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Sample records for plasma spectrometric detection

  1. Mass spectrometric detection of siRNA in plasma samples for doping control purposes.

    Science.gov (United States)

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

    2010-10-01

    Small interfering ribonucleic acid (siRNA) molecules can effect the expression of any gene by inducing the degradation of mRNA. Therefore, these molecules can be of interest for illicit performance enhancement in sports by affecting different metabolic pathways. An example of an efficient performance-enhancing gene knockdown is the myostatin gene that regulates muscle growth. This study was carried out to provide a tool for the mass spectrometric detection of modified and unmodified siRNA from plasma samples. The oligonucleotides are purified by centrifugal filtration and the use of an miRNA purification kit, followed by flow-injection analysis using an Exactive mass spectrometer to yield the accurate masses of the sense and antisense strands. Although chromatography and sensitive mass spectrometric analysis of oligonucleotides are still challenging, a method was developed and validated that has adequate sensitivity (limit of detection 0.25-1 nmol mL(-1)) and performance (precision 11-21%, recovery 23-67%) for typical antisense oligonucleotides currently used in clinical studies.

  2. Inductively coupled plasma emission spectrometric detection of simulated high performance liquid chromatographic peaks

    International Nuclear Information System (INIS)

    Fraley, D.M.; Yates, D.; Manahan, S.E.

    1979-01-01

    Because of its multielement capability, element-specificity, and low detection limits, inductively coupled plasma optical emission spectrometry (ICP) is a very promising technique for the detection of specific elemental species separated by high performance liquid chromatography (HPLC). This paper evaluated ICP as a detector for HPLC peaks containing specific elements. Detection limits for a number of elements have been evaluated in terms of the minimum detectable concentration of the element at the chromatographic peak maximum. The elements studies were Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, Sb, Se, Sr, Ti, V, and Zn. In addition, ICP was compared with atomic absorption spectrometry for the detection of HPLC peaks composed of EDTA and NTA chelates of copper. Furthermore, ICP was compared to uv solution absorption for the detection of copper chelates. 6 figures, 4 tables

  3. Determination of suvorexant in human plasma using 96-well liquid-liquid extraction and HPLC with tandem mass spectrometric detection.

    Science.gov (United States)

    Breidinger, S A; Simpson, R C; Mangin, E; Woolf, E J

    2015-10-01

    A method, using liquid chromatography with tandem mass spectrometric detection (LC-MS/MS), was developed for the determination of suvorexant (MK-4305, Belsomra(®)), a selective dual orexin receptor antagonist for the treatment insomnia, in human plasma over the concentration range of 1-1000ng/mL. Stable isotope labeled (13)C(2)H3-suvorexant was used as an internal standard. The sample preparation procedure utilized liquid-liquid extraction, in the 96-well format, of a 100μL plasma sample with methyl t-butyl ether. The compounds were chromatographed under isocratic conditions on a Waters dC18 (50×2.1mm, 3μm) column with a mobile phase consisting of 30/70 (v/v %) 10mM ammonium formate, pH3/acetonitrile at a flow rate of 0.3mL/min. Multiple reaction monitoring of the precursor-to-product ion pairs for suvorexant (m/z 451→186) and (13)C(2)H3-suvorexant (m/z 455→190) on an Applied Biosystems API 4000 tandem mass spectrometer was used for quantitation. Intraday assay precision, assessed in six different lots of control plasma, was within 10% CV at all concentrations, while assay accuracy ranged from 95.6 to 105.0% of nominal. Quality control (QC) samples in plasma were stored at -20°C. Initial within day analysis of QCs after one freeze-thaw cycle showed accuracy within 9.5% of nominal with precision (CV) of 6.7% or less. The plasma QC samples were demonstrated to be stable for up to 25 months at -20°C. The method described has been used to support clinical studies during Phase I through III of clinical development. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. Determination of rare earth elements by liquid chromatographic separation using inductively coupled plasma mass spectrometric detection

    International Nuclear Information System (INIS)

    Braverman, D.S.

    1992-01-01

    High-performance liquid chromatography (HPLC) is used to separate the rare earth elements (REEs) prior to detection by inductively coupled plasma mass spectrometry (ICP-MS). The use of HPLC-ICP-MS in series combines the separation power and speed of HPLC with the sensitivity, isotopic selectivity and speed of ICP-MS. The detection limits for the REEs are in the sub-ng ml -1 range and the response is linear over four orders of magnitude. A preliminary comparison of isotope dilution and external standard results for the determination of REEs in National Institute of Standards and Technology (NIST) Standard Reference Material (SRM 1633a) Fly Ash is presented. (author)

  5. Determination of itopride in human plasma by liquid chromatography coupled to tandem mass spectrometric detection: application to a bioequivalence study.

    Science.gov (United States)

    Lee, Heon-Woo; Seo, Ji-Hyung; Choi, Seung-Ki; Lee, Kyung-Tae

    2007-01-30

    A simple method using a one-step liquid-liquid extraction (LLE) with butyl acetate followed by high-performance liquid chromatography (HPLC) with positive ion electrospray ionization tandem mass spectrometric (ESI-MS/MS) detection was developed for the determination of itopride in human plasma, using sulpiride as an internal standard (IS). Acquisition was performed in multiple reaction monitoring (MRM) mode, by monitoring the transitions: m/z 359.5>166.1 for itopride and m/z 342.3>111.6 for IS, respectively. Analytes were chromatographed on an YMC C18 reverse-phase chromatographic column by isocratic elution with 1 mM ammonium acetate buffer-methanol (20: 80, v/v; pH 4.0 adjusted with acetic acid). Results were linear (r2=0.9999) over the studied range (0.5-1000 ng mL(-1)) with a total analysis time per run of 2 min for LC-MS/MS. The developed method was validated and successfully applied to bioequivalence studies of itopride hydrochloride in healthy male volunteers.

  6. Carbon-enhanced inductively coupled plasma mass spectrometric detection of arsenic and selenium and its application to arsenic speciation

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Sturup, Stefan

    1994-01-01

    Addition of carbon as methanol or ammonium carbonate to the aqueous analyte solutions in combination with increased plasma power input enhanced the inductively coupled plasma mass spectrometry (ICP-MS) signal intensities of arsenic and selenium. In the presence of the optimum 3% v/v methanol...... (noise) was not increased. Therefore, the observed increase in analyte sensitivity led to a similar increase in signal-to-noise ratio. The addition of carbon as ammonium carbonate enhanced the arsenic signal by a similar factor but caused severe contamination of the ICP-MS instrument by carbon. In the 3....../nebulization efficiency. It is proposed that an increased population of carbon ions or carbon-containing ions in the plasma facilitates a more complete ionization of analytes lower in ionization energy than carbon itself. The enhanced detection power for arsenic was applied to arsenic speciation by high...

  7. Determination of nifedipine in dog plasma by high-performance liquid chromatography with tandem mass spectrometric detection.

    Science.gov (United States)

    Pan, Xigui; Zhou, Shunchang; Fu, Qinqin; Hu, Xianming; Wu, Jianhong

    2014-07-01

    Nifedipine is a dihydropyridine calcium channel blocker used widely in the management of hypertension and other cardiovascular disorders. In this work, a simple, rapid and sensitive liquid chromatography/tandem mass spectrometry method was developed and validated to determine nifedipine in dog plasma using nimodipine as the internal standard. Chromatographic separation was carried out on a C₈ column. The mobile phase consisted of a mixture of acetonitrile, water and formic acid (60:40:0.2, v/v/v) at a flow rate of 0.5 mL/min. Detection was performed on a triple quadrupole tandem mass spectrometer in selected reaction monitoring mode via an atmospheric pressure chemical ionization source. The method has a lower limit of quantification of 0.20 ng/mL with consumption of plasma as low as 0.05 mL. The linear calibration curves were obtained in the concentration range of 0.20-50.0 ng/mL (r = 0.9948). The recoveries of the liquid extraction method were 74.5-84.1%. Intra-day and inter-day precisions were 4.1-8.8 and 6.7-7.4%, respectively. The quantification was not interfered with by other plasma components and the method was applied to determine nifedipine in plasma after a single oral administration of two controlled-release nifedipine tablets to beagle dogs. Copyright © 2013 John Wiley & Sons, Ltd.

  8. Chemometric classification of gunshot residues based on energy dispersive X-ray microanalysis and inductively coupled plasma analysis with mass-spectrometric detection

    International Nuclear Information System (INIS)

    Steffen, S.; Otto, M.; Niewoehner, L.; Barth, M.; Brozek-Mucha, Z.; Biegstraaten, J.; Horvath, R.

    2007-01-01

    A gunshot residue sample that was collected from an object or a suspected person is automatically searched for gunshot residue relevant particles. Particle data (such as size, morphology, position on the sample for manual relocation, etc.) as well as the corresponding X-ray spectra and images are stored. According to these data, particles are classified by the analysis-software into different groups: 'gunshot residue characteristic', 'consistent with gunshot residue' and environmental particles, respectively. Potential gunshot residue particles are manually checked and - if necessary - confirmed by the operating forensic scientist. As there are continuing developments on the ammunition market worldwide, it becomes more and more difficult to assign a detected particle to a particular ammunition brand. As well, the differentiation towards environmental particles similar to gunshot residue is getting more complex. To keep external conditions unchanged, gunshot residue particles were collected using a specially designed shooting device for the test shots revealing defined shooting distances between the weapon's muzzle and the target. The data obtained as X-ray spectra of a number of particles (3000 per ammunition brand) were reduced by Fast Fourier Transformation and subjected to a chemometric evaluation by means of regularized discriminant analysis. In addition to the scanning electron microscopy in combination with energy dispersive X-ray microanalysis results, isotope ratio measurements based on inductively coupled plasma analysis with mass-spectrometric detection were carried out to provide a supplementary feature for an even lower risk of misclassification

  9. Chemometric classification of gunshot residues based on energy dispersive X-ray microanalysis and inductively coupled plasma analysis with mass-spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Steffen, S. [Bundeskriminalamt (BKA), Forensic Science Institute KT23, Thaerstr. 11, D - 65193 Wiesbaden (Germany); Otto, M. [TU Bergakademie Freiberg (TU BAF), Institute for Analytical Chemistry, Leipziger Str. 29, D - 09599 Freiberg (Germany)], E-mail: matthias.otto@chemie.tu-freiberg.de; Niewoehner, L.; Barth, M. [Bundeskriminalamt (BKA), Forensic Science Institute KT23, Thaerstr. 11, D - 65193 Wiesbaden (Germany); Brozek-Mucha, Z. [Instytut Ekspertyz Sadowych (IES), Westerplatte St. 9, PL - 31-033 Krakow (Poland); Biegstraaten, J. [Nederlands Forensisch Instituut (NFI), Fysische Technologie, Laan van Ypenburg 6, NL-2497 GB Den Haag (Netherlands); Horvath, R. [Kriminalisticky a Expertizny Ustav (KEU PZ), Institute of Forensic Science, Sklabinska 1, SK - 812 72 Bratislava (Slovakia)

    2007-09-15

    A gunshot residue sample that was collected from an object or a suspected person is automatically searched for gunshot residue relevant particles. Particle data (such as size, morphology, position on the sample for manual relocation, etc.) as well as the corresponding X-ray spectra and images are stored. According to these data, particles are classified by the analysis-software into different groups: 'gunshot residue characteristic', 'consistent with gunshot residue' and environmental particles, respectively. Potential gunshot residue particles are manually checked and - if necessary - confirmed by the operating forensic scientist. As there are continuing developments on the ammunition market worldwide, it becomes more and more difficult to assign a detected particle to a particular ammunition brand. As well, the differentiation towards environmental particles similar to gunshot residue is getting more complex. To keep external conditions unchanged, gunshot residue particles were collected using a specially designed shooting device for the test shots revealing defined shooting distances between the weapon's muzzle and the target. The data obtained as X-ray spectra of a number of particles (3000 per ammunition brand) were reduced by Fast Fourier Transformation and subjected to a chemometric evaluation by means of regularized discriminant analysis. In addition to the scanning electron microscopy in combination with energy dispersive X-ray microanalysis results, isotope ratio measurements based on inductively coupled plasma analysis with mass-spectrometric detection were carried out to provide a supplementary feature for an even lower risk of misclassification.

  10. A Sensitive and Robust Ultra HPLC Assay with Tandem Mass Spectrometric Detection for the Quantitation of the PARP Inhibitor Olaparib (AZD2281 in Human Plasma for Pharmacokinetic Application

    Directory of Open Access Journals (Sweden)

    Jeffrey Roth

    2014-06-01

    Full Text Available Olaparib (AZD2281 is an orally active PARP-1 inhibitor, primarily effective against cancers with BRCA1/2 mutations. It is currently in Phase III development and has previously been investigated in numerous clinical trials, both as a single agent and in combination with chemotherapy. Despite this widespread testing, there is only one published method that provides assay details and stability studies for olaparib alone. A more sensitive uHPLC-MS/MS method for the quantification of olaparib in human plasma was developed, increasing the range of quantification at both ends (0.5–50,000 ng/mL compared to previously published methods (10–5,000 ng/mL. The wider range encompasses CMAX levels produced by typical olaparib doses and permits better pharmacokinetic modeling of olaparib elimination. This assay also utilizes a shorter analytical runtime, allowing for more rapid quantification and reduced use of reagents. A liquid-liquid extraction was followed by chromatographic separation on a Waters UPLC® BEH C18 column (2.1 × 50 mm, 1.7 µm and mass spectrometric detection. The mass transitions m/z 435.4→281.1 and m/z 443.2→281.1 were used for olaparib and the internal standard [2H8]-olaparib, respectively. The assay proved to be accurate (<9% deviation and precise (CV < 11%. Stability studies showed that olaparib is stable at room temperature for 24 h. in whole blood, at 4 °C for 24 h post-extraction, at −80 °C in plasma for at least 19 months, and through three freeze-thaw cycles. This method proved to be robust for measuring olaparib levels in clinical samples from a Phase I trial.

  11. Speciation of eight arsenic compounds in human urine by high performance liquid chromatography with inductively coupled plasma mass spectrometric detection using antimonate for internal chromatographic standardization

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Pritzl, G.; Hansen, S. H.

    1993-01-01

    Four anionic and four cationic arsenic compounds in urine were separated by anion- and cation-exchange high-performance liquid chromatography and detected by inductively coupled plasma mass spectrometry (ICP-MS) at m/z 75. The species were the anions arsenite, arsenate, monomethylarsonate...... and dimethylarsinate and the cations arsenobetaine, trimethylarsine oxide, arsenocholine and the tetramethylarsonium ion. Hexahydroxyantimonate(III) was co-chromatographed with the arsenic anions but detected at m/z 121 and used as an internal standard for their qualitative analysis. Arsenite was prone to oxidation....... The argon chloride interference at m/z 75 was eliminated by chromatographic separation of the chloride present in the sample from the arsenic analytes. The ClO+ ion detected at m/z 51 and 53 was used to monitor the retention time of chloride in the anion-exchange system. The chloride eluted about 100 s...

  12. High-performance liquid chromatographic separation of biologically important arsenic species utilizing on-line inductively coupled argon plasma atomic emission spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Spall, W.D.; Lynn, J.G.; Andersen, J.L.; Valdez, J.G.; Gurley, L.R.

    1986-06-01

    An anion exchange, high-performance liquid chromatography technique using a 15-min linear gradient from water to 0.5 M ammonium carbonate to separate arsenite, arsenate, methylarsonic acid, and dimethylarsinic acid from neutral arsenic containing compounds was developed for application to a study of arsenic metabolism in cultured cell suspensions. Arsenic detection was accomplished by the direct coupling of the column effluent to an inductively coupled argon plasma atomic emission spectrometer (ICAP-AES) set to monitor the arsenic emission line at 197.19 nm. The analysis requires 20 min and is sensitive to as low as 60 ng of arsenic injected to the column.

  13. Combining asymmetrical flow field-flow fractionation with light-scattering and inductively coupled plasma mass spectrometric detection for characterization of nanoclay used in biopolymer nanocomposites

    DEFF Research Database (Denmark)

    Schmidt, Bjørn; Petersen, Jens Højslev; Koch, C. Bender

    2009-01-01

    mechanical and barrier properties and be more suitable for a wider range of food-packaging applications. Natural or synthetic clay nanofillers are being investigated for this purpose in a project called NanoPack funded by the Danish Strategic Research Council. In order to detect and characterize the size...... of clay nanoparticulates, an analytical system combining asymmetrical flow field-flow fractionation (AF4) with multi-angle light-scattering detection (MALS) and inductively coupled plasma mass spectrometry (ICP-MS) is presented. In a migration study, we tested a biopolymer nanocomposite consisting...... of polylactide (PLA) with 5% Cloisite®30B (a derivatized montmorillonite clay) as a filler. Based on AF4-MALS analyses, we found that particles ranging from 50 to 800 nm in radius indeed migrated into the 95% ethanol used as a food simulant. The full hyphenated AF4-MALS-ICP-MS system showed, however, that none...

  14. Simultaneous determination of codeine, ephedrine, guaiphenesin and chlorpheniramine in beagle dog plasma using high performance liquid chromatography coupled with tandem mass spectrometric detection: application to a bioequivalence study.

    Science.gov (United States)

    Hu, Ziyan; Zou, Qiaogen; Tian, Jixin; Sun, Lili; Zhang, Zunjian

    2011-12-15

    A rapid and sensitive method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the simultaneous determination of codeine, ephedrine, guaiphenesin and chlorpheniramine in beagle dog plasma has been developed and validated. Following liquid-liquid extraction, the analytes were separated on a reversed-phase C(18) column (150 mm × 2.0 mm, 3 μm) using formic acid:10 mM ammonium acetate:methanol (0.2:62:38, v/v/v) as mobile phase at a flow rate of 0.2 mL/min and analyzed by a triple-quadrupole mass spectrometer in the selected reaction monitoring (SRM) mode. The method was linear for all analytes over the following concentration (ng/mL) ranges: codeine 0.08-16; ephedrine 0.8-160; guaiphenesin 80-16,000; chlorpheniramine 0.2-40. Acceptable precision and accuracy were obtained for concentrations over the standard curve range. It is the first time that the validated HPLC-MS/MS method was successfully applied to a bioequivalence study in 6 healthy beagle dogs. Copyright © 2011 Elsevier B.V. All rights reserved.

  15. Mass Spectrometric C-14 Detection Techniques: Progress Report

    Science.gov (United States)

    Synal, H.

    2013-12-01

    Accelerator Mass Spectrometry (AMS) has been established as the best-suited radiocarbon detection technique. In the past years, significant progress with AMS instrumentation has been made resulting in a boom of new AMS facilities around the World. Today, carbon only AMS systems predominantly utilize 1+ charge state and molecule destruction in multiple ion gas collisions in stripper gas cell. This has made possible a significant simplification of the instruments, a reduction of ion energies and related to this less required space of the installations. However, state-of-the-art AMS instruments have still not reached a development stage where they can be regarded as table-top systems. In this respect, more development is needed to further advance the applicability of radiocarbon not only in the traditional fields of dating but also in biomedical research and new fields in Earth and environmental sciences. In a the proof-of-principle experiment the feasibility of radiocarbon detection over the entire range of dating applications was demonstrated using a pure mass spectrometer and ion energies below 50 keV. Now an experimental platform has been completed to test performance and to explore operation and measurement conditions of pure mass spectrometric radiocarbon detection. This contribution will overview the physical principles, which make this development possible and discuss key parameters of the instrumental design and performance of such an instrument.

  16. Status of mass spectrometric radiocarbon detection at ETHZ

    Energy Technology Data Exchange (ETDEWEB)

    Seiler, Martin; Maxeiner, Sascha; Wacker, Lukas; Synal, Hans-Arno

    2015-10-15

    A prototype of a mass spectrometric radiocarbon detection instrument without accelerator stage was built for the first time and set into operation at ETH Zurich. The system is designed as an experimental platform to optimize performance of {sup 14}C detection at low ion energies and to study the most relevant processes that may limit system performance. The optimized stripper unit incorporates differential pumping to maintain a low gas outflow and a revised tube design to better match the phase space volume of the ion beam at low energies. The system is fully operational and has demonstrated true radiocarbon dating capabilities. The overall beam transmission through the stripper tube is about 40% for the 1{sup +} charge state. Radiocarbon analyses with an overall precision of 0.6% were obtained on a single sample under regular measurement conditions. By analyzing multiple targets of the same sample material an uncertainty level of 0.3% has been reached. The background level corresponds to a radiocarbon age of 40,000 years.

  17. Determination of Non-Transferrin Bound Iron, Transferrin Bound Iron, Drug Bound Iron and Total Iron in Serum in a Rats after IV Administration of Sodium Ferric Gluconate Complex by Simple Ultrafiltration Inductively Coupled Plasma Mass Spectrometric Detection

    Directory of Open Access Journals (Sweden)

    Murali K. Matta

    2018-02-01

    Full Text Available A rapid, sensitive and specific ultrafiltration inductively-coupled plasma mass spectrometry method was developed and validated for the quantification of non-transferrin bound iron (NTBI, transferrin bound iron (TBI, drug bound iron (DI and total iron (TI in the same rat serum sample after intravenous (IV administration of iron gluconate nanoparticles in sucrose solution (Ferrlecit®. Ultrafiltration with a 30 kDa molecular cut-off filter was used for sample cleanup. Different elution solvents were used to separate each form of iron from sample serum. Isolated fractions were subjected to inductively-coupled mass spectrometric analysis after microwave digestion in 4% nitric acid. The reproducibility of the method was evaluated by precision and accuracy. The calibration curve demonstrated linearity from 5–500 ng/mL with a regression (r2 of more than 0.998. This method was effectively implemented to quantify rat pharmacokinetic study samples after intravenous administration of Ferrlecit®. The method was successfully applied to a pharmacokinetic (PK study of Ferrlecit in rats. The colloidal iron followed first order kinetics with half-life of 2.2 h and reached background or pre-dose levels after 12 h post-dosing. The drug shown a clearance of 0.31 mL/min/kg and volume of distribution of 0.05 L/kg. 19.4 ± 2.4 mL/h/kg.

  18. Mass spectrometric detection of radiocarbon for dating applications

    OpenAIRE

    Synal Hans-Arno

    2013-01-01

    Radiocarbon is still the most important nuclide measured by accelerator mass spectrometry (AMS). The related capabilities for dating and tracer studies are eminent not only in archaeology but also drive important applications in the earth and environmental sciences as well as in biomedical research. So far standard mass spectrometric systems have not been capable of radiocarbon dating because of interfering molecular isobars which however can be completely eliminated in charge changing proces...

  19. Mass spectrometric detection of radiocarbon for dating applications

    Energy Technology Data Exchange (ETDEWEB)

    Synal, H.-A., E-mail: synal@phys.ethz.ch [ETH Zurich, Laboratory of Ion Beam Physics, Building HPK, 8093 Zurich (Switzerland); Schulze-Koenig, T.; Seiler, M.; Suter, M.; Wacker, L. [ETH Zurich, Laboratory of Ion Beam Physics, Building HPK, 8093 Zurich (Switzerland)

    2013-01-15

    Radiocarbon is still the most important nuclide measured by accelerator mass spectrometry (AMS). The related capabilities for dating and tracer studies are eminent not only in archaeology but also drive important applications in the earth and environmental sciences as well as in biomedical research. So far, standard mass spectrometric systems have not been capable of radiocarbon dating because of interfering molecular isobars which, however, can be completely eliminated in charge changing processes at high ion beam energies (MeV) [1,2]. Here, we present a novel type mass spectrometry system for radiocarbon analyses. Radiocarbon dating was performed using 45 keV {sup 14}C ions from the ion source and a molecule dissociation unit kept at ground potential. This proof-of-principle experiment demonstrates for the first time the feasibility of mass spectrometric radiocarbon dating without an accelerator. The results obtained will be the basis of an optimized design for a radiocarbon dating instrument comparable in size, complexity and cost to standard mass spectrometers.

  20. Mass spectrometric detection of radiocarbon for dating applications

    International Nuclear Information System (INIS)

    Synal, H.-A.; Schulze-König, T.; Seiler, M.; Suter, M.; Wacker, L.

    2013-01-01

    Radiocarbon is still the most important nuclide measured by accelerator mass spectrometry (AMS). The related capabilities for dating and tracer studies are eminent not only in archaeology but also drive important applications in the earth and environmental sciences as well as in biomedical research. So far, standard mass spectrometric systems have not been capable of radiocarbon dating because of interfering molecular isobars which, however, can be completely eliminated in charge changing processes at high ion beam energies (MeV) [1,2]. Here, we present a novel type mass spectrometry system for radiocarbon analyses. Radiocarbon dating was performed using 45 keV 14 C ions from the ion source and a molecule dissociation unit kept at ground potential. This proof-of-principle experiment demonstrates for the first time the feasibility of mass spectrometric radiocarbon dating without an accelerator. The results obtained will be the basis of an optimized design for a radiocarbon dating instrument comparable in size, complexity and cost to standard mass spectrometers.

  1. Mass spectrometric detection of radiocarbon for dating applications

    Science.gov (United States)

    Synal, H.-A.; Schulze-König, T.; Seiler, M.; Suter, M.; Wacker, L.

    2013-01-01

    Radiocarbon is still the most important nuclide measured by accelerator mass spectrometry (AMS). The related capabilities for dating and tracer studies are eminent not only in archaeology but also drive important applications in the earth and environmental sciences as well as in biomedical research. So far, standard mass spectrometric systems have not been capable of radiocarbon dating because of interfering molecular isobars which, however, can be completely eliminated in charge changing processes at high ion beam energies (MeV) [1,2]. Here, we present a novel type mass spectrometry system for radiocarbon analyses. Radiocarbon dating was performed using 45 keV 14C ions from the ion source and a molecule dissociation unit kept at ground potential. This proof-of-principle experiment demonstrates for the first time the feasibility of mass spectrometric radiocarbon dating without an accelerator. The results obtained will be the basis of an optimized design for a radiocarbon dating instrument comparable in size, complexity and cost to standard mass spectrometers.

  2. Retrospective detection of exposure to organophosphorus anti-cholinesterases: Mass spectrometric analysis of phosphylated human butyrylcholinesterase

    NARCIS (Netherlands)

    Fidder, A.; Hulst, A.G.; Noort, D.; Ruiter, R. de; Schans, M.J. van der; Benschop, H.P.; Langenberg, J.P.

    2002-01-01

    In this paper a novel and general procedure is presented for detection of organophosphate-inhibited human butyrylcholinesterase (HuBuChE), which is based on electrospray tandem mass spectrometric analysis of phosphylated nonapeptides obtained after pepsin digestion of the enzyme. The utility of this

  3. Speciation and detection of arsenic in aqueous samples: A review of recent progress in non-atomic spectrometric methods

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Jian [State Key Laboratory of Marine Environmental Science, College of the Environment and Ecology, Xiamen University, Xiamen 361102 (China); Department of Chemistry and Biochemistry, University of Texas, 700 Planetarium Place, Arlington, TX 76019 (United States); Sengupta, Mrinal K. [Department of Chemistry and Biochemistry, University of Texas, 700 Planetarium Place, Arlington, TX 76019 (United States); Thermo Fisher Scientific, Dionex Products, 445 Lakeside Drive, Sunnyvale, CA, 94085 (United States); Yuan, Dongxing [State Key Laboratory of Marine Environmental Science, College of the Environment and Ecology, Xiamen University, Xiamen 361102 (China); Dasgupta, Purnendu K., E-mail: Dasgupta@uta.edu [Department of Chemistry and Biochemistry, University of Texas, 700 Planetarium Place, Arlington, TX 76019 (United States)

    2014-06-01

    Highlights: • Compilation of principal official documents and major review articles, including the toxicology and chemistry of As. • Review of non-atomic spectrometric methods for speciation and detection of arsenic in aqueous samples (2005–2013) of the performance of field-usable methods. - Abstract: Inorganic arsenic (As) displays extreme toxicity and is a class A human carcinogen. It is of interest to both analytical chemists and environmental scientists. Facile and sensitive determination of As and knowledge of the speciation of forms of As in aqueous samples are vitally important. Nearly every nation has relevant official regulations on permissible limits of drinking water As content. The size of the literature on As is therefore formidable. The heart of this review consists of two tables: one is a compilation of principal official documents and major review articles, including the toxicology and chemistry of As. This includes comprehensive official compendia on As speciation, sample treatment, recommended procedures for the determination of As in specific sample matrices with specific analytical instrument(s), procedures for multi-element (including As) speciation and analysis, and prior comprehensive reviews on arsenic analysis. The second table focuses on the recent literature (2005–2013, the coverage for 2013 is incomplete) on As measurement in aqueous matrices. Recent As speciation and analysis methods based on spectrometric and electrochemical methods, inductively coupled plasma-mass spectrometry, neutron activation analysis and biosensors are summarized. We have deliberately excluded atomic optical spectrometric techniques (atomic absorption, atomic fluorescence, inductively coupled plasma-optical emission spectrometry) not because they are not important (in fact the majority of arsenic determinations are possibly carried out by one of these techniques) but because these methods are sufficiently mature and little meaningful innovation has been

  4. Speciation and detection of arsenic in aqueous samples: A review of recent progress in non-atomic spectrometric methods

    International Nuclear Information System (INIS)

    Ma, Jian; Sengupta, Mrinal K.; Yuan, Dongxing; Dasgupta, Purnendu K.

    2014-01-01

    Highlights: • Compilation of principal official documents and major review articles, including the toxicology and chemistry of As. • Review of non-atomic spectrometric methods for speciation and detection of arsenic in aqueous samples (2005–2013) of the performance of field-usable methods. - Abstract: Inorganic arsenic (As) displays extreme toxicity and is a class A human carcinogen. It is of interest to both analytical chemists and environmental scientists. Facile and sensitive determination of As and knowledge of the speciation of forms of As in aqueous samples are vitally important. Nearly every nation has relevant official regulations on permissible limits of drinking water As content. The size of the literature on As is therefore formidable. The heart of this review consists of two tables: one is a compilation of principal official documents and major review articles, including the toxicology and chemistry of As. This includes comprehensive official compendia on As speciation, sample treatment, recommended procedures for the determination of As in specific sample matrices with specific analytical instrument(s), procedures for multi-element (including As) speciation and analysis, and prior comprehensive reviews on arsenic analysis. The second table focuses on the recent literature (2005–2013, the coverage for 2013 is incomplete) on As measurement in aqueous matrices. Recent As speciation and analysis methods based on spectrometric and electrochemical methods, inductively coupled plasma-mass spectrometry, neutron activation analysis and biosensors are summarized. We have deliberately excluded atomic optical spectrometric techniques (atomic absorption, atomic fluorescence, inductively coupled plasma-optical emission spectrometry) not because they are not important (in fact the majority of arsenic determinations are possibly carried out by one of these techniques) but because these methods are sufficiently mature and little meaningful innovation has been

  5. SPECIATION OF SELENIUM AND ARSENIC COMPOUNDS BY CAPILLARY ELECTROPHORESIS WITH HYDRODYNAMICALLY MODIFIED ELECTROOSMOTIC FLOW AND ON-LINE REDUCTION OF SELENIUM(VI) TO SELENIUM(IV) WITH HYDRIDE GENERATION INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRIC DETECTION

    Science.gov (United States)

    Capillary electrophoresis (CE) with hydride generation inductively coupled plasma mass spectrometry was used to determine four arsenicals and two selenium species. Selenate (SeVI) was reduced on-line to selenite (SeIV') by mixing the CE effluent with concentrated HCl. A microporo...

  6. Calibration of a leak detection spectrometer; Calibration d'un spectrometre detecteur de fuites

    Energy Technology Data Exchange (ETDEWEB)

    Geller, R [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1958-07-01

    This paper describes a study of the possible methods for calibrating a leak detection spectrometer, and the estimation of outputs from the leaks is considered. With this in mind the question of sensitivity of leak detection is tackled on a very general level; first the sensitivity of the isolated instrument is determined, and then the sensitivity of an instrument connected to an installation where leaks may be suspected. Finally, practical solutions are proposed. (author) [French] Dans cet article, nous etudions les methodes possibles de calibration d'un spectrometre detecteur de fuites et nous envisageons l'evaluation des debits de fuites trouves. Pour cela, nous abordons la notion de sensibilite de la detection de fuite sur un plan tres general; d'abord nous determinons la sensibilite de l'appareil isole, ensuite la sensibilite d'un appareil connecte sur une installation ou l'on cherche les fuites. Enfin, nous preconisons des solutions pratiques. (auteur)

  7. Gas chromatography of organic microcontaminants using atomic emission and mass spectrometric detection combined in one instrument (GC-AED/MS)

    NARCIS (Netherlands)

    Mol, H.G.J.; Hankemeier, T.; Brinkman, U.A.T.

    1999-01-01

    This study describes the coupling of an atomic-emission detector and mass-spectrometric detector to a single gas chromatograph. Splitting of the column effluent enables simultaneous detection by atomic-emission detection (AED) and mass spectrometry (MS) and yields a powerful system for the target

  8. Identification of volatiles by headspace gas chromatography with simultaneous flame ionization and mass spectrometric detection.

    Science.gov (United States)

    Tiscione, Nicholas B; Yeatman, Dustin Tate; Shan, Xiaoqin; Kahl, Joseph H

    2013-10-01

    Volatiles are frequently abused as inhalants. The methods used for identification are generally nonspecific if analyzed concurrently with ethanol or require an additional analytical procedure that employs mass spectrometry. A previously published technique utilizing a capillary flow technology splitter to simultaneously quantitate and confirm ethyl alcohol by flame ionization and mass spectrometric detection after headspace sampling and gas chromatographic separation was evaluated for the detection of inhalants. Methanol, isopropanol, acetone, acetaldehyde, toluene, methyl ethyl ketone, isoamyl alcohol, isobutyl alcohol, n-butyl alcohol, 1,1-difluoroethane, 1,1,1-trifluoroethane, 1,1,1,2-tetrafluoroethane (Norflurane, HFC-134a), chloroethane, trichlorofluoromethane (Freon®-11), dichlorodifluoromethane (Freon®-12), dichlorofluoromethane (Freon®-21), chlorodifluoromethane (Freon®-22) and 1,2-dichlorotetrafluoroethane (Freon®-114) were validated for qualitative identification by this method. The validation for qualitative identification included evaluation of matrix effects, sensitivity, carryover, specificity, repeatability and ruggedness/robustness.

  9. Analysis of Endocrine Disrupting Pesticides by Capillary GC with Mass Spectrometric Detection

    Directory of Open Access Journals (Sweden)

    Svetlana Hrouzková

    2012-09-01

    Full Text Available Endocrine disrupting chemicals, among them many pesticides, alter the normal functioning of the endocrine system of both wildlife and humans at very low concentration levels. Therefore, the importance of method development for their analysis in food and the environment is increasing. This also covers contributions in the field of ultra-trace analysis of multicomponent mixtures of organic pollutants in complex matrices. With this fact conventional capillary gas chromatography (CGC and fast CGC with mass spectrometric detection (MS has acquired a real importance in the analysis of endocrine disrupting pesticide (EDP residues. This paper provides an overview of GC methods, including sample preparation steps, for analysis of EDPs in a variety of matrices at ultra-trace concentration levels. Emphasis is put on separation method, mode of MS detection and ionization and obtained limits of detection and quantification. Analysis time is one of the most important aspects that should be considered in the choice of analytical methods for routine analysis. Therefore, the benefits of developed fast GC methods are important.

  10. Quantum dots assisted laser desorption/ionization mass spectrometric detection of carbohydrates: qualitative and quantitative analysis.

    Science.gov (United States)

    Bibi, Aisha; Ju, Huangxian

    2016-04-01

    A quantum dots (QDs) assisted laser desorption/ionization mass spectrometric (QDA-LDI-MS) strategy was proposed for qualitative and quantitative analysis of a series of carbohydrates. The adsorption of carbohydrates on the modified surface of different QDs as the matrices depended mainly on the formation of hydrogen bonding, which led to higher MS intensity than those with conventional organic matrix. The effects of QDs concentration and sample preparation method were explored for improving the selective ionization process and the detection sensitivity. The proposed approach offered a new dimension to the application of QDs as matrices for MALDI-MS research of carbohydrates. It could be used for quantitative measurement of glucose concentration in human serum with good performance. The QDs served as a matrix showed the advantages of low background, higher sensitivity, convenient sample preparation and excellent stability under vacuum. The QDs assisted LDI-MS approach has promising application to the analysis of carbohydrates in complex biological samples. Copyright © 2016 John Wiley & Sons, Ltd.

