 10 min and 3 h. 17 elements (Na, K, Ca, Sc, Cr, Mn, Fe, Co, Zn, As, Se, Br, Rb, Sr, Ba, Ce and Sm) were determined by the NAA-k(0) method, showing effectiveness of the present method for environmental sample analysis. The metals observed in the fishes were the highest in Ca and the lowest in Sc, ranging from 10 5 mg/kg-dry weigh in Ca to 10 -2 mg/kg-dry weight in Sc. The differences in metal concentrations were examined by statistical analysis with t-test. Ca, Na and Br concentrations differ between species, Oryzias latipes and Gambusia, and Fe, Sc, Co, Zn and Se concentrations differ among rivers. No difference was observed on K, Rb and Sr concentrations.

  5. Injection Methods and Instrumentation for Serial X-ray Free Electron Laser Experiments

    Science.gov (United States)

    James, Daniel

    Scientists have used X-rays to study biological molecules for nearly a century. Now with the X-ray free electron laser (XFEL), new methods have been developed to advance structural biology. These new methods include serial femtosecond crystallography, single particle imaging, solution scattering, and time resolved techniques. The XFEL is characterized by high intensity pulses, which are only about 50 femtoseconds in duration. The intensity allows for scattering from microscopic particles, while the short pulses offer a way to outrun radiation damage. XFELs are powerful enough to obliterate most samples in a single pulse. While this allows for a "diffract and destroy" methodology, it also requires instrumentation that can position microscopic particles into the X-ray beam (which may also be microscopic), continuously renew the sample after each pulse, and maintain sample viability during data collection. Typically these experiments have used liquid microjets to continuously renew sample. The high flow rate associated with liquid microjets requires large amounts of sample, most of which runs to waste between pulses. An injector designed to stream a viscous gel-like material called lipidic cubic phase (LCP) was developed to address this problem. LCP, commonly used as a growth medium for membrane protein crystals, lends itself to low flow rate jetting and so reduces the amount of sample wasted significantly. This work discusses sample delivery and injection for XFEL experiments. It reviews the liquid microjet method extensively, and presents the LCP injector as a novel device for serial crystallography, including detailed protocols for the LCP injector and anti-settler operation.

  6. Clinical, laboratory and instrumental methods of pre-surgical diagnosis of the parathyroid glands cancer

    Directory of Open Access Journals (Sweden)

    Natalia G. Mokrysheva

    2017-12-01

    Full Text Available Backgraund. When defining symptomatic primary hyperparathyroidism (PHPT, differential diagnosis between a benign and malignant neoplasm of parathyroid glands (PG may be challenging. The diagnosis of carcinoma or a benign tumor determines the extent of the surgical intervention and further observation tactics. Aims. The purpose of the study is to determine the clinical and laboratory and instrumental predictors of PG cancer. Materials and methods. A retrospective study included 385 patients with PHPT (273 with adenomas of the PG, 66 with hyperplasia, and 19 patients with cancer of the PG, who had been examined and operated from 2000 to 2014. The primary goal of the study was to define the level of ionized calcium (Ca++, parathyroid hormone (PTH, and the volume of the tumor PG specific for cancer of the PG. The level of parathyroid hormone (PTH was determined by electrochemoluminescent method on the Roche analyzer Cobas 6000; ionized calcium (Ca++ ion-selective method. The size of the PG was determined by the ellipse formula: V(cm3 = (A × B × C × 0.49 by ultrasound investigation using the Valuson E8 device from General Electric. Results. The group of patients with PG carcinoma showed the increased level of Ca++ of more than 1.60 mmol/l (p = 0.004 and increased level of PTH of more than 600 pg/ml (p = 0.03. The size of tumors of more than 6 cm3 is more typical to malignant neoplasm compared to the adenoma of the PG (p = 0.01. Conclusions. The group of patients with PHPT that are at risk of having PG carcinoma include individuals that have a combination of the following indicators: PTH levels of more than 600 pg/ml, an increase in ionized calcium of more than 1.60 mmol/l, the tumor size of more than 6 cm3.

  7. A damage detection method for instrumented civil structures using prerecorded Green’s functions and cross-correlation

    OpenAIRE

    Heckman, Vanessa; Kohler, Monica; Heaton, Thomas

    2011-01-01

    Automated damage detection methods have application to instrumented structures that are susceptible to types of damage that are difficult or costly to detect. The presented method has application to the detection of brittle fracture of welded beam-column connections in steel moment-resisting frames (MRFs), where locations of potential structural damage are known a priori. The method makes use of a prerecorded catalog of Green’s function templates and a cross-correlation method ...

  8. Method for simultaneous analysis of eight analogues of vitamin D using liquid chromatography tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Shah Iltaf

    2012-10-01

    Full Text Available Abstract Background Despite considerable global investigation over several decades, the roles of vitamin D in health and disease development remains convoluted. One recognised issue is the difficulty of accurately measuring the active forms of vitamin D. Advances made include some new methods addressing the potential interference by excluding epimers and isobars. However, there is no evidence that epimers are without function. Therefore, the aim of this study was to develop and validate, for the first time, a new assay to simultaneously measure levels of six forms of vitamin D along with two epimers. The assay was applied to multilevel certified reference material (CRM and 25 pooled human sera samples, obtained from the Vitamin D External Quality Assessment Scheme (DEQAS, to demonstrate its efficiency. Results The assay is capable of simultaneously measuring eight vitamin D analogues over the calibration ranges and LODs (in nmol/L of: 1α25(OH2D2 [0.015-1; 0.01], 1α25(OH2D3 [0.1-100; 0.01], 25OHD3 [0.5-100, 0.025], 3-epi-25OHD3 [0.1-100, 0.05], 25OHD2 [0.5-100, 0.025], 3-epi-25OHD2 [0.1-100, 0.05], vitamin D3 [0.5-100, 0.05] and vitamin D2 [0.5-100, 0.05], using stanozolol-d3 as internal standard. Certified reference material and external quality control samples (DEQAS were analysed to meet the standards outlined by National Institute of Standards and Technology (NIST. Validation steps included recovery and both precision and accuracy under inter- and intra-day variation limit of detection, and analysis of each analyte over a linear range. All validation parameters were in line with acceptable Food and Drug Administration (FDA guidelines. All eight analogues were quantified with the 25OHD levels being commensurate with DEQAS data. Conclusions This report details the application of a new LC-MS/MS based assay for the efficient analysis of eight analogues of vitamin D over a range of samples, which is a significant advance over the existing

  9. Scope of harmonisation of pharmacopoeial liquid chromatography (LC) methods for diazepam and its related substances

    International Nuclear Information System (INIS)

    Shar, G.Q.; Jatoi, W.B.

    2015-01-01

    Drug analysis is an imperative activity to check the quality of a drug compound. Pharmacopoeial monographs provide important information about the quality of a drug substance. The expected quality of a medicine during period of use is also explained in such monographs. Analytical tools such as spectroscopic and chromatographic methods have been developed for such investigations. We have analysed the purity of a well known anxiolytic drug; diazepam, by using liquid chromatographic (LC) technique. It was noticed that with Zorbax Eclipse XDB - C8 (4.6 x 150 mm, 5 mu m) column and recommended mobile phase comprising acetonitrile - methanol -potassium dihydrogen phosphate (22+34+44 v/v), the desired results obtained were not according the chromatograms provided by European Pharmacopeia (EP), but by using another column (ACE- 5 - C8) (4.6 x 150 mm, 5 ?m), an extra peak of diazepam degradant was obtained, which showed that by using appropriate mobile phase containing CH3CN- CH/sub 3/OH- KH/sub 2/PO/sub 4/ (20+32+48 v/v), the better results can be achieved. The mean retention time for diazepam analysis was 2.9 minutes. (author)

  10. A simple, rapid and validated high-performance liquid chromatography method suitable for clinical measurements of human mercaptalbumin and non-mercaptalbumin.

    Science.gov (United States)

    Yasukawa, Keiko; Shimosawa, Tatsuo; Okubo, Shigeo; Yatomi, Yutaka

    2018-01-01

    Background Human mercaptalbumin and human non-mercaptalbumin have been reported as markers for various pathological conditions, such as kidney and liver diseases. These markers play important roles in redox regulations throughout the body. Despite the recognition of these markers in various pathophysiologic conditions, the measurements of human mercaptalbumin and non-mercaptalbumin have not been popular because of the technical complexity and long measurement time of conventional methods. Methods Based on previous reports, we explored the optimal analytical conditions for a high-performance liquid chromatography method using an anion-exchange column packed with a hydrophilic polyvinyl alcohol gel. The method was then validated using performance tests as well as measurements of various patients' serum samples. Results We successfully established a reliable high-performance liquid chromatography method with an analytical time of only 12 min per test. The repeatability (within-day variability) and reproducibility (day-to-day variability) were 0.30% and 0.27% (CV), respectively. A very good correlation was obtained with the results of the conventional method. Conclusions A practical method for the clinical measurement of human mercaptalbumin and non-mercaptalbumin was established. This high-performance liquid chromatography method is expected to be a powerful tool enabling the expansion of clinical usefulness and ensuring the elucidation of the roles of albumin in redox reactions throughout the human body.