  11. Liquid chromatography-tandem mass spectrometric assay for the tyrosine kinase inhibitor afatinib in mouse plasma using salting-out liquid-liquid extraction

    NARCIS (Netherlands)

    Sparidans, Rolf W; van Hoppe, Stephanie; Rood, Johannes J M; Schinkel, Alfred H; Schellens, Jan H M; Beijnen, Jos H

    2016-01-01

    A quantitative bioanalytical liquid chromatography-tandem mass spectrometric (LC-MS/MS) assay for afatinib, an irreversible inhibitor of the ErbB (erythroblastic leukemia viral oncogene homolog) tyrosine kinase family, was developed and validated. Plasma samples were pre-treated using salting-out

  12. Liquid Chromatography-Tandem Mass Spectrometric Assay for Determination of Stavudine in Human Plasma

    Directory of Open Access Journals (Sweden)

    Fengdan Jin

    2014-01-01

    Full Text Available A LC-MS/MS method for determination of stavudine in human plasma was established and validated, and it was applied to the pharmaceutical formulations bioequivalence study. 0.5 mL plasma sample was extracted by liquid-liquid extraction. Stavudine was detected by a LC-MS/MS system. The pharmacokinetic parameters of stavudine in different formulations were calculated by noncompartment model statistics. The method was linear over the concentration ranges 5.00–1000 ng/mL in plasma. The intra- and interassay relative standard deviation (RSD was <10%. The average accuracies for the assay at three concentrations (5.00, 80.0, and 900 ng/mL were from 100.2% to 102.5%. Pharmacokinetic parameters of stavudine reference formulation were obtained as follows: Tmax was 0.6±0.2 h, Cmax was 480.7±150.9 g/L, t1/2 was 1.7±0.4 h, and AUC0-t was 872.8±227.8 g·h/L, and pharmacokinetic parameters of stavudine test formulation were obtained as follows: Tmax was 0.5±0.2 h, Cmax was 537.5±178.5 g/L, t1/2 was 1.7±0.3 h, and AUC0-t was (914.1±284.5 g·h/L. Calculated with AUC0-t, the bioavailability of two formulations was 105.0%.

  13. Vitamin D-metabolites from human plasma and mass spectrometric analysis by fast heavy ion induced desorption

    Energy Technology Data Exchange (ETDEWEB)

    Fohlman, J; Peterson, P A [Uppsala Univ. (Sweden). Dept. of Cell Research; Kamensky, I; Hakansson, P; Sundqvist, B [Tandemacceleratorlaboratoriet, Uppsala (Sweden)

    1982-07-01

    D-vitamin metabolites have been isolated from human serum employing chromatographic techniques. The serum carrier protein for vitamin D (DBP) was first isolated by immunosorbent chromatography. Lipid ligands associated with DBP were then extracted with hexane and separated by high pressure liquid chromatography (HPLC). Detection of vitamin D metabolites by their absorbance of ultraviolet light is not sufficiently sensitive to monitor all vitamin D derivatives from a few millilitres of serum. Therefore, further analyses are necessary to quantitative these compounds. We have begun to develop a mass spectrometric method to achieve a reliable, quantitative procedure. As a first step towards this goal a number of pure samples of vitamin D compounds have been studied in a time-of-flight mass spectrometer based on fast heavy ion induced desorption. All vitamin D compounds examined could be detected and identified by their molecular ion and fragment spectra.

  14. Vitamin D-metabolites from human plasma and mass spectrometric analysis by fast heavy ion induced desorption

    International Nuclear Information System (INIS)

    Fohlman, J.; Peterson, P.A.

    1982-01-01

    D-vitamin metabolites have been isolated from human serum employing chromatographic techniques. The serum carrier protein for vitamin D (DBP) was first isolated by immunosorbent chromatography. Lipid ligands associated with DBP were then extracted with hexane and separated by high pressure liquid chromatography (HPLC). Detection of vitamin D metabolites by their absorbance of ultraviolet light is not sufficiently sensitive to monitor all vitamin D derivatives from a few millilitres of serum. Therefore, further analyses are necessary to quantitative these compounds. We have begun to develop a mass spectrometric method to achieve a reliable, quantitative procedure. As a first step towards this goal a number of pure samples of vitamin D compounds have been studied in a time-of-flight mass spectrometer based on fast heavy ion induced desorption. All vitamin D compounds examined could be detected and identified by their molecular ion and fragment spectra. (orig.)

  15. Recent progress in the development of CsI(Tl) crystal-Si-photodiode spectrometric detection assemblies

    International Nuclear Information System (INIS)

    Semynozhenko, V.P.; Grinyov, B.V.; Nekrasov, V.V.; Borodenko, Yu.A.

    2005-01-01

    Highly sensitive spectrometric γ-detection assemblies are developed using a comprehensive approach (optimization of crystal growth conditions as well as of treatment and packing of scintillators, creation of low-noise charge-sensitive preamplifiers and shapers). The detection assemblies with CsI(Tl)≤100 cm 3 have a sensitivity of about 20 pulse/s(mcR/h), their energy resolution with respect to 137 Cs γ-line being ≤8.5%. The assemblies with lesser scintillator volumes (1-5 cm 3 ) provide a resolution lower than 6% with respect to 137 Cs and ≤40% with respect to 241 Am

  16. Mass spectrometric detection of proteins in non-aqueous media : the case of prion proteins in biodiesel

    Energy Technology Data Exchange (ETDEWEB)

    Douma, M.D.; Kerr, G.M.; Brown, R.S.; Keller, B.O.; Oleschuk, R.D. [Queen' s Univ., Kingston, ON (Canada). Dept. of Chemistry

    2008-08-15

    This paper presented a filtration method for detecting protein traces in non-aqueous media. The extraction technique used a mixture of acetonitrile, non-ionic detergent and water along with filter disks with embedded C{sub 8}-modified silica particles to capture the proteins from non-aqueous samples. The extraction process was then followed by an elution of the protein from the filter disk and direct mass spectrometric detection and tryptic digestion with peptide mapping and MS/MS fragmentation of protein-specific peptides. The method was used to detect prion proteins in spiked biodiesel samples. A tryptic peptide with the sequence YGQGSPGGNR was used for unambiguous identification. Results of the study showed that the method is suitable for the large-scale testing of protein impurities in tallow-based biodiesel production processes. 33 refs., 6 figs.

  17. Streamer-induced emission and spectrometric determination of basic plasma parameters

    Czech Academy of Sciences Publication Activity Database

    Šimek, Milan

    2004-01-01

    Roč. 54, suppl.C (2004), C778-C783 ISSN 0011-4626. [Symposium on Plasma Physics and Technology /21./. Praha, 14.06.2004-17.06.2004] R&D Projects: GA AV ČR IAA1043403 Institutional research plan: CEZ:AV0Z2043910 Keywords : optical diagnostics * discharge * streamer Subject RIV: BL - Plasma and Gas Discharge Physics Impact factor: 0.292, year: 2004

  18. A spectrometric approach in radiography for detection of materials by their effective atomic number

    CERN Document Server

    Ryzhikov, V D; Onyshchenko, G M; Lecoq, P; Smith, C F

    2009-01-01

    In this paper we report a spectrometric approach to dual-energy digital radiography that has been developed and applied to identify specific organic substances and discern small differences in their effective atomic number. An experimental setup has been designed, and a theoretical description proposed based on the experimental results obtained. The proposed method is based on the application of special reference samples made of materials with different effective atomic number and thickness parameters known to affect X-ray attenuation in the low-energy range. The results obtained can be used in the development of a new generation of multi-energy customs or medical X-ray scanners.

  19. Mass spectrometric evidence for suprathermal ionization in an inductively coupled argon plasma

    International Nuclear Information System (INIS)

    Houk, R.S.; Svec, H.J.; Fassel, V.A.

    1981-01-01

    Mass spectra have been obtained of species in the axial channel of an inductively coupled argon plasma by extracting ions from the inductively coupled plasma into a vacuum system housing a quadrupole mass spectrometer. Ionization temperatures (T/sub ion/) are obtained from relative count rates of m/z-resolved ions according to two general types of ionization equilibrium considerations: (a) the radio of doubly/singly charged ions of the same element, and (b) the ratio of singly charged ions from two elements of different ionization energy. The T/sub ion/ values derived from measurement of Ar +2 /Ar + , Ba +2 /Ba + , Sr +2 /Sr + , and Cd + /I + are all greater than those expected from excitation temperatures measured by other workers. The latter three values for T/sub ion/ are in reasonable agreement with values obtained by optical spectrometry for a variety of argon inductively coupled plasmas

  20. Detection, characterization and quantification of salicylic acid conjugates in plant extracts by ESI tandem mass spectrometric techniques.

    Science.gov (United States)

    Pastor, Victoria; Vicent, Cristian; Cerezo, Miguel; Mauch-Mani, Brigitte; Dean, John; Flors, Victor

    2012-04-01

    An approach for the detection and characterization of SA derivatives in plant samples is presented based on liquid chromatography coupled to electrospray ionization (ESI) tandem mass spectrometric techniques. Precursor ion scan methods using an ESI triple quadrupole spectrometer for samples from plants challenged with the virulent Pseudomonas syringae pv tomato DC3000 allowed us to detect two potential SA derivatives. The criterion used to consider a potential SA derivative is based on the detection of analytes in the precursor ion scan chromatogram upon selecting m/z 137 and m/z 93 that correspond to the salicylate and its main product ion, respectively. Product ion spectra of the newly-detected analytes as well as accurate m/z determinations using an ESI Q-time-of-flight instrument were registered as means of characterization and strongly suggest that glucosylated forms of SA at the carboxylic and at the phenol functional groups are present in plant samples. The specific synthesis and subsequent chromatography of salicylic glucosyl ester (SGE) and glucosyl salicylate (SAG) standards confirmed the chemical identity of both peaks that were obtained applying different tandem mass spectrometric techniques and accurate m/z determinations. A multiple reaction monitoring method has been developed and applied to plant samples. The advantages of this LC-ESI-MS/MS methods with respect to the traditional analysis of glucosyl conjugates are also discussed. Preliminary results revealed that SA and the glucosyl conjugates are accumulated in Arabidopsis thaliana in a time dependent manner, accordingly to the up-regulation of SA-dependent defenses following P. syringae infection. This technique applied to plant hormones or fragment ions may be useful to obtain chemical family members of plant metabolites and help identify their contribution in the signaling of plant defenses. Copyright © 2012 Elsevier Masson SAS. All rights reserved.

  1. High performance liquid chromatographic-mass spectrometric assay for the quantitation of BMS-204352 in dog K(3)EDTA plasma.

    Science.gov (United States)

    Yao, Ming; Mantha, Subbarao; Shah, Vinod R; Vachharajani, Nimish N; Arnold, Mark E; Pursley, Janice M; Srinivas, Nuggehally R

    2002-05-01

    A high performance liquid chromatographic-mass spectrometric (LC/MS) assay was developed and validated for the determination of BMS-204352 in dog K(3)EDTA plasma. A 0.5 mL aliquot of control plasma was spiked with BMS-204352 and internal standard (IS) and buffered with 1 mL of 5 mM ammonium acetate. The mixture was then extracted with 3 mL of toluene. After separation and evaporation of the organic phase to dryness using nitrogen at 40 degrees C, the residue was reconstituted in the mobile phase and 25 microL of the sample were injected onto a Hypersil C(18) column (2 x 50 mm; 3 microm) at a flow rate of 0.5 mL/min. The mobile phase was consisted of two solvent mixtures (A and B). Solvent A was composed of 5 mM ammonium acetate and 0.1% triethylamine in 75:25 v/v water:methanol, pH adjusted to 5.5 with glacial acetic acid, and solvent B was 5 mM ammonium acetate in methanol. A linear gradient system was used to elute the analytes. The mass spectrometer was programmed to admit the de-protonated molecules at m/z 352.7 (IS) and m/z 357.9 (BMS-204352). Standard curves of BMS-204352 were linear (r(2) > or = 0.998) over the concentration range of 0.5-1000 ng/mL. The mean predicted quality control (QC) concentrations deviated less than 5.1% from the corresponding nominal values (ie 4, 80, 400 and 2000 ng/mL); the within- and between-assay precision of the assay were within 5.5% relative standard deviation. Stability of BMS-204352 was confirmed after at least three freeze/thaw cycles and BMS-204532 was stable in dog plasma when stored frozen at or below -20 degrees C for at least 16 weeks in spiked QC samples and for at least 4 1/2 weeks for in vivo study samples. BMS-204352 and IS were stable in the injection solvent at room temperature for at least 24 h. The assay was applied to delineate the pharmacokinetic disposition of BMS-204352 in dogs following a single intravenous dose administration. In conclusion, the assay is accurate, precise, specific, sensitive and

  2. Mass-spectrometric identification of a novel angiotensin peptide in human plasma

    DEFF Research Database (Denmark)

    Jankowski, Vera; Vanholder, Raymond; van der Giet, Markus

    2007-01-01

    Angiotensin peptides play a central role in cardiovascular physiology and pathology. Among these peptides, angiotensin II (Ang II) has been investigated most intensively. However, further angiotensin peptides such as Ang 1-7, Ang III, and Ang IV also contribute to vascular regulation, and may eli...... elicit additional, different, or even opposite effects to Ang II. Here, we describe a novel Ang II-related, strong vasoconstrictive substance in plasma from healthy humans and end-stage renal failure patients....

  3. Plasma dark matter direct detection

    Energy Technology Data Exchange (ETDEWEB)

    Clarke, J.D.; Foot, R., E-mail: j.clarke5@pgrad.unimelb.edu.au, E-mail: rfoot@unimelb.edu.au [ARC Centre of Excellence for Particle Physics at the Terascale, School of Physics, University of Melbourne, Victoria 3010 Australia (Australia)

    2016-01-01

    Dark matter in spiral galaxies like the Milky Way may take the form of a dark plasma. Hidden sector dark matter charged under an unbroken U(1)' gauge interaction provides a simple and well defined particle physics model realising this possibility. The assumed U(1)' neutrality of the Universe then implies (at least) two oppositely charged dark matter components with self-interactions mediated via a massless 'dark photon' (the U(1)' gauge boson). In addition to nuclear recoils such dark matter can give rise to keV electron recoils in direct detection experiments. In this context, the detailed physical properties of the dark matter plasma interacting with the Earth is required. This is a complex system, which is here modelled as a fluid governed by the magnetohydrodynamic equations. These equations are numerically solved for some illustrative examples, and implications for direct detection experiments discussed. In particular, the analysis presented here leaves open the intriguing possibility that the DAMA annual modulation signal is due primarily to electron recoils (or even a combination of electron recoils and nuclear recoils). The importance of diurnal modulation (in addition to annual modulation) as a means of probing this kind of dark matter is also emphasised.

  4. Increased Protein Structural Resolution from Diethylpyrocarbonate-based Covalent Labeling and Mass Spectrometric Detection

    Science.gov (United States)

    Zhou, Yuping; Vachet, Richard W.

    2012-04-01

    Covalent labeling and mass spectrometry are seeing increased use together as a way to obtain insight into the 3-dimensional structure of proteins and protein complexes. Several amino acid specific (e.g., diethylpyrocarbonate) and non-specific (e.g., hydroxyl radicals) labeling reagents are available for this purpose. Diethylpyrocarbonate (DEPC) is a promising labeling reagent because it can potentially probe up to 30% of the residues in the average protein and gives only one reaction product, thereby facilitating mass spectrometric analysis. It was recently reported, though, that DEPC modifications are labile for some amino acids. Here, we show that label loss is more significant and widespread than previously thought, especially for Ser, Thr, Tyr, and His residues, when relatively long protein digestion times are used. Such label loss ultimately decreases the amount of protein structural information that is obtainable with this reagent. We find, however, that the number of DEPC modified residues and, thus, protein structural information, can be significantly increased by decreasing the time between the covalent labeling reaction and the mass spectrometric analysis. This is most effectively accomplished using short (e.g., 2 h) proteolytic digestions with enzymes such as immobilized chymotrypsin or Glu-C rather than using methods (e.g., microwave or ultrasonic irradiation) that accelerate proteolysis in other ways. Using short digestion times, we show that the percentage of solvent accessible residues that can be modified by DEPC increases from 44% to 67% for cytochrome c, 35% to 81% for myoglobin, and 76% to 95% for β-2-microglobulin. In effect, these increased numbers of modified residues improve the protein structural resolution available from this covalent labeling method. Compared with typical overnight digestion conditions, the short digestion times decrease the average distance between modified residues from 11 to 7 Å for myoglobin, 13 to 10 Å for

  5. Mass spectrometric identification of diagnostic markers for chronic prostatitis in seminal plasma by analysis of seminal plasma protein clinical samples.

    Science.gov (United States)

    Rokka, A; Mehik, A; Tonttila, P; Vaarala, M

    2017-08-15

    There are few specific diagnostic markers for chronic prostatitis. Therefore, we used mass spectrometry to evaluate differences in seminal plasma protein expression among patients with prostatitis and young and middle-aged healthy controls. We analysed pooled seminal plasma protein samples from four prostatitis patients (two pools), three young controls (one pool), and three middle-aged controls (one pool). The samples were analysed by liquid chromatography-tandem mass spectrometry. Of the 349 proteins identified, 16 were differentially expressed between the two control pools. Five proteins were up- or down-regulated in both of the prostatitis pools compared to middle-aged controls but not between young and middle-aged pools. Progestagen-associated endometrial protein (PAEP) was over-expressed in prostatitis samples compared to young and middle-aged controls. Our findings and those of previous studies indicate that PAEP is a potential seminal plasma marker for chronic prostatitis. In conclusion, we found age-related changes in seminal plasma protein expression. PAEP expression in seminal plasma should be investigated further to evaluate its potential as a diagnostic marker for chronic prostatitis.

  6. Inductively coupled plasma atomic emission spectrometric determination of tin in canned food.

    Science.gov (United States)

    Sumitani, H; Suekane, S; Nakatani, A; Tatsuka, K

    1993-01-01

    Various canned foods were digested sequentially with HNO3 and HCl, diluted to 100 mL, and filtered, and then tin was determined by inductively coupled plasma atomic emission spectrometry (ICP/AES). Samples of canned Satsuma mandarin, peach, apricot, pineapple, apple juice, mushroom, asparagus, evaporated milk, short-necked clam, spinach, whole tomato, meat, and salmon were evaluated. Sample preparations did not require time-consuming dilutions, because ICP/AES has wide dynamic range. The standard addition method was used to determine tin concentration. Accuracy of the method was tested by analyzing analytical standards containing tin at 2 levels (50 and 250 micrograms/g). The amounts of tin found for the 50 and 250 micrograms/g levels were 50.5 and 256 micrograms/g, respectively, and the repeatability coefficients of variation were 4.0 and 3.8%, respectively. Recovery of tin from 13 canned foods spiked at 2 levels (50 and 250 micrograms/g) ranged from 93.9 to 109.4%, with a mean of 99.2%. The quantitation limit for tin standard solution was about 0.5 microgram/g.

  7. A new ultrafast and high-throughput mass spectrometric approach for the therapeutic drug monitoring of the multi-targeted anti-folate pemetrexed in plasma from lung cancer patients

    NARCIS (Netherlands)

    R.J.W. Meesters (Roland); R. Cornelissen (Robin); R.J. van Klaveren (Rob); R. de Jonge (Robert); E. den Boer (Ethan); J. Lindemans (Jan); T.M. Luider (Theo)

    2010-01-01

    textabstractAn analytical assay has been developed and validated for ultrafast and high-throughput mass spectrometric determination of pemetrexed concentrations in plasma using matrix assisted laser desorption/ionization-triple quadrupole-tandem mass spectrometry. Patient plasma samples spiked with

  8. Mass spectrometric quantification of glucosylsphingosine in plasma and urine of type 1 Gaucher patients using an isotope standard.

    Science.gov (United States)

    Mirzaian, Mina; Wisse, Patrick; Ferraz, Maria J; Gold, Henrik; Donker-Koopman, Wilma E; Verhoek, Marri; Overkleeft, Herman S; Boot, Rolf G; Kramer, Gertjan; Dekker, Nick; Aerts, Johannes M F G

    2015-04-01

    Deficiency of glucocerebrosidase (GBA) leads to Gaucher disease (GD), an inherited disorder characterised by storage of glucosylceramide (GlcCer) in lysosomes of tissue macrophages. Recently, we reported marked increases of deacylated GlcCer, named glucosylsphingosine (GlcSph), in plasma of GD patients. To improve quantification, [5-9] (13)C5-GlcSph was synthesised for use as internal standard with quantitative LC-ESI-MS/MS. The method was validated using plasma of 55 GD patients and 20 controls. Intra-assay variation was 1.8% and inter-assay variation was 4.9% for GlcSph (m/z 462.3). Plasma GlcSph levels with the old and new methods closely correlate (r=0.968, slope=1.038). Next, we analysed GlcSph in 24h urine samples of 30 GD patients prior to therapy. GlcSph was detected in the patient samples (median 1.20nM, range 0.11-8.92nM), but was below the limit of quantification in normal urine. Enzyme replacement therapy led to a decrease of urinary GlcSph of GD patients, coinciding with reductions in plasma GlcSph and markers of Gaucher cells (chitotriosidase and CCL18). In analogy to globotriaosylsphingsone in urine of Fabry disease patients, additional isoforms of GlcSph differing in structure of the sphingosine moiety were identified in GD urine samples. In conclusion, GlcSph can be sensitively detected by LC-ESI-MS/MS with an internal isotope standard. Abnormalities in urinary GlcSph are a hallmark of Gaucher disease allowing biochemical confirmation of diagnosis. Copyright © 2015. Published by Elsevier Inc.

  9. A sensitive mass spectrometric method for hypothesis-driven detection of peptide post-translational modifications: multiple reaction monitoring-initiated detection and sequencing (MIDAS).

    Science.gov (United States)

    Unwin, Richard D; Griffiths, John R; Whetton, Anthony D

    2009-01-01

    The application of a targeted mass spectrometric workflow to the sensitive identification of post-translational modifications is described. This protocol employs multiple reaction monitoring (MRM) to search for all putative peptides specifically modified in a target protein. Positive MRMs trigger an MS/MS experiment to confirm the nature and site of the modification. This approach, termed MIDAS (MRM-initiated detection and sequencing), is more sensitive than approaches using neutral loss scanning or precursor ion scanning methodologies, due to a more efficient use of duty cycle along with a decreased background signal associated with MRM. We describe the use of MIDAS for the identification of phosphorylation, with a typical experiment taking just a couple of hours from obtaining a peptide sample. With minor modifications, the MIDAS method can be applied to other protein modifications or unmodified peptides can be used as a MIDAS target.

  10. A Mass Spectrometric Analysis Method Based on PPCA and SVM for Early Detection of Ovarian Cancer.

    Science.gov (United States)

    Wu, Jiang; Ji, Yanju; Zhao, Ling; Ji, Mengying; Ye, Zhuang; Li, Suyi

    2016-01-01

    Background. Surfaced-enhanced laser desorption-ionization-time of flight mass spectrometry (SELDI-TOF-MS) technology plays an important role in the early diagnosis of ovarian cancer. However, the raw MS data is highly dimensional and redundant. Therefore, it is necessary to study rapid and accurate detection methods from the massive MS data. Methods. The clinical data set used in the experiments for early cancer detection consisted of 216 SELDI-TOF-MS samples. An MS analysis method based on probabilistic principal components analysis (PPCA) and support vector machine (SVM) was proposed and applied to the ovarian cancer early classification in the data set. Additionally, by the same data set, we also established a traditional PCA-SVM model. Finally we compared the two models in detection accuracy, specificity, and sensitivity. Results. Using independent training and testing experiments 10 times to evaluate the ovarian cancer detection models, the average prediction accuracy, sensitivity, and specificity of the PCA-SVM model were 83.34%, 82.70%, and 83.88%, respectively. In contrast, those of the PPCA-SVM model were 90.80%, 92.98%, and 88.97%, respectively. Conclusions. The PPCA-SVM model had better detection performance. And the model combined with the SELDI-TOF-MS technology had a prospect in early clinical detection and diagnosis of ovarian cancer.

  11. Characterization of a microwave microstrip helium plasma with gas-phase sample introduction for the optical emission spectrometric determination of bromine, chlorine, sulfur and carbon using a miniaturized optical fiber spectrometer

    International Nuclear Information System (INIS)

    Pohl, Pawel; Zapata, Israel Jimenez; Amberger, Martin A.; Bings, Nicolas H.; Broekaert, Jose A.C.

    2008-01-01

    Continuous flow generation of Br 2 , Cl 2 and H 2 S coupled to a low-power 2.45 GHz microwave microstrip He plasma exiting from a capillary gas channel in a micro-fabricated sapphire wafer with microstrip lines has been used for the optical emission spectrometric determination of Br, Cl and S using a miniaturized optical fiber CCD spectrometer. Under optimized conditions, detection limits (3σ) of 330, 190 and 220 μg l -1 for Br, Cl and S, respectively, under the use of the Br II 478.5 nm, Cl I 439.0 nm and S I 469.0 nm lines were obtained and the calibration curves were found to be linear over 2 orders of magnitude. In addition, when introducing CO 2 and using the rotational line of the CN molecular band at 385.7 nm the detection limit for C was 4.6 μg l -1 . The procedure developed was found to be free from interferences from a number of metal cations and non-metal anions. Only the presence of CO 3 2- and CN - was found to cause severe spectral interferences as strong CN and C 2 molecular bands occurred as a result of an introduction of co-generated CO 2 and HCN into the plasma. With the procedure described Br, Cl and S could be determined at a concentration level of 10-30 mg l -1 with accuracy and precision better than 2%

  12. Mass Spectrometric Detection of Botulinum Neurotoxin by Measuring its Activity in Serum and Milk

    Science.gov (United States)

    Kalb, Suzanne R.; Pirkle, James L.; Barr, John R.

    Botulinum neurotoxins (BoNTs) are bacterial protein toxins which are considered likely agents for bioterrorism due to their extreme toxicity and high availability. A new mass spectrometry based assay called Endopep MS detects and defines the toxin serotype in clinical and food matrices via toxin activity upon a peptide substrate which mimics the toxin's natural target. Furthermore, the subtype of the toxin is differentiated by employing mass spectrometry based proteomic techniques on the same sample. The Endopep-MS assay selectively detects active BoNT and defines the serotype faster and with sensitivity greater than the mouse bioassay. One 96-well plate can be analyzed in under 7 h. On higher level or "hot" samples, the subtype can then be differentiated in less than 2 h with no need for DNA.

  13. A small azide-modified thiazole-based reporter molecule for fluorescence and mass spectrometric detection

    Directory of Open Access Journals (Sweden)

    Stefanie Wolfram

    2014-10-01

    Full Text Available Molecular probes are widely used tools in chemical biology that allow tracing of bioactive metabolites and selective labeling of proteins and other biomacromolecules. A common structural motif for such probes consists of a reporter that can be attached by copper(I-catalyzed 1,2,3-triazole formation between terminal alkynes and azides to a reactive headgroup. Here we introduce the synthesis and application of the new thiazole-based, azide-tagged reporter 4-(3-azidopropoxy-5-(4-bromophenyl-2-(pyridin-2-ylthiazole for fluorescence, UV and mass spectrometry (MS detection. This small fluorescent reporter bears a bromine functionalization facilitating the automated data mining of electrospray ionization MS runs by monitoring for its characteristic isotope signature. We demonstrate the universal utility of the reporter for the detection of an alkyne-modified small molecule by LC–MS and for the visualization of a model protein by in-gel fluorescence. The novel probe advantageously compares with commercially available azide-modified fluorophores and a brominated one. The ease of synthesis, small size, stability, and the universal detection possibilities make it an ideal reporter for activity-based protein profiling and functional metabolic profiling.

  14. Determination of trace elements in Egyptian cane sugar (Deshna Factories) by neutron activation, atomic absorption spectrophotometric and inductively coupled plasma-atomic emission spectrometric analysis

    International Nuclear Information System (INIS)

    Awadallah, R.M.; Sherif, M.K.; Mohamed, A.E.; Grass, F.

    1986-01-01

    Multielement instrumental neutron activation (INAA), inductively coupled plasma-atomic emission spectrometric (ICP-AES) and atomic absorption spectrophotometric (AAS) analyses were utilized for the determination of Ag, Al, As, Au, Ba, Be, Br, Ca, Cd, Ce, Cl, Co, Cr, Cu, Eu, Fe, Ga, Hf, K, La, Li, Lu, Mg, Mn, Na, Nb, Ni, P, Pb, Sb, Sc, Se, Sm, Sn, Sr, Ta, Th, Ti, U, V, W and Zn in sugar cane plant, raw juice, juice in different stages, syrup, deposits, molasses, A, B and C sugar, refinery 1 and 2 sugar, and in soil samples picked up from the immediate vicinity of the cane plant roots at surface, 30 and 60 cm depth, respectively. (author)

  15. Simulation for photon detection in spectrometric system of high purity (HPGe) using MCNPX code

    International Nuclear Information System (INIS)

    Correa, Guilherme Jorge de Souza

    2013-01-01

    The Brazilian National Commission of Nuclear Energy defines parameters for classification and management of radioactive waste in accordance with the activity of materials. The efficiency of a detection system is crucial to determine the real activity of a radioactive source. When it's possible, the system's calibration should be performed using a standard source. Unfortunately, there are only a few cases that it can be done this way, considering the difficulty of obtaining appropriate standard sources for each type of measurement. So, computer simulations can be performed to assist in calculating of the efficiency of the system and, consequently, also auxiliary the classification of radioactive waste. This study aims to model a high purity germanium (HPGe) detector with MCNPX code, approaching the spectral values computationally obtained of the values experimentally obtained for the photopeak of 137 Cs. The approach will be made through changes in outer dead layer of the germanium crystal modeled. (author)

  16. Towards an automatic lab-on-valve-ion mobility spectrometric system for detection of cocaine abuse.

    Science.gov (United States)

    Cocovi-Solberg, David J; Esteve-Turrillas, Francesc A; Armenta, Sergio; de la Guardia, Miguel; Miró, Manuel

    2017-08-25

    A lab-on-valve miniaturized system integrating on-line disposable micro-solid phase extraction has been interfaced with ion mobility spectrometry for the accurate and sensitive determination of cocaine and ecgonine methyl ester in oral fluids. The method is based on the automatic loading of 500μL of oral fluid along with the retention of target analytes and matrix clean-up by mixed-mode cationic/reversed-phase solid phase beads, followed by elution with 100μL of 2-propanol containing (3% v/v) ammonia, which are online injected into the IMS. The sorptive particles are automatically discarded after every individual assay inasmuch as the sorptive capacity of the sorbent material is proven to be dramatically deteriorated with reuse. The method provided a limit of detection of 0.3 and 0.14μgL -1 for cocaine and ecgonine methyl ester, respectively, with relative standard deviation values from 8 till 14% with a total analysis time per sample of 7.5min. Method trueness was evaluated by analyzing oral fluid samples spiked with cocaine at different concentration levels (1, 5 and 25μgL -1 ) affording relative recoveries within the range of 85±24%. Fifteen saliva samples were collected from volunteers and analysed following the proposed automatic procedure, showing a 40% cocaine occurrence with concentrations ranging from 1.3 to 97μgL -1 . Field saliva samples were also analysed by reference methods based on lateral flow immunoassay and gas chromatography-mass spectrometry. The application of this procedure to the control of oral fluids of cocaine consumers represents a step forward towards the development of a point-of-care cocaine abuse sensing system. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Quantitative analysis of flavonols, flavones, and flavanones in fruits, vegetables and beverages by high-performance liquid chromatography with photo-diode array and mass spectrometric detection

    DEFF Research Database (Denmark)

    Justesen, U.; Knuthsen, Pia; Leth, Torben

    1998-01-01

    after acid hydrolysis of freeze-dried food material. Identification was based on retention time, UV and mass spectra by comparison with commercial standards, and the UV peak areas were used for quantitation of the flavonoid contents. Examples of HPLC-MS analyses of orange pulp, tomato, and apple......A high-performance liquid chromatographic (HPLC) separation method viith photo-diode array (PDA) and mass spectrometric (MS) detection was developed to determine and quantify flavonols, flavones, and flavanones in fruits, vegetables and beverages. The compounds were analysed as aglycones, obtained...

  18. The composition of bile acids in patients with cholelithiasis according to the data of liquid chromatography with mass spectrometric detection

    Directory of Open Access Journals (Sweden)

    V. M. Klymenko

    2017-12-01

    Full Text Available Bile acids play a leading role in the physical and colloidal properties of bile stabilization. Lack of bile acids consequences result in the formation of cholesterol stones in the gall bladder, diarrhea and steatorrhea, fat-soluble vitamins impaired absorption, and kidney stones formation (oxalates. Investigation of altered bile composition, especially the content of bile acids, in patients with gallstone disease by means of modern analytical analysis methods (liquid chromatography with mass spectrometric detection would complement the modern ideas about mechanisms of lithogenesis and aim efforts at prevention of stone formation in the gall bladder, that was the purpose of our work. Materials and methods. Bile samples were tested for bile acid content using liquid chromatography with mass spectrometry. 14 samples of bile from patients with cholelithiasis were included in the main group, and control group consisted of 7 bile samples from practically healthy persons. Results. In patients with cholelithiasis there is an increase in the content of conjugated forms of bile acids – glycolic acid in 2 times (p = 0.002, taurocholic acid in 1.57 times (p = 0.062 compared with practically healthy persons. In patients with cholelithiasis, the ratio of taurocholic to glycolic acidі content (0.95 vs. 1.27, p = 0.0179, as well as glycogenodeoxycholic to glycodeoxycholic acid (1.11 vs. 1.58, p = 0.027 is significantly less than that in practically healthy persons. In addition, one in two patients with cholelithiasis does not reveal the presence of ursodeoxycholic acid in the bile. Conclusions. The lithogenic properties of bile are primarily caused by conjugated forms of cholic acid with glycine and taurine content violation. The ratio of taurocholic to glycolic acid content in patients with cholelithiasis is significantly lower than the similar index in practically healthy persons (0.95 vs. 1.27, p = 0.0179. The ratio of glycine conjugated bile acids

  19. Rapid dating of recent sediments in Loch Ness. Inductively coupled plasma mass spectrometric measurements of global fallout plutonium

    International Nuclear Information System (INIS)

    Ketterer, Michael E.; Hafer, Kevin M.; Jones, Vivienne J.; Appleby, Peter G.

    2004-01-01

    The 239+240 Pu activity profile is determined for a sediment core collected from 170-m depth at Loch Ness, Scotland. These measurements use magnetic sector inductively coupled plasma mass spectrometry for rapid determination of Pu activities and 240 Pu/ 239 Pu atom ratios. A 239+240 Pu detection limit of 0.1 Bq/kg is obtained for 2 g of acid-leached sediment; 242 Pu is used as a spike isotope. The Pu activity profile exhibits a maximum of 42.7±0.3 Bq/kg 239+240 Pu in the 9-10-cm depth interval. The position of this maximum coincides with peaks in the 241 Am and 137 Cs activity profiles. These peak activities are ascribed to the 1963/1964 peak fallout from atmospheric testing of nuclear weapons. The 240 Pu/ 239 Pu atom ratios are in the range 0.15-0.20, in agreement with the expected range of 0.166-0.194 for Northern Hemisphere fallout, and do not suggest the presence of other contributing sources. This study demonstrates that ICPMS has considerable potential for rapid determination of the chronology of post-1950 sediments, and also for validating 210 Pb dates where chronologies over longer time-scales are needed

  20. Rapid dating of recent sediments in Loch Ness. Inductively coupled plasma mass spectrometric measurements of global fallout plutonium

    Energy Technology Data Exchange (ETDEWEB)

    Ketterer, Michael E.; Hafer, Kevin M. [Department of Chemistry, Northern Arizona University, Flagstaff, AZ 86011-5698 (United States); Jones, Vivienne J. [Environmental Change Research Centre, University College London, 26 Bedford Way, London WC1H 0AP (United Kingdom); Appleby, Peter G. [Department of Mathematical Sciences, University of Liverpool, P.O. Box 147, Liverpool L69 3BX (United Kingdom)

    2004-04-25

    The {sup 239+240}Pu activity profile is determined for a sediment core collected from 170-m depth at Loch Ness, Scotland. These measurements use magnetic sector inductively coupled plasma mass spectrometry for rapid determination of Pu activities and {sup 240}Pu/{sup 239}Pu atom ratios. A {sup 239+240}Pu detection limit of 0.1 Bq/kg is obtained for 2 g of acid-leached sediment; {sup 242}Pu is used as a spike isotope. The Pu activity profile exhibits a maximum of 42.7{+-}0.3 Bq/kg {sup 239+240}Pu in the 9-10-cm depth interval. The position of this maximum coincides with peaks in the {sup 241}Am and {sup 137}Cs activity profiles. These peak activities are ascribed to the 1963/1964 peak fallout from atmospheric testing of nuclear weapons. The {sup 240}Pu/{sup 239}Pu atom ratios are in the range 0.15-0.20, in agreement with the expected range of 0.166-0.194 for Northern Hemisphere fallout, and do not suggest the presence of other contributing sources. This study demonstrates that ICPMS has considerable potential for rapid determination of the chronology of post-1950 sediments, and also for validating {sup 210}Pb dates where chronologies over longer time-scales are needed.

  1. APPLICATION OF THE SPECTROMETRIC METHOD FOR CALCULATING THE DOSE RATE FOR CREATING CALIBRATION HIGHLY SENSITIVE INSTRUMENTS BASED ON SCINTILLATION DETECTION UNITS

    Directory of Open Access Journals (Sweden)

    R. V. Lukashevich

    2017-01-01

    Full Text Available Devices based on scintillation detector are highly sensitive to photon radiation and are widely used to measure the environment dose rate. Modernization of the measuring path to minimize the error in measuring the response of the detector to gamma radiation has already reached its technological ceiling and does not give the proper effect. More promising for this purpose are new methods of processing the obtained spectrometric information. The purpose of this work is the development of highly sensitive instruments based on scintillation detection units using a spectrometric method for calculating dose rate.In this paper we consider the spectrometric method of dosimetry of gamma radiation based on the transformation of the measured instrumental spectrum. Using predetermined or measured functions of the detector response to the action of gamma radiation of a given energy and flux density, a certain function of the energy G(E is determined. Using this function as the core of the integral transformation from the field to dose characteristic, it is possible to obtain the dose value directly from the current instrumentation spectrum. Applying the function G(E to the energy distribution of the fluence of photon radiation in the environment, the total dose rate can be determined without information on the distribution of radioisotopes in the environment.To determine G(E by Monte-Carlo method instrumental response function of the scintillator detector to monoenergetic photon radiation sources as well as other characteristics are calculated. Then the whole full-scale energy range is divided into energy ranges for which the function G(E is calculated using a linear interpolation.Spectrometric method for dose calculation using the function G(E, which allows the use of scintillation detection units for a wide range of dosimetry applications is considered in the article. As well as describes the method of calculating this function by using Monte-Carlo methods

  2. Separation of gold, palladium and platinum in chromite by anion exchange chromatography for inductively coupled plasma atomic emission spectrometric analysis

    International Nuclear Information System (INIS)

    Choi, Kwang Soon; Lee, Chang Heon; Park, Yeong Jae; Joe, Kih Soo; Kim, Won Ho

    2001-01-01

    A study has been carried out on the separation of gold, iridium, palladium, rhodium, ruthenium and platinum in chromite samples and their quantitative determination using inductively coupled plasma atomic emission spectrometry (ICP-AES). The dissolution condition of the minerals by fusion with sodium peroxide was optimized and chromatographic elution behavior of the rare metals was investigated by anion exchange chromatography. Spectral interference of chromium, a matrix of the minerals, was investigated on determination of gold. Chromium interfered on determination of gold at the concentration of 500 mg/L and higher. Gold plus trace amounts of iridium, palladium, rhodium and ruthenium, which must be preconcentrated before ICP-AES was separated by anion exchange chromatography after reducing Cr(VI) to Cr(III) by H 2 O 2 . AuCl - 4 retained on the resin column was selectively eluted with acetone- HNO 3 -H 2 O as an eluent. In addition, iridium, palladium, rhodium and ruthenium remaining on the resin column were eluted as a group with concentrated HCl. However, platinum was eluted with concentrated HNO 3 . The recovery yield of gold with acetone-HNO 3 -H 2 O was 100.7 ± 2.0 % , and the yields of palladium and platinum with concentrated HCl and HNO 3 were 96.1 ± 1.8% and 96.6 ± 1.3%, respectively. The contents of gold and platinum in a Mongolian chromite sample were 32.6 ± 2.2 μg/g and 1.6 ± 0.14 μg/g, respectively. Palladium was not detected

  3. Characterization of a microwave microstrip helium plasma with gas-phase sample introduction for the optical emission spectrometric determination of bromine, chlorine, sulfur and carbon using a miniaturized optical fiber spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Pohl, Pawel; Zapata, Israel Jimenez; Amberger, Martin A.; Bings, Nicolas H. [Universitaet Hamburg, Institut fuer Anorganische und Angewandte Chemie, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany); Broekaert, Jose A.C. [Universitaet Hamburg, Institut fuer Anorganische und Angewandte Chemie, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)], E-mail: jose.broekaert@chemie.uni-hamburg.de

    2008-03-15

    Continuous flow generation of Br{sub 2}, Cl{sub 2} and H{sub 2}S coupled to a low-power 2.45 GHz microwave microstrip He plasma exiting from a capillary gas channel in a micro-fabricated sapphire wafer with microstrip lines has been used for the optical emission spectrometric determination of Br, Cl and S using a miniaturized optical fiber CCD spectrometer. Under optimized conditions, detection limits (3{sigma}) of 330, 190 and 220 {mu}g l{sup -1} for Br, Cl and S, respectively, under the use of the Br II 478.5 nm, Cl I 439.0 nm and S I 469.0 nm lines were obtained and the calibration curves were found to be linear over 2 orders of magnitude. In addition, when introducing CO{sub 2} and using the rotational line of the CN molecular band at 385.7 nm the detection limit for C was 4.6 {mu}g l{sup -1}. The procedure developed was found to be free from interferences from a number of metal cations and non-metal anions. Only the presence of CO{sub 3}{sup 2-} and CN{sup -} was found to cause severe spectral interferences as strong CN and C{sub 2} molecular bands occurred as a result of an introduction of co-generated CO{sub 2} and HCN into the plasma. With the procedure described Br, Cl and S could be determined at a concentration level of 10-30 mg l{sup -1} with accuracy and precision better than 2%.

  4. 'Age' Determination of Irradiated Materials Utilizing Inductively Coupled Plasma Mass Spectrometric (ICP-MS) Detection

    International Nuclear Information System (INIS)

    Sommers, James; Giglio, Jeffrey J.; Cummings, Daniel; Carney, Kevin P.

    2009-01-01

    A gas pressurized extraction chromatography (GPEC) system has been developed to perform elemental separations on radioactive samples to determine total and isotopic compositions of Cs and Ba from an irradiated salt sample, fuel sample and two sealed radiation sources. The separation is necessary to remove isobaric interferences in the determination of 137Cs, 135Cs, 137Ba, 135Ba, which are used to determine the age of a sample from radioactive decay or purification. The micro-column extraction chromatography system employs compressed nitrogen to move liquid through the system, compared to gravity or pumped liquids that are typically used for separations. The use of compressed gas allows for accurate and precise recovery of all liquids put into the chromatography system, enabling very accurate dilutions. The use of a small analytical column permits the use of very small amounts of liquids to be used. As a benefit, the amount of radiological waste that is generated in the separation process is minimized. For this work, a commercially available Sr-Resin(trademark) was used to perform the separation for the above mentioned analytes. The column consists of a 7 inch piece of 1/16 in. O.D. x 0.030 in I.D. Teflon(trademark) tubing having an internal volume of 81 (micro)L. To this column, 49 mg of resin was added. The columns are re-usable after regeneration with 3 M HNO3. All samples were separated using batch collection, although real time analysis is possible with the current experimental design. A 1 % acetic acid solution was determined to be the best extractant for Ba. A flow rate of 0.1 mL/min was determined to be optimal for the separation of Ba. Complete recovery of the Cs and Ba was achieved, within the systematic error of the experiments.

  5. 'Age' determination of irradiated materials utilizing inductively coupled plasma mass spectrometric (ICP-MS) detection

    International Nuclear Information System (INIS)

    Sommers, J.; Cummings, D.; Giglio, J.; Carney, K.

    2009-01-01

    A gas pressurized extraction chromatography (GPEC) system has been developed to perform elemental separations on radioactive samples to determine total and isotopic compositions of Cs and Ba from an irradiated salt sample, fuel sample and two sealed radiation sources. The GPEC system employs compressed nitrogen to move liquid through the system, compared to gravity or pumped liquids that are typically used for separations. A commercially available Sr-Resin TM was used to perform the separation for the above mentioned analytes. A 1% acetic acid solution was determined to be the best extractant for Ba. A flow rate of 0.1 mL/min was determined to be optimal for the separation of Ba. Complete recovery of the Cs and Ba was achieved, within the systematic uncertainties of the experiments. (author)

  6. Separation of silver ions and starch modified silver nanoparticles using high performance liquid chromatography with ultraviolet and inductively coupled mass spectrometric detection

    International Nuclear Information System (INIS)

    Hanley, Traci A.; Saadawi, Ryan; Zhang, Peng; Caruso, Joseph A.; Landero-Figueroa, Julio

    2014-01-01

    The production of commercially available products marketed to contain silver nanoparticles is rapidly increasing. Species-specific toxicity is a phenomenon associated with many elements, including silver, making it imperative to develop a method to identify and quantify the various forms of silver (namely, silver ions vs. silver nanoparticles) possibly present in these products. In this study a method was developed using high performance liquid chromatography (HPLC) with ultraviolet (UV–VIS) and inductively coupled mass spectrometric (ICP-MS) detection to separate starch stabilized silver nanoparticles (AgNPs) and silver ions (Ag + ) by cation exchange chromatography with 0.5 M nitric acid mobile phase. The silver nanoparticles and ions were baseline resolved with an ICP-MS response linear over four orders of magnitude, 0.04 mg kg −1 detection limit, and 90% chromatographic recovery for silver solutions containing ions and starch stabilized silver nanoparticles smaller than 100 nm

  7. Separation of silver ions and starch modified silver nanoparticles using high performance liquid chromatography with ultraviolet and inductively coupled mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Hanley, Traci A.; Saadawi, Ryan; Zhang, Peng; Caruso, Joseph A., E-mail: joseph.caruso@uc.edu; Landero-Figueroa, Julio

    2014-10-01

    The production of commercially available products marketed to contain silver nanoparticles is rapidly increasing. Species-specific toxicity is a phenomenon associated with many elements, including silver, making it imperative to develop a method to identify and quantify the various forms of silver (namely, silver ions vs. silver nanoparticles) possibly present in these products. In this study a method was developed using high performance liquid chromatography (HPLC) with ultraviolet (UV–VIS) and inductively coupled mass spectrometric (ICP-MS) detection to separate starch stabilized silver nanoparticles (AgNPs) and silver ions (Ag{sup +}) by cation exchange chromatography with 0.5 M nitric acid mobile phase. The silver nanoparticles and ions were baseline resolved with an ICP-MS response linear over four orders of magnitude, 0.04 mg kg{sup −1} detection limit, and 90% chromatographic recovery for silver solutions containing ions and starch stabilized silver nanoparticles smaller than 100 nm.

  8. Automated sequential injection-microcolumn approach with on-line flame atomic absorption spectrometric detection for implementing metal fractionation schemes of homogeneous and non-homogeneous solid samples of environmental interest

    DEFF Research Database (Denmark)

    Chomchoei, Roongrat; Miró, Manuel; Hansen, Elo Harald

    2005-01-01

    spectrometric detection and used for the determination of Cu as a model analyte, the potentials of this novel hyphenated approach are demonstrated by the ability of handling up to 300 mg sample of a nonhomogeneous sewage amended soil (viz., CRM 483). The three steps of the endorsed Standards, Measurements...

  9. NZG 201 portable spectrometric unit

    International Nuclear Information System (INIS)

    Jursa, P.; Novakova, O.; Slezak, V.

    The NZG 201 spectrometric unit is a portable single-channel processing unit supplied from the mains or a battery which allows the qualitative and quantitative measurement of different types of ionizing radiation when connected to a suitable detection unit. The circuit layout and the choice of control elements makes the spectrometric unit suitable for use with scintillation detector units. The spectrometric unit consists of a pulse amplifier, an amplitude pulse analyzer, a pulse counter, a pulse rate counter with an output for a recorder, a high voltage source and a low voltage source. The block diagram is given. All circuits are modular and are mounted on PCB's. The apparatus is built in a steel cabinet with a raised edge which protects the control elements. The linear pulse amplifier has a maximum gain of 1024, the pulse counter has a maximum capacity of 10 6 -1 imp and time resolution better than 0.5 μs. The temperature interval at which the apparatus is operational is 0 to 45 degC, its weight is 12.5 kg and dimensions 36x280x310 mm, energy range O.025 to 2.5 MeV, for 137 Cs the energy resolution is 8 to 10%. The spectrometric unit NZG 2O1 may, with regard to its parameters, number and range of control elements, be used as a universal measuring unit. (J.P.)

  10. Visual and light scattering spectrometric method for the detection of melamine using uracil 5‧-triphosphate sodium modified gold nanoparticles

    Science.gov (United States)

    Liang, Lijiao; Zhen, Shujun; Huang, Chengzhi

    2017-02-01

    A highly selective method was presented for colorimetric determination of melamine using uracil 5‧-triphosphate sodium modified gold nanoparticles (UTP-Au NPs) in this paper. Specific hydrogen-bonding interaction between uracil base (U) and melamine resulted in the aggregation of AuNPs, displaying variations of localized surface plasmon resonance (LSPR) features such as color change from red to blue and enhanced localized surface plasmon resonance light scattering (LSPR-LS) signals. Accordingly, the concentration of melamine could be quantified based on naked eye or a spectrometric method. This method was simple, inexpensive, environmental friendly and highly selective, which has been successfully used for the detection of melamine in pretreated liquid milk products with high recoveries.

  11. Quantification of rifampicin in human plasma and cerebrospinal fluid by a highly sensitive and rapid liquid chromatographic–tandem mass spectrometric method

    OpenAIRE

    Srivastava, Abhishek; Waterhouse, David; Ardrey, Alison; Ward, Stephen A.

    2012-01-01

    A highly sensitive and rapid liquid chromatography tandem mass spectrometry (LC–MS/MS) method has been developed to measure the levels of the antitubercular drug rifampicin (RIF) in human plasma and cerebrospinal fluid (CSF). The analyte and internal standard (IS) were isolated from plasma and CSF by a simple organic solvent based precipitation of proteins followed by centrifugation. Detection was carried out by electrospray positive ionization mass spectrometry in the multiple-reaction monit...

  12. Photometric and emission-spectrometric determination of boron in steels

    International Nuclear Information System (INIS)

    Thierig, D.

    1982-01-01

    A method for the photometric determination of boron in unalloyed and alloyed steels is described, in which Curcumine is used as reagent. A separation of boron is not necessary. Limit of detection: 0.0003% B. The decomposition of boron nitride in the steel is achieved by heating the whole sample in fuming sulphuric acid/phosphoric acid. For the emission spectrometric investigation of solid steel samples and for the spectrochemical analysis of solutions with plasma excitation working parameters are given and possibilities of interferences are demonstrated. (orig.) [de

  13. Quantitative Mass spectrometric Analysis of Ropivacaine and Bupivacaine in Authentic, Pharmaceutical and Spiked Human Plasma without Chromatographic Separation

    Directory of Open Access Journals (Sweden)

    Nahla N. Salama

    2009-01-01

    Full Text Available The present study employs time of flight mass spectrometry for quantitative analysis of the local anesthetic drugs ropivacaine and bupivacaine in authentic, pharmaceutical and spiked human plasma as well as in the presence of their impurities 2,6-dimethylaniline and alkaline degradation product. The method is based on time of flight electron spray ionization mass spectrometry technique without preliminary chromatographic separation and makes use of bupivacaine as internal standard for ropivacaine, which is used as internal standard for bupivacaine. A linear relationship between drug concentrations and the peak intensity ratio of ions of the analyzed substances is established. The method is linear from 23.8 to 2380.0 ng mL-1 for both drugs. The correlation coefficient was ≥0.996 in authentic and spiked human plasma. The average percentage recoveries in the ranges of 95.39%–102.75% was obtained. The method is accurate (% RE < 5% and reproducible with intra- and inter-assay precision (RSD% < 8.0%. The quantification limit is 23.8 ng mL-1 for both drugs. The method is not only highly sensitive and selective, but also simple and effective for determination or identification of both drugs in authentic and biological fluids. The method can be applied in purity testing, quality control and stability monitoring for the studied drugs.

  14. Quantitative Mass Spectrometric Analysis of Ropivacaine and Bupivacaine in Authentic, Pharmaceutical and Spiked Human Plasma without Chromatographic Separation

    Directory of Open Access Journals (Sweden)

    Nahla N. Salama

    2009-01-01

    Full Text Available The present study employs time of flight mass spectrometry for quantitative analysis of the local anesthetic drugs ropivacaine and bupivacaine in authentic, pharmaceutical and spiked human plasma as well as in the presence of their impurities 2,6-dimethylaniline and alkaline degradation product. The method is based on time of flight electron spray ionization mass spectrometry technique without preliminary chromatographic separation and makes use of bupivacaine as internal standard for ropivacaine, which is used as internal standard for bupivacaine. A linear relationship between drug concentrations and the peak intensity ratio of ions of the analyzed substances is established. The method is linear from 23.8 to 2380.0 ng mL −1 for both drugs. The correlation coefficient was ≥0.996 in authentic and spiked human plasma. The average percentage recoveries in the ranges of 95.39%-102.75% was obtained. The method is accurate (% RE <; 5% and reproducible with intra- and inter-assay precision (RSD% <; 8.0%. The quantification limit is 23.8 ng mL −1 for both drugs. The method is not only highly sensitive and selective, but also simple and effective for determination or identification of both drugs in authentic and biological fluids. The method can be applied in purity testing, quality control and stability monitoring for the studied drugs.

  15. Direct atomic spectrometric analysis by slurry atomisation: Pt. 7. Analysis of coal using inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ebdon, Les; Foulkes, M E; Parry, H G.M.; Tye, C T

    1988-09-01

    The application of slurry atomisation - inductively coupled plasma mass spectrometry (ICP-MS) to major, minor and trace element determination in coals has been investigated. Eight certified reference material (CRM) coals have been ground by the bottle and bead method and analysed using both rapid scan semi-quantitative analysis, employing a single rhodium internal standard, and full quantitative analysis using simple aqueous standards for calibration. The semi-quantitative mode, which determines the concentration using the mass-response curve for 68 elements against the single internal standard, produced values which were within a factor of two of the certified reference value, in most instances. The full quantitative determination gave excellent agreement with the certified reference material coals for a large number of elemental constituents. The results from the determination of 16 elements of interest are discussed including the effects of polyatomic interferents and isotope sensitivity.

  16. The leakage problem in vacuum system. Realization of a mass spectrometer detecting leaks; Le probleme des fuites en technique du vide. Realisation d'un spectrometre de masse detecteur de fuite

    Energy Technology Data Exchange (ETDEWEB)

    Geller, R [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1954-11-15

    In the first part of this paper we consider the problem of leaks in vacuum systems, and their detection. We consider in particular the method of detection by means of a helium spectrometer. The second part deals with the experimental set p. The analyser and the ion source have been studied in great detail, and we have also discussed the technological and mechanical aspects of the apparatus and its performances. (author) [French] Dans la premiere partie de ce travail, nous traitons le probleme des fuites en technique du vide et leur detection en general. La methode de detection par spectrometre a helium y est envisagee plus particulierement. La deuxieme partie de l'article est consacree a la realisation du spectrometre. Le tube analyseur et la source d'ions y sont etudies en detail. Nous exposons de meme les conceptions technologiques et mecaniques de l'appareil ainsi que ses performances. (auteur)

  17. Inductively coupled plasma mass-spectrometric determination of platinum in excretion products of client-owned pet dogs.

    Science.gov (United States)

    Janssens, T; Brouwers, E E M; de Vos, J P; de Vries, N; Schellens, J H M; Beijnen, J H

    2015-06-01

    Residues of antineoplastic drugs in canine excretion products may represent exposure risks to veterinary personnel, owners of pet dogs and other animal care-takers. The aim of this study was to measure the extent and duration of platinum (Pt) excretion in pet dogs treated with carboplatin. Samples were collected before and up to 21 days after administration of carboplatin. We used validated, ultra-sensitive, inductively coupled plasma-mass spectrometry assays to measure Pt in canine urine, faeces, saliva, sebum and cerumen. Results showed that urine is the major route of elimination of Pt in dogs. In addition, excretion occurs via faeces and saliva, with the highest amounts eliminated during the first 5 days. The amount of excreted Pt decreased over time but was still quantifiable at 21 days after administration of carboplatin. In conclusion, increased Pt levels were found in all measured excretion products up to 21 days after administration of carboplatin to pet dogs, with urine as the main route of excretion. These findings may be used to further adapt current veterinary guidelines on safe handling of antineoplastic drugs and treated animals. © 2013 Blackwell Publishing Ltd.

  18. Validation and application of a liquid chromatography-electrospray ionization mass spectrometric method for determination of mazindol in human plasma and urine.

    Science.gov (United States)

    de Oliveira, Marcella Herbstrith; Ferreira, Pâmela Cristina Lukasewicz; Carlos, Graciela; Salazar, Fernanda Rodrigues; Bergold, Ana Maria; Pechansky, Flavio; Limberger, Renata Pereira; Fröehlich, Pedro Eduardo

    2016-01-01

    Even after removal of some stimulants, like fenproporex, amfepramone and mazindol, from Brazilian market, the use of these substances is still high, especially by drivers. Mazindol is the second most used anorectic agent in the world acting as an indirect sympathomimetic agonist, having stimulatory action on central nervous system. Plasma is a good matrix to monitor since it reflects the psychomotor effects of these drugs, but unlike urine has an invasive collection; drug levels and detection time are quite low. The method involved a liquid-liquid extraction of the samples and a LC-MS analysis was fully validated. Method was used to analyze samples of urine and plasma collected from health volunteers in a period of 24h. Metabolite of mazindol was synthesized using alkaline conditions. After validation the method proved to be adequate to analyze samples collected from health volunteers. Method was linear in the concentration range of 0.1-10ng/mL (r=0.9982) for plasma and 5-50ng/mL (r=0.9973) for urine. Analysis of the samples showed that mazindol can be detected after 1h of administration and that concentration levels in urine were always higher than in plasma. Mazindol metabolite was detected only in urine. Copyright © 2015 Elsevier Inc. All rights reserved.

  19. 电感耦合等离子体发射光谱法测定纯银焊丝中杂质元素%Measuring the Impurity Elements in Sterling Silver Wire by the Method of Inductively Coupled Plasma Atomic Emission Spectrometric

    Institute of Scientific and Technical Information of China (English)

    张雅丽; 李立东

    2014-01-01

    Continuous determination of impurity elements in sterling silver wire by the method of inductively coupled plasma atomic emission spectrometric has been established to discuss the analysis of the selection of spectral line, not only optimizing the analytical conditions,but also checking the limit of detection and recovery of standard addition, which can meet the requirement of industrial analysis as well as has a simple method.%研究建立了电感耦合等离子体发射光谱法对纯银焊丝中杂质元素的连续测定方法,讨论了分析谱线的选择问题,优化了分析条件,对检出限与加标回收率进行了检验,方法简便、可满足工业分析要求。

  20. Barley husk carbon as the fiber coating for the solid-phase microextraction of twelve pesticides in vegetables prior to gas chromatography-mass spectrometric detection.

    Science.gov (United States)

    Liang, Weiqian; Wang, Juntao; Zang, Xiaohuan; Dong, Wenhuan; Wang, Chun; Wang, Zhi

    2017-03-31

    In this work, a barley husk biomaterial was successfully carbonized by hydrothermal method. The carbon had a high specific surface area and good stability. It was coated onto a stainless steel wire through sol-gel technique to prepare a solid-phase microextraction fiber for the extraction of trace levels of twelve pesticides (tsumacide, fenobucarb, indoxacarb, diethofencarb, thimet, terbufos, malathion, thiamethoxam, imidacloprid, buprofezin, acetamiprid, thiamethoxam) from vegetable samples prior to gas chromatography-mass spectrometric (GC-MS) detection. The main experimental parameters that could influence the extraction efficiency such as extraction time, extraction temperature, sample pH, sample salinity, stirring rate, desorption temperature and desorption time, were investigated. Under the optimized conditions, the linearity was observed in the range of 0.2-75.0μgkg -1 for tomato samples, and 0.3-60.0μgkg -1 for cucumber samples, with the correlation coefficients (r) ranging from 0.9959 to 0.9983. The limits of detection of the method were 0.01-0.05μgkg -1 for tomato samples, and 0.03-0.10μgkg -1 for cucumber samples. The recoveries of the analytes for the method from spiked samples were in the range of 76%-104%, and the precision, expressed as the relative standard deviations, was less than 12%. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Identification of Polish cochineal (Porphyrophora polonica L.) in historical textiles by high-performance liquid chromatography coupled with spectrophotometric and tandem mass spectrometric detection.

    Science.gov (United States)

    Lech, Katarzyna; Jarosz, Maciej

    2016-05-01

    The present work reports a method for identification of Polish cochineal (Porphyrophora polonica L.) in historical fabrics by the use of high-performance liquid chromatography coupled with diode array and tandem mass spectrometric detection with electrospray ionization (HPLC-DAD-ESI MS/MS). This hyphened technique allows detection and identification of 16 new minor colorants present in the discussed scale insect (including two previously observed by Wouters and Verhecken (Ann Soc Entomol Fr. 1989;25:393-410), but specified only as compounds of unknown structures) that do not occur (e.g., in American cochineal). The MS/MS experiments, complemented with UV-VIS data, enable identification of mono- and di-, C- and O-hexosides of kermesic and flavokermesic acids or their derivatives. The present paper introduces a fingerprint of color compounds present in Polish cochineal and defines them, particularly pp6 (ppI, O-hexoside of flavokermesic acid), as its markers allow distinguishing of Polish-cochineal reds from the American ones. Usefulness of the selected set of markers for identification of Polish cochineal has been demonstrated in the examination of textiles from the collection of the National Museum in Warsaw using the multiple reaction monitoring (MRM) method, originally elaborated on the basis of this study.

  2. Quantification of rifampicin in human plasma and cerebrospinal fluid by a highly sensitive and rapid liquid chromatographic-tandem mass spectrometric method.

    Science.gov (United States)

    Srivastava, Abhishek; Waterhouse, David; Ardrey, Alison; Ward, Stephen A

    2012-11-01

    A highly sensitive and rapid liquid chromatography tandem mass spectrometry (LC-MS/MS) method has been developed to measure the levels of the antitubercular drug rifampicin (RIF) in human plasma and cerebrospinal fluid (CSF). The analyte and internal standard (IS) were isolated from plasma and CSF by a simple organic solvent based precipitation of proteins followed by centrifugation. Detection was carried out by electrospray positive ionization mass spectrometry in the multiple-reaction monitoring (MRM) mode. The assay was linear in the concentration range 25-6400 ng/mL with intra- and inter-day precision of <7% and <8%, respectively. The validated method was applied to the study of RIF pharmacokinetics in human CSF and plasma over 25 h period after a 10 mg/kg oral dose. Copyright © 2012 Elsevier B.V. All rights reserved.

  3. Spectrometric techniques 4

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume IV discusses three widely diversified areas of spectrometric techniques. The book focuses on three spectrometric methods. Chapter 1 discusses the phenomenology and applications of Coherent Anti-Stokes Raman Spectroscopy (CARS), the most commonly used optical technique that exploit the Raman effect. The second chapter is concerned with diffraction gratings and mountings for the Vacuum Ultraviolet Spectral Region. Chapter 3 accounts the uses of mass spectrometry, detectors, types of spectrometers, and ion sources. Physicists and chemists will find the book a go

  4. Optical emission spectrometric determination of arsenic and antimony by continuous flow chemical hydride generation and a miniaturized microwave microstrip argon plasma operated inside a capillary channel in a sapphire wafer

    International Nuclear Information System (INIS)

    Pohl, Pawel; Zapata, Israel Jimenez; Bings, Nicolas H.; Voges, Edgar; Broekaert, Jose A.C.

    2007-01-01

    Continuous flow chemical hydride generation coupled directly to a 40 W, atmospheric pressure, 2.45 GHz microwave microstrip Ar plasma operated inside a capillary channel in a sapphire wafer has been optimized for the emission spectrometric determination of As and Sb. The effect of the NaBH 4 concentration, the concentration of HCl, HNO 3 and H 2 SO 4 used for sample acidification, the Ar flow rate, the reagent flow rates, the liquid volume in the separator as well as the presence of interfering metals such as Fe, Cu, Ni, Co, Zn, Cd, Mn, Pb and Cr, was investigated in detail. A considerable influence of Fe(III) (enhancement of up to 50 %) for As(V) and of Fe(III), Cu(II) and Cr(III) (suppression of up to 75%) as well as of Cd(II) and Mn(II) (suppression by up to 25%) for Sb(III) was found to occur, which did not change by more than a factor of 2 in the concentration range of 2-20 μg ml -1 . The microstrip plasma tolerated the introduction of 4.2 ml min -1 of H 2 in the Ar working gas, which corresponded to an H 2 /Ar ratio of 28%. Under these conditions, the excitation temperature as measured with Ar atom lines and the electron number density as determined from the Stark broadening of the H β line was of the order of 5500 K and 1.50 . 10 14 cm -3 , respectively. Detection limits (3σ) of 18 ng ml -1 for As and 31 ng ml -1 for Sb were found and the calibration curves were linear over 2 orders of magnitude. With the procedure developed As and Sb could be determined at the 45 and 6.4 μg ml -1 level in a galvanic bath solution containing 2.5% of NiSO 4 . Additionally, As was determined in a coal fly ash reference material (NIST SRM 1633a) with a certified concentration of As of 145 ± 15 μg g -1 and a value of 144 ± 4 μg g -1 was found

  5. Quantitative determination of plant phenolics in Urtica dioica extracts by high-performance liquid chromatography coupled with tandem mass spectrometric detection.

    Science.gov (United States)

    Orčić, Dejan; Francišković, Marina; Bekvalac, Kristina; Svirčev, Emilija; Beara, Ivana; Lesjak, Marija; Mimica-Dukić, Neda

    2014-01-15

    A method for quantification of 45 plant phenolics (including benzoic acids, cinnamic acids, flavonoid aglycones, C- and O-glycosides, coumarins, and lignans) in plant extracts was developed, based on reversed phase HPLC separation of extract components, followed by tandem mass spectrometric detection. The phenolic profile of 80% MeOH extracts of the stinging nettle (Urtica dioica L.) herb, root, stem, leaf and inflorescence was obtained by using this method. Twenty-one of the investigated compounds were present at levels above the reliable quantification limit, with 5-O-caffeoylquinic acid, rutin and isoquercitrin as the most abundant. The inflorescence extracts were by far the richest in phenolics, with the investigated compounds amounting 2.5-5.1% by weight. As opposed to this, the root extracts were poor in phenolics, with only several acids and derivatives being present in significant amounts. The results obtained by the developed method represent the most detailed U. dioica chemical profile so far. Copyright © 2013 Elsevier Ltd. All rights reserved.

  6. Determination of Triazine Herbicides in Drinking Water by Dispersive Micro Solid Phase Extraction with Ultrahigh-Performance Liquid Chromatography-High-Resolution Mass Spectrometric Detection.

    Science.gov (United States)

    Chen, Dawei; Zhang, Yiping; Miao, Hong; Zhao, Yunfeng; Wu, Yongning

    2015-11-11

    A novel dispersive micro solid phase extraction (DMSPE) method based on a polymer cation exchange material (PCX) was applied to the simultaneous determination of the 30 triazine herbicides in drinking water with ultrahigh-performance liquid chromatography-high-resolution mass spectrometric detection. Drinking water samples were acidified with formic acid, and then triazines were adsorbed by the PCX sorbent. Subsequently, the analytes were eluted with ammonium hydroxide/acetonitrile. The chromatographic separation was performed on an HSS T3 column using water (4 mM ammonium formate and 0.1% formic acid) and acetonitrile (0.1% formic acid) as the mobile phase. The method achieved LODs of 0.2-30.0 ng/L for the 30 triazines, with recoveries in the range of 70.5-112.1%, and the precision of the method was better than 12.7%. These results indicated that the proposed method had the advantages of convenience and high efficiency when applied to the analysis of the 30 triazines in drinking water.

  7. Analysis of phenolic compounds from different morphological parts of Helichrysum devium by liquid chromatography with on-line UV and electrospray ionization mass spectrometric detection.

    Science.gov (United States)

    Gouveia, Sandra C; Castilho, Paula C

    2009-12-01

    A simple and rapid method has been used for the screening and identification of the main phenolic compounds from Helichrysum devium using high-performance liquid chromatography with on-line UV and electrospray ionization mass spectrometric detection (LC-DAD/ESI-MS(n)). The total aerial parts and different morphological parts of the plant, namely leaves, flowers and stems, were analyzed separately. A total of 34 compounds present in the methanolic extract from Helichrysum devium were identified or tentatively characterized based on their UV and mass spectra and retention times. Three of these compounds were positively identified by comparison with reference standards. The phenolic compounds included derivatives of quinic acid, O-glycosylated flavonoids, a caffeic acid derivative and a protocatechuic acid derivative. The characteristic loss of 206 Da from malonylcaffeoyl quinic acid was used to confirm the malonyl linkage to the caffeoyl group. This contribution presents one of the first reports on the analysis of phenolic compounds from Helichrysum devium using LC-DAD/ESI-MS(n) and highlights the prominence of quinic acid derivatives as the main group of phenolic compounds present in these extracts. We also provide evidence that the methanolic extract from the flowers was significantly more complex when compared to that of other morphological parts. Copyright 2009 John Wiley & Sons, Ltd.

  8. Detection of tokamak plasma positrons using annihilation photons

    Energy Technology Data Exchange (ETDEWEB)

    Guanying, Yu; Liu, Jian; Xie, Jinlin [University of Science and Technology, Hefei, Anhui, 230027 (China); Li, Jiangang, E-mail: j_li@ipp.ac.cn [Institute of Plasma Physics, Chinese Academy of Sciences, Hefei, Anhui 230031 (China)

    2017-05-15

    Highlights: • A design for detection of tokamak plasma positrons is given. • Identify the main obstacle toward experimental confirmation of fusion plasma positrons. • Signal to noise ratio in a plasma disruption is estimated. • Unique potential applications of fusion plasma positrons are discussed. - Abstract: A massive amount of positrons (plasma positrons), produced by the collision between runaway electrons and nuclei during fusion plasma disruption, was first predicted theoretically in 2003. To help confirm this prediction, we report here the design of an experimental system to detect tokamak plasma positrons. Because a substantial amount of positrons (material positrons) are produced when runaway electrons impact plasma-facing materials, we proposed maximizing the ratio of plasma to material positrons by inserting a thin carbon target at the plasma edge as a plasma positron bombing target and producing a plasma disruption scenario triggered by massive gas injection. Meanwhile, the coincidence detection of positron annihilation photons was used to filter out the noise of annihilation photons from locations other than the carbon target and that of bremsstrahlung photons near 511 keV. According to our simulation, the overall signal-to-noise ratio should be more than 10:1.