  11. An analytical method for cyclosporine using liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Kanduru, Srividya V; Somayaji, Vishwa; Lavasanifar, Afsaneh; Brocks, Dion R

    2010-02-01

    A liquid chromatographic mass spectrometric (LC-MS) assay has been developed for cyclosporine A (CyA) in rat plasma using amiodarone as internal standard (IS). Rat plasma (100 microL) containing drug and IS were extracted using liquid-liquid extraction with 4 mL of 95:5 ether:methanol. After evaporation of the organic layer the residue was reconstituted with 500 microL of water. Then the aqueous layer was transferred to LC-MS sample vials. A 10 microL volume was injected. The analysis was performed on a C(8) column 3.5 microm (2.1 x 50 mm) heated to 60 degrees C with a mobile phase consisting of acetonitrile:methanol:0.2% NH(4)OH (60:20:20) at an isocratic flow-rate of 0.2 mL/min. The ions used for quantitation of CyA and IS were m/z 1202.8 and 645.9, with retention times of 3.35 and 4.72 min, respectively. Linear relationships (r(2) > 0.99) were achieved between plasma or blood concentration and peak height ratios (drug:IS) over the concentration range 50-5000 ng/mL. The CV% and mean error were <19%. Based on validation data, the lower limit of quantification for the assay was 50 ng/mL. The reported assay method displayed high measures of linearity, sensitivity, reliability and precision, allowing its applicability in pharmacokinetic studies in rat. (c) 2009 John Wiley & Sons, Ltd.

  12. Assessing learning outcomes in middle-division classical mechanics: The Colorado Classical Mechanics and Math Methods Instrument

    Science.gov (United States)

    Caballero, Marcos D.; Doughty, Leanne; Turnbull, Anna M.; Pepper, Rachel E.; Pollock, Steven J.

    2017-06-01

    Reliable and validated assessments of introductory physics have been instrumental in driving curricular and pedagogical reforms that lead to improved student learning. As part of an effort to systematically improve our sophomore-level classical mechanics and math methods course (CM 1) at CU Boulder, we have developed a tool to assess student learning of CM 1 concepts in the upper division. The Colorado Classical Mechanics and Math Methods Instrument (CCMI) builds on faculty consensus learning goals and systematic observations of student difficulties. The result is a 9-question open-ended post test that probes student learning in the first half of a two-semester classical mechanics and math methods sequence. In this paper, we describe the design and development of this instrument, its validation, and measurements made in classes at CU Boulder and elsewhere.

  13. Assessing learning outcomes in middle-division classical mechanics: The Colorado Classical Mechanics and Math Methods Instrument

    Directory of Open Access Journals (Sweden)

    Marcos D. Caballero

    2017-04-01

    Full Text Available Reliable and validated assessments of introductory physics have been instrumental in driving curricular and pedagogical reforms that lead to improved student learning. As part of an effort to systematically improve our sophomore-level classical mechanics and math methods course (CM 1 at CU Boulder, we have developed a tool to assess student learning of CM 1 concepts in the upper division. The Colorado Classical Mechanics and Math Methods Instrument (CCMI builds on faculty consensus learning goals and systematic observations of student difficulties. The result is a 9-question open-ended post test that probes student learning in the first half of a two-semester classical mechanics and math methods sequence. In this paper, we describe the design and development of this instrument, its validation, and measurements made in classes at CU Boulder and elsewhere.

  14. Trace elements determination in silicon and ferrosilicon reference materials by instrumental neutron activation analysis method

    International Nuclear Information System (INIS)

    Moreira, Edson Goncalves; Vasconcellos, Marina Beatriz Agostini; Saiki, Mitiko; Iamashita, Celia Omine

    2002-01-01

    The use of certified reference materials, CRM, is of uppermost importance in the rastreability realization of the measurement process. At times, CRM use is restricted by the non existence of a suitable CRM with similarity to the sample in respect to matrix composition or with element levels in different orders of magnitude. IPT Chemical Division launched a project to prepare a metallic silicon CRM, due to the requirements of the industries in this field. To characterize this new CRM, IPEN Nuclear Reactor Center is able to perform instrumental neutron activation analysis, INAA, a very suitable method for silicon matrix samples because they produce basically the short lived radionuclide 3 1 Si under thermal neutrons flux, which after radioactive decay, does not interfere in the determination of other elements. In this paper, it is presented the determination of As, Br, Co, Cr, K, Eu, Fe, La, Mn, Na Nb, Sb, Sm, Sc, Th, Tb, U, V, W and Yb in silicon CRM NBS SRM 57; ferrosilicon CRM IPT 56; IPT 70; NBS SRM 58a; NBS SRM 59a and silicon RM under preparation IPT 132. From the results, the accuracy and the precision of the process were assessed. (author)

  15. Waste minimization methods for treating analytical instrumentation effluents at the source

    International Nuclear Information System (INIS)

    Ritter, J.A.; Barnhart, C.

    1995-01-01

    The primary goal of this project was to reduce the amount of hazardous waste being generated by the Savannah River Siste Defense Waste Processing Technology-analytical Laboratory (DWPT-AL). A detailed characterization study was performed on 12 of the liquid effluent streams generated within the DWPT-AL. Two of the streams were not hazardous, and are now being collected separately from the 10 hazardous streams. A secondary goal of the project was to develop in-line methods using primarily adsorption/ion exchange columns to treat liquid effluent as it emerges from the analytical instrument as a slow, dripping flow. Samples from the 10 hazardous streams were treated by adsorption in an experimental apparatus that resembled an in-line or at source column apparatus. The layered adsorbent bed contained activated carbon and ion exchange resin. The column technique did not work on the first three samples of the spectroscopy waste stream, but worked well on the next three samples which were treated in a different column. It was determined that an unusual form of mercury was present in the first three samples. Similarly, two samples of a combined waste stream were rendered nonhazardous, but the last two samples contained acetylnitrile that prevented analysis. The characteristics of these streams changed from the initial characterization study; therefore, continual, in-deptch stream characterization is the key to making this project successful

  16. The alignment of the LHC low beta triplets. Review of instrumentation and methods

    International Nuclear Information System (INIS)

    Coosemans, W.; Mainaud Durand, H.; Marin, A.; Quesnel, J-P.

    2003-01-01

    Alignment tolerances for the LHC insertions are particularly stringent regarding the low beta quadrupoles, which induce strict positioning tolerances, in a severe environment (high radiation fluxes and magnetic fields): positioning of one inner triplet with respect to the other (left/right side): ±0.5 mm (3σ), stability of the positioning of one quadrupole inside its triplet: a few microns. We propose to continuously monitor the relative position of the quadrupoles of one inner triplet with respect to a reference frame materialized by a wire and a water surface, and to use common references to link a triplet on one side to the triplet on the other side of the experiment. When the offset between real and reference position becomes too great, the quadrupole will be moved using remote motorized jacks. Instrumentation (HLS, WPS, radial measuring system, etc.) and methods will be detailed as well as the first results obtained on a cryo-magnet prototype named TAP used as test facility. The TAP is equipped with HLS linked by two types of hydraulic networks (two pipes with air and water separated, one pipe half filled), WPS and one inclinometer. It is installed on three polyurethane motorized jacks in order to study and compare servo positioning using the different sensors. (author)

  17. Instant thin layer chromatography (ITLC) - the most true and convenient method for the determination of radiochemical purity of Tc-99m Labeled radiopharmaceuticals

    International Nuclear Information System (INIS)

    Anwar-Ul-Azim, M.; Ansari, M.I.H.

    2007-01-01

    Full text: Determination of radiochemical purity usually involves paper chromatography method or some column chromatography such as ion exchange or gel filtration technique. In this study, a modified chromatography method with thin-layer support called instant thin Layer chromatography (ITLC) was used for the measurement of radiochemical purity. The aim of the study was to present instant thin layer chromatography-Silica-Gel (ITLC-SG) technique as a fairly rapid , convenient and inexpensive system for the screening of radiochemical impurities of 99mTc-labeled radiopharmaceuticals resulting from physical , chemical and/or radiation decomposition. Materials and Methods: The experiment was carried out at the Institute of Nuclear Medicine and Ultrasound, Dhaka for a period of 10 months from August '05 to May '06. Radiochemical purity of seven types of 99mTc-labeled radiopharmaceuticals, namely 99mTc-DTPA,99mTc- MI I, 99m Tc - HDP, 99m Tc - DMSA, 99m Tc - Tetofosmin, 99mTc-Fyton and 99mTc-ECD were measured by the use of two solvent dual-instant thin layer chromatography systems. Commercially available instant thin layer chromatography plate ( 20cm x20cm) impregnated with silica gel (ITLC-SG: Merck, Germany) was used as a stationary phase for the measurement of radiochemical impurities.Acetone, Ethyl methyl ketone, chloroform and methanol were used to measure the amount of free pertechnetate in the labelled radiopharmaceuticals and 0.9% saline was used in all cases as solvent (Mobile phase) to measure the amount of the hydrolyzed-reduced technetium colloid. Results: The results showed that the measured radiochemical purity of 99mTc-DTPA, 99mTc-MIBI, 99mTc-HDP, 99mTc-DMSA, 99mTc-Tetofosmin, 99mTc-Fyton and 99mTc-ECD were acceptable for all the studied samples except two samples of 99mTc-MIBI, one sample of 99mTc-Fyton and two samples of 99mTc-ECD, where the measured radiochemical purity were not within the acceptable RCP limits of commonly used radiopharmaceuticals (RCP

  18. A simple and selective liquid chromatography- tandem mass spectrometry method for determination of ε-aminocaproic acid in human plasma

    Directory of Open Access Journals (Sweden)