  9. Forensic Drug Identification, Confirmation, and Quantification Using Fully Integrated Gas Chromatography with Fourier Transform Infrared and Mass Spectrometric Detection (GC-FT-IR-MS).

    Science.gov (United States)

    Lanzarotta, Adam; Lorenz, Lisa; Voelker, Sarah; Falconer, Travis M; Batson, JaCinta S

    2018-05-01

    This manuscript is a continuation of a recent study that described the use of fully integrated gas chromatography with direct deposition Fourier transform infrared detection and mass spectrometric detection (GC-FT-IR-MS) to identify and confirm the presence of sibutramine and AB-FUBINACA. The purpose of the current study was to employ the GC-FT-IR portion of the same instrument to quantify these compounds, thereby demonstrating the ability to identify, confirm, and quantify drug substances using a single GC-FT-IR-MS unit. The performance of the instrument was evaluated by comparing quantitative analytical figures of merit to those measured using an established, widely employed method for quantifying drug substances, high performance liquid chromatography with ultraviolet detection (HPLC-UV). The results demonstrated that GC-FT-IR was outperformed by HPLC-UV with regard to sensitivity, precision, and linear dynamic range (LDR). However, sibutramine and AB-FUBINACA concentrations measured using GC-FT-IR were not significantly different at the 95% confidence interval compared to those measured using HPLC-UV, which demonstrates promise for using GC-FT-IR as a semi-quantitative tool at the very least. The most significant advantage of GC-FT-IR compared to HPLC-UV is selectivity; a higher level of confidence regarding the identity of the analyte being quantified is achieved using GC-FT-IR. Additional advantages of using a single GC-FT-IR-MS instrument for identification, confirmation, and quantification are efficiency, increased sample throughput, decreased consumption of laboratory resources (solvents, chemicals, consumables, etc.), and thus cost.

  10. In-source collision induced dissociation of inorganic explosives for mass spectrometric signature detection and chemical imaging

    Energy Technology Data Exchange (ETDEWEB)

    Forbes, Thomas P., E-mail: thomas.forbes@nist.gov; Sisco, Edward

    2015-09-10

    The trace detection, bulk quantification, and chemical imaging of inorganic explosives and components was demonstrated utilizing in-source collision induced dissociation (CID) coupled with laser desorption/ionization mass spectrometry (LDI-MS). The incorporation of in-source CID provided direct control over the extent of adduct and cluster fragmentation as well as organic noise reduction for the enhanced detection of both the elemental and molecular ion signatures of fuel-oxidizer mixtures and other inorganic components of explosive devices. Investigation of oxidizer molecular anions, specifically, nitrates, chlorates, and perchlorates, identified that the optimal in-source CID existed at the transition between fragmentation of the ionic salt bonds and molecular anion bonds. The chemical imaging of oxidizer particles from latent fingerprints was demonstrated, including both cation and anion components in positive and negative mode mass spectrometry, respectively. This investigation demonstrated LDI-MS with in-source CID as a versatile tool for security fields, as well as environmental monitoring and nuclear safeguards, facilitating the detection of elemental and molecular inorganic compounds at nanogram levels. - Highlights: • In-source CID enhanced detection of elemental inorganics up to 1000-fold. • In-source CID optimization of polyatomic oxidizers enhanced detection up to 100-fold. • Optimal CID identified at transition from breaking ionic salt to molecular anion bonds. • Trace detection of inorganic explosives at nanogram levels was demonstrated. • Oxidizer particles were chemically imaged directly from latent fingerprints.

  11. Spectrometric assembly for portable installations

    International Nuclear Information System (INIS)

    Kluger, A.; Popescu, C.

    1997-01-01

    The components of the portable spectrometric assembly are: - the detecting probe with Na I(Tl) crystal and air-tight case of industrial type; - a microcomputer; - a unit of analogical processing of the signal from the detecting probe; - a single-channel analyzer with adjustable threshold; - commands and display module; - a source of high voltage; - an electrical supply battery. The device uses the method of gamma photons detection in energetic windows. Through theoretical and experimental studies carried out during the prototype development phase, the superiority of this method has been proved as compared with the installations which make use of the classical principle of photon integral detection. The achieved prototype has a basic program enabling the setting of all working parameters (measuring time, discriminating thresholds, discriminators operating conditions, etc.). Through the included interface RS232 it is possible to transmit the data to a more powerful computer in order to continually process the results. The spectrometric assembly, realized on the basis of micro-computers, can be used in a wide range of applications: measurement of thickness and erosion of walls and tubes, measurement of level in closed containers, of soil density, etc. The adjustment for specific application is performed only through a program modification. (authors)

  12. Bioactivity screening and mass spectrometric confirmation for the detection of PPAR-delta agonists that increase type 1 muscle fibres

    NARCIS (Netherlands)

    Bovee, T.F.H.; Blokland, M.H.; Kersten, A.H.; Hamers, A.R.M.; Heskamp, H.H.; Essers, M.L.; Nielen, M.W.F.; Ginkel, van L.A.

    2014-01-01

    Sensitive and robust bioassays able to detect nuclear receptor activation are very useful for veterinary and doping control, pharmaceutical industry and environmental scientists. Here, we used bioassays based on human leukemic monocyte lymphoma U937 and human liver hepatocellular carcinoma HepG2

  13. Continuous fraction collection of gas chromatographic separations with parallel mass spectrometric detection applied to cell-based bioactivity analysis

    NARCIS (Netherlands)

    Jonker, Willem; Zwart, Nick; Stockl, Jan B.; de Koning, Sjaak; Schaap, Jaap; Lamoree, Marja H.; Somsen, Govert W.; Hamers, Timo; Kool, Jeroen

    2017-01-01

    We describe the development and evaluation of a GC-MS fractionation platform that combines high-resolution fraction collection of full chromatograms with parallel MS detection. A y-split at the column divides the effluent towards the MS detector and towards an inverted y-piece where vaporized trap

  14. On-line two-dimensional capillary electrophoresis with mass spectrometric detection using a fully electric isolated mechanical valve.

    Science.gov (United States)

    Kohl, Felix J; Montealegre, Cristina; Neusüß, Christian

    2016-04-01

    CE is becoming more and more important in many fields of bioanalytical chemistry. Besides optical detection, hyphenation to ESI-MS detection is increasingly applied for sensitive identification purposes. Unfortunately, many CE techniques and methods established in research and industry are not compatible to ESI-MS since essential components of the background electrolyte interfere in ES ionization. In order to identify unknown peaks in established CE methods, here, a heart-cut 2D-CE separation system is introduced using a fully isolated mechanical valve with an internal loop of only 20 nL. In this system, the sample is separated using potentially any non-ESI compatible method in the first separation dimension. Subsequently, the portion of interest is cut by the internal sample loop of the valve and reintroduced to the second dimension where the interfering compounds are removed, followed by ESI-MS detection. When comparing the separation efficiency of the system with the valve to a system using a continuous capillary only a slight increase in peak width is observed. Ultraviolet/visible detection is integrated in the first dimension for switching time determination, enabling reproducible cutting of peaks of interest. The feasibility of the system is successfully demonstrated by a 2D analysis of a BSA tryptic digest sample using a nonvolatile (phosphate based) background electrolyte in the first dimension. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Anti-aggregation-based spectrometric detection of Hg(II) at physiological pH using gold nanorods

    Energy Technology Data Exchange (ETDEWEB)

    Rajeshwari, A.; Karthiga, D.; Chandrasekaran, Natarajan; Mukherjee, Amitava, E-mail: amit.mookerjea@gmail.com

    2016-10-01

    An efficient detection method for Hg (II) ions at physiological pH (pH 7.4) was developed using tween 20-modified gold nanorods (NRs) in the presence of dithiothreitol (DTT). Thiol groups (-SH) at the end of DTT have a higher affinity towards gold atoms, and they can covalently interact with gold NRs and leads to their aggregation. The addition of Hg(II) ions prevents the aggregation of gold NRs due to the covalent bond formation between the -SH group of DTT and Hg(II) ions in the buffer system. The changes in the longitudinal surface plasmon resonance peak of gold NRs were characterized using a UV–visible spectrophotometer. The absorption intensity peak of gold NRs at 679 nm was observed to reduce after interaction with DTT, and the absorption intensity was noted to increase by increasing the concentration of Hg(II) ions. The TEM analysis confirms the morphological changes of gold NRs before and after addition of Hg(II) ions in the presence of DTT. Further, the aggregation and disaggregation of gold NRs were confirmed by particle size and zeta potential analysis. The developed method shows an excellent linearity (y = 0.001 x + 0.794) for the graph plotted between the absorption ratio and Hg(II) concentration (1 to 100 pM) under the optimized conditions. The limit of detection was noted to be 0.42 pM in the buffer system. The developed method was tested in simulated body fluid, and it was found to have a good recovery rate. - Highlights: • Tween-20 modified gold NRs used as a probe for Hg(II) at physiological pH. • TEM, particle size and surface charge analysis confirm the aggregation and • disaggregation of NRs • The sensitivity of the probe for Hg(II) ions detection was 0.42 pM. • Hg(II) estimation in simulated body fluids with good recovery.

  16. Brimstone chemistry under laser light assists mass spectrometric detection and imaging the distribution of arsenic in minerals.

    Science.gov (United States)

    Lal, Swapnil; Zheng, Zhaoyu; Pavlov, Julius; Attygalle, Athula B

    2018-05-23

    Singly charged As2n+1 ion clusters (n = 2-11) were generated from elemental arsenic by negative-ion laser-ablation mass spectrometry. The overall abundance of the gaseous As ions generated upon laser irradiation was enhanced nearly a hundred times when As-bearing samples were admixed with sulfur. However, sulfur does not act purely as an inert matrix: irradiating arsenic-sulfur mixtures revealed a novel pathway to generate and detect a series of [AsSn]- clusters (n = 2-6). Intriguingly, the spectra recorded from As2O3, NaAsO2, Na3AsO4, cacodylic acid and 3-amino-4-hydroxyphenylarsonic acid together with sulfur as the matrix were remarkably similar to that acquired from an elemental arsenic and sulfur mixture. This result indicated that arsenic sulfide cluster-ions are generated directly from arsenic compounds by a hitherto unknown pathway. The mechanism of elemental sulfur extracting chemically bound arsenic from compounds and forming [AsSn]- clusters is enigmatic; however, this discovery has a practical value as a general detection method for arsenic compounds. For example, the method was employed for the detection of As in its minerals, and for the imaging of arsenic distribution in minerals such as domeykite. LDI-MS data recorded from a latent image imprinted on a piece of paper from a flat mineral surface, and wetting the paper with a solution of sulfur, enabled the localization of arsenic in the mineral. The distribution of As was visualized as false-color images by extracting from acquired data the relative intensities of m/z 139 (AsS2-) and m/z 171 (AsS3-) ions.

  17. Determination of free amino compounds in betalainic fruits and vegetables by gas chromatography with flame ionization and mass spectrometric detection.

    Science.gov (United States)

    Kugler, Florian; Graneis, Stephan; Schreiter, Pat P-Y; Stintzing, Florian C; Carle, Reinhold

    2006-06-14

    Amino acids and amines are the precursors of betalains. Therefore, the profiles of free amino compounds in juices obtained from cactus pears [Opuntia ficus-indica (L.) Mill. cv. Bianca, cv. Gialla, and cv. Rossa], pitaya fruits [Selenicereus megalanthus (K. Schumann ex Vaupel) Moran, Hylocereus polyrhizus (Weber) Britton & Rose, and Hylocereus undatus (Haworth) Britton & Rose], and in extracts from differently colored Swiss chard [Beta vulgaris L. ssp. cicla (L.) Alef. cv. Bright Lights] petioles and red and yellow beets (B. vulgaris L. ssp. vulgaris var. conditiva Alef. cv. Burpee's Golden) were investigated for the first time. Amino compounds were derivatized with propyl chloroformate. While gas chromatography (GC) with mass spectrometry was used for peak assignment, GC flame ionization detection was applied for quantification of individual compounds. Whereas proline was the major free amino compound of cactus pear and pitaya fruit juices, glutamine dominated in Swiss chard stems and beets, respectively. Interestingly, extremely high concentrations of dopamine were detected in Swiss chard stems and beets. Furthermore, the cleavage of betaxanthins caused by derivatization in alkaline reaction solutions is demonstrated for the first time. Amino acids and amines thus released might increase the actual free amino compound contents of the respective sample. To evaluate the contribution of betaxanthin cleavage to total amino acid and amine concentration, isolated betaxanthins were derivatized according to the "EZ:faast" method prior to quantification of the respective amino compounds released. On a molar basis, betaxanthin contribution to overall amino compound contents was always below 6.4%.

  18. Spectrometric techniques 3

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume III presents the applications of spectrometric techniques to atmospheric and space studies. This book reviews the spectral data processing and analysis techniques that are of broad applicability.Organized into five chapters, this volume begins with an overview of the instrumentation used for obtaining field data. This text then reviews the contribution that space-borne spectroscopy in the thermal IR has made to the understanding of the planets. Other chapters consider the instruments that have recorded the planetary emission spectra. This book discusses as well

  19. Plasma wave detection in laser spectroscopy and gas chromatography

    International Nuclear Information System (INIS)

    Franzke, J.; Irmer, A. von; Veza, D.; Niemax, K.

    1995-01-01

    Frequency changes of plasma oscillations in low-pressure discharges are used for sensitive detection of atomic or molecular trace gases. Analyte selectivity can be either obtained by resonant laser excitation or by gas chromatography

  20. Analysis of multiple quaternary ammonium compounds in the brain using tandem capillary column separation and high resolution mass spectrometric detection.

    Science.gov (United States)

    Falasca, Sara; Petruzziello, Filomena; Kretz, Robert; Rainer, Gregor; Zhang, Xiaozhe

    2012-06-08

    Endogenous quaternary ammonium compounds are involved in various physiological processes in the central nervous system. In the present study, eleven quaternary ammonium compounds, including acetylcholine, choline, carnitine, acetylcarnitine and seven other acylcarnitines of low polarity, were analyzed from brain extracts using a two dimension capillary liquid chromatography-Fourier transform mass spectrometry method. To deal with their large difference in hydrophobicities, tandem coupling between reversed phase and hydrophilic interaction chromatography columns was used to separate all the targeted quaternary ammonium compounds. Using high accuracy mass spectrometry in selected ion monitoring mode, all the compounds could be detected from each brain sample with high selectivity. The developed method was applied for the relative quantification of these quaternary ammonium compounds in three different brain regions of tree shrews: prefrontal cortex, striatum, and hippocampus. The comparative analysis showed that quaternary ammonium compounds were differentially distributed across the three brain areas. The analytical method proved to be highly sensitive and reliable for simultaneous determination of all the targeted analytes from brain samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  1. Identification of organic sulfur compounds in coal bitumen obtained by different extraction techniques using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Machado, Maria Elisabete; Cappelli Fontanive, Fernando; Bastos Caramao, Elina; Alcaraz Zini, Claudia [Universidade Federal do Rio Grande do Sul, Instituto de Quimica, Porto Alegre, RS (Brazil); Oliveira, Jose Vladimir de [URI, Universidade Regional Integrada do Alto Uruguai e das Missoes, Erechim, RS (Brazil)

    2011-11-15

    The determination of organic sulfur compounds (OSC) in coal is of great interest. Technically and operationally these compounds are not easily removed and promote corrosion of equipment. Environmentally, the burning of sulfur compounds leads to the emission of SO{sub x} gases, which are major contributors to acid rain. Health-wise, it is well known that these compounds have mutagenic and carcinogenic properties. Bitumen can be extracted from coal by different techniques, and use of gas chromatography coupled to mass spectrometric detection enables identification of compounds present in coal extracts. The OSC from three different bitumens were tentatively identified by use of three different extraction techniques: accelerated solvent extraction (ASE), ultrasonic extraction (UE), and supercritical-fluid extraction (SFE). Results obtained from one-dimensional gas chromatography (1D GC) coupled to quadrupole mass spectrometric detection (GC-qMS) and from two-dimensional gas chromatography with time-of-flight mass spectrometric detection (GC x GC-TOFMS) were compared. By use of 2D GC, a greater number of OSC were found in ASE bitumen than in SFE and UE bitumens. No OSC were identified with 1D GC-qMS, although some benzothiophenes and dibenzothiophenes were detected by use of EIM and SIM modes. GC x GC-TOFMS applied to investigation of OSC in bitumens resulted in analytical improvement, as more OSC classes and compounds were identified (thiols, sulfides, thiophenes, naphthothiophenes, benzothiophenes, and benzonaphthothiophenes). The roof-tile effect was observed for OSC and PAH in all bitumens. Several co-elutions among analytes and with matrix interferents were solved by use of GC x GC. (orig.)

  2. Marine gamma spectrometric survey

    International Nuclear Information System (INIS)

    Kostoglodov, V.V.

    1979-01-01

    Presented are theoretical problems physical and geochemical prerequisites and possibilities of practical application of the method of continuous submarine gamma-spectrometric survey and radiometric survey destined for rapid study of the surface layer of marine sediments. Shown is high efficiency and advantages of this method in comparison with traditional and widely spread in marine geology methods of bottom sediments investigation

  3. Mobile spectrometric laboratory

    International Nuclear Information System (INIS)

    Isajenko, K.A.; Lipinski, P.

    2002-01-01

    The article presents the Mobile Spectrometric Laboratory used by Central Laboratory for Radiological Protection since year 2000. The equipment installed in the Mobile Laboratory and its uses is described. The results of international exercises and intercalibrations, in which the Laboratory participated are presented. (author)

  4. Study of matrix effects on the direct trace analysis of acidic pesticides in water using various liquid chromatographic modes coupled to tandem mass spectrometric detection.

    Science.gov (United States)

    Dijkman, E; Mooibroek, D; Hoogerbrugge, R; Hogendoorn, E; Sancho, J V; Pozo, O; Hernández, F

    2001-08-10

    This study investigated the effects of matrix interferences on the analytical performance of a triple quadrupole mass spectrometric (MS-MS) detector coupled to various reversed-phase liquid chromatographic (LC) modes for the on-line determination of various types of acidic herbicides in water using external calibration for quantification of the analytes tested at a level of 0.4 microg/l. The LC modes included (i) a single-column configuration (LC), (ii) precolumn switching (PC-LC) and (iii) coupled-column LC (LC-LC). As regards detection, electrospray (ESI) and atmospheric pressure chemical ionization (APCI) in both positive (PI) and negative (NI) ionization modes were examined. Salinity and dissolved organic carbon (DOC) were selected as interferences to study matrix effects in this type of analysis. Therefore, Milli-Q and tap water samples both fortified with 12 mg/l DOC and spiked with sulfometuron-methyl, bentazone, bromoxynil, 2-methyl-4-chlorophenoxyacetic acid, and 2-methyl-4-chlorophenoxypropionic acid at a level of about 0.4 microg/l were analyzed with the various LC-MS approaches. Direct sample injection was performed with volumes of 0.25 ml or 2.0 ml on a column of 2.1 mm I.D. or 4.6 mm I.D. for the ESI and APCI modes, respectively. The recovery data were used to compare and evaluate the analytical performance of the various LC approaches. As regards matrix effects, the salinity provided a dramatic decrease in response for early eluting analytes (k value of about 1) when using the LC mode. Both PC-LC and LC-LC efficiently eliminated this problem. The high DOC content hardly effected the responses of analytes in the ESI mode, while in most cases the responses increased when using APCI-MS-MS detection. Of all the tested configurations, LC-LC-ESI-MS-MS with the column combination Discovery C18/ABZ+ was the most favorable as regards elimination of matrix effects and provided reliable quantification of all compounds using external calibration at the tested

  5. Development and validation of a sensitive liquid chromatographic-tandem mass spectrometric method for the simultaneous analysis of granisetron and 7-hydroxy granisetron in human plasma and urine samples: application in a clinical pharmacokinetic study in pregnant subject.

    Science.gov (United States)

    Zhao, Yang; Chen, Hui-Jun; Caritis, Steve; Venkataramanan, Raman

    2016-02-01

    A liquid chromatography-tandem mass spectrometric method for the quantification of granisetron and its major metabolite, 7-hydroxy granisetron in human plasma and urine samples was developed and validated. Respective stable isotopically labeled granisetron and 7-hydroxy granisetron were used as internal standards (IS). Chromatography was performed using an Xselect HSS T3 analytical column with a mobile phase of 20% acetonitrile in water (containing 0.2 mM ammonium formate and 0.14% formic acid, pH 4) delivered in an isocratic mode. Tandem mass spectrometry operating in positive electrospray ionization mode with multiple reaction monitoring was used for quantification. The standard curves were linear in the concentration ranges of 0.5-100 ng/mL for granisetron and 0.1-100 ng/mL for 7-hydroxy granisetron in human plasma samples, and 2-2000 ng/mL for granisetron and 2-1000 ng/mL for 7-hydroxy granisetron in human urine samples, respectively. The accuracies were >85% and the precision as determined by the coefficient of variations was granisetron or 7-hydroxy granisetron in either plasma or urine samples. Granisetron was stable under various storage and experimental conditions. This validated method was successfully applied to a pharmacokinetic study after intravenous administration of 1 mg granisetron to a pregnant subject. Copyright © 2015 John Wiley & Sons, Ltd.

  6. Quantitation of donepezil and its active metabolite 6-O-desmethyl donepezil in human plasma by a selective and sensitive liquid chromatography-tandem mass spectrometric method

    Energy Technology Data Exchange (ETDEWEB)

    Patel, Bhavin N. [Chemistry Department, School of Sciences, Gujarat University, Navrangpura, Ahmedabad 380 009, Gujarat (India); Analytical Laboratory, BA Research India Ltd., Bodakdev, Ahmedabad 380 054, Gujarat (India); Sharma, Naveen [Analytical Laboratory, BA Research India Ltd., Bodakdev, Ahmedabad 380 054, Gujarat (India); Sanyal, Mallika [Chemistry Department, St. Xaviers' College, Navrangpura, Ahmedabad 380 009, Gujarat (India); Shrivastav, Pranav S. [Chemistry Department, School of Sciences, Gujarat University, Navrangpura, Ahmedabad 380 009, Gujarat (India)], E-mail: pranav_shrivastav@yahoo.com

    2008-11-23

    A sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay for the simultaneous determination of donepezil (D) and its pharmacologically active metabolite, 6-O-desmethyl donepezil (6-ODD) in human plasma is developed using galantamine as internal standard (IS). The analytes and IS were extracted from 500 {mu}L aliquots of human plasma via solid-phase extraction (SPE) on Waters Oasis HLB cartridges. Chromatographic separation was achieved in a run time of 6.0 min on a Waters Novapak C18 (150 mm x 3.9 mm, 4 {mu}m) column under isocratic conditions. Detection of analytes and IS was done by tandem mass spectrometry, operating in positive ion and multiple reaction monitoring (MRM) acquisition mode. The protonated precursor to product ion transitions monitored for D, 6-ODD and IS were at m/z 380.1 {yields} 91.2, 366.3 {yields} 91.3 and 288.2 {yields} 213.2, respectively. The method was fully validated for its selectivity, interference check, sensitivity, linearity, precision and accuracy, recovery, matrix effect, ion suppression/enhancement, cross-specificity, stability and dilution integrity. A linear dynamic range of 0.10-50.0 ng mL{sup -1} for D and 0.02-10.0 ng mL{sup -1} for 6-ODD was evaluated with mean correlation coefficient (r) of 0.9975 and 0.9985, respectively. The intra-batch and inter-batch precision (%CV, coefficient of variation) across five quality control levels was less than 7.5% for both the analytes. The method was successfully applied to a bioequivalence study of 10 mg donepezil tablet formulation in 24 healthy Indian male subjects under fasting condition.

  7. Plasma functionalized surface of commodity polymers for dopamine detection

    Energy Technology Data Exchange (ETDEWEB)

    Fabregat, Georgina [Departament d’Enginyeria Química, E.T.S. d’Enginyeria Industrial de Barcelona, Universitat Politècnica de Catalunya, Diagonal 647, 08028, Barcelona (Spain); Center for Research in Nano-Engineering, Universitat Politècnica de Catalunya, Campus Sud, Edifici C’, C/Pasqual i Vila s/n, Barcelona, E-08028 (Spain); Osorio, Joaquin [Departament d’Enginyeria Química, E.T.S. d’Enginyeria Industrial de Barcelona, Universitat Politècnica de Catalunya, Diagonal 647, 08028, Barcelona (Spain); Castedo, Alejandra [Center for Research in Nano-Engineering, Universitat Politècnica de Catalunya, Campus Sud, Edifici C’, C/Pasqual i Vila s/n, Barcelona, E-08028 (Spain); Institut de Tècniques Energètiques, E.T.S. d’Enginyeria Industrial de Barcelona, Universitat Politècnica de Catalunya, Diagonal 647, 08028, Barcelona (Spain); Armelin, Elaine [Departament d’Enginyeria Química, E.T.S. d’Enginyeria Industrial de Barcelona, Universitat Politècnica de Catalunya, Diagonal 647, 08028, Barcelona (Spain); Center for Research in Nano-Engineering, Universitat Politècnica de Catalunya, Campus Sud, Edifici C’, C/Pasqual i Vila s/n, Barcelona, E-08028 (Spain); and others

    2017-03-31

    Highlights: • Electrochemically inert polymers become electroactive after plasma functionalization. • Selective dopamine detection has been achieved functionalizing polymers with plasma. • Plasma-functionalized polymers are sensitive dopamine detectors. • XPS analyses reflect the transformation of inert polymers into electrosensors. - Abstract: We have fabricated potentially generalizable sensors based on polymeric-modified electrodes for the electrochemical detection of dopamine. Sensitive and selective sensors have been successfully obtained by applying a cold-plasma treatment during 1–2 min not only to conducting polymers but also to electrochemically inert polymers, such as polyethylene, polypropylene, polyvinylpyrrolidone, polycaprolactone and polystyrene. The effects of the plasma in the electrode surface activation, which is an essential requirement for the dopamine detection when inert polymers are used, have been investigated using X-ray photoelectron spectroscopy. Results indicate that exposure of polymer-modified electrodes to cold-plasma produces the formation of a large variety of reactive species adsorbed on the electrode surface, which catalyse the dopamine oxidation. With this technology, which is based on the application of a very simple physical functionalization, we have defined a paradox-based paradigm for the fabrication of electrochemical sensors by using inert and cheap plastics.

  8. Emission spectrometric isotope analyzer

    International Nuclear Information System (INIS)

    Mauersberger, K.; Meier, G.; Nitschke, W.; Rose, W.; Schmidt, G.; Rahm, N.; Andrae, G.; Krieg, D.; Kuefner, W.; Tamme, G.; Wichlacz, D.

    1982-01-01

    An emission spectrometric isotope analyzer has been designed for determining relative abundances of stable isotopes in gaseous samples in discharge tubes, in liquid samples, and in flowing gaseous samples. It consists of a high-frequency generator, a device for defined positioning of discharge tubes, a grating monochromator with oscillating slit and signal converter, signal generator, window discriminator, AND connection, read-out display, oscillograph, gas dosing device and chemical conversion system with carrier gas source and vacuum pump

  9. Enhanced Detection of Human Plasma Proteins on Nanostructured Silver Surfaces

    Directory of Open Access Journals (Sweden)

    Zuzana Orságová Králová

    2013-08-01

    enhancement factor of 3.6×102 was achieved for a band with a Raman shift of 2104cm‐1 for globulin deposited onto silver nanostructured film on unpolished stainless steel substrate. The detection limit was 400g/mL. Plasma or serum could present a preferable material for non‐ invasive cancer disease diagnosis using the SERS method.

  10. Flaw detection device for plasma facing wall in thermonuclear device

    International Nuclear Information System (INIS)

    Doi, Akira.

    1996-01-01

    The present invention concerns plasma facing walls of a thermonuclear device and provides a device for detecting a thickness of amour tiles accurately and efficiently with no manual operation. Namely, the position of the plasma facing surface of the amour tile is measured using a structure to which the amour tiles are to be disposed as a reference. Also in a case of disposing new armor tiles, the position of the plasma facing surface of the armor tiles is measured to thereby measure the wearing amount of the amour tiles based on the difference between the reference and the measured value. If a measuring means capable of measuring a plurality of amour tiles at once is used efficiency of the measurement and the detection can be enhanced. Several ten thousands of amour tiles are disposed to the plasma facing wall in a large scaled thermonuclear device, and a plenty of time was required for the detection. However, the present invention can improve the accuracy for the measurement and detection and provide time and labors-saving. (I.S.)

  11. Validation of a liquid chromatography-triple quadrupole mass spectrometric method for the determination of 5-nitro-5'-hydroxy-indirubin-3'-oxime (AGM-130) in human plasma and its application to microdose clinical trial.

    Science.gov (United States)

    Park, Min-Ho; Lee, Yun Young; Cho, Kyung Hee; La, Sookie; Lee, Hee Joo; Yim, Dong-Seok; Ban, Sooho; Park, Moon-Young; Kim, Yong-Chul; Kim, Yoon-Gyoon; Shin, Young G

    2016-03-01

    A liquid chromatography-triple quadrupole mass spectrometric (LC-MS/MS) method was developed and validated for the determination of 5-nitro-5'-hydroxy-indirubin-3'-oxime (AGM-130) in human plasma to support a microdose clinical trial. The method consisted of a liquid-liquid extraction for sample preparation and LC-MS/MS analysis in the positive ion mode using TurboIonSpray(TM) for analysis. d3 -AGM-130 was used as the internal standard. A linear regression (weighted 1/concentration) was used to fit calibration curves over the concentration range of 10-2000 pg/mL for AGM-130. There were no endogenous interference components in the blank human plasma tested. The accuracy at the lower limit of quantitation was 96.6% with a precision (coefficient of variation, CV) of 4.4%. For quality control samples at 30, 160 and 1600 pg/mL, the between run CV was ≤5.0 %. Between-run accuracy ranged from 98.1 to 101.0%. AGM-130 was stable in 50% acetonitrile for 168 h at 4°C and 6 h at room temperature. AGM-130 was also stable in human plasma at room temperature for 6 h and through three freeze-thaw cycles. The variability of selected samples for the incurred sample reanalysis was ≤12.7% when compared with the original sample concentrations. This validated LC-MS/MS method for determination of AGM-130 was used to support a phase 0 microdose clinical trial. Copyright © 2015 John Wiley & Sons, Ltd.

  12. Characterization of phenolic and other polar compounds in peel and flesh of pink guava (Psidium guajava L. cv. 'Criolla') by ultra-high performance liquid chromatography with diode array and mass spectrometric detection.

    Science.gov (United States)

    Rojas-Garbanzo, Carolina; Zimmermann, Benno F; Schulze-Kaysers, Nadine; Schieber, Andreas

    2017-10-01

    Pink guava (Psidium guajava L.) is a highly consumed fruit in tropical countries. Despite of interesting research on health effects of this fruit, investigations into the profile of secondary plant metabolites are scarce. In this study, the phenolic compounds in the peel and flesh of pink guava were characterized by ultra-high performance liquid chromatography with diode array and mass spectrometric detection. Sixty phenolic compounds were characterized by MS 2 and classified as ellagitannins, flavones, flavonols, flavanols, proanthocyanidins, dihydrochalcones, and anthocyanidins, and non-flavonoids such as phenolic acid derivatives, stilbenes, acetophenones, and benzophenones. Forty-two polyphenols are reported for the first time in both peel and flesh, and twenty-four compounds were detected for the first time in P. guajava, e.g., phlorizin, nothofagin, astringin, chrysin-C-glucoside, valoneic acid bilactone, cinnamoyl-glucoside, and two dimethoxycinnamoyl-hexosides. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. Spectrometric techniques 2

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume II provides information pertinent to vacuum ultraviolet techniques to complete the demonstration of the diversity of methods available to the spectroscopist interested in the ultraviolet visible and infrared spectral regions. This book discusses the specific aspects of the technique of Fourier transform spectroscopy.Organized into five chapters, this volume begins with an overview of the large number of systematic effects in the recording of an interferogram. This text then examines the design approach for a Fourier transform spectrometer with focus on optics.

  14. Aerosol detection efficiency in inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Hubbard, Joshua A.; Zigmond, Joseph A.

    2016-05-01

    An electrostatic size classification technique was used to segregate particles of known composition prior to being injected into an inductively coupled plasma mass spectrometer (ICP-MS). Size-segregated particles were counted with a condensation nuclei counter as well as sampled with an ICP-MS. By injecting particles of known size, composition, and aerosol concentration into the ICP-MS, efficiencies of the order of magnitude aerosol detection were calculated, and the particle size dependencies for volatile and refractory species were quantified. Similar to laser ablation ICP-MS, aerosol detection efficiency was defined as the rate at which atoms were detected in the ICP-MS normalized by the rate at which atoms were injected in the form of particles. This method adds valuable insight into the development of technologies like laser ablation ICP-MS where aerosol particles (of relatively unknown size and gas concentration) are generated during ablation and then transported into the plasma of an ICP-MS. In this study, we characterized aerosol detection efficiencies of volatile species gold and silver along with refractory species aluminum oxide, cerium oxide, and yttrium oxide. Aerosols were generated with electrical mobility diameters ranging from 100 to 1000 nm. In general, it was observed that refractory species had lower aerosol detection efficiencies than volatile species, and there were strong dependencies on particle size and plasma torch residence time. Volatile species showed a distinct transition point at which aerosol detection efficiency began decreasing with increasing particle size. This critical diameter indicated the largest particle size for which complete particle detection should be expected and agreed with theories published in other works. Aerosol detection efficiencies also displayed power law dependencies on particle size. Aerosol detection efficiencies ranged from 10- 5 to 10- 11. Free molecular heat and mass transfer theory was applied, but

  15. Standard test methods for chemical and mass spectrometric analysis of nuclear-grade gadolinium oxide (Gd2O3) powder

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2006-01-01

    1.1 These test methods cover procedures for the chemical and mass spectrometric analysis of nuclear-grade gadolinium oxide powders to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Carbon by Direct CombustionThermal Conductivity C1408 Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method Total Chlorine and Fluorine by Pyrohydrolysis Ion Selective Electrode C1502 Test Method for Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide Loss of Weight on Ignition 7-13 Sulfur by CombustionIodometric Titration Impurity Elements by a Spark-Source Mass Spectrographic C761 Test Methods for Chemical, Mass Spectrometric, Spectrochemical,Nuclear, and Radiochemical Analysis of Uranium Hexafluoride C1287 Test Method for Determination of Impurities In Uranium Dioxide By Inductively Coupled Plasma Mass Spectrometry Gadolinium Content in Gadolinium Oxid...

  16. Detection of electric field around field-reversed configuration plasma

    International Nuclear Information System (INIS)

    Ikeyama, Taeko; Hiroi, Masanori; Nogi, Yasuyuki; Ohkuma, Yasunori

    2010-01-01

    Electric-field probes consisting of copper plates are developed to measure electric fields in a vacuum region around a plasma. The probes detect oscillating electric fields with a maximum strength of approximately 100 V/m through a discharge. Reproducible signals from the probes are obtained with an unstable phase dominated by a rotational instability. It is found that the azimuthal structure of the electric field can be explained by the sum of an n=2 mode charge distribution and a convex-surface electron distribution on the deformed separatrix at the unstable phase. The former distribution agrees with that anticipated from the diamagnetic drift motions of plasma when the rotational instability occurs. The latter distribution suggests that an electron-rich plasma covers the separatrix.

  17. Liquid chromatography-tandem mass spectrometric assay for the T790M mutant EGFR inhibitor osimertinib (AZD9291) in human plasma

    NARCIS (Netherlands)

    Rood, Johannes J M; van Bussel, Mark T J; Schellens, Jan H M; Beijnen, Jos H; Sparidans, Rolf W

    2016-01-01

    A method for the quantitative analysis by ultra-performance liquid chromatography-tandem mass spectrometry of the highly selective irreversible covalent inhibitor of EGFR-TK, osimertinib in human plasma was developed and validated, using pazopanib as an internal standard. The validation was

  18. Liquid chromatography-tandem mass spectrometric assay for the quantitative determination of the tyrosine kinase inhibitor quizartinib in mouse plasma using salting-out liquid-liquid extraction

    NARCIS (Netherlands)

    Retmana, Irene A; Wang, Jing; Schinkel, Alfred H; Schellens, Jan H M; Beijnen, Jos H; Sparidans, Rolf W

    2017-01-01

    A bioanalytical assay for quizartinib -a potent, and selective FLT3 tyrosine kinase inhibitor- in mouse plasma was developed and validated. Salting-out assisted liquid-liquid extraction (SALLE), using acetonitrile and magnesium sulfate, was selected as sample pretreatment with deuterated quizartinib

  19. Au nanoparticle-based sensor for apomorphine detection in plasma

    Directory of Open Access Journals (Sweden)

    Chiara Zanchi

    2015-11-01

    Full Text Available Artificially roughened gold surfaces with controlled nanostructure produced by pulsed laser deposition have been investigated as sensors for apomorphine detection aiming at clinical application. The use of such gold surfaces has been optimized using aqueous solutions of apomorphine in the concentration range between 3.3 × 10−4 M and 3.3 × 10−7 M. The experimental parameters have been investigated and the dynamic concentration range of the sensor has been assessed by the selection of two apomorphine surface enhanced Raman scattering (SERS peaks. The sensor behavior used to detect apomorphine in unfiltered human blood plasma is presented and discussed.

  20. Commercial Applications of X Ray Spectrometric Techniques

    International Nuclear Information System (INIS)

    Wegrzynek, D.

    2013-01-01

    In the 21st century, the X-ray fluorescence (XRF) technique is widely used in process control, industrial applications and for routine elemental analysis. The technique has a multielement capability capable of detecting elements with Z ≥ 10, with a few instruments capable of detecting also elements with Z ≥ 5. It is characterized by a non-destructive analysis process and relatively good detection limits, typically one part per million, for a wide range of elements. The first commercial XRF instruments were introduced to the market about 50 years ago. They were the wavelength dispersive X ray fluorescence (WDXRF) spectrometers utilizing Bragg’s law and reflection on crystal lattices for sequential elemental analysis of sample composition. The advances made in radiation detector technology, especially the introduction of semiconductor detectors, improvements in signal processing electronics, availability and exponential growth of personal computer market led to invention of energy dispersive X ray fluorescence (EDXRF) technique. The EDXRF is more cost effective as compared to WDXRF. It also allows for designing compact instruments. Such instruments can be easily tailored to the needs of different customers, integrated with industrial installations, and also miniaturized for the purpose of in-situ applications. The versatility of the technique has been confirmed in a spectacular way by using the XRF and X-ray spectrometric techniques, among few others, during the NASA and ESA missions in search for the evidence of life and presence of water on the surface of Mars. The XRF technique has achieved its strong position within the atomic spectroscopy group of analytical techniques not only due to its versatility but also due to relatively low running costs, as compared to the commonly used methods, e.g., atomic absorption spectrometry (AAS) or inductively coupled plasma atomic emission/mass spectrometry (ICP-AES/MS). Presently, the XRF technique together with X ray

  1. Commercial Applications of X Ray Spectrometric Techniques

    Energy Technology Data Exchange (ETDEWEB)

    Wegrzynek, D., E-mail: D.Wedgrznek@iaea.org [International Atomic Energy Agency, The IAEA Laboratories, Seibersdorf, Vienna (Austria)

    2013-07-15

    In the 21st century, the X-ray fluorescence (XRF) technique is widely used in process control, industrial applications and for routine elemental analysis. The technique has a multielement capability capable of detecting elements with Z {>=} 10, with a few instruments capable of detecting also elements with Z {>=} 5. It is characterized by a non-destructive analysis process and relatively good detection limits, typically one part per million, for a wide range of elements. The first commercial XRF instruments were introduced to the market about 50 years ago. They were the wavelength dispersive X ray fluorescence (WDXRF) spectrometers utilizing Bragg's law and reflection on crystal lattices for sequential elemental analysis of sample composition. The advances made in radiation detector technology, especially the introduction of semiconductor detectors, improvements in signal processing electronics, availability and exponential growth of personal computer market led to invention of energy dispersive X ray fluorescence (EDXRF) technique. The EDXRF is more cost effective as compared to WDXRF. It also allows for designing compact instruments. Such instruments can be easily tailored to the needs of different customers, integrated with industrial installations, and also miniaturized for the purpose of in-situ applications. The versatility of the technique has been confirmed in a spectacular way by using the XRF and X-ray spectrometric techniques, among few others, during the NASA and ESA missions in search for the evidence of life and presence of water on the surface of Mars. The XRF technique has achieved its strong position within the atomic spectroscopy group of analytical techniques not only due to its versatility but also due to relatively low running costs, as compared to the commonly used methods, e.g., atomic absorption spectrometry (AAS) or inductively coupled plasma atomic emission/mass spectrometry (ICP-AES/MS). Presently, the XRF technique together with X ray

  2. Ultrasensitive liquid chromatography-tandem mass spectrometric methodologies for quantification of five HIV-1 integrase inhibitors in plasma for a microdose clinical trial.

    Science.gov (United States)

    Sun, Li; Li, Hankun; Willson, Kenneth; Breidinger, Sheila; Rizk, Matthew L; Wenning, Larissa; Woolf, Eric J

    2012-10-16

    HIV-1 integrase strand transfer inhibitors are an important class of compounds targeted for the treatment of HIV-1 infection. Microdosing has emerged as an attractive tool to assist in drug candidate screening for clinical development, but necessitates extremely sensitive bioanalytical assays, typically in the pg/mL concentration range. Currently, accelerator mass spectrometry is the predominant tool for microdosing support, which requires a specialized facility and synthesis of radiolabeled compounds. There have been few studies attempted to comprehensively assess a liquid chromatography-tandem mass spectrometry (LC-MS/MS) approach in the context of microdosing applications. Herein, we describe the development of automated LC-MS/MS methods to quantify five integrase inhibitors in plasma with the limits of quantification at 1 pg/mL for raltegravir and 2 pg/mL for four proprietary compounds. The assays involved double extractions followed by UPLC coupled with negative ion electrospray MS/MS analysis. All methods were fully validated to the rigor of regulated bioanalysis requirements, with intraday precision between 1.20 and 14.1% and accuracy between 93.8 and 107% at the standard curve concentration range. These methods were successfully applied to a human microdose study and demonstrated to be accurate, reproducible, and cost-effective. Results of the study indicate that raltegravir displayed linear pharmacokinetics between a microdose and a pharmacologically active dose.

  3. DETECTION AND ISOLATION OF CD59 FROM HUMAN SEMINAL PLASMA

    Directory of Open Access Journals (Sweden)

    A REZAIE

    2002-06-01

    Full Text Available Introduction. CD59 is one of the complement regulatory proteins (CRPs which exert inhibitory function by blocking the formation of C5b-9 complex or Membrane Attacks complex (MAC. Regarding the therapeutic role of CD59 in treatment of pathological effects in uncontrolled activation of complements system and its efficiency to overcome the hyper-acute rejection, CD59 was suggested for maintenance of transplanted organ. In this study We determined and isolated CD59 from seminal plasma. Methods. Six normospermic sample according to WHO standards were chosen. Plasma of samples was separated and to remove the postasomes, the seminal plama was ultra centrifuged. CD59 was detected by Dot-Blot using CD59 mAb (MEM43. The molecular weight and purity of protein was detected by SOS-PAGE method follwed by Westerm Blot. Results. Protein was present in the 6.5 ml and 15ml of gel fitration fractions. Molecular weight based on marker size in these two fractions was 65 and 21KD respectively. Discussion. CD59 had previously beem purified by lysis of erythrocyte cell membrane. Because of use of detergent and preservative agents, this method decreased physiologic effects of the protein. In this study the isolation was performed from prostasome granules" without using of any detergent and preservative agents.

  4. Mass Spectrometric Analysis for Nuclear Safeguards

    International Nuclear Information System (INIS)

    Boulyga, S.

    2013-01-01

    The release of man-made radionuclides into the environment results in contamination that carries specific isotopic signatures according to the release scenarios and the previous usage of materials and facilities. In order to trace the origin of such contamination and/or to assess the potential impact on the public and environmental health, it is necessary to determine the isotopic composition and activity concentrations of radionuclides in environmental samples in an accurate and timely fashion. Mass spectrometric techniques, such as thermal ionization mass spectrometry (TIMS), secondary ion mass spectrometry (SIMS), and inductively coupled plasma mass spectrometry (ICP-MS) belong to the most powerful methods for analysis of nuclear and related samples in nuclear safeguards, forensics, and environmental monitoring. This presentation will address the potential of mass spectrometric analysis of actinides at ultra-trace concentration levels, isotopic analysis of micro-samples, age determination of nuclear materials as well as identification and quantification of elemental and isotopic signatures of nuclear samples in general. (author)

  5. Effect of operation conditions of the drop-on-demand aerosol generator on aerosol characteristics: Pseudo-cinematographic and plasma mass spectrometric studies

    International Nuclear Information System (INIS)

    Orlandini von Niessen, Jan O.; Krone, Karin M.; Bings, Nicolas H.

    2014-01-01

    The recently presented drop-on-demand (DOD) aerosol generator overcomes some of the drawbacks of pneumatic nebulization, as its aerosol is no longer generated by gas–liquid interaction. In the current study, an advanced imaging technique is presented, based on a CCD camera equipped with magnifying telecentric optics to allow for fast, automated and precise aerosol characterization as well as fundamental studies on the droplet generation processes by means of pseudo-cinematography. The DOD aerosol generator is thoroughly characterized regarding its droplet size distribution, which shows few distinct populations rather than a continuous distribution. Other important figures, such as the Sauter diameter (D 3,2 ) of 22 μm and the span of 0.4 were also determined. Additionally, the influence of the electrical operation conditions of the dosing device on the aerosol generation process is described. The number and volume of the generated droplets were found to be very reproducible and user-variable, e.g. from 17 to 27 μm (D 3,2 ), within a span of 0.07–0.89. The performances of different setups of the DOD as liquid sample introduction system in ICP-MS are correlated to the respective achievable aerosol characteristics and are also compared to the performance of a state-of-the-art μ-flow nebulizer (EnyaMist). The DOD system allowed for improved sensitivity, but slightly elevated signal noise and overall comparable limits of detection. The results are critically discussed and future directions are outlined. - Graphical abstract: Further characterization of the drop-on-demand aerosol generator for sample introduction in atomic spectrometry. - Highlights: • Significantly improved ICP-MS sensitivity using the DOD vs. EnyaMist. • Comparable detection limits but slightly worse short-term precision. • Superior flexibility compared with conventional/miniaturized pneumatic nebulizers. • Electrical operation conditions of the DOD influence aerosol characteristics.

  6. Effect of operation conditions of the drop-on-demand aerosol generator on aerosol characteristics: Pseudo-cinematographic and plasma mass spectrometric studies

    Energy Technology Data Exchange (ETDEWEB)

    Orlandini von Niessen, Jan O.; Krone, Karin M.; Bings, Nicolas H., E-mail: bings@uni-mainz.de

    2014-02-01

    The recently presented drop-on-demand (DOD) aerosol generator overcomes some of the drawbacks of pneumatic nebulization, as its aerosol is no longer generated by gas–liquid interaction. In the current study, an advanced imaging technique is presented, based on a CCD camera equipped with magnifying telecentric optics to allow for fast, automated and precise aerosol characterization as well as fundamental studies on the droplet generation processes by means of pseudo-cinematography. The DOD aerosol generator is thoroughly characterized regarding its droplet size distribution, which shows few distinct populations rather than a continuous distribution. Other important figures, such as the Sauter diameter (D{sub 3,2}) of 22 μm and the span of 0.4 were also determined. Additionally, the influence of the electrical operation conditions of the dosing device on the aerosol generation process is described. The number and volume of the generated droplets were found to be very reproducible and user-variable, e.g. from 17 to 27 μm (D{sub 3,2}), within a span of 0.07–0.89. The performances of different setups of the DOD as liquid sample introduction system in ICP-MS are correlated to the respective achievable aerosol characteristics and are also compared to the performance of a state-of-the-art μ-flow nebulizer (EnyaMist). The DOD system allowed for improved sensitivity, but slightly elevated signal noise and overall comparable limits of detection. The results are critically discussed and future directions are outlined. - Graphical abstract: Further characterization of the drop-on-demand aerosol generator for sample introduction in atomic spectrometry. - Highlights: • Significantly improved ICP-MS sensitivity using the DOD vs. EnyaMist. • Comparable detection limits but slightly worse short-term precision. • Superior flexibility compared with conventional/miniaturized pneumatic nebulizers. • Electrical operation conditions of the DOD influence aerosol

  7. Effect of operation conditions of the drop-on-demand aerosol generator on aerosol characteristics: Pseudo-cinematographic and plasma mass spectrometric studies

    Science.gov (United States)

    Orlandini v. Niessen, Jan O.; Krone, Karin M.; Bings, Nicolas H.

    2014-02-01

    The recently presented drop-on-demand (DOD) aerosol generator overcomes some of the drawbacks of pneumatic nebulization, as its aerosol is no longer generated by gas-liquid interaction. In the current study, an advanced imaging technique is presented, based on a CCD camera equipped with magnifying telecentric optics to allow for fast, automated and precise aerosol characterization as well as fundamental studies on the droplet generation processes by means of pseudo-cinematography. The DOD aerosol generator is thoroughly characterized regarding its droplet size distribution, which shows few distinct populations rather than a continuous distribution. Other important figures, such as the Sauter diameter (D3,2) of 22 μm and the span of 0.4 were also determined. Additionally, the influence of the electrical operation conditions of the dosing device on the aerosol generation process is described. The number and volume of the generated droplets were found to be very reproducible and user-variable, e.g. from 17 to 27 μm (D3,2), within a span of 0.07-0.89. The performances of different setups of the DOD as liquid sample introduction system in ICP-MS are correlated to the respective achievable aerosol characteristics and are also compared to the performance of a state-of-the-art μ-flow nebulizer (EnyaMist). The DOD system allowed for improved sensitivity, but slightly elevated signal noise and overall comparable limits of detection. The results are critically discussed and future directions are outlined.

  8. Viral protein Nef is detected in plasma of half of HIV-infected adults with undetectable plasma HIV RNA.

    Directory of Open Access Journals (Sweden)

    Jana Ferdin

    Full Text Available To address the role of translationally active HIV reservoir in chronic inflammation and non-AIDS related disorders, we first need a simple and accurate assay to evaluate viral protein expression in virally suppressed subjects.We optimized an HIV Nef enzyme-linked immunosorbent assay (ELISA and used it to quantify plasma Nef levels as an indicator of the leaky HIV reservoir in an HIV-infected cohort.This study accessed 134 plasma samples from a well-characterized cohort study of HIV-infected and uninfected adults in San Francisco (the SCOPE cohort. We optimized an ELISA for detection of plasma Nef in HIV-negative subjects and HIV-infected non-controllers, and evaluated its utility to quantify plasma Nef levels in a cross-sectional study of ART-suppressed and elite controller HIV-infected subjects.Here, we describe the performance of an optimized HIV Nef ELISA. When we applied this assay to the study cohort we found that plasma Nef levels were correlated with plasma HIV RNA levels in untreated disease. However, we were able to detect Nef in plasma of approximately half of subjects on ART or with elite control, despite the lack of detectable plasma HIV RNA levels using standard assays. Plasma Nef levels were not consistently associated with CD4+ T-cell count, CD8+ T-cell count, self-reported nadir CD4+ T-cell count or the CD4+/CD8+ T-cell ratio in HIV-infected subjects.Since plasma HIV RNA levels are undetectable in virally suppressed subjects, it is reasonable to assume that viral protein expression in leaky reservoir, and not plasma virions, is the source of Nef accumulating in plasma. To examine this further, improvements of the assay sensitivity, by lowering the background through improvements in the quality of Nef antibodies, and detailed characterization of the HIV reservoirs are needed.

  9. Microwave receivers for fast-ion detection in fusion plasmas

    International Nuclear Information System (INIS)

    Furtula, V.

    2012-02-01

    The main objectives of this thesis are to determine fundamental properties of a millimeter wave radiometer used to detect radiation associated with dynamics of fast ions and to investigate possibilities for improvements and new designs. The detection of fast ions is based on a principle called collective Thomson scattering (CTS). The Danish CTS group has been involved in fusion plasma experiments for more than 10 years and the future plans will most probably include the International Thermonuclear Experimental Reactor (ITER). Current CTS systems designed by the Danish group are specified for the frequency range from 100 to 110 GHz. In this thesis we follow the path of the radiation from a fusion plasma to the data acquisition unit. Firstly, the scattered radiation passes through the quasi-optical system. Quasi-optical elements required to be installed on the high field side (HFS) on the ITER are assessed. For the ITER HFS receiver we have designed and measured the quasi-optical components that form a transmission link between the plasma and the radio frequency (RF) electronics. This HFS receiver is required to resolve the near parallel velocity components created by the alpha particles. Secondly, the radiation will encounter the RF part. This part is not yet designed for ITER, but instead the solution is addressed to the CTS receiver installed at ASDEX Upgrade (AUG).We have put effort to thoroughly examine and evaluate the performance of the receiver components and the receiver as an assembled unit. We have measured and analyzed all the receiver components starting from the two notch filters to the fifty square-law detector diodes. The receiver sensitivity is calculated from the system measurements and compared with the expected sensitivity based on the individual component measurements. Besides the system considerations we have also studied improvements of two critical components of the receiver. The first component is the notch filter, which is needed to block

  10. Simultaneous determination of ethyl carbamate and urea in Korean rice wine by ultra-performance liquid chromatography coupled with mass spectrometric detection.

    Science.gov (United States)

    Lee, Gyeong-Hweon; Bang, Dae-Young; Lim, Jung-Hoon; Yoon, Seok-Min; Yea, Myeong-Jai; Chi, Young-Min

    2017-10-15

    In this study, a rapid method for simultaneous detection of ethyl carbamate (EC) and urea in Korean rice wine was developed. To achieve quantitative analysis of EC and urea, the conditions for Ultra-performance liquid chromatography (UPLC) separation and atmospheric-pressure chemical ionization tandem mass spectrometry (APCI-MS/MS) detection were first optimized. Under the established conditions, the detection limit, relative standard deviation and linear range were 2.83μg/L, 3.75-5.96%, and 0.01-10.0mg/L, respectively, for urea; the corresponding values were 0.17μg/L, 1.06-4.01%, and 1.0-50.0μg/L, respectively, for EC. The correlation between the contents of EC and its precursor urea was determined under specific pH (3.5 and 4.5) and temperature (4, 25, and 50°C) conditions using the developed method. As a result, EC content was increased with greater temperature and lower pH. In Korean rice wine, urea was detected 0.19-1.37mg/L and EC was detected 2.0-7.7μg/L. The method developed in this study, which has the advantages of simplified sample preparation, low detection limits, and good selectivity, was successfully applied for the rapid analysis of EC and urea. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Effects of sample injection amount and time-of-flight mass spectrometric detection dynamic range on metabolome analysis by high-performance chemical isotope labeling LC-MS.

    Science.gov (United States)

    Zhou, Ruokun; Li, Liang

    2015-04-06

    The effect of sample injection amount on metabolome analysis in a chemical isotope labeling (CIL) liquid chromatography-mass spectrometry (LC-MS) platform was investigated. The performance of time-of-flight (TOF) mass spectrometers with and without a high-dynamic-range (HD) detection system was compared in the analysis of (12)C2/(13)C2-dansyl labeled human urine samples. An average of 1635 ± 21 (n = 3) peak pairs or putative metabolites was detected using the HD-TOF-MS, compared to 1429 ± 37 peak pairs from a conventional or non-HD TOF-MS. In both instruments, signal saturation was observed. However, in the HD-TOF-MS, signal saturation was mainly caused by the ionization process, while in the non-HD TOF-MS, it was caused by the detection process. To extend the MS detection range in the non-HD TOF-MS, an automated switching from using (12)C to (13)C-natural abundance peaks for peak ratio calculation when the (12)C peaks are saturated has been implemented in IsoMS, a software tool for processing CIL LC-MS data. This work illustrates that injecting an optimal sample amount is important to maximize the metabolome coverage while avoiding the sample carryover problem often associated with over-injection. A TOF mass spectrometer with an enhanced detection dynamic range can also significantly increase the number of peak pairs detected. In chemical isotope labeling (CIL) LC-MS, relative metabolite quantification is done by measuring the peak ratio of a (13)C2-/(12)C2-labeled peak pair for a given metabolite present in two comparative samples. The dynamic range of peak ratio measurement does not need to be very large, as only subtle changes of metabolite concentrations are encountered in most metabolomic studies where relative metabolome quantification of different groups of samples is performed. However, the absolute concentrations of different metabolites can be very different, requiring a technique to provide a wide detection dynamic range to allow the detection of as

  12. Electrolyte system strategies for anionic isotachophoresis with electrospray-ionization mass-spectrometric detection. 1. Regular isotachophoresis and free-acid isotachophoresis

    Czech Academy of Sciences Publication Activity Database

    Malá, Zdeňka; Gebauer, Petr; Boček, Petr

    2013-01-01

    Roč. 34, 20-21 (2013), s. 3072-3078 ISSN 0173-0835 R&D Projects: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : Diclofenac * ESI-MS detection * Ibuprofen * isotachophoresis * water analysis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.161, year: 2013

  13. Intercomparisons to evaluate the suitability of gaschromatographic, electron-spin-resonance spectrometric and thermoluminescence methods to detect irradiated foods in routine control

    International Nuclear Information System (INIS)

    Schreiber, G.A.; Helle, N.; Schulzki, G.; Spiegelberg, A.; Linke, B.; Wagner, U.; Boegl, K.W.

    1993-01-01

    The results of four different intercomparisons to detect irradiated fish and chicken meat containing bones, chicken-, pork-, and beef-meat without bones, spices, herbs as well as spice- and herb mixtures, various fruit and vegetables as well as pistachio nuts using gas chromatographic methods, electron-spin resonance spectroscopy or thermoluminescence analyses are reported. (author)

  14. Data correlation in on-line solid-phase extraction-gas chromatography-atomic emission/mass spectrometric detection of unknown microcontaminants

    NARCIS (Netherlands)

    Hankemeier, Th.; Rozenbrand, J.; Abhadur, M.; Vreuls, J.J.; Brinkman, U.A.Th.

    1998-01-01

    A procedure is described for the (non-target) screening of hetero-atom-containing compounds in tap and waste water by correlating data obtained by gas chromatography (GC) using atomic emission (AED) and mass selective (MS) detection. Solid-phase extraction (SPE) was coupled on-line to both GC

  15. Electrolyte system strategies for anionic isotachophoresis with electrospray-ionization mass-spectrometric detection. 2. Isotachophoresis in moving-boundary systems

    Czech Academy of Sciences Publication Activity Database

    Gebauer, Petr; Malá, Zdeňka; Boček, Petr

    2013-01-01

    Roč. 34, č. 24 (2013), s. 3245-3251 ISSN 0173-0835 R&D Project s: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : electrolyte systems * ESI-MS detection * isotachophoresis * moving-boundary electrophoresis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.161, year: 2013

  16. Development, validation and application of an ultra high performance liquid chromatographic-tandem mass spectrometric method for the simultaneous detection and quantification of five different classes of veterinary antibiotics in swine manure.

    Science.gov (United States)

    Van den Meersche, Tina; Van Pamel, Els; Van Poucke, Christof; Herman, Lieve; Heyndrickx, Marc; Rasschaert, Geertrui; Daeseleire, Els

    2016-01-15

    In this study, a fast, simple and selective ultra high performance liquid chromatographic-tandem mass spectrometric (UHPLC-MS/MS) method for the simultaneous detection and quantification of colistin, sulfadiazine, trimethoprim, doxycycline, oxytetracycline and ceftiofur and for the detection of tylosin A in swine manure was developed and validated. First, a simple extraction procedure with acetonitrile and 6% trichloroacetic acid was carried out. Second, the supernatant was evaporated and the pellet was reconstituted in 1 ml of water/acetonitrile (80/20) and 0.1% formic acid. Extracts were filtered and analyzed by UHPLC-MS/MS on a Kinetex C18 column using gradient elution. The method developed was validated according to the criteria of Commission Decision 2002/657/EC. Recovery percentages varied between 94% and 106%, repeatability percentages were within the range of 1.7-9.2% and the intralaboratory reproducibility varied between 2.8% and 9.3% for all compounds, except for tylosin A for which more variation was observed resulting in a higher measurement uncertainty. The limit of detection and limit of quantification varied between 1.1 and 20.2 and between 3.5 and 67.3 μg/kg, respectively. This method was used to determine the presence and concentration of the seven antibiotic residues in swine manure sampled from ten different manure pits on farms where the selected antibiotics were used. A link was found between the antibiotics used and detected, except for ceftiofur which is injected at low doses and degraded readily in swine manure and was therefore not recovered in any of the samples. To the best of our knowledge, this is the first method available for the simultaneous extraction and quantification of colistin with other antibiotic classes. Additionally, colistin was never extracted from swine manure before. Another innovative aspect of this method is the simultaneous detection and quantification of five different classes of antibiotic residues in swine manure

  17. Speciation of selenoamino acids, selenonium ions and inorganic selenium by ion exchange HPLC with mass spectrometric detection and its application to yeast and algae

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Hansen, M.; Fan, T.

    2001-01-01

    Cation and anion exchange HPLC were used to separate a mixture of 12 selenium species comprising selenoamino acids, selenonium ions and inorganic selenium. The cationic species were separated from each other and from the co-injected anions using a cation exchange column with gradient elution...... by aqueous pyridinium formate at pH similar to 3 as the mobile phase. The anionic species were separated using an anion exchange column with isocratic elution by an aqueous salicylate-TRIS mobile phase at pH 8.5. The separated selenium species were detected as Se-80 by ICP-dynamic reaction cell (DRC...... acid extract of Chlorella algae contained dimethylselenonium propionate (DMSeP), which was verified by HPLC-ES-MS. Se-allylselenocysteine and selenoethionine was detected at the low ng g(-1) concentration level based on co-chromatography with the standard substances spiked to the algal extract....

  18. Comparison of various liquid chromatographic methods involving UV and atmospheric pressure chemical ionization mass spectrometric detection for the efficient trace analysis of phenylurea herbicides in various types of water samples.

    Science.gov (United States)

    van der Heeft, E; Dijkman, E; Baumann, R A; Hogendoorn, E A

    2000-05-19

    The performance of mass spectrometric (MS) detection and UV detection in combination with reversed-phase liquid chromatography without and with the use of coupled column RPLC (LC-LC) has been compared for the trace analysis of phenylurea herbicides in environmental waters. The selected samples of this comparative study originated from an inter-laboratory study. For both detection modes, a 50 mm x 4.6 mm I.D. column and a 100 mm x 4.6 mm I.D. column packed with 3 microm C18 were used as the first (C-1) and second (C-2) column, respectively. Atmospheric pressure chemical ionization mass spectrometry was performed on a magnetic sector instrument. The LC-LC-MS analysis was carried out on-line by means of direct large volume (11.7 ml) injection (LVI). The performance of both on-line (LVI, 4 ml of sample) and off-line LC-LC-UV (244 nm) analysis was investigated. The latter procedure consisted of a solid-phase extraction (SPE) of 250 ml of water sample on a 500 mg C18 cartridge. The comparative study showed that LC-LC-MS is more selective then LC-LC-UV and, in most cases, more sensitive. The LVI-LC-LC-MS approach combines direct quantification and confirmation of most of the analytes down to a level of 0.01 microg/l in water samples in less then 30 min. As regards LC-LC-UV, the off-line method appeared to be a more viable approach in comparison with the on-line procedure. This method allows the screening of phenylurea's in various types of water samples down to a level of at least 0.05 microg/l. On-line analysis with LVI provided marginal sensitivity (limits of detection of about 0.1 microg/l) and selectivity was sometimes less in case of surface water samples. Both the on-line LVI-LC-LC-MS method and the LC-LC-UV method using off-line SPE were validated by analysing a series of real-life reference samples. These samples were part of an inter-laboratory test and contained residues of herbicides ranging from 0.02 to 0.8 microg/l. Beside good correlation between the methods

  19. Spectrometric properties of crystals for low-energy x-ray diagnostics

    International Nuclear Information System (INIS)

    Barrus, D.m.; Blake, R.L.; Felthauser, H.; Fenimore, E.E.

    1981-01-01

    Quantitative diagnostics of fusion and astrophysical plasmas require knowledge of crystal spectrometric properties. To provide more reliable and versatile diagnostics of plasma conditions, increasingly accurate knowledge of crystal spectrometric properties is becoming necessary. A summary is presented of the following accurately measured parameters for the crystals KAP, RbAP, TlAP, NH 4 AP, NaAP, ADP, and EDDT: the interplanar spacing of atoms; the angle correction for normal and anomalous dispersion that is required for application of the Bragg formula; the thermal expansion coefficient near room temperature for commonly used planes; and the integrated coefficient of reflection

  20. Methodology of analysis of very weak acids by isotachophoresis with electrospray-ionization mass-spectrometric detection: Anionic electrolyte systems for the medium-alkaline pH range.

    Science.gov (United States)

    Malá, Zdena; Gebauer, Petr

    2018-01-15

    This work describes for the first time a functional electrolyte system setup for anionic isotachophoresis (ITP) with electrospray-ionization mass-spectrometric (ESI-MS) detection in the neutral to medium-alkaline pH range. So far no application was published on the analysis of very weak acids by anionic ITP-MS although there is a broad spectrum of potential analytes with pK a values in the range 5-10, where application of this technique promises interesting gains in both sensitivity and specificity. The problem so far was the lack of anionic ESI-compatible ITP systems in the mentioned pH range as all typical volatile anionic system components are fully ionized at neutral and alkaline pH and thus too fast to suit as terminators. We propose an original solution of the problem based on the combination of two ITP methods: (i) use of the hydroxyl ion as a natural and ESI-compatible terminator, and (ii) use of configurations based on moving-boundary ITP. The former method ensures effective stacking of analytes by an alkaline terminator of sufficiently low mobility and the latter offers increased flexibility for tuning of the separation window and selectivity according to actual needs. A theoretical description of the proposed model is presented and applied to the design of very simple functional electrolyte configurations. The properties of example systems are demonstrated by both computer simulation and experiments with a group of model analytes. Potential effects of carbon dioxide present in the solutions are demonstrated for particular systems. Experimental results confirm that the proposed methodology is well capable of performing sensitive and selective ITP-MS analyses of very weak acidic analytes (e.g. sulfonamides or chlorophenols). Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Spectrometric microbiological analyzer

    Science.gov (United States)

    Schlager, Kenneth J.; Meissner, Ken E.

    1996-04-01

    Currently, there are four general approaches to microbiological analysis, i.e., the detection, identification and quantification of micro-organisms: (1) Traditional culturing and staining procedures, metabolic fermentations and visual morphological characteristics; (2) Immunological approaches employing microbe-specific antibodies; (3) Biotechnical techniques employing DNA probes and related genetic engineering methods; and (4) Physical measurement techniques based on the biophysical properties of micro-organisms. This paper describes an instrumentation development in the fourth of the above categories, physical measurement, that uses a combination of fluorometric and light scatter spectra to detect and identify micro-organisms at the species level. A major advantage of this approach is the rapid turnaround possible in medical diagnostic or water testing applications. Fluorometric spectra serve to define the biochemical characteristics of the microbe, and light scatter spectra the size and shape morphology. Together, the two spectra define a 'fingerprint' for each species of microbe for detection, identification and quantification purposes. A prototype instrument has been developed and tested under NASA sponsorship based on fluorometric spectra alone. This instrument demonstrated identification and quantification capabilities at the species level. The paper reports on test results using this instrument, and the benefits of employing a combination of fluorometric and light scatter spectra.

  2. Coupling continuous ultrasound-assisted extraction, preconcentration and flame atomic absorption spectrometric detection for the determination of cadmium and lead in mussel samples

    International Nuclear Information System (INIS)

    Yebra-Biurrun, M.C.; Cancela-Perez, S.; Moreno-Cid-Barinaga, A.

    2005-01-01

    Continuous ultrasound-assisted extraction has been coupled with preconcentration and flame atomic absorption spectrometry for the determination of cadmium and lead in mussel samples. Experimental designs were used for the optimisation of the leaching and preconcentration steps. The use of diluted nitric acid as extractant in the continuous mode at a flow rate of 3.5 ml min -1 and room temperature was sufficient for quantitative extraction of these trace metals. A minicolumn containing a chelating resin (Chelite P, with aminomethylphosphoric acid groups) was proved as an excellent material for the quantitative preconcentration of cadmium and lead prior to their flame atomic absorption detection. A flow injection manifold was used as interface for coupling the three analytical steps, which allowed the automation of the whole analytical process. A good precision of the whole procedure (2.0 and 2.3%), high enrichment factors (20.5 and 11.8) and a detection limit of 0.011 and 0.25 μg g -1 for cadmium and lead, respectively, were obtained for 80 mg of sample. The sample throughputs were ca. 16 and 14 samples h -1 for cadmium and lead, respectively. The accuracy of the analytical procedures was verified by using a standard reference material (BCR 278-R, mussel tissue) and the results were in good agreement with the certified values. The method was successfully applied to the determination of trace amounts of cadmium and lead in mussel samples from the coast of Galicia (NW, Spain)

  3. Analysis of polycyclic aromatic hydrocarbons in water and beverages using membrane-assisted solvent extraction in combination with large volume injection-gas chromatography-mass spectrometric detection.

    Science.gov (United States)

    Rodil, Rosario; Schellin, Manuela; Popp, Peter

    2007-09-07

    Membrane-assisted solvent extraction (MASE) in combination with large volume injection-gas chromatography-mass spectrometry (LVI-GC-MS) was applied for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. The MASE conditions were optimized for achieving high enrichment of the analytes from aqueous samples, in terms of extraction conditions (shaking speed, extraction temperature and time), extraction solvent and composition (ionic strength, sample pH and presence of organic solvent). Parameters like linearity and reproducibility of the procedure were determined. The extraction efficiency was above 65% for all the analytes and the relative standard deviation (RSD) for five consecutive extractions ranged from 6 to 18%. At optimized conditions detection limits at the ng/L level were achieved. The effectiveness of the method was tested by analyzing real samples, such as river water, apple juice, red wine and milk.

  4. Standoff detection of bioaerosols over wide area using a newly developed sensor combining a cloud mapper and a spectrometric LIF lidar

    Science.gov (United States)

    Buteau, Sylvie; Simard, Jean-Robert; Roy, Gilles; Lahaie, Pierre; Nadeau, Denis; Mathieu, Pierre

    2013-10-01

    A standoff sensor called BioSense was developed to demonstrate the capacity to map, track and classify bioaerosol clouds from a distant range and over wide area. The concept of the system is based on a two steps dynamic surveillance: 1) cloud detection using an infrared (IR) scanning cloud mapper and 2) cloud classification based on a staring ultraviolet (UV) Laser Induced Fluorescence (LIF) interrogation. The system can be operated either in an automatic surveillance mode or using manual intervention. The automatic surveillance operation includes several steps: mission planning, sensor deployment, background monitoring, surveillance, cloud detection, classification and finally alarm generation based on the classification result. One of the main challenges is the classification step which relies on a spectrally resolved UV LIF signature library. The construction of this library relies currently on in-chamber releases of various materials that are simultaneously characterized with the standoff sensor and referenced with point sensors such as Aerodynamic Particle Sizer® (APS). The system was tested at three different locations in order to evaluate its capacity to operate in diverse types of surroundings and various environmental conditions. The system showed generally good performances even though the troubleshooting of the system was not completed before initiating the Test and Evaluation (T&E) process. The standoff system performances appeared to be highly dependent on the type of challenges, on the climatic conditions and on the period of day. The real-time results combined with the experience acquired during the 2012 T & E allowed to identify future ameliorations and investigation avenues.

  5. Gas chromatography interfaced with atmospheric pressure ionization-quadrupole time-of-flight-mass spectrometry by low-temperature plasma ionization

    DEFF Research Database (Denmark)

    Norgaard, Asger W.; Kofoed-Sorensen, Vivi; Svensmark, Bo

    2013-01-01

    A low temperature plasma (LTP) ionization interface between a gas chromatograph (GC) and an atmospheric pressure inlet mass spectrometer, was constructed. This enabled time-of-flight mass spectrometric detection of GC-eluting compounds. The performance of the setup was evaluated by injection...