    Ganesh S. Moorthy

    2015-07-01

    Full Text Available Understanding the clinical pharmacology of the antifibrinolytic drug epsilon-aminocaproic acid (EACA is critical for rational drug administration in children. The aim of this study is to develop a reliable assay for the determination of EACA in human plasma. We describe a high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS assay for EACA in human plasma. Sample preparation involved plasma dilution (1:2040, followed by reversed-phase chromatographic separation and selective detection using tandem mass spectrometry. EACA had a linear range of 1 - 250 μg/mL. The intraday precision based on the standard deviation of replicates of quality control samples ranged from 4.7 to 10.4% and the accuracy ranged from 92-106%. The interday precision ranged from 4.6 to 9.8% and the accuracy ranged from 95-103%. Stability studies showed that EACA was stable during the conditions for sample preparation and storage. The described method is robust and successfully employed for clinical studies of EACA in children

  19. A rapid liquid chromatography tandem mass spectrometry-based method for measuring propranolol on dried blood spots.

    Science.gov (United States)

    Della Bona, Maria Luisa; Malvagia, Sabrina; Villanelli, Fabio; Giocaliere, Elisa; Ombrone, Daniela; Funghini, Silvia; Filippi, Luca; Cavallaro, Giacomo; Bagnoli, Paola; Guerrini, Renzo; la Marca, Giancarlo

    2013-05-05

    Propranolol, a non-selective beta blocker drug, is used in young infants and newborns for treating several heart diseases; its pharmacokinetics has been extensively evaluated in adult patients using extrapolation to treat pediatric population. The purpose of the present study was to develop and validate a method to measure propranolol levels in dried blood spots. The analysis was performed by using liquid chromatography/tandem mass spectrometry operating in multiple reaction monitoring mode. The calibration curve in matrix was linear in the concentration range of 2.5-200 μg/L with correlation coefficient r=0.9996. Intra-day and inter-day precisions and biases were less than 8.0% (n=10) and 11.5% (n=10) respectively. The recoveries ranged from 94 to 100% and the matrix effect did not result in a severe signal suppression. Propranolol on dried blood spot showed a good stability at three different temperatures for one month. This paper describes a micromethod for measuring propranolol levels on dried blood spot, which determines a great advantage in neonates or young infants during pharmacokinetic studies because of less invasive sampling and small blood volume required. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Simultaneous determination of some ultraviolet-absorbing chemicals in sunscreen cosmetics using a high-performance liquid chromatography method.

    Science.gov (United States)

    Liu, T; Wu, D

    2011-10-01

    A method of gradient elution high-performance liquid chromatography (HPLC) for simultaneous determination of 11 different ultraviolet-absorbing chemicals of phenylbenzlmldazole sulphonic acid, 4-aminobenzoic acid, benzophenone-4, benzophenone-3, isoamyl p-methoxycinnamate, 4-methylbenzylidene camphor, octocrylene, ethylhexyl methoxycinnamate, homosalate, ethylhexyl salicylate, methylene bis-benzotriazolyl tetramethylbutyl phenol was developed for the application to sunscreen cosmetic products. In this study, an Agilent SB-C18 analytical column (250 × 4.6 mm, 5 μm) was utilized and methanol, tetrahydrofuran and perchloric acid aqueous solution (0.2 mL HClO(4) + 300 mL H(2)O) were used for gradient elution at a total flow rate of 1.0 mL min(-1). The optimum conditions for 11 different ultraviolet-absorbing chemicals analyses were investigated. All calibration curves showed good linear regression with UV detection (311 nm) within test ranges. The correlation coefficients were better than 0.999 in all cases. The assay was simple, selective, convenient and reproducible and is suitable for the determination of ultraviolet-absorbing chemicals in commercial sunscreen cosmetic products. The use frequency of 11 different ultraviolet absorbents in 100 sunscreen cosmetics was investigated and statistically analysed. The ultraviolet absorbent of maximum use frequency was ethylhexyl methoxycinnamate. © 2011 The Authors. ICS © 2011 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

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

    Science.gov (United States)

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

    2016-09-06

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

  2. Liquid chromatography/tandem mass spectrometry method for quantitative estimation of solutol HS15 and its applications

    Directory of Open Access Journals (Sweden)

    V. Vijaya Bhaskar

    2015-04-01

    Full Text Available A rapid, sensitive and selective pseudoMRM (pMRM-based method for the determination of solutol HS15 (SHS15 in rat plasma was developed using liquid chromatography/tandem mass spectrometry (LC–MS/MS. The most abundant ions corresponding to SHS15 free polyethyleneglycol (PEG oligomers at m/z 481, 525, 569, 613, 657, 701, 745, 789, 833, 877, 921 and 965 were selected for pMRM in electrospray mode of ionization. Purity of the lipophilic and hydrophilic components of SHS15 was estimated using evaporative light scattering detector (ELSD. Plasma concentrations of SHS15 were measured after oral administration at 2.50 g/kg dose and intravenous administration at 1.00 g/kg dose in male Sprague Dawley rats. SHS15 has poor oral bioavailability of 13.74% in rats. Differences in pharmacokinetics of oligomers were studied. A novel proposal was conveyed to the scientific community, where formulation excipient could be analyzed as a qualifier in the analysis of new chemical entities (NCEs to address the spiky plasma concentration profiles. Keywords: SHS15, LC–MS/MS, Spiky profiles, Validation

  3. Liquid chromatography/tandem mass spectrometry method for quantitative estimation of solutol HS15 and its applications.

    Science.gov (United States)

    Bhaskar, V Vijaya; Middha, Anil; Srivastava, Pratima; Rajagopal, Sriram

    2015-04-01

    A rapid, sensitive and selective pseudoMRM (pMRM)-based method for the determination of solutol HS15 (SHS15) in rat plasma was developed using liquid chromatography/tandem mass spectrometry (LC-MS/MS). The most abundant ions corresponding to SHS15 free polyethyleneglycol (PEG) oligomers at m / z 481, 525, 569, 613, 657, 701, 745, 789, 833, 877, 921 and 965 were selected for pMRM in electrospray mode of ionization. Purity of the lipophilic and hydrophilic components of SHS15 was estimated using evaporative light scattering detector (ELSD). Plasma concentrations of SHS15 were measured after oral administration at 2.50 g/kg dose and intravenous administration at 1.00 g/kg dose in male Sprague Dawley rats. SHS15 has poor oral bioavailability of 13.74% in rats. Differences in pharmacokinetics of oligomers were studied. A novel proposal was conveyed to the scientific community, where formulation excipient could be analyzed as a qualifier in the analysis of new chemical entities (NCEs) to address the spiky plasma concentration profiles.

  4. Validation of a Multiresidue Analysis Method for 379 Pesticides in Human Serum Using Liquid Chromatography-Tandem Mass Spectrometry.

    Science.gov (United States)

    Shin, Yongho; Lee, Jonghwa; Lee, Jiho; Lee, Junghak; Kim, Eunhye; Liu, Kwang-Hyeon; Lee, Hye Suk; Kim, Jeong-Han

    2018-04-04

    A screening method for simultaneous analysis of 379 pesticides in human serum was developed using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Electrospray ionization with positive/negative switching mode of LC-MS/MS was adopted, and scheduled multiple reaction monitoring for each target compound was established. The limit of quantitation was 10 ng/mL for 94.5% of the total pesticides, and the correlation coefficients of calibration were ≥0.990 for 93.9% of the pesticides. For the sample preparation, scaled-down QuEChERS were used. Serum (100 μL) was extracted with acetonitrile (400 μL), partitioned with magnesium sulfate (40 mg) and sodium chloride (10 mg), and the upper layer was used for analysis without further cleanup steps. For the accuracy and precision tests, most of the pesticides showed excellent results in intra- and interday conditions. In the recovery tests at 10, 50, and 250 ng/mL, 85.8-91.8% of all target compounds satisfied the recovery range of 70-120% (relative standard deviation ≤20%).

  5. The separation of [32P]inositol phosphates by ion-pair chromatography: Optimization of the method and biological applications

    International Nuclear Information System (INIS)

    Sulpice, J.C.; Gascard, P.; Journet, E.; Rendu, F.; Renard, D.; Poggioli, J.; Giraud, F.

    1989-01-01

    We have developed an ion-pair reverse-phase HPLC method to measure inositol phosphates in 32 P-labeled cells. The different chromatographic parameters were analyzed to optimize the resolution of the 32 P-labeled metabolites. Analysis of inositol phosphates in biological samples was improved by a single charcoal pretreatment which eliminated interfering nucleotides without removing inositol phosphates. The kinetics of production of inositol phosphates in calcium-activated erythrocytes, vasopressin-stimulated hepatocytes, and thrombin-activated platelets were analyzed. Original data on the activation of phosphoinositide phospholipase C were obtained in intact erythrocytes by direct measurement of inositol (1,4,5)P3. Data from agonist-stimulated hepatocytes and platelets were consistent with those from previous studies. In conclusion, this technique offers many advantages over the methodologies currently employed involving anion-exchange chromatography and [ 3 H]inositol labeling: (i) 32 P labeling is less expensive and more efficient than 3 H labeling and can be used with all types of cells without permeabilization treatments and (ii) ion-pair HPLC gives good resolution of inositol phosphates from nucleotides with shorter retention times, and long reequilibration periods are not required

  6. Re-evaluation of thin layer chromatography as an alternative method for the quantification of prostaglandins from rat Kupffer cells.

    Science.gov (United States)

    Pestel, Sabine; Jungermann, Kurt; Schieferdecker, Henrike L

    2005-01-01

    In contrast to conventionally used immunoassays, thin layer chromatography (TLC)--by prelabeling of cells with radioactive arachidonic acid (AA)--allows to differentiate between cellularly built and added prostanoids and thus to investigate feedback effects of prostanoids on their own release. PGD2, TXB2 and PGE2 released from zymosan-stimulated Kupffer cells were separated with distinct RF-values, corresponding to those of the pure substances. Quantification of PGD2 and PGE2 gave comparable results with TLC and immunoassays, but measurement in the presence of added prostanoids was only possible with TLC. Moreover TLC was superior to immunoassays in having a longer linear range while being comparably sensitive. Cellularly built TXB2 in its radioactively labeled form was not detectable by TLC. Inhibition of TXB2 release by externally added AA or technical artifacts were excluded, suggesting that the cellular AA-pools used for prostaglandin and thromboxane synthesis differ in their accessibility for added AA. Thus, TLC is a simple, sensitive and precise method for the quantification of cellularly built prostaglandins but not of thromboxane even in the presence of added prostanoids.

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

    Science.gov (United States)

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

    2017-07-01

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

  8. Rapid methods to determine procyanidins, anthocyanins, theobromine and caffeine in rat tissues by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Serra, Aida; Macià, Alba; Romero, Maria-Paz; Piñol, Carme; Motilva, Maria-José

    2011-06-01

    Rapid, selective and sensitive methods were developed and validated to determine procyanidins, anthocyanins and alkaloids in different biological tissues, such as liver, brain, the aorta vein and adipose tissue. For this purpose, standards of procyanidins (catechin, epicatechin, and dimer B(2)), anthocyanins (cyanidin-3-glucoside and malvidin-3-glucoside) and alkaloids (theobromine, caffeine and theophylline) were used. The methods included the extraction of homogenized tissues by off-line liquid-solid extraction, and then solid-phase extraction to analyze alkaloids, or microelution solid-phase extraction plate for the analysis of procyanidins and anthocyanins. The eluted extracts were then analyzed by ultra-performance liquid chromatography-electrospray ionization-tandem mass spectrometry, using a triple quadrupole as the analyzer. The optimum extraction solution was water/methanol/phosphoric acid 4% (94/4.5/1.5, v/v/v). The extraction recoveries were higher than 81% for all the studied compounds in all the tissues, except the anthocyanins, which were between 50 and 65% in the liver and brain. In order to show the applicability of the developed methods, different rat tissues were analyzed to determine the procyanidins, anthocyanins and alkaloids and their generated metabolites. The rats had previously consumed 1g of a grape pomace extract (to analyze procyanidins and anthocyanins) or a cocoa extract (to analyze alkaloids) per kilogram of body weight. Different tissues were extracted 4h after administration of the respective extracts. The analysis of the metabolites revealed a hepatic metabolism of procyanidins. The liver was the tissue which produced a greater accumulation of these metabolites. Copyright © 2011 Elsevier B.V. All rights reserved.

  9. Quantitative determination of hederagenin in rat plasma and cerebrospinal fluid by ultra fast liquid chromatography-tandem mass spectrometry method.

    Science.gov (United States)

    Yang, Xuemei; Li, Guoliang; Chen, Lingyun; Zhang, Cong; Wan, Xinxiang; Xu, Jiangping

    2011-07-01

    A rapid, sensitive and selective method was developed for the quantitative determination of hederagenin in rat plasma and cerebrospinal fluid (CSF) by ultra fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS). It has been successfully applied in a pharmacokinetic study of hederagenin in the central nervous system (CNS). Sample pretreatment involved a simple protein precipitation with methanol and a one-step extraction with ethyl acetate. Separation was carried out in a Shim-pack XR-ODS II (75 mm × 2.0 mm, i.d., 2.1 μm) column with gradient elution at a flow rate of 0.35 mL/min. The mobile phase was 5mM ammonium acetate and acetonitrile. Detection was performed in a triple-quadruple tandem mass spectrometer by multiple-reaction-monitoring mode via electrospray ionization. A linear calibration curve for hederagenin was obtained over a concentration range of 0.406 (lower limit of quantification, LLOQ) to 203 ng/mL (r² > 0.99) for both plasma and CSF. The intra-day and inter-day precision (relative standard deviation, RSD) values were less than 15%. At all quality control (QC) levels, the accuracy (relative error, RE) was within -9.0% and 11.1% for plasma and CSF, respectively. The pharmacokinetics results indicated that hederagenin could pass through the blood-brain barrier. This UFLC-MS/MS method demonstrates higher sensitivity and sample throughput than previous methods. It was also successfully applied to the pharmacokinetic study of hederagenin following oral administration of Fructus akebiae extract in rats. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Development of a method based on on-line reversed phase liquid chromatography and gas chromatography coupled by means of an adsorption-desorption interface for the analysis of selected chiral volatile compounds in methyl jasmonate treated strawberries.

    Science.gov (United States)

    de la Peña Moreno, Fernando; Blanch, Gracia Patricia; Flores, Gema; Ruiz Del Castillo, Maria Luisa

    2010-02-12

    A method based on the use of the through oven transfer adsorption-desorption (TOTAD) interface in on-line coupling between reversed phase liquid chromatography and gas chromatography (RPLC-GC) for the determination of chiral volatile compounds was developed. In particular, the method was applied to the study of the influence of methyl jasmonate (MJ) treatment on the production and enantiomeric composition of selected aroma compounds in strawberry. The compounds studied were ethyl 2-methylbutanoate, linalool and 4-hydroxy-2,5-dimethyl-3(2H)-furanone (i.e. furaneol), which were examined on days 3, 6 and 9 after treatment. The method developed resulted in relative standard deviations (RSDs) of 21.6%, 8.1% and 9.8% and limits of detection (LD) of 0.04, 0.07 and 0.02mg/l for ethyl 2-methylbutanoate, linalool and furaneol, respectively. The application of the RPLC-TOTAD-GC method allowed higher levels of ethyl 2-methylbutanoate, linalool and furaneol to be detected, particularly after 9 days of treatment. Besides, MJ demonstrated to affect the enantiomeric distribution of ethyl 2-methylbutanoate. On the contrary, the enantiomeric composition of linalool and furaneol kept constant in both control and MJ-treated strawberries throughout the study. These results are discussed. Copyright 2009 Elsevier B.V. All rights reserved.

  11. Study of extraction chromatography methods of separation of neptunium and its radiometric determination

    International Nuclear Information System (INIS)

    Reich, M.

    2009-04-01

    elution solutions for securing the highest recovery of 239 Np were tested. Isolated 239 Np is suitable as a tracer for the determination of recovery of 237 Np after separation from environmental samples. This method is suitable for preparation of 239 Np generator because the radioactive equilibrium of mother radionuclide/daughter radionuclide occurs after relatively short period of time (33.6 d.). 5. The separation procedure was optimized in order to particular steps followed without useless steps like for example evaporation of solvent solution and subsequent change of chemical composition of system. 6. The scheme was optimised for reaching the highest recovery of separation 237 Np from matrix of model solution of known composition. The matrix of soils is complicated and recovery of 237 Np in separation process lower, but in measured alpha spectrum peaks coming from interfering radionuclides were not observed. The mass of soil sample for analyses influence the salinity of solution which caused decreasing the yield of 237 Np due to competing effect in separation process. 7 .The optimal composition of elution solution used in separation procedure was 0.5 mol.dm -3 HCI - 0.02 mol · dm -3 HF. This solution is compatible with solution suitable for preparation of sample for measuring of alpha activity by alpha spectrometry. It was not necessary to change solution for alpha sample preparation. 8. Dependencies of recoveries of neptunium separation from mass of soil sample and mass of present iron in model solution were observed. Increasing mass of soil sample and mass of iron in the model solution causes decreasing of the recoveries of neptunium. (author)

  12. Validation of a high performance liquid chromatography method for quantitation of L-proline in 20 % tincture from Murraya paniculata L. Jack

    International Nuclear Information System (INIS)

    Varona Torres, Noel; Gutierrez Gaiten, Yamilet Irene; Casado Martin, Celia Magaly

    2014-01-01

    The search for analytical methods that may monitor the quality of drugs is an issue of great interest in the pharmaceutical field, even more if they are directed to studying chemical markers of medicinal plants, their extracts and phytomedicines. To validate a high-resolution liquid chromatography (HPLC) method for the quantitative determination of the L-proline amino acid as a marker substance in Murraya paniculata L. Jack tincture

  13. Use of the mathematical modelling method for the investigation of dynamic characteristics of acoustical measuring instruments

    Science.gov (United States)

    Vasilyev, Y. M.; Lagunov, L. F.

    1973-01-01

    The schematic diagram of a noise measuring device is presented that uses pulse expansion modeling according to the peak or any other measured values, to obtain instrument readings at a very low noise error.

  14. Aroma composition of red wines by different extraction methods and Gas Chromatography-SIM/MASS spectrometry analysis.

    Science.gov (United States)

    Genovese, Alessandro; Dimaggio, Rosa; Lisanti, Maria Tiziana; Piombino, Paola; Moio, Luigi

    2005-06-01

    One hundred and one volatile compounds, reported in literature as powerful odorants of wine, were quantified by Gas Chromatography-Selective Ion Monitoring/Mass Spectrometry (GC-SIM/MS) in Primitivo, Aglianico, Merlot and Cabernet Sauvignon red wines. Wine samples were extracted by 3 different extraction methods: 1) separation of the alcoholic fraction from the aqueous phase by salting-out and subsequent extraction by liquid-liquid micro-extraction with 1,1,2-trichlorotrifluoroethane (Freon 113); 2) extraction by liquid-liquid micro-extraction with dichloromethane; 3) solid phase extraction (SPE cartridge: 800 mg of LiChrolut EN resin) with pentane-dichloromethane (20:1) and dichloromethane. The selection of the ion fragments used for quantification was directly performed on a red wine sample. For each compound the area of the corresponding peak was normalized respect to the peak of the internal standard and then interpolated in a calibration curve obtained analysing a model wine solution (water, ethanol, tartaric acid and known amounts of analytes and of internal standard). The methods showed a good linearity: r2>0.990, except for farnesol (isomer a and c), octanal, decanal, furaneol and phenylacetic acid with 0.966 furaneol and sotolon. The Aglianico wines were characterised by the major fermentation compounds (esters, fatty acids and 2-phenylethanol), beta-damascenone, beta-ionone and linalool. The Primitivo wines were characterized by furaneol, methoxypyrazine, gamma-nonalactone and acetaldehyde, while Cabernet Sauvignon and Merlot wines principally by cask derivates (vanillin, (Z) 3-methyl-gamma-octalactone [(Z) wiskylactone], maltol and eugenol), some aldehydes and 3-isopropyl-2-methoxypyrazine.