  6. An overview on the study of quark gluon plasma with Alice dimuon spectrometer; Apercu sur l'etude du plasma de Quarks et de gluons a l'aide du spectrometre dimuons d'Alice

    Energy Technology Data Exchange (ETDEWEB)

    Espagnon, B

    2007-10-15

    The Alice experiment is one of the four main LHC (Large Hadron Collider) experiments. It is dedicated to the study of a new state of matter: the quark gluon plasma, where quarks and gluons are no longer confined within hadrons. In this document, the physics issues that led to the construction of Alice dimuon spectrometer, are described. Then, the research and development on the dimuon spectrometer is presented. The different absorbers are described and experimental tests used to determine their dimensions are presented. The dimuon trigger built using the RPC (Resistive Plate Chamber) streamer mode is then described along with the associated beam and cosmic tests and results. Finally, the tracking system is described in detail and more particularly all its electronics and the first station. The physics constraints on the expected performances of all these systems are clearly defined. (author)

  7. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection

    International Nuclear Information System (INIS)

    Nakamoto, Akihiro; Nishida, Manami; Saito, Takeshi; Kishiyama, Izumi; Miyazaki, Shota; Murakami, Katsunori; Nagao, Masataka; Namura, Akira

    2010-01-01

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d 5 was used as an internal standard. The linear ranges were 0.01-5.0 μg mL -1 for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 μg mL -1 for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation ≥0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 μg mL -1 of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio ≥ 3) in urine was 5 ng mL -1 for MA and MDMA and 10 ng mL -1 for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.

  8. “Measure Your Gradient”: A New Way to Measure Gradients in High Performance Liquid Chromatography by Mass Spectrometric or Absorbance Detection

    Science.gov (United States)

    Magee, Megan H.; Manulik, Joseph C.; Barnes, Brian B.; Abate-Pella, Daniel; Hewitt, Joshua T.; Boswell, Paul G.

    2014-01-01

    The gradient produced by an HPLC is never the same as the one it is programmed to produce, but non-idealities in the gradient can be taken into account if they are measured. Such measurements are routine, yet only one general approach has been described to make them: both HPLC solvents are replaced with water, solvent B is spiked with 0.1% acetone, and the gradient is measured by UV absorbance. Despite the widespread use of this procedure, we found a number of problems and complications with it, mostly stemming from the fact that it measures the gradient under abnormal conditions (e.g. both solvents are water). It is also generally not amenable to MS detection, leaving those with only an MS detector no way to accurately measure their gradients. We describe a new approach called “Measure Your Gradient” that potentially solves these problems. One runs a test mixture containing 20 standards on a standard stationary phase and enters their gradient retention times into open-source software available at www.measureyourgradient.org. The software uses the retention times to back-calculate the gradient that was truly produced by the HPLC. Here we present a preliminary investigation of the new approach. We found that gradients measured this way are comparable to those measured by a more accurate, albeit impractical, version of the conventional approach. The new procedure worked with different gradients, flow rates, column lengths, inner diameters, on two different HPLCs, and with six different batches of the standard stationary phase. PMID:25441073

  9. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Nakamoto, Akihiro [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nishida, Manami [Hiroshima University Technical Center, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Saito, Takeshi [Department of Emergency and Critical Care Medicine, Tokai University School of Medicine, Shimokasuya 143, Isehara, Kanagawa 259-1143 (Japan); Kishiyama, Izumi; Miyazaki, Shota [GL Sciences Inc., Sayamagahara 237-2, Iruma, Saitama 358-0032 (Japan); Murakami, Katsunori [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nagao, Masataka [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Namura, Akira, E-mail: namera@hiroshima-u.ac.jp [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan)

    2010-02-19

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d{sub 5} was used as an internal standard. The linear ranges were 0.01-5.0 {mu}g mL{sup -1} for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 {mu}g mL{sup -1} for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation {>=}0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 {mu}g mL{sup -1} of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio {>=} 3) in urine was 5 ng mL{sup -1} for MA and MDMA and 10 ng mL{sup -1} for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.

  10. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection.

    Science.gov (United States)

    Nakamoto, Akihiro; Nishida, Manami; Saito, Takeshi; Kishiyama, Izumi; Miyazaki, Shota; Murakami, Katsunori; Nagao, Masataka; Namura, Akira

    2010-02-19

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d(5) was used as an internal standard. The linear ranges were 0.01-5.0 microg mL(-1) for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 microg mL(-1) for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation > or = 0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 microg mL(-1) of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio > or = 3) in urine was 5 ng mL(-1) for MA and MDMA and 10 ng mL(-1) for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation. Copyright 2009 Elsevier B.V. All rights reserved.

  11. Stability of arsenic peptides in plant extracts: off-line versus on-line parallel elemental and molecular mass spectrometric detection for liquid chromatographic separation.

    Science.gov (United States)

    Bluemlein, Katharina; Raab, Andrea; Feldmann, Jörg

    2009-01-01

    The instability of metal and metalloid complexes during analytical processes has always been an issue of an uncertainty regarding their speciation in plant extracts. Two different speciation protocols were compared regarding the analysis of arsenic phytochelatin (As(III)PC) complexes in fresh plant material. As the final step for separation/detection both methods used RP-HPLC simultaneously coupled to ICP-MS and ES-MS. However, one method was the often used off-line approach using two-dimensional separation, i.e. a pre-cleaning step using size-exclusion chromatography with subsequent fraction collection and freeze-drying prior to the analysis using RP-HPLC-ICP-MS and/or ES-MS. This approach revealed that less than 2% of the total arsenic was bound to peptides such as phytochelatins in the root extract of an arsenate exposed Thunbergia alata, whereas the direct on-line method showed that 83% of arsenic was bound to peptides, mainly as As(III)PC(3) and (GS)As(III)PC(2). Key analytical factors were identified which destabilise the As(III)PCs. The low pH of the mobile phase (0.1% formic acid) using RP-HPLC-ICP-MS/ES-MS stabilises the arsenic peptide complexes in the plant extract as well as the free peptide concentration, as shown by the kinetic disintegration study of the model compound As(III)(GS)(3) at pH 2.2 and 3.8. But only short half-lives of only a few hours were determined for the arsenic glutathione complex. Although As(III)PC(3) showed a ten times higher half-life (23 h) in a plant extract, the pre-cleaning step with subsequent fractionation in a mobile phase of pH 5.6 contributes to the destabilisation of the arsenic peptides in the off-line method. Furthermore, it was found that during a freeze-drying process more than 90% of an As(III)PC(3) complex and smaller free peptides such as PC(2) and PC(3) can be lost. Although the two-dimensional off-line method has been used successfully for other metal complexes, it is concluded here that the fractionation and

  12. An integrative time-varying frequency detection and channel sounding method for dynamic plasma sheath

    Science.gov (United States)

    Shi, Lei; Yao, Bo; Zhao, Lei; Liu, Xiaotong; Yang, Min; Liu, Yanming

    2018-01-01

    The plasma sheath-surrounded hypersonic vehicle is a dynamic and time-varying medium and it is almost impossible to calculate time-varying physical parameters directly. The in-fight detection of the time-varying degree is important to understand the dynamic nature of the physical parameters and their effect on re-entry communication. In this paper, a constant envelope zero autocorrelation (CAZAC) sequence based on time-varying frequency detection and channel sounding method is proposed to detect the plasma sheath electronic density time-varying property and wireless channel characteristic. The proposed method utilizes the CAZAC sequence, which has excellent autocorrelation and spread gain characteristics, to realize dynamic time-varying detection/channel sounding under low signal-to-noise ratio in the plasma sheath environment. Theoretical simulation under a typical time-varying radio channel shows that the proposed method is capable of detecting time-variation frequency up to 200 kHz and can trace the channel amplitude and phase in the time domain well under -10 dB. Experimental results conducted in the RF modulation discharge plasma device verified the time variation detection ability in practical dynamic plasma sheath. Meanwhile, nonlinear phenomenon of dynamic plasma sheath on communication signal is observed thorough channel sounding result.

  13. Gravitational wave detection by bounded cold electronic plasma in a long pipe

    OpenAIRE

    Jalili, O.; Rouhani, S.; Takook, M. V.

    2013-01-01

    We intend to propose an experimental sketch to detect gravitational waves (GW) directly, using an cold electronic plasma in a long pipe. By considering an cold electronic plasma in a long pipe, the Maxwell equations in 3+1 formalism will be invoked to relate gravitational waves to the perturbations of plasma particles. It will be shown that the impact of GW on cold electronic plasma causes disturbances on the paths of the electrons. Those electrons that absorb energy from GW will pass through...

  14. Microwave Receivers for Fast-Ion Detection in Fusion Plasmas

    DEFF Research Database (Denmark)

    Furtula, Vedran

    for the frequency range from 100 to 110 GHz. In this thesis we follow the path of the radiation from a fusion plasma to the data acquisition unit. Firstly, the scattered radiation passes through the quasi-optical system. Quasi-optical elements required to be installed on the high field side (HFS) on the ITER...... are assessed. For the ITER HFS receiver we have designed and measured the quasioptical components that form a transmission link between the plasma and the radio frequency (RF) electronics. This HFS receiver is required to resolve the near parallel velocity components created by the alpha particles. Secondly...... is the mixer. The conversion loss of the mixer, together with loss in waveguide components and quasi-optic parts, is the main contributor to the noise and thereby degrades the signal to-noise ratio. The architecture of the mixer is a subharmonic type, optimized to be driven by a double local oscillator (LO...

  15. Detection of methylated CDO1 in plasma of colorectal cancer; a PCR study.

    Directory of Open Access Journals (Sweden)

    Keishi Yamashita

    Full Text Available BACKGROUND: Cysteine biology is important for the chemosensitivity of cancer cells. Our research has focused on the epigenetic silencing of cysteine dioxygenase type 1 (CDO1 in colorectal cancer (CRC. In this study, we describe detection of CDO1 methylation in the plasma of CRC patients using methylation specific PCR (Q-MSP and extensive analysis of the PCR reaction. METHODS: DNA was extracted from plasma, and analysed for methylation of the CDO1 gene using Q-MSP. The detection rate of CDO1 gene methylation was calculated and compared with that of diluted DNA extracted from "positive control" DLD1 cells. CDO1 gene methylation in the plasma of 40 CRC patients that were clinicopathologically analysed was then determined. RESULTS: (1 The cloned sequence analysis detected 93.3% methylation of the promoter CpG islands of the CDO1 gene of positive control DLD1 cells and 4.7% methylation of the negative control HepG2 CDO1 gene. (2 DLD1 CDO1 DNA could not be detected in this assay if the extracted DNA was diluted ∼1000 fold. The more DNA that was used for the PCR reaction, the more effectively it was amplified in Q-MSP. (3 By increasing the amount of DNA used, methylated CDO1 could be clearly detected in the plasma of 8 (20% of the CRC patients. However, the percentage of CRC patients detected by methylated CDO1 in plasma was lower than that detected by CEA (35.9% or CA19-9 (23.1% in preoperative serum. Combination of CEA/CA19-9 plus plasma methylated CDO1 could increase the rate of detection of curable CRC patients (39.3% as compared to CEA/CA19-9 (25%. CONCLUSION: We have described detection of CDO1 methylation in the plasma of CRC patients. Although CDO1 methylation was not detected as frequently as conventional tumor markers, analysis of plasma CDO1 methylation in combination with CEA/CA19-9 levels increases the detection rate of curable CRC patients.

  16. A method for studies on interactions between a gold-based drug and plasma proteins based on capillary electrophoresis with inductively coupled plasma mass spectrometry detection

    DEFF Research Database (Denmark)

    Nguyen, Tam T T N; Østergaard, Jesper; Gammelgaard, Bente

    2015-01-01

    An analytical method based on capillary electrophoresis (CE) and inductively coupled plasma mass spectrometry (ICP-MS) detection was developed for studies on the interaction of gold-containing drugs and plasma proteins using auranofin as example. A detection limit of 18 ng/mL of auranofin corresp...

  17. Arsenic speciation in seafood samples with emphasis on minor constituents. An investigation by high performance liquid chromatography with inductively coupled plasma mass spectrometric detection

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Pritzl, G.; Hansen, S. H.

    1993-01-01

    Extracts of 11 samples of shrimp, crab, fish, fish liver, shellfish and lobster digestive gland (hepatopancreas), including five certified reference materials, were investigated for their contents of arsenic compounds (arsenic speciation). The cation-exchange high performance liquid chromatography...... (as arsenic atom) relative to the total arsenic extracted from the samples were: arsenobetaine 19-98%, arsenocholine and trimethylarsine oxide 0-0.6% and the trimethylarsonium ion 0-2.2%. Additionally, an unknown arsenic species (U1) was present at 3.1-18% in the shellfish and in the lobster digestive...

  18. Clinical significance of detection of plasma natriuretic peptide in the diagnosis of patients with heart failure

    International Nuclear Information System (INIS)

    Song Chunli; Liu Haihong; Zhao Ning; Li Jie; Huang Jianmin

    2009-01-01

    To explore the clinical significance of plasma natriuretic peptide in the diagnosis of patients with heart failure (HF), the plasma atrial natriuretic peptide (ANP), brain natriuretic peptide (BNP), NT-pro brain natriuretic peptide (NT-proBNP) levels in 129 patients with heart failure and 30 healthy controls were detected by RIA and ELISA. The results showed that the plasma ANP, BNP, NT-proBNP levels in patients with heart failure were significantly higher than the healthy controls. As the cardiac function deteriorated from NYHA I to IV, the BNP and NT-proBNP levels increased consecutively with significant differences from each other. There was a negative correlation between the plasma ANP and NT-proBNP levels and LVEF. The determination of plasma ANP, BNP and NT-proBNP levels in patients with HF were helpful to the study of the severity and diagnosis of disease. (authors)

  19. Quantitative detection of plasma-generated radicals in liquids by electron paramagnetic resonance spectroscopy

    International Nuclear Information System (INIS)

    Tresp, H; Hammer, M U; Winter, J; Reuter, S; Weltmann, K-D

    2013-01-01

    In this paper the qualitative and quantitative detection of oxygen radicals in liquids after plasma treatment with an atmospheric pressure argon plasma jet by electron paramagnetic resonance spectroscopy is investigated. Absolute values for · OH and O 2 ·- radical concentration and their net production rate in plasma-treated liquids are determined without the use of additional scavenging chemicals such as superoxide dismutase (SOD) or mannitol (D-MAN). The main oxygen-centred radical generation in PBS was found to originate from the superoxide radical. It is shown that hidden parameters such as the manufacturer of chemical components could have a big influence on the comparability and reproducibility of the results. Finally, the effect of a shielding gas device for the investigated plasma jet with a shielding gas composition of varying oxygen-to-nitrogen ratio on radical generation after plasma treatment of phosphate-buffered saline solution was investigated. (paper)

  20. Mass Spectrometric Characteristics of Prenylated Indole Derivatives from Marine-Derived Penicillium sp. NH-SL.

    Science.gov (United States)

    Ding, Hui; Ding, Wanjing; Ma, Zhongjun

    2017-03-22

    Two prenylated indole alkaloids were isolated from the ethyl acetate extracts of a marine-derived fungus Penicillium sp. NH-SL and one of them exhibited potent cytotoxic activity against mouse hepa 1c1c7 cells. In order to detect other bioactive analogs, we used liquid chromatogram tandem mass spectrometry (LC-MS/MS) to analyze the mass spectrometric characteristics of the isolated compounds as well as the crude extracts. As a result, three other analogs were detected, and their structures were deduced according to the similar fragmentation patterns. This is the first systematic report on the mass spectrometric characteristics of prenylated indole derivatives.

  1. Concentrations of Nicotinamide in Plasma by RP-HPLC With Fluorescence Detection

    Directory of Open Access Journals (Sweden)

    Pan Zhipeng

    2016-01-01

    Full Text Available The purpose of this study is to establish a new method for detecting nicotinamide concentration in plasma. In the experiment, the high performance liquid chromatography (HPLC method was used, with a fluorescence detector. The nicotinamide in the plasma was first converted to N1- methylnicotinamide, then reacted with acetophenone under certain conditions to produce fluorescent derivatives for testing. The method is a kind of highly sensitive detection, of which the lower limit is 10 ng/mL, the recovery rate is between 92.75% and 105.13%, and the relative standard deviation (RSD is between 3.76% and 4.43%. The results showed that this measurement method is accurate, sensitive and rapid. It meets the requirements of the experiment, and applies to the detection of nicotinamide concentration in plasma.

  2. Detection of inverse Compton scattering in plasma wakefield experiments

    Energy Technology Data Exchange (ETDEWEB)

    Bohlen, Simon

    2016-12-15

    Inverse Compton scattering (ICS) is the process of scattering of photons and electrons, where the photons gain a part of the electrons energy. In combination with plasma wakefield acceleration (PWA), ICS offers a compact MeV γ-ray source. A numerical study of ICS radiation produced in PWA experiments at FLASHForward was performed, using an ICS simulation code and the results from particle-in-cell modelling. The possibility of determining electron beam properties from measurements of the γ-ray source was explored for a wide range of experimental conditions. It was found that information about the electron divergence, the electron spectrum and longitudinal information can be obtained from measurements of the ICS beams for some cases. For the measurement of the ICS profile at FLASHForward, a CsI(Tl) scintillator array was chosen, similar to scintillators used in other ICS experiments. To find a suitable detector for spectrum measurements, an experimental test of a Compton spectrometer at the RAL was conducted. This test showed that a similar spectrometer could also be used at FLASHForward. However, changes to the spectrometer could be needed in order to use the pair production effect. In addition, further studies using Geant4 could lead to a better reconstruction of the obtained data. The studies presented here show that ICS is a promising method to analyse electron parameters from PWA experiments in further detail.

  3. Non-invasive prenatal detection of achondroplasia using circulating fetal DNA in maternal plasma.

    Science.gov (United States)

    Lim, Ji Hyae; Kim, Mee Jin; Kim, Shin Young; Kim, Hye Ok; Song, Mee Jin; Kim, Min Hyoung; Park, So Yeon; Yang, Jae Hyug; Ryu, Hyun Mee

    2011-02-01

    To perform a reliable non-invasive detection of the fetal achondroplasia using maternal plasma. We developed a quantitative fluorescent-polymerase chain reaction (QF-PCR) method suitable for detection of the FGFR3 mutation (G1138A) causing achondroplasia. This method was applied in a non-invasive detection of the fetal achondroplasia using circulating fetal-DNA (cf-DNA) in maternal plasma. Maternal plasmas were obtained at 27 weeks of gestational age from women carrying an achondroplasia fetus or a normal fetus. Two percent or less achondroplasia DNA was reliably detected by QF-PCR. In a woman carrying a normal fetus, analysis of cf-DNA showed only one peak of the wild-type G allele. In a woman expected an achondroplasia fetus, analysis of cf-DNA showed the two peaks of wild-type G allele and mutant-type A allele and accurately detected the fetal achondroplasia. The non-invasive method using maternal plasma and QF-PCR may be useful for diagnosis of the fetal achondroplasia.

  4. Ex vivo spontaneous generation of 19-norandrostenedione and nandrolone detected in equine plasma and urine.

    Science.gov (United States)

    Guan, Fuyu; Uboh, Cornelius E; Soma, Lawrence R; You, Youwen; Li, Xiaoqing; McDonnell, Sue

    2012-01-01

    19-Norandrostenedione (NAED) and nandrolone are anabolic-androgenic steroids (AASs). Nandrolone was regarded solely as a synthetic AAS until the 1980s when trace concentrations of apparently endogenous nandrolone were detected in urine samples obtained from intact male horses (stallions). Since then, its endogenous origin has been reported in boars and bulls; endogenous NAED and nandrolone have been identified in plasma and urine samples collected from stallions. More recently, however, it was suggested that NAED and nandrolone detected in urine samples from stallions are primarily artifacts due to the analytical procedure. The present study was undertaken to determine whether NAED and nandrolone detected in plasma and urine samples collected from stallions are truly endogenous or artifacts from sample processing. To answer this question, fresh plasma and urine samples from ≥8 stallions were analyzed for the two AASs, soon after collection, by liquid chromatography hyphenated to tandem mass spectrometry (LC-MS/MS). NAED and nandrolone were not detected in fresh plasma samples but detected in the same samples post storage. Concentrations of both AASs increased with storage time, and the increases were greater at a higher storage temperature (37°C versus 4°C, and ambient temperature versus 4°C). Although NAED was detected in some fresh stallion urine samples, its concentration (samples post storage (at ambient temperature for 15 days). Nandrolone was not detected in most of fresh urine samples but detected in the same samples post storage. Based on these results, it is concluded that all NAED and nandrolone detected in stored plasma samples of stallions and most of them in the stored urine samples are not from endogenous origins but spontaneously generated during sample storage, most likely from spontaneous decarboxylation of androstenedione-19-oic acid and testosterone-19-oic acid. To our knowledge, it is the first time that all NAED and nandrolone detected in

  5. Detection of erbB2 copy number variations in plasma of patients with esophageal carcinoma

    International Nuclear Information System (INIS)

    Andolfo, Immacolata; Orditura, Michele; Ciardiello, Fortunato; De Vita, Fernando; Zollo, Massimo; Petrosino, Giuseppe; Vecchione, Loredana; De Antonellis, Pasqualino; Capasso, Mario; Montanaro, Donatella; Gemei, Marica; Troncone, Giancarlo; Iolascon, Achille

    2011-01-01

    Mortality is high in patients with esophageal carcinoma as tumors are rarely detected before the disease has progressed to an advanced stage. Here, we sought to isolate cell-free DNA released into the plasma of patients with esophageal carcinoma, to analyze copy number variations of marker genes in the search for early detection of tumor progression. Plasma of 41 patients with esophageal carcinoma was prospectively collected before tumor resection and chemotherapy. Our dataset resulted heterogeneous for clinical data, resembling the characteristics of the tumor. DNA from the plasma was extracted to analyze copy number variations of the erbB2 gene using real-time PCR assays. The real-time PCR assays for erbB2 gene showed significant (P = 0.001) copy number variations in the plasma of patients with esophageal carcinoma, as compared to healthy controls with high sensitivity (80%) and specificity (95%). These variations in erbB2 were negatively correlated to the progression free survival of these patients (P = 0.03), and revealed a further risk category stratification of patients with low VEGF expression levels. The copy number variation of erbB2 gene from plasma can be used as prognostic marker for early detection of patients at risk of worse clinical outcome in esophageal cancer

  6. Microcolumn high pressure liquid chromatography with a glass-frit nebulizer interface for plasma emission detection

    International Nuclear Information System (INIS)

    Ibrahim, M.; Nisamaneepong, W.; Caruso, J.

    1985-01-01

    Microcolumn high pressure liquid chromatography (micro-HPLC) is rapidly gaining recognition as a practical separation tool for organometallic compounds. The use of the inductively coupled plasma (ICP) as a detector for micro-HPLC is studied. Several miniaturized glass-frit nebulizers are investigated as interfaces between the output of the microbore column and the ICP torch. Their performance with aqueous and methanolic solutions is evaluated by direct nebulization and flow injection analysis. The most efficient of these nebulizers is used in the micro-HPLC/ICP study of some Cd, Pb, and Zn organometallic compounds. Detection limits of 1.92 ng of Pb for tetramethyllead and 5.01 ng of Pb for tetraethyllead are obtained and compared with regular HPLC/ICP of these same compounds. Approximately equivalent detection limits were obtained when using a microwave induced plasma as an alternate plasma source

  7. Plasma TIMP-1 and CEA as markers for detection of primary colorectal cancer

    DEFF Research Database (Denmark)

    Christensen, Ib Jarle; Brünner, Nils; Dowell, Barry

    2015-01-01

    endoscopy were prospectively included (N=1965). Baseline data and co-morbidity were recorded. The primary end-point was the detection of CRC. Plasma was obtained before endoscopy and TIMP-1 and CEA levels were determined using an automated analysis platform when all samples were collected. RESULTS: CRC...

  8. Detection of melanoma cells suspended in mononuclear cells and blood plasma using photoacoustic generation

    Science.gov (United States)

    Spradling, Emily M.; Viator, John A.

    2009-02-01

    Melanoma is the deadliest form of skin cancer. Although the initial malignant cells are removed, it is impossible to determine whether or not the cancer has metastasized until a secondary tumor forms that is large enough to detect with conventional imaging. Photoacoustic detection of circulating melanoma cells in the bloodstream has shown promise for early detection of metastasis that may aid in treatment of this aggressive cancer. When blood is irradiated with energy from an Nd:YAG laser at 532 nm, photoacoustic signals are created and melanoma cells can be differentiated from the surrounding cells based on waveforms produced by an oscilloscope. Before this can be used as a diagnostic technique, however, we needed to investigate several parameters. Specifically, the current technique involves the in vitro separation of blood through centrifugation to isolate and test only the white blood cell layer. Using this method, we have detected a single cultured melanoma cell among a suspension of white blood cells. However, the process could be made simpler if the plasma layer were used for detection instead of the white blood cell layer. This layer is easier to obtain after blood separation, the optical difference between plasma and melanoma cells is more pronounced in this layer than in the white blood cell layer, and the possibility that any stray red blood cells could distort the results is eliminated. Using the photoacoustic apparatus, we detected no melanoma cells within the plasma of whole blood samples spiked with cultured melanoma cells.

  9. Plasma membrane damage detected by nucleic acid leakage

    International Nuclear Information System (INIS)

    Fortunati, E.; Bianchi, V.

    1989-01-01

    Among the indicators of membrane damage, the leakage of intracellular components into the medium is the most directly related to the perturbations of the membrane molecular organization. The extent of the damage can be evaluated from the size of the released components. We have designed a protocol for the detection of membrane leakage based on the preincubation of cells with tritiated adenine for 24 h, followed by a 24-h chase in nonradioactive medium. The treatment takes place when the distribution of the precursor among its end products has reached the plateau, and thus the differences of radioactivity in the fractions obtained from the control and treated cultures (medium, nucleotide pool, RNA, DNA) correspond to actual quantitative variations induced by the test chemical. Aliquots of the medium are processed to determine which percentage of the released material is macromolecular, in order to distinguish between mild and severe membrane damage. The origin of the extracellular radioactivity can be recognized from the variations of RNA counts in the treated cells. DNA radioactivity is used to evaluate the number of cells that remain attached to the plates in the different conditions of treatment. By this means, generalized permeabilization of membranes to macromolecules is distinguished from complete solubilization of only a subpopulation of cells. We present some examples of application of the protocol with detergents (LAS, SDS, Triton X-100) and with Cr(VI), which damages cell membranes by a different mechanism of action

  10. Quantitative mass-spectrometric analysis of hydrogen helium isotope mixtures

    International Nuclear Information System (INIS)

    Langer, U.

    1998-12-01

    This work deals with the mass-spectrometric method for the quantitative analysis of hydrogen-helium-isotope mixtures, with special attention to fusion plasma diagnostics. The aim was to use the low-resolution mass spectrometry, a standard measuring method which is well established in science and industry. This task is solved by means of the vector mass spectrometry, where a mass spectrum is repeatedly measured, but with stepwise variation of the parameter settings of a quadruple mass spectrometer. In this way, interfering mass spectra can be decomposed and, moreover, it is possible to analyze underestimated mass spectra of complex hydrogen-helium-isotope mixtures. In this work experimental investigations are presented which show that there are different parameters which are suitable for the UMS-method. With an optimal choice of the parameter settings hydrogen-helium-isotope mixtures can be analyzed with an accuracy of 1-3 %. In practice, a low sensitivity for small helium concentration has to be noted. To cope with this task, a method for selective hydrogen pressure reduction has been developed. Experimental investigations and calculations show that small helium amounts (about 1 %) in a hydrogen atmosphere can be analyzed with an accuracy of 3 - 10 %. Finally, this work deals with the effects of the measuring and calibration error on the resulting error in spectrum decomposition. This aspect has been investigated both in general mass-spectrometric gas analysis and in the analysis of hydrogen-helium-mixtures by means of the vector mass spectrometry. (author)

  11. Significance of Airborne Gamma-ray spectrometric data of Umm bisilla Area, central Eastern Desert, Egypt

    Energy Technology Data Exchange (ETDEWEB)

    Rabie, S I [Nuclear materials authority, Maadi, Cairo, (Egypt)

    1995-10-01

    Umm bisilla area, located in the Central Eastern Desert of Egypt, consists mainly of basement rocks. The present investigation of the airborne spectrometric data is to define the meaningful anomalies from the raw data by applying the significance factor techniques, by calculating the significant radioactive provinces. Determination of the gross structural pattern and broad variations in composition of the crystalline basement, to define the relationships between the tectonic features of the area as interpreted from aeromagnetic data, with the significant anomalies revealed from spectrometric data was carried out through the application of different magnetic techniques. Five significant uraniferous zones were detected associated with Umm Bisilla granite, amphibolite, and grey granite. The intersection of the structural lineaments interpreted from aeromagnetic data illustrated good correlation with the significant uranium anomalous zones interpreted from spectrometric data, and indicated that the concentration is structurally. 15 figs.

  12. Plasma diagnostics: Detection of laser scattering: Final report, September 1, 1978 to August 31, 1982

    International Nuclear Information System (INIS)

    Dutta, J.M.; Jones, C.R.

    1985-01-01

    Submillimeter (SMM) radiation is the optimum radiation to use in studying some parameters of plasmas produced in Tokamak machines. The ultimate objective has been in constructing a low-noise SMM receiver suitable for application to the diagnosis of Tokamak plasmas. In this connection, a compact, stable SMM laser has been designed and constructed, and its performance as a local oscillator in the heterodyne detection has been tested. The performance of Schottky diodes as mixer elements has been evaluated by utilizing them in a quasi-optical modulation for the heterodyne generation of tunable sidebands

  13. Liquid chromatography-tandem mass spectrometric assay for the simultaneous determination of the irreversible BTK inhibitor ibrutinib and its dihydrodiol-metabolite in plasma and its application in mouse pharmacokinetic studies

    NARCIS (Netherlands)

    Rood, Johannes J M; van Hoppe, Stephanie; Schinkel, Alfred H.; Schellens, Jan H M; Beijnen, Jos H.; Sparidans, Rolf W.

    2016-01-01

    A validated simple, fast and sensitive bio-analytical assay for ibrutinib and its dihydrodiol metabolite in human and mouse plasma was set up. Sample preparation was performed by protein precipitation, and addition of the respective deuterated internal standards, followed by LC-MS/MS analysis.

  14. Hybrid Synthetic Receptors on MOSFET Devices for Detection of Prostate Specific Antigen in Human Plasma.

    Science.gov (United States)

    Tamboli, Vibha K; Bhalla, Nikhil; Jolly, Pawan; Bowen, Chris R; Taylor, John T; Bowen, Jenna L; Allender, Chris J; Estrela, Pedro

    2016-12-06

    The study reports the use of extended gate field-effect transistors (FET) for the label-free and sensitive detection of prostate cancer (PCa) biomarkers in human plasma. The approach integrates for the first time hybrid synthetic receptors comprising of highly selective aptamer-lined pockets (apta-MIP) with FETs for sensitive detection of prostate specific antigen (PSA) at clinically relevant concentrations. The hybrid synthetic receptors were constructed by immobilizing an aptamer-PSA complex on gold and subjecting it to 13 cycles of dopamine electropolymerization. The polymerization resulted in the creation of highly selective polymeric cavities that retained the ability to recognize PSA post removal of the protein. The hybrid synthetic receptors were subsequently used in an extended gate FET setup for electrochemical detection of PSA. The sensor was reported to have a limit of detection of 0.1 pg/mL with a linear detection range from 0.1 pg/mL to 1 ng/mL PSA. Detection of 1-10 pg/mL PSA was also achieved in diluted human plasma. The present apta-MIP sensor developed in conjunction with FET devices demonstrates the potential for clinical application of synthetic hybrid receptors for the detection of clinically relevant biomarkers in complex samples.

  15. Mass spectrometric methods for trace analysis of metals

    International Nuclear Information System (INIS)

    Bahr, U.; Schulten, H.R.

    1981-01-01

    A brief outline is given of the principles of mass spectrometry (MS) and the fundamentals of qualitative and quantitative mass spectrometric analysis emphasizing recent developments and results. Classical methods of the analysis of solids, i.e. spark-source MS and thermal ionization MS, as well as recent methods of metal analysis are described. Focal points in this survey of recently developed techniques include secondary ion MS, laser probe MS, plasma ion source MS, gas discharge MS and field desorption MS. Here, a more detailed description is given and the merits of these emerging methods are discussed more explicitly. In particular, the results of the field desorption techniques in elemental analyses are reviewed and critically evaluated

  16. Structure elucidation of metabolite x17299 by interpretation of mass spectrometric data.

    Science.gov (United States)

    Zhang, Qibo; Ford, Lisa A; Evans, Anne M; Toal, Douglas R

    2017-01-01

    A major bottleneck in metabolomic studies is metabolite identification from accurate mass spectrometric data. Metabolite x17299 was identified in plasma as an unknown in a metabolomic study using a compound-centric approach where the associated ion features of the compound were used to determine the true molecular mass. The aim of this work is to elucidate the chemical structure of x17299, a new compound by de novo interpretation of mass spectrometric data. An Orbitrap Elite mass spectrometer was used for acquisition of mass spectra up to MS 4 at high resolution. Synthetic standards of N,N,N -trimethyl-l-alanyl-l-proline betaine (l,l-TMAP), a diastereomer, and an enantiomer were chemically prepared. The planar structure of x17299 was successfully proposed by de novo mechanistic interpretation of mass spectrometric data without any laborious purification and nuclear magnetic resonance spectroscopic analysis. The proposed structure was verified by deuterium exchanged mass spectrometric analysis and confirmed by comparison to a synthetic standard. Relative configuration of x17299 was determined by direct chromatographic comparison to a pair of synthetic diastereomers. Absolute configuration was assigned after derivatization of x17299 with a chiral auxiliary group followed by its chromatographic comparison to a pair of synthetic standards. The chemical structure of metabolite x17299 was determined to be l,l-TMAP.

  17. Active Detectors for Plasma Soft X-Ray Detection at PALS

    Directory of Open Access Journals (Sweden)

    C. Granja

    2010-01-01

    Full Text Available This paper summarizes the work carried out for an experimental study of low-energy nuclear excitation by laser-produced plasma at the PALS Prague laser facility. We describe the adaptation and shielding of single-quantum active radiation detectors developed at IEAP CTU Prague to facilitate their operation inside the laser interaction chamber in the vicinity of the plasma target. The goal of this effort is direct real-time single-quantum detection of plasma soft X-ray radiation with energy above a few keV and subsequent identification of the decay of the excited nuclear states via low-energy gamma rays in a highly radiative environment with strong electromagnetic interference.

  18. Influenza A plasma and serum virus antibody detection comparison in dogs using blocking enzyme-linked immunosorbent assay

    Directory of Open Access Journals (Sweden)

    H. T. Lin

    2015-05-01

    Full Text Available Background and Aim: The influenza A virus (IAV is an important zoonotic pathogen with infections also reported in dogs. IAV infections can be detected through the presence of antibodies using the enzyme-linked immunosorbent assay (ELISA. Serum is the only standard sample source; however, there is no information on the availability of other sample sources for IAV antibody detection in dogs. Compared with serum, plasma is more widely employed in most animal hospitals. The object of this study is to investigate whether plasma collected in ethylenediaminetetraacetic acid (EDTA tubes (EDTA plasma or heparin tubes (heparin plasma could be used in the ELISA protocol instead of serum for IAV antibody detection in dogs. Materials and Methods: Totally, 82 matched EDTA plasma and serum sample pairs and 79 matched heparin plasma and serum sample pairs were employed using blocking enzyme-linked immunosorbent assay (bELISA. The agreement and correlation between the plasma (EDTA or heparin plasma and serum were assessed using the agreement index kappa (kD calculation and Pearson correlation coefficient, respectively. Results: The agreement index kD of EDTA plasma and serum was 1.0, and that of heparin plasma and serum was 0.85. The Pearson correlation coefficient of EDTA plasma and serum was 0.87 (p<0.01, and that of heparin plasma and serum was 0.82 (p<0.01. Conclusion: The results proved that plasma, especially EDTA plasma, could be substituted for serum in the bELISA test. This might greatly expand the clinical applicability of IAV antibody detection in dogs.