  15. First liquid chromatography method for the simultaneous determination of levofloxacin, pazufloxacin, gatifloxacin, moxifloxacin and trovafloxacin in human plasma.

    Science.gov (United States)

    Sousa, Joana; Alves, Gilberto; Campos, Gonçalo; Fortuna, Ana; Falcão, Amílcar

    2013-07-01

    For the first time a simple, selective and sensitive liquid chromatography method was developed and validated for the simultaneous determination of levofloxacin (LEV), pazufloxacin (PAZ), gatifloxacin (GAT), moxifloxacin (MOX) and trovafloxacin (TRO) in human plasma. Samples were pre-treated with acetonitrile for precipitation of plasma proteins followed by evaporation and reconstitution steps. Chromatographic separation of the analytes and norfloxacin, used as internal standard (IS), was performed under gradient elution on a LiChroCART(®) Purospher Star C18 column (55mm×4mm, 3μm). The mobile phase comprised a mixture of 0.1% aqueous formic acid adjusted to pH 3.0 with triethylamine, acetonitrile and methanol pumped at a flow rate of 1.0mL/min. The detector was set at excitation/emission wavelengths of 260/455nm. Calibration curves were linear (r(2)≥0.9923) in the ranges of 0.005-5μg/mL for GAT, 0.02-5μg/mL for LEV, PAZ and MOX and 0.04-5μg/mL for TRO. The intra and interday precision did not exceed 7.32% and the intra and interday accuracy ranged from -11.73 to 8.92%. The limits of quantification were established at 0.005μg/mL for GAT, 0.02μg/mL for LEV, PAZ and MOX and 0.04μg/mL for TRO. No endogenous or tested exogenous compounds were found to interfere at the retention times of the analytes and IS. Since the proposed method proved to be reliable for the quantitative determination of LEV, PAZ, GAT, MOX and TRO it may be a useful tool for routine analysis and to support clinical pharmacokinetic and toxicological studies involving these antibiotics. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. A comprehensive review of sensors and instrumentation methods in devices for musical expression.

    Science.gov (United States)

    Medeiros, Carolina Brum; Wanderley, Marcelo M

    2014-07-25

    Digital Musical Instruments (DMIs) are musical instruments typically composed of a control surface where user interaction is measured by sensors whose values are mapped to sound synthesis algorithms. These instruments have gained interest among skilled musicians and performers in the last decades leading to artistic practices including musical performance, interactive installations and dance. The creation of DMIs typically involves several areas, among them: arts, design and engineering. The balance between these areas is an essential task in DMI design so that the resulting instruments are aesthetically appealing, robust, and allow responsive, accurate and repeatable sensing. In this paper, we review the use of sensors in the DMI community as manifested in the proceedings of the International Conference on New Interfaces for Musical Expression (NIME 2009-2013). Focusing on the sensor technologies and signal conditioning techniques used by the NIME community. Although it has been claimed that specifications for artistic tools are harder than those for military applications, this study raises a paradox showing that in most of the cases, DMIs are based on a few basic sensors types and unsophisticated engineering solutions, not taking advantage of more advanced sensing, instrumentation and signal processing techniques that could dramatically improve their response. We aim to raise awareness of limitations of any engineering solution and to assert the benefits of advanced electronics instrumentation design in DMIs. For this, we propose the use of specialized sensors such as strain gages, advanced conditioning circuits and signal processing tools such as sensor fusion. We believe that careful electronic instrumentation design may lead to more responsive instruments.

  17. A Comprehensive Review of Sensors and Instrumentation Methods in Devices for Musical Expression

    Directory of Open Access Journals (Sweden)

    Carolina Brum Medeiros

    2014-07-01

    Full Text Available Digital Musical Instruments (DMIs are musical instruments typically composed of a control surface where user interaction is measured by sensors whose values are mapped to sound synthesis algorithms. These instruments have gained interest among skilled musicians and performers in the last decades leading to artistic practices including musical performance, interactive installations and dance. The creation of DMIs typically involves several areas, among them: arts, design and engineering. The balance between these areas is an essential task in DMI design so that the resulting instruments are aesthetically appealing, robust, and allow responsive, accurate and repeatable sensing. In this paper, we review the use of sensors in the DMI community as manifested in the proceedings of the International Conference on New Interfaces for Musical Expression (NIME 2009–2013. Focusing on the sensor technologies and signal conditioning techniques used by the NIME community. Although it has been claimed that specifications for artistic tools are harder than those for military applications, this study raises a paradox showing that in most of the cases, DMIs are based on a few basic sensors types and unsophisticated engineering solutions, not taking advantage of more advanced sensing, instrumentation and signal processing techniques that could dramatically improve their response. We aim to raise awareness of limitations of any engineering solution and to assert the benefits of advanced electronics instrumentation design in DMIs. For this, we propose the use of specialized sensors such as strain gages, advanced conditioning circuits and signal processing tools such as sensor fusion. We believe that careful electronic instrumentation design may lead to more responsive instruments.

  18. Development of an analytical method coupling cell membrane chromatography with gas chromatography-mass spectrometry via microextraction by packed sorbent and its application in the screening of volatile active compounds in natural products.

    Science.gov (United States)

    Li, Miao; Wang, Sicen; He, Langchong

    2015-01-01

    Natural products (NPs) are important sources of lead compounds in modern drug discovery. To facilitate the screening of volatile active compounds in NPs, we have developed a new biochromatography method that uses rat vascular smooth muscle cells (VSMC), which are rich in L-type calcium channels (LCC), to prepare the stationary phase. This integrated method, which couples cell membrane chromatography (CMC) with gas chromatography-mass spectrometry (GC-MS) via microextraction by packed sorbent (MEPS) technology, has been termed VSMC/CMC-MEPS-GC-MS. Methodological validation confirmed its specificity, reliability and convenience. Screening results for Radix Angelicae Dahuricae and Fructus Cnidii obtained using VSMC/CMC-MEPS-GC-MS were consistent with those obtained using VSMC/CMC-offline-GC-MS. MEPS connection plays as simplified solid-phase extraction and replaces the uncontrollable evaporation operation in reported offline connections, so our new method is supposed to be more efficient and reliable than the offline ones, especially for compounds that are volatile, thermally unstable or difficult to purify. In application, senkyunolide A and ligustilide were preliminary identified as the volatile active components in Rhizoma Chuanxiong. We have thus confirmed the suitability of VSMC/CMC-MEPS-GC-MS for volatile active compounds screening in NP. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. The instruments in the first psychological laboratory in Mexico: antecedents, influence, and methods.

    Science.gov (United States)

    Escobar, Rogelio

    2014-11-01

    Enrique O. Aragón established the first psychological laboratory in Mexico in 1916. This laboratory was inspired by Wundt's laboratory and by those created afterward in Germany and the United States. It was equipped with state-of-the art instruments imported from Germany in 1902 from Ernst Zimmermann who supplied instruments for Wundt's laboratory. Although previous authors have described the social events leading to the creation of the laboratory, there are limited descriptions of the instruments, their use, and their influence. With the aid of archival resources, the initial location of the laboratory was determined. The analysis of instruments revealed a previously overlooked relation with a previous laboratory of experimental physiology. The influence of the laboratory was traced by describing the careers of 4 students, 3 of them women, who worked with the instruments during the first 2 decades of the 20th century, each becoming accomplished scholars. In addition, this article, by identifying and analyzing the instruments shown in photographs of the psychological laboratory and in 1 motion film, provides information of the class demonstrations and the experiments conducted in this laboratory.

  20. A method for screening active components from Chinese herbs by cell membrane chromatography-offline-high performance liquid chromatography/mass spectrometry and an online statistical tool for data processing.

    Science.gov (United States)

    Cao, Yan; Wang, Shaozhan; Li, Yinghua; Chen, Xiaofei; Chen, Langdong; Wang, Dongyao; Zhu, Zhenyu; Yuan, Yongfang; Lv, Diya

    2018-03-09

    Cell membrane chromatography (CMC) has been successfully applied to screen bioactive compounds from Chinese herbs for many years, and some offline and online two-dimensional (2D) CMC-high performance liquid chromatography (HPLC) hyphenated systems have been established to perform screening assays. However, the requirement of sample preparation steps for the second-dimensional analysis in offline systems and the need for an interface device and technical expertise in the online system limit their extensive use. In the present study, an offline 2D CMC-HPLC analysis combined with the XCMS (various forms of chromatography coupled to mass spectrometry) Online statistical tool for data processing was established. First, our previously reported online 2D screening system was used to analyze three Chinese herbs that were reported to have potential anti-inflammatory effects, and two binding components were identified. By contrast, the proposed offline 2D screening method with XCMS Online analysis was applied, and three more ingredients were discovered in addition to the two compounds revealed by the online system. Then, cross-validation of the three compounds was performed, and they were confirmed to be included in the online data as well, but were not identified there because of their low concentrations and lack of credible statistical approaches. Last, pharmacological experiments showed that these five ingredients could inhibit IL-6 release and IL-6 gene expression on LPS-induced RAW cells in a dose-dependent manner. Compared with previous 2D CMC screening systems, this newly developed offline 2D method needs no sample preparation steps for the second-dimensional analysis, and it is sensitive, efficient, and convenient. It will be applicable in identifying active components from Chinese herbs and practical in discovery of lead compounds derived from herbs. Copyright © 2018 Elsevier B.V. All rights reserved.

  1. Determination of vegetable oils and fats adulterants in diesel oil by high performance liquid chromatography and multivariate methods.

    Science.gov (United States)

    Brandão, Luiz Filipe Paiva; Braga, Jez Willian Batista; Suarez, Paulo Anselmo Ziani

    2012-02-17

    The current legislation requires the mandatory addition of biodiesel to all Brazilian road diesel oil A (pure diesel) marketed in the country and bans the addition of vegetable oils for this type of diesel. However, cases of irregular addition of vegetable oils directly to the diesel oil may occur, mainly due to the lower cost of these raw materials compared to the final product, biodiesel. In Brazil, the situation is even more critical once the country is one of the largest producers of oleaginous products in the world, especially soybean, and also it has an extensive road network dependent on diesel. Therefore, alternatives to control the quality of diesel have become increasingly necessary. This study proposes an analytical methodology for quality control of diesel with intention to identify and determine adulterations of oils and even fats of vegetable origin. This methodology is based on detection, identification and quantification of triacylglycerols on diesel (main constituents of vegetable oils and fats) by high performance liquid chromatography in reversed phase with UV detection at 205nm associated with multivariate methods. Six different types of oils and fats were studied (soybean, frying oil, corn, cotton, palm oil and babassu) and two methods were developed for data analysis. The first one, based on principal component analysis (PCA), nearest neighbor classification (KNN) and univariate regression, was used for samples adulterated with a single type of oil or fat. In the second method, partial least square regression (PLS) was used for the cases where the adulterants were mixtures of up to three types of oils or fats. In the first method, the techniques of PCA and KNN were correctly classified as 17 out of 18 validation samples on the type of oil or fat present. The concentrations estimated for adulterants showed good agreement with the reference values, with mean errors of prediction (RMSEP) ranging between 0.10 and 0.22% (v/v). The PLS method was

  2. An analysis method for flavan-3-ols using high performance liquid chromatography coupled with a fluorescence detector

    Directory of Open Access Journals (Sweden)

    Liuqing Wang

    2017-07-01

    Full Text Available Procyanidins belong to a family of flavan-3-ols, which consist of monomers, (+-catechin and (−-epicatechin, and their oligomers and polymers, and are distributed in many plant-derived foods. Procyanidins are reported to have many beneficial physiological activities, such as antihypertensive and anticancer effects. However, the bioavailability of procyanidins is not well understood owing to a lack of convenient and high-sensitive analysis methods. The aim of this study was to develop an improved method for determining procyanidin content in both food materials and biological samples. High performance liquid chromatography (HPLC coupled with a fluorescence detector was used in this study. The limits of detection (LODs of (+-catechin, (−-epicatechin, procyanidin B2, procyanidin C1, and cinnamtannin A2 were 3.0×10−3 ng, 4.0×10−3 ng, 14.0×10−3 ng, 18.5×10−3 ng, and 23.0×10−3 ng, respectively; the limits of quantification (LOQs were 10.0×10−3 ng, 29.0×10−3 ng, 28.5×10−3 ng, 54.1×10−3 ng, and 115.0×10−3 ng, respectively. The LOD and LOQ values indicated that the sensitivity of the fluorescence detector method was around 1000 times higher than that of conventional HPLC coupled with a UV-detector. We applied the developed method to measure procyanidins in black soybean seed coat extract (BE prepared from soybeans grown under three different fertilization conditions, namely, conventional farming, basal manure application, and intertillage. The amount of flavan-3-ols in these BEs decreased in the order intertillage > basal manure application > conventional farming. Commercially available BE was orally administered to mice at a dose of 250 mg/kg body weight, and we measured the blood flavan-3-ol content. Data from plasma analysis indicated that up to the tetramer oligomerization, procyanidins were detectable and flavan-3-ols mainly existed in conjugated forms in the plasma. In conclusion, we developed a highly

  3. Data Quality Control: Challenges, Methods, and Solutions from an Eco-Hydrologic Instrumentation Network

    Science.gov (United States)

    Eiriksson, D.; Jones, A. S.; Horsburgh, J. S.; Cox, C.; Dastrup, D.

    2017-12-01

    Over the past few decades, advances in electronic dataloggers and in situ sensor technology have revolutionized our ability to monitor air, soil, and water to address questions in the environmental sciences. The increased spatial and temporal resolution of in situ data is alluring. However, an often overlooked aspect of these advances are the challenges data managers and technicians face in performing quality control on millions of data points collected every year. While there is general agreement that high quantities of data offer little value unless the data are of high quality, it is commonly understood that despite efforts toward quality assurance, environmental data collection occasionally goes wrong. After identifying erroneous data, data managers and technicians must determine whether to flag, delete, leave unaltered, or retroactively correct suspect data. While individual instrumentation networks often develop their own QA/QC procedures, there is a scarcity of consensus and literature regarding specific solutions and methods for correcting data. This may be because back correction efforts are time consuming, so suspect data are often simply abandoned. Correction techniques are also rarely reported in the literature, likely because corrections are often performed by technicians rather than the researchers who write the scientific papers. Details of correction procedures are often glossed over as a minor component of data collection and processing. To help address this disconnect, we present case studies of quality control challenges, solutions, and lessons learned from a large scale, multi-watershed environmental observatory in Northern Utah that monitors Gradients Along Mountain to Urban Transitions (GAMUT). The GAMUT network consists of over 40 individual climate, water quality, and storm drain monitoring stations that have collected more than 200 million unique data points in four years of operation. In all of our examples, we emphasize that scientists

  4. The Signal Validation method of Digital Process Instrumentation System on signal conditioner for SMART

    International Nuclear Information System (INIS)

    Moon, Hee Gun; Park, Sang Min; Kim, Jung Seon; Shon, Chang Ho; Park, Heui Youn; Koo, In Soo

    2005-01-01

    The function of PIS(Process Instrumentation System) for SMART is to acquire the process data from sensor or transmitter. The PIS consists of signal conditioner, A/D converter, DSP(Digital Signal Process) and NIC(Network Interface Card). So, It is fully digital system after A/D converter. The PI cabinet and PDAS(Plant Data Acquisition System) in commercial plant is responsible for data acquisition of the sensor or transmitter include RTD, TC, level, flow, pressure and so on. The PDAS has the software that processes each sensor data and PI cabinet has the signal conditioner, which is need for maintenance and test. The signal conditioner has the potentiometer to adjust the span and zero for test and maintenance. The PIS of SMART also has the signal conditioner which has the span and zero adjust same as the commercial plant because the signal conditioner perform the signal condition for AD converter such as 0∼10Vdc. But, To adjust span and zero is manual test and calibration. So, This paper presents the method of signal validation and calibration, which is used by digital feature in SMART. There are I/E(current to voltage), R/E(resistor to voltage), F/E(frequency to voltage), V/V(voltage to voltage). Etc. In this paper show only the signal validation and calibration about I/E converter that convert level, pressure, flow such as 4∼20mA into signal for AD conversion such as 0∼10Vdc

  5. Development of a quality instrument for assessing the spontaneous reports of ADR/ADE using Delphi method in China.

    Science.gov (United States)

    Chen, Lixun; Jiang, Ling; Shen, Aizong; Wei, Wei

    2016-09-01

    The frequently low quality of submitted spontaneous reports is of an increasing concern; to our knowledge, no validated instrument exists for assessing case reports' quality comprehensively enough. This work was conducted to develop such a quality instrument for assessing the spontaneous reports of adverse drug reaction (ADR)/adverse drug event (ADE) in China. Initial evaluation indicators were generated using systematic and literature data analysis. Final indicators and their weights were identified using Delphi method. The final quality instrument was developed by adopting the synthetic scoring method. A consensus was reached after four rounds of Delphi survey. The developed quality instrument consisted of 6 first-rank indicators, 18 second-rank indicators, and 115 third-rank indicators, and each rank indicator has been weighted. It evaluates the quality of spontaneous reports of ADR/ADE comprehensively and quantitatively on six parameters: authenticity, duplication, regulatory, completeness, vigilance level, and reporting time frame. The developed instrument was tested with good reliability and validity, which can be used to comprehensively and quantitatively assess the submitted spontaneous reports of ADR/ADE in China.

  6. Comparative determination of phenytoin by spectrophotometry, gas chromatography, liquid chromatography, enzyme immunoassay, and radioimmunoassay

    International Nuclear Information System (INIS)

    Castro, A.; Ibanez, J.; DiCesare, J.L.; Adams, R.F.; Malkus, H.