  19. Plasma-derived exosomal survivin, a plausible biomarker for early detection of prostate cancer.

    Directory of Open Access Journals (Sweden)

    Salma Khan

    Full Text Available Survivin is expressed in prostate cancer (PCa, and its downregulation sensitizes PCa cells to chemotherapeutic agents in vitro and in vivo. Small membrane-bound vesicles called exosomes, secreted from the endosomal membrane compartment, contain RNA and protein that they readily transport via exosome internalization into recipient cells. Recent progress has shown that tumor-derived exosomes play multiple roles in tumor growth and metastasis and may produce these functions via immune escape, tumor invasion and angiogenesis. Furthermore, exosome analysis may provide novel biomarkers to diagnose or monitor PCa treatment.Exosomes were purified from the plasma and serum from 39 PCa patients, 20 BPH patients, 8 prostate cancer recurrent and 16 healthy controls using ultracentrifugation and their quantities and qualities were quantified and visualized from both the plasma and the purified exosomes using ELISA and Western blotting, respectively.Survivin was significantly increased in the tumor-derived samples, compared to those from BPH and controls with virtually no difference in the quantity of Survivin detected in exosomes collected from newly diagnosed patients exhibiting low (six or high (nine Gleason scores. Exosome Survivin levels were also higher in patients that had relapsed on chemotherapy compared to controls.These studies demonstrate that Survivin exists in plasma exosomes from both normal, BPH and PCa subjects. The relative amounts of exosomal Survivin in PCa plasma was significantly higher than in those with pre-inflammatory BPH and control plasma. This differential expression of exosomal Survivin was seen with both newly diagnosed and advanced PCa subjects with high or low-grade cancers. Analysis of plasma exosomal Survivin levels may offer a convenient tool for diagnosing or monitoring PCa and may, as it is elevated in low as well as high Gleason scored samples, be used for early detection.

  20. Liquid chromatographic-mass spectrometric method for ...

    African Journals Online (AJOL)

    Tropical Journal of Pharmaceutical Research ... Purpose: To develop and validate a simple, efficient and reliable Liquid chromatographic-mass spectrometric (LC-MS/MS) method for the quantitative determination of two dermatological drugs, ... By Country · List All Titles · Free To Read Titles This Journal is Open Access.

  1. Mass spectrometric researches in isotope cosmochemistry

    International Nuclear Information System (INIS)

    Gopalan, K.

    1979-01-01

    Recent advances in the understanding of solar system processes, past and present, based on mass spectrometric researches on meteorites and moon samples are reviewed. The topics include the following : (1) Duration of nebular condensation, (2) Terminal stages of nucleosynthesis, (3) Planetary formation and evolution, (4) Heterogeneities in the solar nebula and (5) Solar wind composition. (auth.)

  2. Plasma-treated polyethylene film: A smart material applied for Salmonella Typhimurium detection

    Energy Technology Data Exchange (ETDEWEB)

    Peng-Ubol, Triranat [Department of Chemistry, Faculty of Science, Mahidol University, Rama 6 Rd, Phayathai, Bangkok 10400 (Thailand); Phinyocheep, Pranee, E-mail: scppo@mahidol.ac.th [Department of Chemistry, Faculty of Science, Mahidol University, Rama 6 Rd, Phayathai, Bangkok 10400 (Thailand); Daniel, Philippe [Laboratoire de Physique de l' Etat Condense (LPEC-UMR CNRS 6087), Universite du Maine, Avenue Olivier Messiaen, 72085, Le Mans Cedex 9 (France); Panbangred, Watanalai [Department of Biotechnology and Mahidol University-Osaka University Collaborative Research Center for Bioscience and Biotechnology (MU-OU: CRC), Faculty of Science, Mahidol University, Rama 6 Rd, Phayathai, Bangkok 10400 (Thailand); Pilard, Jean-Francois [Unite de Chimie Organique Moleculaire et Macromoleculaire (UCO2M-UMR CNRS 6011), Universite du Maine, Avenue Olivier Messiaen, 72085 Le Mans Cedex 9 (France); Thouand, Gerald; Durand-Thouand, Marie-Jose [Genie des Procedes Environnement et Agroalimentaire (GEPEA UMR CNRS 6144), Departement Genie Biologique, IUT de la Roche/Yon, Universite de Nantes, 18 Bd G. Defferre, 85035 La Roche sur Yon (France)

    2012-12-01

    Salmonella is a major cause of foodborne illness worldwide and is not allowed to be present in any food in all countries. The purpose of this study is to develop a simple alternative method for the detection of Salmonella based on functionalized polyethylene (PE) surfaces. Salmonella Typhimurium was used as a model bacterium. PE film was treated using dielectric plasma in order to alter the wettability of the PE surface and consequently introduce functionality on the surface. The PE film characterized by ATR-FTIR spectroscopy revealed the presence of C=O stretching of ketones, aldehydes and carboxylic acids. The antibodies against O or H antigens of Salmonella and S. Typhimurium were then respectively immobilized on the PE surface after activation of the carboxylic group using NHS/EDC followed by protein A. The evidences from ATR-FTIR, scanning electron microscopy and optical microscopy showed the presence of S. Typhimurium attached to the plasma treated PE surfaces via the two types of anti-Salmonella antibody. The plasma treated PE film developed is simple and allows efficient association of bacterial cells on the treated surfaces without the necessity of time-consuming centrifugation and washing steps for isolation of the cells. This material is considered to be a smart material applicable for S. Typhimurium detection. Highlights: Black-Right-Pointing-Pointer We developed a functionalized polyethylene film for bacterial detection. Black-Right-Pointing-Pointer We modified the surface of polyethylene film by plasma treatment. Black-Right-Pointing-Pointer ATR-FTIR spectroscopy was used to analyze the functionality on the PE surface. Black-Right-Pointing-Pointer We introduced Salmonella Typhimurium on the modified PE film. Black-Right-Pointing-Pointer SEM revealed the presence of S. Typhimurium on the plasma treated PE film.

  3. Plasma-treated polyethylene film: A smart material applied for Salmonella Typhimurium detection

    International Nuclear Information System (INIS)

    Peng-Ubol, Triranat; Phinyocheep, Pranee; Daniel, Philippe; Panbangred, Watanalai; Pilard, Jean-François; Thouand, Gerald; Durand-Thouand, Marie-José

    2012-01-01

    Salmonella is a major cause of foodborne illness worldwide and is not allowed to be present in any food in all countries. The purpose of this study is to develop a simple alternative method for the detection of Salmonella based on functionalized polyethylene (PE) surfaces. Salmonella Typhimurium was used as a model bacterium. PE film was treated using dielectric plasma in order to alter the wettability of the PE surface and consequently introduce functionality on the surface. The PE film characterized by ATR-FTIR spectroscopy revealed the presence of C=O stretching of ketones, aldehydes and carboxylic acids. The antibodies against O or H antigens of Salmonella and S. Typhimurium were then respectively immobilized on the PE surface after activation of the carboxylic group using NHS/EDC followed by protein A. The evidences from ATR-FTIR, scanning electron microscopy and optical microscopy showed the presence of S. Typhimurium attached to the plasma treated PE surfaces via the two types of anti-Salmonella antibody. The plasma treated PE film developed is simple and allows efficient association of bacterial cells on the treated surfaces without the necessity of time-consuming centrifugation and washing steps for isolation of the cells. This material is considered to be a smart material applicable for S. Typhimurium detection. Highlights: ► We developed a functionalized polyethylene film for bacterial detection. ► We modified the surface of polyethylene film by plasma treatment. ► ATR-FTIR spectroscopy was used to analyze the functionality on the PE surface. ► We introduced Salmonella Typhimurium on the modified PE film. ► SEM revealed the presence of S. Typhimurium on the plasma treated PE film.

  4. Spectrometric methods for the determination of chlorine in crude oil and petroleum derivatives — A review

    International Nuclear Information System (INIS)

    Doyle, Adriana; Saavedra, Alvaro; Tristão, Maria Luiza B.; Mendes, Luiz A.N.; Aucélio, Ricardo Q.

    2013-01-01

    Chlorine determination in crude oil is made in order to guarantee that the oil does not contain levels of this element that might cause damages in the oil processing equipment. In petroleum products, the determination of chlorine is made, for instance, to evaluate if there are proper concentrations of organochloride compounds, which are used as additives. Such determinations are currently performed following official guidelines from the ASTM International and from the United States Environmental Protection Agency as well as protocols indicated by the Universal Oil Products. X-ray fluorescence spectroscopy plays an important role in many of these official methods. In contrast, other spectrometric methods based on optical and mass detection are plagued by limitations related to both the fundamental characteristics of non-metals and to the complex sample matrices, which reflects in the small number of articles devoted to these applications. In this review, the current status of the spectrometric methods, especially the role played by X-ray fluorescence spectrometry, is evaluated in terms of the determination of chlorine in crude oil and petroleum derivatives. Comparison of the performance of the methods, limitations and potential new approaches to ensure proper spectrometric determinations of chlorine is indicated. - Highlights: • Critical evaluation of spectrometric methods for chlorine in petroleum products. • Reviews on element determination in petroleum have not address the case of chlorine. • Peculiarities of the spectrometric determination of Cl in petroleum are discussed. • The spectrometric approaches are detailed and compared to the official methods. • New trends in chlorine determination in petroleum products are indicated

  5. Detecting subtle plasma membrane perturbation in living cells using second harmonic generation imaging.

    Science.gov (United States)

    Moen, Erick K; Ibey, Bennett L; Beier, Hope T

    2014-05-20

    The requirement of center asymmetry for the creation of second harmonic generation (SHG) signals makes it an attractive technique for visualizing changes in interfacial layers such as the plasma membrane of biological cells. In this article, we explore the use of lipophilic SHG probes to detect minute perturbations in the plasma membrane. Three candidate probes, Di-4-ANEPPDHQ (Di-4), FM4-64, and all-trans-retinol, were evaluated for SHG effectiveness in Jurkat cells. Di-4 proved superior with both strong SHG signal and limited bleaching artifacts. To test whether rapid changes in membrane symmetry could be detected using SHG, we exposed cells to nanosecond-pulsed electric fields, which are believed to cause formation of nanopores in the plasma membrane. Upon nanosecond-pulsed electric fields exposure, we observed an instantaneous drop of ~50% in SHG signal from the anodic pole of the cell. When compared to the simultaneously acquired fluorescence signals, it appears that the signal change was not due to the probe diffusing out of the membrane or changes in membrane potential or fluidity. We hypothesize that this loss in SHG signal is due to disruption in the interfacial nature of the membrane. The results show that SHG imaging has great potential as a tool for measuring rapid and subtle plasma membrane disturbance in living cells. Copyright © 2014 Biophysical Society. Published by Elsevier Inc. All rights reserved.

  6. Lack of detection of XMRV in seminal plasma from HIV-1 infected men in The Netherlands.

    Directory of Open Access Journals (Sweden)

    Marion Cornelissen

    Full Text Available BACKGROUND: Xenotropic murine leukaemia virus-related virus (XMRV is a recently discovered human gammaretrovirus with yet unknown prevalence and transmission route(s. Its presence in prostate stromal fibroblasts and prostatic secretions suggests that XMRV might be sexually transmitted. We chose to study a compartment closely connected to the prostate, a location where XMRV was detected in independent studies. Seminal plasma samples from HIV-1 infected men were examined as they have an increased probability of acquiring sexually transmitted pathogens. METHODOLOGY/PRINCIPAL FINDINGS: We studied the prevalence of XMRV in 93 seminal plasma samples of 54 HIV-1 infected men living in The Netherlands with a nested PCR amplification specifically targeting the XMRV gag gene. As a control for the presence and integrity of retrovirus particles, HIV-1 was amplified from the same samples with a PCR amplification targeting the env gene of the virus, or HIV-1 was quantified with a real-time PCR amplifying part of the pol gene. CONCLUSIONS/SIGNIFICANCE: Although HIV-1 was amplified from 25% of the seminal plasma samples, no XMRV was detected, suggesting that either the prevalence of XMRV is very low in The Netherlands, or that XMRV is not naturally present in the seminal plasma.

  7. Quantification of pharmaceutical peptides in human plasma by LC-ICP-MS sulfur detection

    DEFF Research Database (Denmark)

    Møller, Laura Hyrup; Macherius, André; Hansen, Thomas Hesselhøj

    2016-01-01

    A method for quantification of a pharmaceutical peptide in human plasma was developed using gradient elution LC-ICP-MS. A membrane desolvation (MD) system was applied to remove organic solvents from the eluent prior to the detection as SO+ in the dynamic reaction cell (DRC) of the ICP-DRC-MS inst......A method for quantification of a pharmaceutical peptide in human plasma was developed using gradient elution LC-ICP-MS. A membrane desolvation (MD) system was applied to remove organic solvents from the eluent prior to the detection as SO+ in the dynamic reaction cell (DRC) of the ICP......-DRC-MS instrument and subsequent quantification by post-column isotope dilution (IDA). Plasma proteins were precipitated prior to analysis. Analytical figures of merit including linearity, precision, LOD, LOQ and accuracy were considered satisfactory for analysis of plasma samples. The selectivity of the developed...... method was demonstrated for five pharmaceutically relevant peptides: desmopressin, penetratin, substance P, PTH (1-34) and insulin. Preliminary experiments on an ICP-MS/MS system using oxygen to reduce the effect of organic solvents were also performed to compare sensitivity. The results of the study...

  8. Surface plasmon resonance investigation of optical detection in plasma-modified phospholipid layers

    International Nuclear Information System (INIS)

    Park, Byoungchoo; Cho, Chanyoun; Choi, Kyoungho; Jeon, Honggoo

    2012-01-01

    We herein report on a study of surface plasmon resonance (SPR) in thin gold (Au) films coated with thin layers of phospholipid material, which had been exposed to an atmospheric pressure (AP) plasma containing both pure Ar and Ar mixed with O 2 (Ar/O 2 , 0.8%). The phospholipid material that we used for the SPR experiments was lecithin, and the AP plasma system was applied in air by means of a radio-frequency (RF) plasma generator. A thin (∼60 nm) film of Au and a thin (∼15 nm) layer of lecithin were deposited and attached to the face of a prism, and surface plasmon modes were excited along the interfaces of the prism-Au-lecithin-air system by means of prism coupling using a He-Ne Laser (632.8 nm). The experimental SPR reflectance curves of the Au-lecithin-air modes were found to be shifted towards those of the Au-air mode with increasing applications of AP RF plasma treatment. From the shifts in the SPR curves, we found that the estimated thickness of the lecithin layer treated with a pure Ar plasma showed a linear decrease with etching rate of about 3 nm per treatment while the thickness of the lecithin layer treated with a mixed Ar/O 2 plasma showed a tendency to saturate following a large initial decrease (ca. 14 nm). All these results demonstrate that the use of SPR sensing could facilitate the detection of extremely small variations in plasma-treated films of biomaterials.

  9. Methods for detecting and correcting inaccurate results in inductively coupled plasma-atomic emission spectrometry

    Science.gov (United States)

    Chan, George C. Y. [Bloomington, IN; Hieftje, Gary M [Bloomington, IN

    2010-08-03

    A method for detecting and correcting inaccurate results in inductively coupled plasma-atomic emission spectrometry (ICP-AES). ICP-AES analysis is performed across a plurality of selected locations in the plasma on an unknown sample, collecting the light intensity at one or more selected wavelengths of one or more sought-for analytes, creating a first dataset. The first dataset is then calibrated with a calibration dataset creating a calibrated first dataset curve. If the calibrated first dataset curve has a variability along the location within the plasma for a selected wavelength, errors are present. Plasma-related errors are then corrected by diluting the unknown sample and performing the same ICP-AES analysis on the diluted unknown sample creating a calibrated second dataset curve (accounting for the dilution) for the one or more sought-for analytes. The cross-over point of the calibrated dataset curves yields the corrected value (free from plasma related errors) for each sought-for analyte.

  10. Identification of organic iodocompounds in the PUREX process with the help of methods for chromatographic separation and spectrometric detection as well as characterization of their behavior during extraction. Final report

    International Nuclear Information System (INIS)

    Gaul, G.; Gibau, F.; Knoechel, A.

    1993-01-01

    In the system HNO 3 KI, Dodecan and TBP the radiolytic reactive behaviour of the described compounds during the dissolution of nuclear fuel elements was simulated. External γ-irradiation gave the best informations. As a consequence of radiolyticly induced reactions several volatile and non-volatile iodoorganic compounds like iodoalkanes, iodonitroalkanes and iodonitroalkylphosphates are formed. They were separated by gaschromatography (GC) and high performance liquid chromatography (HPLC). For HPLC a special photolytic/electrochemical detector with comparable sensitivity like the electroncapture detector in the GC-field was developed. With the help of the two described chromatographic techniques the different iodoorganic compounds could be separated singularily or in groups of isomers. The separation of all compounds demands two-dimensional chromatographies including the capillary-SFC, which was not available for this project. Most of the iodoorganic compounds could be identified by comparison of the retention times of well known compounds. In the other cases, the compounds were studied mass-spectrometrically. Unfortunately all available ionisation techniques (EI; CI; FAB) were too hard for the labile C-I-bond. Therefore an identification of these compounds was not possible. In any case, instructive fingerprint spectra are available enabling relationships between the generation of the iodoorganic compounds and the reaction conditions during their formation. (orig.) [de

  11. HPLC/Fluorometric Detection of Carvedilol in Real Human Plasma Samples Using Liquid-Liquid Extraction.

    Science.gov (United States)

    Yilmaz, Bilal; Arslan, Sakir

    2016-03-01

    A simple, rapid and sensitive high-performance liquid chromatography (HPLC) method has been developed to quantify carvedilol in human plasma using an isocratic system with fluorescence detection. The method included a single-step liquid-liquid extraction with diethylether and ethylacetate mixture (3 : 1, v/v). HPLC separation was carried out by reversed-phase chromatography with a mobile phase composed of 20 mM phosphate buffer (pH 7)-acetonitrile (65 : 35, v/v), pumped at a flow rate of 1.0 mL/min. Fluorescence detection was performed at 240 nm (excitation) and 330 nm (emission). The calibration curve for carvedilol was linear from 10 to 250 ng/mL. Intra- and interday precision values for carvedilol in human plasma were plasma averaged out to 91.8%. The limits of detection and quantification of carvedilol were 3.0 and 10 ng/mL, respectively. Also, the method was successfully applied to three patients with hypertension who had been given an oral tablet of 25 mg carvedilol. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  12. Detection of tetracosactide in plasma by enzyme-linked immunosorbent assay (ELISA).

    Science.gov (United States)

    Martin, Laurent; Chaabo, Ayman; Lasne, Françoise

    2015-06-01

    As a synthetic analogue of adrenocorticotropic hormone (ACTH), tetracosactide is prohibited in sport by the World Anti-Doping Agency (WADA). An enzyme-linked immunosorbent assay (ELISA) method is proposed for detection of this drug in plasma. Since its structure corresponds to the 24 N-terminal of the 39 amino acids of the natural endogenous peptide ACTH, tetracosactide can be detected with a commercial ELISA kit for ACTH that uses antibodies, the epitopes of which are located in the 1-24 part of ACTH. However, an essential condition for detection specificity is the preliminary total clearance of endogenous ACTH in the plasma samples. This is achieved by a preparative step based on cation-exchange chromatography before ELISA. The method is specific and sensitive (LOD: 30 pg/mL) and may be used as a screening analysis in anti-doping control. The pre-analytical conditions are shown to be of the upmost importance and recommendations for blood collection (EDTA tubes), sample transport (4 °C) and plasma sample storage (-20 °C) are presented. Copyright © 2014 John Wiley & Sons, Ltd.

  13. Sheath-lens probe for negative ion detection in reactive plasmas

    International Nuclear Information System (INIS)

    Stamate, E.; Sugai, H.; Takai, O.; Ohe, K.

    2004-01-01

    A method that allows easy and inexpensive detection of negative ions is introduced. The method is based upon the electrostatic lens effect of the sheath layer evolving to a positively biased planar probe that focuses the negative charges to distinct regions on the surface. Trajectories of negative ions inside the sheath are obtained after computing the potential and electric field distribution by solving in three dimensions the nonlinear Poisson equation. The negative ions' flux to square and disk probes is developed in Ar/SF 6 and O 2 plasmas. The method allows negative ion detection with sensitivity higher than that of Langmuir probes

  14. Bioanalytical development and validation of liquid chromatographic–tandem mass spectrometric methods for the quantification of total and free cefazolin in human plasma and cord blood

    Directory of Open Access Journals (Sweden)

    Christopher A. Crutchfield

    2015-04-01

    Full Text Available Objectives: Cefazolin is a commonly prescribed β-lactam antibiotic for prophylaxis against skin infections following surgery, including caesarean sections. Assessment of maternal and neonatal exposure is important for correlating drug concentrations to clinical outcomes. Thus, bioanalytical methods for the quantification of both total and free cefazolin in maternal plasma and cord blood can assist in the comprehensive evaluation of cefazolin exposure. Design and methods: Specimen preparation for the measurement of total cefazolin was performed via protein precipitation with acetonitrile containing the internal standard cloxacillin. Ultrafiltration was used to isolate free cefazolin. Processed samples were analyzed on a Prelude SPLC system coupled to a TSQ triple quadrupole Vantage mass spectrometer. Methods were validated following FDA bioanalytical guidelines. Results: The analytical measuring ranges of these methods were 0.48–480 µg/mL and 0.048–48 µg/mL for total and free drug, respectively. Calibration curves were generated using 1/x2 weighted linear regression analysis. Total cefazolin demonstrated inter- and intra-assay precision of ≤20% at the LLOQ and ≤11.2% at other levels. Free cefazolin demonstrated inter- and intra-assay precision of ≤18.5% at the LLOQ and ≤12.6% at other levels, respectively. Accuracy (%DEV, carryover, matrix effects, recovery and stability studies were also acceptable based on FDA recommendations. Furthermore, it was demonstrated that samples prepared in cord blood can be accurately quantified from an adult plasma calibration curve, with recoveries ≤9.1% DIF and ≤11.9% DIF for total and free cefazolin, respectively. Conclusions: The described LC–MS/MS methods allow for the measurement of total and free cefazolin in both plasma and cord blood. Keywords: Mass spectrometry, Method validation, Cefazolin, Antibiotic, Ultrafiltration

  15. MYC protein expression is detected in plasma cell myeloma but not in monoclonal gammopathy of undetermined significance (MGUS).

    Science.gov (United States)

    Xiao, Ruobing; Cerny, Jan; Devitt, Katherine; Dresser, Karen; Nath, Rajneesh; Ramanathan, Muthalagu; Rodig, Scott J; Chen, Benjamin J; Woda, Bruce A; Yu, Hongbo

    2014-06-01

    It has been recognized that monoclonal gammopathy of undetermined significance (MGUS) precedes a diagnosis of plasma cell myeloma in most patients. Recent gene expression array analysis has revealed that an MYC activation signature is detected in plasma cell myeloma but not in MGUS. In this study, we performed immunohistochemical studies using membrane CD138 and nuclear MYC double staining on bone marrow biopsies from patients who met the diagnostic criteria of plasma cell myeloma or MGUS. Our study demonstrated nuclear MYC expression in CD138-positive plasma cells in 22 of 26 (84%) plasma cell myeloma samples and in none of the 29 bone marrow samples from patients with MGUS. In addition, our data on the follow-up biopsies from plasma cell myeloma patients with high MYC expression demonstrated that evaluation of MYC expression in plasma cells can be useful in detecting residual disease. We also demonstrated that plasma cells gained MYC expression in 5 of 8 patients (62.5%) when progressing from MGUS to plasma cell myeloma. Analysis of additional lymphomas with plasmacytic differentiation, including lymphoplasmacytic lymphoma, marginal zone lymphoma, and plasmablastic lymphoma, reveals that MYC detection can be a useful tool in the diagnosis of plasma cell myeloma.

  16. Speciation of four selenium compounds using high performance liquid chromatography with on-line detection by inductively coupled plasma mass spectrometry or flame atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Pedersen, Gitte Alsing; Larsen, Erik Huusfeldt

    1997-01-01

    An analytical method for the speciation of selenomethionine, selenocystine, selenite and selenate by high performance liquid chromatography (HPLC) with atomic spectrometric detection is presented. An organic polymeric strong anion exchange column was used as the stationary phase in combination...... spectrometry (ICP-MS). The signal-to-noise ratio of the FAAS detector was optimized using a hydrogen-argon entrained-air flame and a slotted-tube atom trap (STAT) in the flame. The limit of detection (3 sigma) achieved by the HPLC-FAAS system was 1 mg L-1 of selenium (100 mu L injections) for each of the four...

  17. Mass spectrometric confirmation criterion for product-ion spectra generated in flow-injection analysis. Environmental application

    NARCIS (Netherlands)

    Geerdink, R.B.; Niessen, W.M.A.; Brinkman, U.A.T.

    2001-01-01

    The suitability of a confirmation criterion recently recommended in the Netherlands for gas chromatography with mass spectrometric detection (GC-MS), was evaluated for flow-injection analysis (FIA) with atmospheric pressure chemical ionisation MS-MS detection. The main feature of the criterion is

  18. The coupling of capillary electrophoresis-inductively coupled plasma mass spectrometer as a speciation instrument for actinides at trace level; Le couplage electrophorese capillaire-spectrometre de masse a source plasma en tant qu'instrument de speciation des actinides a l'etat de traces

    Energy Technology Data Exchange (ETDEWEB)

    Delorme, A

    2004-07-01

    An interface between the separation technique (capillary electrophoresis) and the analytical technique (Inductively Coupled Plasma - Mass Spectrometer) was developed. In that sense, bibliographic and parametric studies allowed to define necessary conditions for the good working of both techniques. The results obtained led to the realisation of an interface capillary electrophoresis / ICP-MS (CE / ICP-MS). This one was experimentally validated on classical separations (alkalis / earth-alkalis and lanthanides) and the detection limit of the analytical system was determined equal to 4 x 10{sup -11} mol.L{sup -1} for plutonium. This result exhibits a gain in detection limit of a factor higher than 10{sup 4} compared to the capillary electrophoresis in standard detection (UV). The studies were made in order to check the capacity of the CE / ICP-MS coupling as a speciation instrument for actinides at trace level and to define the associated analytical procedures. The coupling turned out to be a suited instrument for the determination of absolute electrophoretic mobilities at infinite dilution (physico-chemical property which allows to predict the migration time of an ion under an electrical field in a given electrolyte), for the determination of thermodynamic constants and for the separation of different actinide oxidation states in solution. (author)

  19. Detection of an electron beam in a high density plasma via an electrostatic probe

    Science.gov (United States)

    Majeski, Stephen; Yoo, Jongsoo; Zweben, Stewart; Yamada, Masaaki; Ji, Hantao

    2017-10-01

    The perturbation in floating potential by an electron beam is detected by a 1D floating potential probe array to evaluate the use of an electron beam for magnetic field line mapping in the Magnetic Reconnection Experiment (MRX) plasma. The MRX plasma is relatively high density (1013 cm-3) and low temperature (5 eV). Beam electrons are emitted from a tungsten filament and are accelerated by a 200 V potential across the sheath. They stream along the magnetic field lines towards the probe array. The spatial electron beam density profile is assumed to be a Gaussian along the radial axis of MRX and the effective beam width is determined from the radial profile of the floating potential. The magnitude of the perturbation is in agreement with theoretical predictions and the location of the perturbation is also in agreement with field line mapping. In addition, no significant broadening of the electron beam is observed after propagation for tens of centimeters through the high density plasma. These results demonstrate that this method of field line mapping is, in principle, feasible in high density plasmas. This work is supported by the DOE Contract No. DE-AC0209CH11466.

  20. Magnetic spires for the detection of the position of the plasma column in a Tokamak (linear approximation)

    International Nuclear Information System (INIS)

    Colunga S, S.

    1990-07-01

    In this report the simplified analysis of a method to detect the movement of the plasma column of a tokamak in the vertical direction and of the biggest radius is given. The peculiar case of the Tokamak Novillo of the Plasma Physics Laboratory of the ININ is studied. (Author)

  1. Detection of nanoflare-heated plasma in the solar corona by the FOXSI-2 sounding rocket

    Science.gov (United States)

    Ishikawa, Shin-nosuke; Glesener, Lindsay; Krucker, Säm; Christe, Steven; Buitrago-Casas, Juan Camilo; Narukage, Noriyuki; Vievering, Juliana

    2017-11-01

    The processes that heat the solar and stellar coronae to several million kelvins, compared with the much cooler photosphere (5,800 K for the Sun), are still not well known1. One proposed mechanism is heating via a large number of small, unresolved, impulsive heating events called nanoflares2. Each event would heat and cool quickly, and the average effect would be a broad range of temperatures including a small amount of extremely hot plasma. However, detecting these faint, hot traces in the presence of brighter, cooler emission is observationally challenging. Here we present hard X-ray data from the second flight of the Focusing Optics X-ray Solar Imager (FOXSI-2), which detected emission above 7 keV from an active region of the Sun with no obvious individual X-ray flare emission. Through differential emission measure computations, we ascribe this emission to plasma heated above 10 MK, providing evidence for the existence of solar nanoflares. The quantitative evaluation of the hot plasma strongly constrains the coronal heating models.

  2. Mass spectrometric characterization of circulating and functional antigens derived from piperacillin in patients with cystic fibrosis1

    Science.gov (United States)

    Whitaker, Paul; Meng, Xiaoli; Lavergne, Sidonie N.; El-Ghaiesh, Sabah; Monshi, Manal; Earnshaw, Caroline; Peckham, Daniel; Gooi, Jimmy; Conway, Steve; Pirmohamed, Munir; Jenkins, Rosalind E.; Naisbitt, Dean J.; Park, B. Kevin

    2011-01-01

    A mechanistic understanding of the relationship between the chemistry of drug antigen formation and immune function is lacking. Thus, mass spectrometric methods were employed to detect and fully characterize circulating antigens derived from piperacillin in patients undergoing therapy and the nature of the drug derived-epitopes on protein which can function as an antigen to stimulate T-cells. Albumin modification with piperacillin in vitro resulted in the formation of two distinct haptens, one formed directly from piperacillin and a second in which the dioxopiperazine ring had undergone hydrolysis. Modification was time- and concentration-dependent, with selective modification of Lys541 observed at low concentrations, whereas at higher concentrations up to 13/59 lysine residues were modified, four of which (Lys190, 195, 432 and 541) were detected in patients’ plasma. Piperacillin-specific T-lymphocyte responses (proliferation, cytokines and granzyme-B release) were detected ex vivo with cells from hypersensitive patients, and analysis of incubation medium showed that modification of the same lysine residues in albumin occurred in situ. The antigenicity of piperacillin-modified albumin was confirmed by stimulation of T-cells with characterized synthetic conjugates. Analysis of minimally-modified T-cell stimulatory albumin conjugates revealed peptide sequences incorporating Lys190, 432 and 541 as principal functional epitopes for T-cells. This study has characterized the multiple haptenic structures on albumin in patients, and showed that they constitute functional antigenic determinants for T-cells. PMID:21606251

  3. Detection efficiencies in nano- and femtosecond laser ablation inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Waelle, M.; Koch, J.; Flamigni, L.; Heiroth, S.; Lippert, T.; Hartung, W.; Guenther, D.

    2009-01-01

    Detection efficiencies of laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), defined as the ratio of ions reaching the detector and atoms released by LA were measured. For this purpose, LA of silicate glasses, zircon, and pure silicon was performed using nanosecond (ns) as well as femtosecond (fs) LA. For instance, ns-LA of silicate glass using helium as in-cell carrier gas resulted in detection efficiencies between approximately 1E-7 for low and 3E-5 for high mass range elements which were, in addition, almost independent on the laser wavelength and pulse duration chosen. In contrast, the application of argon as carrier gas was found to suppress the detection efficiencies systematically by a factor of up to 5 mainly due to a less efficient aerosol-to-ion conversion and ion transmission inside the ICP-MS

  4. Validation and application of a high-performance liquid chromatography-tandem mass spectrometric method for simultaneous quantification of lopinavir and ritonavir in human plasma using semi-automated 96-well liquid-liquid extraction.

    Science.gov (United States)

    Wang, Perry G; Wei, Jack S; Kim, Grace; Chang, Min; El-Shourbagy, Tawakol

    2006-10-20

    Kaletra is an important antiretroviral drug, which has been developed by Abbott Laboratories. It is composed of lopinavir (low-pin-a-veer) and ritonavir (ri-toe-na-veer). Both have been proved to be human immunodeficiency virus (HIV) protease inhibitors and have substantially reduced the morbidity and mortality associated with HIV-1 infection. We have developed and validated an assay, using liquid chromatography coupled with atmospheric pressure chemical ionization tandem mass spectrometry (LC/MS/MS), for the routine quantification of lopinavir and ritonavir in human plasma, in which lopinavir and ritonavir can be simultaneously analyzed with high throughput. The sample preparation consisted of liquid-liquid extraction with a mixture of hexane: ethyl acetate (1:1, v/v), using 100 microL of plasma. Chromatographic separation was performed on a Waters Symmetry C(18) column (150 mm x 3.9 mm, particle size 5 microm) with reverse-phase isocratic using mobile phase of 70:30 (v/v) acetonitrile: 2 mM ammonium acetate aqueous solution containing 0.01% formic acid (v/v) at a flow rate of 1.0 mL/min. A Waters symmetry C(18) guard column (20 mm x 3.9 mm, particle size 5 microm) was connected prior to the analytical column, and a guard column back wash was performed to reduce the analytical column contamination using a mixture of tetrahydrofuran (THF), methanol and water (45:45:10, v/v/v). The analytical run was 4 min. The use of a 96-well plate autosampler allowed a batch size up to 73 study samples. A triple-quadrupole mass spectrometer was operated in a positive ion mode and multiple reaction monitoring (MRM) was used for drug quantification. The method was validated over the concentration ranges of 19-5,300 ng/mL for lopinavir and 11-3,100 ng/mL for ritonavir. A-86093 was used as an internal standard (I.S.). The relative standard deviation (RSD) were <6% for both lopinavir and ritonavir. Mean accuracies were between the designed limits (+/-15%). The robust and rapid LC

  5. Processing of gamma-ray spectrometric logs

    International Nuclear Information System (INIS)

    Umiastowski, K.; Dumesnil, P.

    1984-10-01

    CEA (Commissariat a l'Energie Atomique) has developped a gamma-ray spectrometric tool, containing an analog-to-digital converter. This new tool permits to perform very precise uranium logs (natural gamma-ray spectrometry), neutron activation logs and litho-density logs (gamma-gamma spectrometric logs). Specific processing methods were developped to treate the particular problems of down-hole gamma-ray spectrometry. Extraction of the characteristic gamma-ray peak, even if they are superposed on the background radiation of very high intensity, is possible. This processing methode enables also to obtain geological informations contained in the continuous background of the spectrum. Computer programs are written in high level language for SIRIUS (VICTOR) and APOLLO computers. Exemples of uranium and neutron activation logs treatment are presented [fr

  6. Effective method for the detection of piroxicam in human plasma using HPLC.

    Science.gov (United States)

    Calvo, Adriana Maria; Prado, Mariel Tavares de Oliveira; Dionísio, Thiago José; Marques, Maria Paula; Brozoski, Daniel Thomas; Lanchote, Vera Lúcia; Faria, Flávio Augusto Cardoso; Santos, Carlos Ferreira

    2016-05-20

    Non-steroidal anti-inflammatory drugs (NSAIDs) are widely used by the general population to alleviate inflammation and pain after oral surgeries. Piroxicam is among the most commonly used NSAIDs and excels in controlling pain, swelling, trismus and other common symptoms of inflammation. This study aimed to evaluate different concentrations of piroxicam and its major metabolite, 5'-hydroxypiroxicam, in human plasma samples over time using high performance liquid chromatography (HPLC) after liquid-liquid extraction. Briefly, 10 volunteers participated in this study after approval by the Ethics Committee of Bauru School of Dentistry, Universidade de São Paulo - USP, Brazil. Volunteers received a single dose oral of piroxicam (20 mg) and had blood collected at various times following an established protocol. The methodology of liquid-liquid extraction was effective for determining concentrations of piroxicam in plasma using HPLC in 10 out of 10 volunteers while 5'-hydroxypiroxicam was only detected in 2 out of 10 volunteers.