    1978-01-01

    Sera from patients being treated with phenytoin were analyzed for the drug by spectrophotometry, gas chromatography, radioimmunoasay, enzyme immunoassay, and liquid chromatography. The assay values obtained were intercompared statistically. Enzyme immunoassay and liquid chromatography appear to be attractive alternatives to the more traditional methods of spectrophotometry and gas chromatography. Our radioimmunoassay data correlated poorly with results by the four other methods

  7. Identification of Hepatoprotective Constituents in Limonium tetragonum and Development of Simultaneous Analysis Method using High-performance Liquid Chromatography

    Science.gov (United States)

    Lee, Jae Sun; Kim, Yun Na; Kim, Na-Hyun; Heo, Jeong-Doo; Yang, Min Hye; Rho, Jung-Rae; Jeong, Eun Ju

    2017-01-01

    Background: Limonium tetragonum, a naturally salt-tolerant halophyte, has been studied recently and is of much interest to researchers due to its potent antioxidant and hepatoprotective activities. Objective: In the present study, we attempted to elucidate bioactive compounds from ethyl acetate (EtOAc) soluble fraction of L. tetragonum extract. Furthermore, the simultaneous analysis method of bioactive EtOAc fraction of L. tetragonum has been developed using high-performance liquid chromatography (HPLC). Materials and Methods: Thirteen compounds have been successfully isolated from EtOAc fraction of L. tetragonum, and the structures of 1–13 were elucidated by extensive one-dimensional and two-dimensional spectroscopic methods including 1H-NMR, 13C-NMR, 1H-1H COSY, heteronuclear single quantum coherence, heteronuclear multiple bond correlation, and nuclear Overhauser effect spectroscopy. Hepatoprotection of the isolated compounds against liver fibrosis was evaluated by measuring inhibition on hepatic stellate cells (HSCs) undergoing proliferation. Results: Compounds 1–13 were identified as gallincin (1), apigenin-3-O-β-D-galactopyranoside (2), quercetin (3), quercetin-3-O-β-D-galactopyranoside (4), (−)-epigallocatechin (5), (−)-epigallocatechin-3-gallate (6), (−)-epigallocatechin-3-(3″-O-methyl) gallate (7), myricetin-3-O-β-D-galactopyranoside (8), myricetin-3-O-(6″-O-galloyl)-β-D-galactopyranoside (9), myricetin-3-O-α-L-rhamnopyranoside (10), myricetin-3-O-(2″-O-galloyl)-α-L-rhamnopyranoside (11), myricetin-3-O-(3″-O-galloyl)-α-L-rhamnopyranoside (12), and myricetin-3-O-α-L-arabinopyranoside (13), respectively. All compounds except for 4, 8, and 10 are reported for the first time from this plant. Conclusion: Myricetin glycosides which possess galloyl substituent (9, 11, and 12) showed most potent inhibitory effects on the proliferation of HSCs. SUMMARY In the present study, we have successfully isolated 13 compounds from bioactive fraction

  8. Qualitative to Quantitative and Spectrum to Report: An Instrument-Focused Research Methods Course for First-Year Students

    Science.gov (United States)

    Thomas, Alyssa C.; Boucher, Michelle A.; Pulliam, Curtis R.

    2015-01-01

    Our Introduction to Research Methods course is a first-year majors course built around the idea of helping students learn to work like chemists, write like chemists, and think like chemists. We have developed this course as a hybrid hands-on/ lecture experience built around instrumentation use and report preparation. We take the product from one…

  9. Solid-phase microextraction/gas chromatography-mass spectrometry method optimization for characterization of surface adsorption forces of nanoparticles.

    Science.gov (United States)

    Omanovic-Miklicanin, Enisa; Valzacchi, Sandro; Simoneau, Catherine; Gilliland, Douglas; Rossi, Francois

    2014-10-01

    A complete characterization of the different physico-chemical properties of nanoparticles (NPs) is necessary for the evaluation of their impact on health and environment. Among these properties, the surface characterization of the nanomaterial is the least developed and in many cases limited to the measurement of surface composition and zetapotential. The biological surface adsorption index approach (BSAI) for characterization of surface adsorption properties of NPs has recently been introduced (Xia et al. Nat Nanotechnol 5:671-675, 2010; Xia et al. ACS Nano 5(11):9074-9081, 2011). The BSAI approach offers in principle the possibility to characterize the different interaction forces exerted between a NP's surface and an organic--and by extension biological--entity. The present work further develops the BSAI approach and optimizes a solid-phase microextraction gas chromatography-mass spectrometry (SPME/GC-MS) method which, as an outcome, gives a better-defined quantification of the adsorption properties on NPs. We investigated the various aspects of the SPME/GC-MS method, including kinetics of adsorption of probe compounds on SPME fiber, kinetic of adsorption of probe compounds on NP's surface, and optimization of NP's concentration. The optimized conditions were then tested on 33 probe compounds and on Au NPs (15 nm) and SiO2 NPs (50 nm). The procedure allowed the identification of three compounds adsorbed by silica NPs and nine compounds by Au NPs, with equilibrium times which varied between 30 min and 12 h. Adsorption coefficients of 4.66 ± 0.23 and 4.44 ± 0.26 were calculated for 1-methylnaphtalene and biphenyl, compared to literature values of 4.89 and 5.18, respectively. The results demonstrated that the detailed optimization of the SPME/GC-MS method under various conditions is a critical factor and a prerequisite to the application of the BSAI approach as a tool to characterize surface adsorption properties of NPs and therefore to draw any further

  10. Vitamins in fruits and vegetables of the Amazon. 1. Methods for the determination of β—carotene, tocopherol and ascorbic acid with high performance liquid chromatography (HPLC)

    OpenAIRE

    Marx, F.; Maia, J.G.S.

    1983-01-01

    Summary At the beginning of on inventory of the chemical composition of regional fruits and vegetables of the Amazon, analytical methods were adapted for the high performance liquid chromatography (HPLC) determination of pro-vitamin A (β—carotene), vitamin C (ascorbic acid) and vitamin E (tocopherol) The first analyses indicate as excellent sources of β—carotene, Mauritia flexuosa L., Astrocaryum tucuma Mart. and Cucurbita pepa L.; of asco bic acid Theobroma grandiflorum (Culis ex Spreng.) Sc...

  11. [Ablation on the undersurface of a LASIK flap. Instrument and method for continuous eye tracking].

    Science.gov (United States)

    Taneri, S; Azar, D T

    2007-02-01

    The risk of iatrogenic keratectasia after laser in situ keratomileusis (LASIK) increases with thinner posterior stromal beds. Ablations on the undersurface of a LASIK flap could only be performed without the guidance of an eye tracker, which may lead to decentration. A new method for laser ablation with flying spot lasers on the undersurface of a LASIK flap was developed that enables the use of an active eye tracker by utilizing a novel instrument. The first clinical results are reported. Patients wishing an enhancement procedure were eligible for a modified repeat LASIK procedure if the flaps cut in the initial procedure were thick enough to perform the intended additional ablation on the undersurface leaving at least 90 microm of flap thickness behind. (1) The horizontal axis and the center of the entrance pupil were marked on the epithelial side of the flap using gentian violet dye. (2) The flap was reflected on a newly designed flap holder which had a donut-shaped black marking. (3) The eye tracker was centered on the mark visible in transparency on the flap. (4) Ablation with a flying spot Bausch & Lomb Technolas 217z laser was performed on the undersurface of the flap with a superior hinge taking into account that in astigmatic ablations the cylinder axis had to be mirrored according to the formula: axis on the undersurface=180 degrees -axis on the stromal bed. (5) The flap was repositioned. Detection of the marking on the modified flap holder and continuous tracking instead of the real pupil was possible in all of the 12 eyes treated with this technique. It may be necessary to cover the real pupil during ablation in order not to confuse the eye tracker. Ablation could be performed without decentration or loss of best spectacle-corrected visual acuity. Refractive results in minor corrections were good without nomogram adjustment. Using this novel flap holder with a marking that is tracked instead of the real pupil, centered ablations with a flying spot laser

  12. Advanced Instrumentation and Control Methods for Small and Medium Reactors with IRIS Demonstration

    Energy Technology Data Exchange (ETDEWEB)

    J. Wesley Hines; Belle R. Upadhyaya; J. Michael Doster; Robert M. Edwards; Kenneth D. Lewis; Paul Turinsky; Jamie Coble

    2011-05-31

    Development and deployment of small-scale nuclear power reactors and their maintenance, monitoring, and control are part of the mission under the Small Modular Reactor (SMR) program. The objectives of this NERI-consortium research project are to investigate, develop, and validate advanced methods for sensing, controlling, monitoring, diagnosis, and prognosis of these reactors, and to demonstrate the methods with application to one of the proposed integral pressurized water reactors (IPWR). For this project, the IPWR design by Westinghouse, the International Reactor Secure and Innovative (IRIS), has been used to demonstrate the techniques developed under this project. The research focuses on three topical areas with the following objectives. Objective 1 - Develop and apply simulation capabilities and sensitivity/uncertainty analysis methods to address sensor deployment analysis and small grid stability issues. Objective 2 - Develop and test an autonomous and fault-tolerant control architecture and apply to the IRIS system and an experimental flow control loop, with extensions to multiple reactor modules, nuclear desalination, and optimal sensor placement strategy. Objective 3 - Develop and test an integrated monitoring, diagnosis, and prognosis system for SMRs using the IRIS as a test platform, and integrate process and equipment monitoring (PEM) and process and equipment prognostics (PEP) toolboxes. The research tasks are focused on meeting the unique needs of reactors that may be deployed to remote locations or to developing countries with limited support infrastructure. These applications will require smaller, robust reactor designs with advanced technologies for sensors, instrumentation, and control. An excellent overview of SMRs is described in an article by Ingersoll (2009). The article refers to these as deliberately small reactors. Most of these have modular characteristics, with multiple units deployed at the same plant site. Additionally, the topics focus

  13. Factor analysis methods and validity evidence: A systematic review of instrument development across the continuum of medical education

    Science.gov (United States)

    Wetzel, Angela Payne

    Previous systematic reviews indicate a lack of reporting of reliability and validity evidence in subsets of the medical education literature. Psychology and general education reviews of factor analysis also indicate gaps between current and best practices; yet, a comprehensive review of exploratory factor analysis in instrument development across the continuum of medical education had not been previously identified. Therefore, the purpose for this study was critical review of instrument development articles employing exploratory factor or principal component analysis published in medical education (2006--2010) to describe and assess the reporting of methods and validity evidence based on the Standards for Educational and Psychological Testing and factor analysis best practices. Data extraction of 64 articles measuring a variety of constructs that have been published throughout the peer-reviewed medical education literature indicate significant errors in the translation of exploratory factor analysis best practices to current practice. Further, techniques for establishing validity evidence tend to derive from a limited scope of methods including reliability statistics to support internal structure and support for test content. Instruments reviewed for this study lacked supporting evidence based on relationships with other variables and response process, and evidence based on consequences of testing was not evident. Findings suggest a need for further professional development within the medical education researcher community related to (1) appropriate factor analysis methodology and reporting and (2) the importance of pursuing multiple sources of reliability and validity evidence to construct a well-supported argument for the inferences made from the instrument. Medical education researchers and educators should be cautious in adopting instruments from the literature and carefully review available evidence. Finally, editors and reviewers are encouraged to recognize

  14. Comparative urine analysis by liquid chromatography-mass spectrometry and multivariate statistics : Method development, evaluation, and application to proteinuria

    NARCIS (Netherlands)

    Kemperman, Ramses F. J.; Horvatovich, Peter L.; Hoekman, Berend; Reijmers, Theo H.; Muskiet, Frits A. J.; Bischoff, Rainer

    2007-01-01

    We describe a platform for the comparative profiling of urine using reversed-phase liquid chromatography-mass spectrometry (LC-MS) and multivariate statistical data analysis. Urinary compounds were separated by gradient elution and subsequently detected by electrospray Ion-Trap MS. The lower limit

  15. NONLINEAR-REGRESSION METHODS FOR MODELING OF HETEROSCEDASTIC RETENTION DATA IN REVERSED-PHASE HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY

    NARCIS (Netherlands)

    HENDRIKS, MMWB; COENEGRACHT, PMJ; DOORNBOS, DA

    1994-01-01

    New models have been developed that accurately describe the response surfaces of capacity factors that are a function of changes in the pH and the fraction of organic modifier in reversed-phase high-performance liquid chromatography (RP-HPLC). The purpose of this article is to illustrate one of the

  16. Development and evaluation of a liquid chromatography tandem mass spectrometry method for simultaneous determination of salivary melatonin, cortisol and testosterone

    DEFF Research Database (Denmark)

    Jensen, Marie Aarrebo; Hansen, Åse Marie; Abrahamsson, Peter

    2011-01-01

    saliva. We used liquid-liquid extraction (LLE) followed by liquid chromatography coupled to electrospray tandem mass spectrometry (LC-ESI-MS/MS) recorded in positive ion mode. Saliva samples were collected by spitting directly into tubes and 250 µL were used for analysis. The limits of detection were 4...

  17. Exploring Liquid Sequential Injection Chromatography to Teach Fundamentals of Separation Methods: A Very Fast Analytical Chemistry Experiment

    Science.gov (United States)

    Penteado, Jose C.; Masini, Jorge Cesar

    2011-01-01

    Influence of the solvent strength determined by the addition of a mobile-phase organic modifier and pH on chromatographic separation of sorbic acid and vanillin has been investigated by the relatively new technique, liquid sequential injection chromatography (SIC). This technique uses reversed-phase monolithic stationary phase to execute fast…

  18. A simple solid-phase extraction method for the analysis of red cell phospholipids by liquid chromatography- tandem mass spectrometry.

    Science.gov (United States)

    Nguyen, Van Long

    2018-02-25

    There has been increasing interest in the analysis of phospholipids in red blood cells as potential long-term biomarkers of different disease states. Here, we describe a simple method for the analysis of two phospholipids: 1-Palmitoyl-2-oleoyl-sn-glycero-3-phosphoethanol (PE 16:0/18:1) and 1-Palmitoyl-2-linoleoyl-sn-glycero-3-phosphoethanol (PE 16:/0/18:2) in erythrocytes by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Whole blood samples were removed free of plasma and washed in isotonic saline. Red cells were lysed with ultrapure water. Lysate samples were processed using a hybrid solid-phase extraction (SPE) phospholipid cartridge (1 mL, 30 mg). Both PE 16:0/18:1 and PE 16:0/18:2 and their deuterated internal standards were separated on an ACE C4 (150 mm × 2.1 mm, 2.7 μm particle size) by gradient elution at a flow rate of 0.5 mL per minute using mobile phases consisting of 0.01 mol/L ammonium acetate in: water (A), methanol (B), and isopropanol (C). The phospholipid species were quantified by the following transitions: PE 16:0/18:1: 701.5→281.3 and PE 16:0/18:2: 699.5→279.3. Both PE species displayed linearity ranging from 10 to 500 μg/L. The coefficient of variation (CV%) of PE 16:0/18:1 concerning intraday and interday precision was between 1.9%-2.6% and 3.0%-4.3%, respectively. For PE 16:0/18:2, this was between 1.8%-3.4% and 3.7%-4.1%, respectively. Both phospholipid species had accuracy (PE 16:0/18:1: 91%-98% and PE 16:0/18:2: 94%-103%) and extraction recovery (PE 16:0/18:1: 95%-106% and PE 16:0/18:2: 92%-102%) exceeding 90% over the analytical range. The limit of detection was 5 μg/L. Here we propose a simple SPE LC-MS/MS method for analyzing phospholipids in erythrocytes, which can be easily adopted. © 2018 Wiley Periodicals, Inc.

  19. Rapid quantitative analysis of individual anthocyanin content based on high-performance liquid chromatography with diode array detection with the pH differential method.

    Science.gov (United States)

    Wang, Huayin

    2014-09-01

    A new quantitative technique for the simultaneous quantification of the individual anthocyanins based on the pH differential method and high-performance liquid chromatography with diode array detection is proposed in this paper. The six individual anthocyanins (cyanidin 3-glucoside, cyanidin 3-rutinoside, petunidin 3-glucoside, petunidin 3-rutinoside, and malvidin 3-rutinoside) from mulberry (Morus rubra) and Liriope platyphylla were used for demonstration and validation. The elution of anthocyanins was performed using a C18 column with stepwise gradient elution and individual anthocyanins were identified by high-performance liquid chromatography with tandem mass spectrometry. Based on the pH differential method, the high-performance liquid chromatography peak areas of maximum and reference absorption wavelengths of anthocyanin extracts were conducted to quantify individual anthocyanins. The calibration curves for these anthocyanins were linear within the range of 10-5500 mg/L. The correlation coefficients (r(2)) all exceeded 0.9972, and the limits of detection were in the range of 1-4 mg/L at a signal-to-noise ratio ≥5 for these anthocyanins. The proposed quantitative analysis was reproducible with good accuracy of all individual anthocyanins ranging from 96.3 to 104.2% and relative recoveries were in the range 98.4-103.2%. The proposed technique is performed without anthocyanin standards and is a simple, rapid, accurate, and economical method to determine individual anthocyanin contents. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Development and validation of a rapid ultra-high performance liquid chromatography diode array detector method for Vitex agnus-castus.

    Science.gov (United States)

    Högner, C; Sturm, S; Seger, C; Stuppner, H

    2013-05-15

    A rapid ultra-high performance liquid chromatography diode array detector (UHPLC-DAD) method was developed and validated for the simultaneous determination of all classes of non-volatile phytochemicals (iridoids, flavonoids and diterpenes) in Vitex agnus-castus (Lamiaceae) fruits, a traditional medicinal plant used against premenstrual symptoms (PMS) and other disorders. Seven marker compounds, 3,4-dihydroxybenzoic acid, p-hydroxybenzoic acid, agnuside, 5-hydroxykaempferol-3,6,7,4'-tetramethylether, 1,2-dibenzoic acid glucose, methoxy-vitexilactone, and vitetrifolin D were isolated from the methanol extract of V. agnus-castus to be used as reference substances. Chromatographic separation was performed on a Zorbax Eclipse XDB-C18 (50mm×2.1mm) UHPLC column with 1.8μm particle size, within 20min. A solvent gradient from 0.5% acetic acid to acetonitrile at a flow rate of 0.6mL/min was used as mobile phase. Analyte detection and quantification was realized at 210nm and 260nm. The UHPLC-DAD assay was validated for the quantitative analysis of agnuside, isovitexin, casticin, 5-hydroxykaempferol-3,6,7,4'-tetramethylether and vitetrifolin D. It was found to be specific, accurate, precise, and reproducible for the quantification of these compound within a concentration range of 0.7-500.0μg/mL for casticin and 5-hydroxykaempferol-3,6,7,4'-tetramethylether, 1.4-1000.0μg/mL for isovitexin and agnuside, and 12.4-1000.0μg/mL for vitetrifolin D. Intra- and inter-day variations showed relative standard deviations (RSD) of less than 3.9% and 6.4%, respectively. Tentatively assignment of 62 chromatographic features found in the UHPLC-DAD assay was carried out by coupling the UHPLC instrument to a quadrupole time-of-flight mass spectrometer via an electrospray ionization interface (ESI-QTOF-MS) operated in positive and negative ion mode. By using the established quantitative UHPLC-DAD assay to asses agnuside, isovitexin, casticin, 5-hydroxykaempferol-3,6,7,4'-tetramethylether and