  7. Electronic equipment for spectrometric data processing

    International Nuclear Information System (INIS)

    Antonov, L.J.; Trenev, A.M.; Todorova, E.I.; Dimitrov, V.D.

    1978-01-01

    Electronic equipment carrying out logical operations and a full set of the arithmetic operations was developed for spectrometric data processing. The flowsheet of the computing part of the device, made on the basis of a specialized integral circuit, is given. The device includes input registers, multiplexor, matrix commutator, arithmetic unit and indication unit. The equipment is rated to carry out calculations according to comparatively complex formulae in several seconds

  8. Quench detection of fast plasma events for the JT-60SA central solenoid

    International Nuclear Information System (INIS)

    Murakami, Haruyuki; Kizu, Kaname; Tsuchiya, Katsuhiko; Kamiya, Koji; Takahashi, Yoshikazu; Yoshida, Kiyoshi

    2012-01-01

    Highlights: ► Pick-up coil method is used for the quench detection of JT-60SA magnet system. ► Disk-shaped pick-up coils are inserted in CS module to compensate inductive voltage. ► Applicability of pick-up coil is evaluated by two dimensional analysis. ► Pick-up coil is applicable whenever disruption, mini collapse and other plasma event. - Abstract: The JT-60 is planned to be modified to a full-superconducting tokamak referred to as the JT-60 Super Advanced (JT-60SA). The maximum temperature of the magnet during its quench might reach the temperature of higher than several hundreds Kelvin that will damage the superconducting magnet itself. The high precision quench detection system, therefore, is one of the key technologies in the superconducting magnet protection system. The pick-up coil method, which is using voltage taps to detect the normal voltage, is used for the quench detection of the JT-60SA superconducting magnet system. The disk-shaped pick-up coils are inserted in the central solenoid (CS) module to compensate the inductive voltage. In the previous study, the quench detection system requires a large number of pick-up coils. The reliability of quench detection system would be higher by simplifying the detection system such as reducing the number of pick-up coils. Simplifying the quench detection system is also important to reduce the total cost of the protection system. Hence the design method is improved by increasing optimizing parameters. The improved design method can reduce the number of pick-up coils without reducing the sensitivity of detection; consequently the protection system can be designed with higher reliability and lower cost. The applicability of the disk-shaped pick-up coil for quench detection system is evaluated by the two dimensional analysis. In the previous study, however, the analysis model only took into account the CS, EF (equilibrium field) coils and plasma. Therefore, applicability of the disk-shaped pick-up coil for

  9. Detection of Antibodies in Blood Plasma Using Bioluminescent Sensor Proteins and a Smartphone.

    Science.gov (United States)

    Arts, Remco; den Hartog, Ilona; Zijlema, Stefan E; Thijssen, Vito; van der Beelen, Stan H E; Merkx, Maarten

    2016-04-19

    Antibody detection is of fundamental importance in many diagnostic and bioanalytical assays, yet current detection techniques tend to be laborious and/or expensive. We present a new sensor platform (LUMABS) based on bioluminescence resonance energy transfer (BRET) that allows detection of antibodies directly in solution using a smartphone as the sole piece of equipment. LUMABS are single-protein sensors that consist of the blue-light emitting luciferase NanoLuc connected via a semiflexible linker to the green fluorescent acceptor protein mNeonGreen, which are kept close together using helper domains. Binding of an antibody to epitope sequences flanking the linker disrupts the interaction between the helper domains, resulting in a large decrease in BRET efficiency. The resulting change in color of the emitted light from green-blue to blue can be detected directly in blood plasma, even at picomolar concentrations of antibody. Moreover, the modular architecture of LUMABS allows changing of target specificity by simple exchange of epitope sequences, as demonstrated here for antibodies against HIV1-p17, hemagglutinin (HA), and dengue virus type I. The combination of sensitive ratiometric bioluminescent detection and the intrinsic modularity of the LUMABS design provides an attractive generic platform for point-of-care antibody detection that avoids the complex liquid handling steps associated with conventional immunoassays.

  10. Optimization of an anion-exchange high performance liquid chromatography-inductively coupled plasma-mass spectrometric method for the speciation analysis of oxyanion-forming metals and metalloids in leachates from cement-based materials.

    Science.gov (United States)

    Mulugeta, Mesay; Wibetoe, Grethe; Engelsen, Christian J; Lund, Walter

    2010-10-01

    A method was developed for the speciation analysis of the oxyanions of As(III), As(V), Cr(VI), Mo(VI), Sb(III), Sb(V), Se(IV), Se(VI) and V(V) in leachates from cement-based materials, based on anion-exchange HPLC coupled with ICP-MS. The method was optimized in a two-step multivariate approach: the effect of sample pH and mobile phase composition on resolution, peak symmetry and analysis time was studied. Optimum conditions were then identified for the significant experimental factors by studying their interdependence. A mobile phase composition of 20 mM ammonium nitrate, 50 mM ammonium tartrate and pH 9.5 was found to be a compromise optimum for the separation of the target analytes using isocratic elution. The optimum condition provided separation of the analytes in less than 6 min, at a mobile phase flow rate of 1.0 mL/min. The signal intensities of the analytes were improved by adding 1% methanol to the mobile phase. The limit of detection of the method was in the range 0.2-2.2 μg/L for the various species. The effect of sample constituents was studied using spiked concrete leachates. The method was used to determine the target oxyanionic species in leachates generated from a concrete material in the pH range 3.5-12.4; CrO(4)(2-), MoO(4)(2-) and VO(4)(3-) were detected in most of the leachates. Copyright © 2010 Elsevier B.V. All rights reserved.

  11. Advance in plasma SEPT9 gene methylation assay for colorectal cancer early detection.

    Science.gov (United States)

    Wang, Yu; Chen, Pei-Min; Liu, Rong-Bin

    2018-01-15

    This review article summarizes the research advances of the plasma-based SEPT9 gene methylation assay for the clinical detection of colorectal cancer and its limitations. Colorectal cancer is a common malignancy with a poor prognosis and a high mortality, for which early detection and diagnosis are particularly crucial for the high-risk groups. Increasing evidence supported that SEPT9 gene methylation is associated with the pathogenesis of colorectal cancer and that detecting the level of methylation of SEPT9 in the peripheral blood can be used for screening of colorectal cancer in susceptible populations. In recent years, the data obtained in clinical studies demonstrated that the SEPT9 gene methylation assay has a good diagnostic performance with regard to both sensitivity and specificity with the advantage of better acceptability, convenience and compliance with serological testing compared with fecal occult blood tests and carcinoembryonic antigen for colorectal cancer (CRC). Furthermore, the combination of multiple methods or markers has become a growing trend for CRC detection and screening. Nevertheless, the clinical availability of the methylated SEPT9 assay is still limited because of the large degree of sample heterogeneity caused by demographic characteristics, pathological features, comorbidities and/or technique selection. Another factor is the cost-effectiveness of colorectal cancer screening strategies that hinders its large-scale application. In addition, improvements in its accuracy in detecting adenomas and premalignant polyps are required.

  12. The improvement of the detection power of a U-shaped DC plasma

    Directory of Open Access Journals (Sweden)

    DRAGAN MARKOVIC

    2001-04-01

    Full Text Available Optimization of the operating parameters of U-shpaed DC arc plasma and spectrometer parameters has been undertaken to explore the possibilities of improving its detection power. It is demonstrated, with a U-shaped arc as an example, that the limits of detection, in addition to well-defined parameters as described by Boumans and Winge, depend on the signal integration time. It is shown that with increasing integration time, the limits of detection are decreased within some limits and that the precision and concentration sensitivity are improved as well. A mathematical expression for the dependence of the detection limit on the integration time is presented. To increase the reliability of the measurement of the mentioned parameters, the working conditions were optimized for the following analytes: Ag, Al, Au, Cr, Fe, Mn, Ni, Pb, Pd, Pt, and V. The obtained limits of detection are comparable or better than those obtained by ICP for the elements studied. Itwas estimed that the possibility exists for their further improvement up to 10 times.

  13. Label Free Detection of Biomolecules Using Charge-Plasma-Based Gate Underlap Dielectric Modulated Junctionless TFET

    Science.gov (United States)

    Wadhwa, Girish; Raj, Balwinder

    2018-05-01

    Nanoscale devices are emerging as a platform for detecting biomolecules. Various issues were observed during the fabrication process such as random dopant fluctuation and thermal budget. To reduce these issues charge-plasma-based concept is introduced. This paper proposes the implementation of charge-plasma-based gate underlap dielectric modulated junctionless tunnel field effect transistor (DM-JLTFET) for the revelation of biomolecule immobilized in the open cavity gate channel region. In this p+ source and n+ drain regions are introduced by employing different work function over the intrinsic silicon. Also dual material gate architecture is implemented to reduce short channel effect without abandoning any other device characteristic. The sensitivity of biosensor is studied for both the neutral and charge-neutral biomolecules. The effect of device parameters such as channel thickness, cavity length and cavity thickness on drain current have been analyzed through simulations. This paper investigates the performance of charge-plasma-based gate underlap DM-JLTFET for biomolecule sensing applications while varying dielectric constant, charge density at different biasing conditions.

  14. Clinical significance of plasma atrial natriuretic factor and endothelin detection in hyperthyroidism and hypothyroidism

    International Nuclear Information System (INIS)

    Zhu Yalin; Huo Ying; Pan Yunlong

    2005-01-01

    Plasma at rial natriuretic factor (ANF) and endothelin (ET) were detected by RIA in 58 cases of hyperthyroidism and 47 cases of hypothyroidism. Before the ANF and ET concentration of untreatment hyperthyroid patients was much higher than that of treatment hyperthyroid patients, hypothyroid patients before and after treatment and the normal group (P 3 and FT 4 . Compared with the normal group, ANF concentration in treatment hyperthyroid patients, hypothyroid patients before and after treatment was no significantly different (P>0.05), but that in hypothyroid patients before treatment was significantly decreased compared with hypothyroid patients after treatment (P 0.05), but that in hypothyroid patients before treatment was significantly decreased compared with others (P<0.01 and P<0.05). Detection of ANF and ET level may be have a role in supplementary diagnosis and curative effect observation of hyperthyroidism and hypothyroidism. (authors)

  15. Determination of long-lived actinides in soil leachates by inductively coupled plasma: Mass spectrometry

    International Nuclear Information System (INIS)

    Crain, J.S.; Smith, L.L.; Yaeger, J.S.; Alvarado, J.A.

    1994-01-01

    Inductively coupled plasma -- mass spectrometry (ICP-MS) was used to concurrently determine multiple long-lived (t 1/2 > 10 4 y) actinide isotopes in soil samples. Ultrasonic nebulization was found to maximize instrument sensitivity. Instrument detection limits for actinides in solution ranged from 50 mBq L -1 ( 239 Pu) to 2 μBq L -1 ( 235 U) Hydride adducts of 232 Th and 238 U interfered with the determinations of 233 U and 239 Pu; thus, extraction chromatography was, used to eliminate the sample matrix, concentrate the analytes, and separate uranium from the other actinides. Alpha spectrometric determinations of 230 Th, 239 Pu, and the 234 U/ 238 U activity ratio in soil leachates compared well with ICP-MS determinations; however, there were some small systematic differences (ca. 10%) between ICP-MS and a-spectrometric determinations of 234 U and 238 U activities

  16. Dielectric barrier discharge micro-plasma emission spectrometry for the detection of acetone in exhaled breath.

    Science.gov (United States)

    Yang, Ting; Gao, Dong-Xue; Yu, Yong-Liang; Chen, Ming-Li; Wang, Jian-Hua

    2016-01-01

    Acetone is a predominant volatile organic compound (VOC) in the exhaled breath and a promising biomarker for diabetes and ketoacidosis. A non-thermal micro-plasma generated in a planar dielectric barrier discharge (DBD) is used as a radiation source for the excitation of gaseous acetone followed by its quantification with optical emission spectrometry (OES). Gaseous acetone can be directly sampled, while liquid acetone is evaporated by heated tungsten coil and then introduced into the DBD micro-plasma by a helium carrier flow for performing optical emission and detection at a 519 nm emission line. In the present study, the exhaled breath is collected and transferred into aqueous medium for sampling. With a sampling volume of 7 μL in a micro-drop, a linear range of 40-1600 mg L(-1) is obtained along with a detection limit of 44 ng and a precision of 5.7% RSD. The present system is successfully applied to the determination of breath acetone for both diabetic patients and healthy volunteers. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. A Detection of the Same Hot Plasma in the Corona: During a CME and Later at Ulysses

    Science.gov (United States)

    Suess, S. T.; Poletto, G.

    2004-01-01

    We show direct evidence for the same very hot plasma being detected remotely from SOHO in the corona and subsequently, at Ulysses in the solar wind. This is, to our knowledge, the first time that such an unambiguous identification has been made in the case of hot plasma. This detection complements studies correlating other plasma and field properties observed to the properties measured at the source in the corona. This observation takes advantage of a SOHO-Sun-Ulysses quadrature, during which the Sun-Ulysses included angle is $90^\\circ$ and it is possible to observe with Ulysses instruments the same plasma that has previously been remotely observed with SOHO instruments in the corona on the limb of the Sun. The identification builds on an existing base of separate SOHO and interplanetary detections of hot plasma. SOHO/UVCS has found evidence for very hot coronal plasma in current sheets in the aftermath of CMEs in the [Fe XVIII] $\\lambda$ \\AA\\ line, implying a temperature on the order of $6\\times 10(exp 6)$ K. This temperature is unusually high even for active regions, but is compatible with the high temperature predicted in current sheets. In the solar wind, ACE data from early 1998 to middle 2000 revealed high frozen-in Fe charge state in many cases to be present in interplanetary plasma.

  18. PCR/LDR/capillary electrophoresis for detection of single-nucleotide differences between fetal and maternal DNA in maternal plasma.

    Science.gov (United States)

    Yi, Ping; Chen, Zhuqin; Zhao, Yan; Guo, Jianxin; Fu, Huabin; Zhou, Yuanguo; Yu, Lili; Li, Li

    2009-03-01

    The discovery of fetal DNA in maternal plasma has opened up an approach for noninvasive diagnosis. We have now assessed the possibility of detecting single-nucleotide differences between fetal and maternal DNA in maternal plasma by polymerase chain reaction (PCR)/ligase detection reaction((LDR)/capillary electrophoresis. PCR/LDR/capillary electrophoresis was applied to detect the genotype of c.454-397T>gene (ESR1) from experimental DNA models of maternal plasma at different sensitivity levels and 13 maternal plasma samples.alphaC in estrogen receptor. (1) Our results demonstrated that the technique could discriminate low abundance single-nucleotide mutation with a mutant/normal allele ratio up to 1:10 000. (2) Examination of ESR1 c.454-397T>C genotypes by using the method of restriction fragment length analysis was performed in 25 pregnant women, of whom 13 pregnant women had homozygous genotypes. The c.454-397T>C genotypes of paternally inherited fetal DNA in maternal plasma of these 13 women were detected by PCR/LDR/capillary electrophoresis, which were accordant with the results of umbilical cord blood. PCR/LDR/capillary electrophoresis has very high sensitivity to distinguish low abundance single nucleotide differences and can discriminate point mutations and single-nucleotide polymorphisms(SNPs) of paternally inherited fetal DNA in maternal plasma.

  19. High Magnetic Field in THz Plasma Wave Detection by High Electron Mobility Transistors

    Science.gov (United States)

    Sakowicz, M.; Łusakowski, J.; Karpierz, K.; Grynberg, M.; Valusis, G.

    The role of gated and ungated two dimensional (2D) electron plasma in THz detection by high electron mobility transistors (HEMTs) was investigated. THz response of GaAs/AlGaAs and GaN/AlGaN HEMTs was measured at 4.4K in quantizing magnetic fields with a simultaneous modulation of the gate voltage UGS. This allowed us to measure both the detection signal, S, and its derivative dS/dUGS. Shubnikov - de-Haas oscillations (SdHO) of both S and dS/dUGS were observed. A comparison of SdHO observed in detection and magnetoresistance measurements allows us to associate unambiguously SdHO in S and dS/dUGS with the ungated and gated parts of the transistor channel, respectively. This allows us to conclude that the entire channel takes part in the detection process. Additionally, in the case of GaAlAs/GaAs HEMTs, a structure related to the cyclotron resonance transition was observed.

  20. Spectrometric control of radionuclides production parameters

    International Nuclear Information System (INIS)

    Zhuk, I.; Potarenko, A.; Yarochevich, O.; Hluboky, N.; Kerko, P.; Bogdanov, V.; Dyatel, N.

    2006-01-01

    Full text: A radioactive preparations and sources are widely used all over the world for scientific, industrial and medical purposes. These preparations in Belarus are planned to produce by the Joint Belarussian-Russian Closed Joint Stock Company 'Isotope technologies' (CJSC IT). The company was created in 1998 by two leading scientific centers-SSI 'Joint Institute of Power and Nuclear Research-Sosny' the National Academy of Sciences of Belarus and the State Center of Science of the Russian Federation 'Scientific research institute of nuclear reactors'. One of the mainstream directions in CJSC IT activities is production of radioactive preparations for the industrial and scientific application (such as 133 Ba, 109 Cd, 63 Ni, 60 Co) and for the medical purposes (such as 19 '2Ir, 60 Co). All radioactive preparations have a good export potential and adequate to modern technical and consumer requirements. X-γ spectrometric analysis of considered radioactive sources is one of the basic methods for quality control of radioactive sources. At present, we are developing x-γ spectrometric support of purification process from contaminating radionuclides of 109 Cd -γ preparation and 63 Ni - β preparation. Work on x-γ spectrometric quality control of 133 Ba preparation is carried out. The description of the used equipment is given. Techniques of contaminating radionuclides determination (contents ∼10 - '6 from activity of the basic radionuclide) are presented. Problems of the choice of geometry of measurements of sources with activity about 10 7 -10 9 Bq and possible sources of errors are discussed. (author)

  1. Similarity ratio analysis for early stage fault detection with optical emission spectrometer in plasma etching process.

    Directory of Open Access Journals (Sweden)

    Jie Yang

    Full Text Available A Similarity Ratio Analysis (SRA method is proposed for early-stage Fault Detection (FD in plasma etching processes using real-time Optical Emission Spectrometer (OES data as input. The SRA method can help to realise a highly precise control system by detecting abnormal etch-rate faults in real-time during an etching process. The method processes spectrum scans at successive time points and uses a windowing mechanism over the time series to alleviate problems with timing uncertainties due to process shift from one process run to another. A SRA library is first built to capture features of a healthy etching process. By comparing with the SRA library, a Similarity Ratio (SR statistic is then calculated for each spectrum scan as the monitored process progresses. A fault detection mechanism, named 3-Warning-1-Alarm (3W1A, takes the SR values as inputs and triggers a system alarm when certain conditions are satisfied. This design reduces the chance of false alarm, and provides a reliable fault reporting service. The SRA method is demonstrated on a real semiconductor manufacturing dataset. The effectiveness of SRA-based fault detection is evaluated using a time-series SR test and also using a post-process SR test. The time-series SR provides an early-stage fault detection service, so less energy and materials will be wasted by faulty processing. The post-process SR provides a fault detection service with higher reliability than the time-series SR, but with fault testing conducted only after each process run completes.

  2. A measuring generator for testing spectrometric channels

    International Nuclear Information System (INIS)

    Dinh Sy Hien; Kalinkin, A.I.

    1984-01-01

    A measuring generator for testing and tuning an amplitude spectrometric channel is described. The device consists of a pseudo random pulse generator, constructed on shifters, a sawtooth wave generator and a shaper of stable amplitude pulses with exponential decay times. The device is made as CAMAC unit width modules and has the following specifications: average pulse repetition rate of pseudo random pulses is 3.1; 25; 50; 100; 200 kHz; peak amplitude of 2 Hz pulse repetition of saw tooth pulses is 6 V; peak amplitude of exponential shape pulses is 5 V. The block-diagram and basic circuits of the device are given

  3. Uncertainty assessment in gamma spectrometric measurements of plutonium isotope ratios and age

    Energy Technology Data Exchange (ETDEWEB)

    Ramebaeck, H., E-mail: henrik.ramebeck@foi.se [Swedish Defence Research Agency, FOI, Division of CBRN Defence and Security, SE-901 82 Umea (Sweden); Chalmers University of Technology, Department of Chemical and Biological Engineering, Nuclear Chemistry, SE-412 96 Goeteborg (Sweden); Nygren, U.; Tovedal, A. [Swedish Defence Research Agency, FOI, Division of CBRN Defence and Security, SE-901 82 Umea (Sweden); Ekberg, C.; Skarnemark, G. [Chalmers University of Technology, Department of Chemical and Biological Engineering, Nuclear Chemistry, SE-412 96 Goeteborg (Sweden)

    2012-09-15

    A method for the assessment of the combined uncertainty in gamma spectrometric measurements of plutonium composition and age was evaluated. Two materials were measured. Isotope dilution inductively coupled plasma sector field mass spectrometry (ID-ICP-SFMS) was used as a reference method for comparing the results obtained with the gamma spectrometric method for one of the materials. For this material (weapons grade plutonium) the measurement results were in agreement between the two methods for all measurands. Moreover, the combined uncertainty in all isotope ratios considered in this material (R{sub Pu238/Pu239}, R{sub Pu240/Pu239}, R{sub Pu241/Pu239}, and R{sub Am241/Pu241} for age determination) were limited by counting statistics. However, the combined uncertainty for the other material (fuel grade plutonium) were limited by the response fit, which shows that the uncertainty in the response function is important to include in the combined measurement uncertainty of gamma spectrometric measurements of plutonium.

  4. The determination of fenspiride in human plasma and urine by liquid chromatography with electrochemical or ultraviolet detection.

    Science.gov (United States)

    Sauveur, C; Baune, A; Vergnes, N; Jeanniot, J P

    1989-01-01

    A selective and sensitive method for the determination of fenspiride in biological fluids is described. The method involves liquid-liquid extraction followed by separation on a reversed-phase column with electrochemical detection for low levels of the drug in plasma (less than or equal to 100 ng ml-1) or UV absorption for higher concentrations in plasma or urine. The method is suitable for pharmacokinetic analyses and drug monitoring studies.

  5. Carbohydrate-based electrochemical biosensor for detection of a cancer biomarker in human plasma.

    Science.gov (United States)

    Devillers, Marion; Ahmad, Lama; Korri-Youssoufi, Hafsa; Salmon, Laurent

    2017-10-15

    Autocrine motility factor (AMF) is a tumor-secreted cytokine that stimulates tumor cell motility in vitro and metastasis in vivo. AMF could be detected in serum or urine of cancer patients with worse prognosis. Reported as a cancer biomarker, AMF secretion into body fluids might be closely related to metastases formation. In this study, a sensitive and specific carbohydrate-based electrochemical biosensor was designed for the detection and quantification of a protein model of AMF, namely phosphoglucose isomerase from rabbit muscle (RmPGI). Indeed, RmPGI displays high homology with AMF and has been shown to have AMF activity. The biosensor was constructed by covalent binding of the enzyme substrate d-fructose 6-phosphate (F6P). Immobilization was achieved on a gold surface electrode following a bottom-up approach through an aminated surface obtained by electrochemical patterning of ethylene diamine and terminal amine polyethylene glycol chain to prevent non-specific interactions. Carbohydrate-protein interactions were quantified in a range of 10 fM to 100nM. Complex formation was analyzed through monitoring of the redox couple Fe 2+ /Fe 3+ by electrochemical impedance spectroscopy and square wave voltammetry. The F6P-biosensor demonstrates a detection limit of 6.6 fM and high selectivity when compared to other non-specific glycolytic proteins such as d-glucose-6-phosphate dehydrogenase. Detection of protein in spiked plasma was demonstrated and accuracy of 95% is obtained compared to result obtained in PBS (phosphate buffered saline). F6P-biosensor is a very promising proof of concept required for the design of a carbohydrate-based electrochemical biosensor using the enzyme substrate as bioreceptor. Such biosensor could be generalized to detect other protein biomarkers of interest. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Improved mass spectrometry assay for plasma hepcidin: detection and characterization of a novel hepcidin isoform.

    Directory of Open Access Journals (Sweden)

    Coby M M Laarakkers

    Full Text Available Mass spectrometry (MS-based assays for the quantification of the iron regulatory hormone hepcidin are pivotal to discriminate between the bioactive 25-amino acid form that can effectively block the sole iron transporter ferroportin and other naturally occurring smaller isoforms without a known role in iron metabolism. Here we describe the design, validation and use of a novel stable hepcidin-25(+40 isotope as internal standard for quantification. Importantly, the relative large mass shift of 40 Da makes this isotope also suitable for easy-to-use medium resolution linear time-of-flight (TOF platforms. As expected, implementation of hepcidin-25(+40 as internal standard in our weak cation exchange (WCX TOF MS method yielded very low inter/intra run coefficients of variation. Surprisingly, however, in samples from kidney disease patients, we detected a novel peak (m/z 2673.9 with low intensity that could be identified as hepcidin-24 and had previously remained unnoticed due to peak interference with the formerly used internal standard. Using a cell-based bioassay it was shown that synthetic hepcidin-24 was, like the -22 and -20 isoforms, a significantly less potent inducer of ferroportin degradation than hepcidin-25. During prolonged storage of plasma at room temperature, we observed that a decrease in plasma hepcidin-25 was paralleled by an increase in the levels of the hepcidin-24, -22 and -20 isoforms. This provides first evidence that all determinants for the conversion of hepcidin-25 to smaller inactive isoforms are present in the circulation, which may contribute to the functional suppression of hepcidin-25, that is significantly elevated in patients with renal impairment. The present update of our hepcidin TOF MS assay together with improved insights in the source and preparation of the internal standard, and sample stability will further improve our understanding of circulating hepcidin and pave the way towards further optimization and

  7. Effective method for the detection of piroxicam in human plasma using HPLC

    Directory of Open Access Journals (Sweden)

    Adriana Maria CALVO

    2016-01-01

    Full Text Available Abstract Non-steroidal anti-inflammatory drugs (NSAIDs are widely used by the general population to alleviate inflammation and pain after oral surgeries. Piroxicam is among the most commonly used NSAIDs and excels in controlling pain, swelling, trismus and other common symptoms of inflammation. This study aimed to evaluate different concentrations of piroxicam and its major metabolite, 5’-hydroxypiroxicam, in human plasma samples over time using high performance liquid chromatography (HPLC after liquid-liquid extraction. Briefly, 10 volunteers participated in this study after approval by the Ethics Committee of Bauru School of Dentistry, Universidade de São Paulo – USP, Brazil. Volunteers received a single dose oral of piroxicam (20 mg and had blood collected at various times following an established protocol. The methodology of liquid-liquid extraction was effective for determining concentrations of piroxicam in plasma using HPLC in 10 out of 10 volunteers while 5’-hydroxypiroxicam was only detected in 2 out of 10 volunteers.

  8. Li-BES detection system for plasma turbulence measurements on the COMPASS tokamak

    Energy Technology Data Exchange (ETDEWEB)

    Berta, M. [Institute of Plasma Physics AS CR, Prague (Czech Republic); Széchenyi István University, Győr (Hungary); Anda, G.; Bencze, A.; Dunai, D. [Wigner – RCP, HAS, Budapest (Hungary); Háček, P., E-mail: hacek@ipp.cas.cz [Institute of Plasma Physics AS CR, Prague (Czech Republic); Faculty of Mathematics and Physics, Charles University in Prague, Prague (Czech Republic); Hron, M. [Institute of Plasma Physics AS CR, Prague (Czech Republic); Kovácsik, A. [Wigner – RCP, HAS, Budapest (Hungary); Department of Nuclear Techniques, Budapest University of Technology and Economics, Budapest (Hungary); Krbec, J. [Institute of Plasma Physics AS CR, Prague (Czech Republic); Faculty of Nuclear Sciences and Physical Engineering, Czech Technical University in Prague, Prague (Czech Republic); Pánek, R. [Institute of Plasma Physics AS CR, Prague (Czech Republic); Réfy, D.; Veres, G. [Wigner – RCP, HAS, Budapest (Hungary); Weinzettl, V. [Institute of Plasma Physics AS CR, Prague (Czech Republic); Zoletnik, S. [Wigner – RCP, HAS, Budapest (Hungary)

    2015-10-15

    Highlights: • Li-BES detection system on the COMPASS tokamak is optimized observation system with high temporal resolution. • High sensitivity to low level light fluctuations. • Optics and detectors with electronics are placed in thermally stabilized compact box. • Fast deflection system allows us to measure background corrected electron density profiles on microsecond time-scale. - Abstract: A new Li beam emission spectroscopy (Li-BES) diagnostic system with a ∼ cm spatial resolution, and with beam energy ranging from 10 keV up to 120 keV and a 18 channel Avalanche photo diode (APD) detector system sampled at 2 MHz has been recently installed and tested on the COMPASS tokamak. This diagnostic allows to reconstruct density profile based on directly measured light profiles, and to follow turbulent behaviour of the edge plasma. The paper reports technical capabilities of this new system designed for fine spatio-temporal measurements of plasma electron density. Focusing on turbulence-induced fluctuation measurements, we demonstrate how physically relevant information can be extracted using the COMPASS Li-BES system.

  9. Automated mass spectrometric analysis of urinary and plasma serotonin

    NARCIS (Netherlands)

    de Jong, Wilhelmina H. A.; Wilkens, Marianne H. L. I.; de Vries, Elisabeth G. E.; Kema, Ido P.

    Serotonin emerges as crucial neurotransmitter and hormone in a growing number of different physiologic processes. Besides extensive serotonin production previously noted in patients with metastatic carcinoid tumors, serotonin now is implicated in liver cell regeneration and bone formation. The aim

  10. Detection of metal ions by atomic emission spectroscopy from liquid-electrode discharge plasma

    International Nuclear Information System (INIS)

    Wu Jian; Yu Jing; Li Jun; Wang Jianping; Ying Yibin

    2007-01-01

    In this paper, the discharge ignited in a capillary connecting two beakers filled with electrolyte solution is investigated. During the experiment, an external electrical voltage is applied through two platinum electrodes dipped in the beakers. A gas bubble forms inside the capillary when the applied voltage is higher than 1000 V. Since the beakers are tilted slightly, after generation, the bubble moves slowly to the uphill outlet of the capillary due to buoyancy. When the bubble reaches the end of the capillary, it cracks and a bright discharge is ignited. The emission spectra of the discharge plasma are related to the metal ions dissolved in the solution and thus can be used for metal ion detection. An application of the system to measurement of water hardness is shown

  11. Longitudinal Bank for Serum, Plasma, and DNA for Detection of Biomarkers

    Energy Technology Data Exchange (ETDEWEB)

    Vogelzang, Nicolas [Nevada Cancer Inst., Las Vegas, NV (United States); Fink, Louis [Nevada Cancer Inst., Las Vegas, NV (United States)

    2007-11-12

    The discovery of genetic or biochemical markers to discriminate malignant cancers from normal or benign disease states, markers to stage cancer or monitor disease progression and markers that provide an early indication of an individual’s response to chemotherapy have become a major research objectives of the oncology community over the past few years. The goal of the project is to create a patient specimen bank of serum, plasma, urine and tissues from approximately 1500 individuals. The collection of samples from individuals on a longitudinal basis provided proteomic and biochemical data to be correlated with clinical endpoints. This greatly enhanced our ability to identify biomarkers for staging different cancers and to detect patient responsiveness to therapy at an early state in the treatment process.

  12. Filterless preconcentration, flow injection analysis and detection by inductively-coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Andersen, Jens Enevold Thaulov

    The influence of interferences in the analysis of elements by inductively-coupled-plasma mass-spectrometry (ICP-MS) may be significantly diminished by utilising a protocol of flow-injection analysis (FIA). The method is based on filterless preconcentration of metallic elements at the walls...... of a knotted reactor that was made of nylon tubings. In the load mode, the preconcentration was accomplished by precipitation of metallic species in alkaline-buffered carriers onto the inner walls of the hydrofilic tube. After a preconcen-tration period of 40-120 seconds using sample volumes of 4-10 m...... of 10-30 were obtained in the analysis of aluminium, of chromium and of iron, which resulted in detection limits (3) down to 20 g/L at a sampling frequency of 50 per hour. The preconcentration protocol improves the selectivity thus allowing direct determination of the elements in saline media. Anionic...

  13. Droplet digital PCR for detection and quantification of circulating tumor DNA in plasma of head and neck cancer patients.

    Science.gov (United States)

    van Ginkel, Joost H; Huibers, Manon M H; van Es, Robert J J; de Bree, Remco; Willems, Stefan M

    2017-06-19

    During posttreatment surveillance of head and neck cancer patients, imaging is insufficiently accurate for the early detection of relapsing disease. Free circulating tumor DNA (ctDNA) may serve as a novel biomarker for monitoring tumor burden during posttreatment surveillance of these patients. In this exploratory study, we investigated whether low level ctDNA in plasma of head and neck cancer patients can be detected using Droplet Digital PCR (ddPCR). TP53 mutations were determined in surgically resected primary tumor samples from six patients with high stage (II-IV), moderate to poorly differentiated head and neck squamous cell carcinoma (HNSCC). Subsequently, mutation specific ddPCR assays were designed. Pretreatment plasma samples from these patients were examined on the presence of ctDNA by ddPCR using the mutation-specific assays. The ddPCR results were evaluated alongside clinicopathological data. In all cases, plasma samples were found positive for targeted TP53 mutations in varying degrees (absolute quantification of 2.2-422 mutational copies/ml plasma). Mutations were detected in wild-type TP53 background templates of 7667-156,667 copies/ml plasma, yielding fractional abundances of down to 0.01%. Our results show that detection of tumor specific TP53 mutations in low level ctDNA from HNSCC patients using ddPCR is technically feasible and provide ground for future research on ctDNA quantification for the use of diagnostic biomarkers in the posttreatment surveillance of HNSCC patients.

  14. [Determination of trace cobalt in human urine by graphite furnace atomic absorption spectrometr].

    Science.gov (United States)

    Zhong, L X; Ding, B M; Jiang, D; Liu, D Y; Yu, B; Zhu, B L; Ding, L

    2016-05-20

    To establish a method to determine cobalt in human urine by graphite furnace atomic absorption spectrometry. Urine with 2% nitric acid diluted two-fold, to quantify the curve, graphite furnace atomic absorption spectrometric detection. Co was linear within 2.5~40.0 ng/ml with r>0.999. Spike experiment showed that Co received good recovery rate, which was 90.8%~94.8%. Intra-assay precisions were 3.2%~5.1% for Co, inter-assay precisions were 4.4%~5.2% for Co. The method by using graphite furnace atomic absorption spectrometr to determine urine Co was fast, accurate and with low matrix effect. It could meet the requirement in GBZ/T 210.5-2008.

  15. The fast gamma spectrometric method of the Am-241 determination in Chernobyl restricted zone soils

    International Nuclear Information System (INIS)

    Gleisberg, B.; Lukachina, V.V.; Kirsenko, V.N.; Tepikin, V.E.; Rajevsky, V.S.; Libman, V.A.; Stoljarevsky, I.P.; Isajev, A.G.

    1997-01-01

    The known methods of the 241 Am contents determination in environmental objects, as a rule, is based on ion-chromatographic or extraction separation techniques. This approach reflects widespread opinion, that only the α-spectrometric analysis termination is suitable to ensure necessary sensitivity of the overall method of 241 Am actively determination. Really, the minimal detectable activity for such methods is about 0.05 Bq/kg (considering that Am is usually concentrated during separation procedure). However, because of α-spectrometry does not permit to separate the α-peaks of the 241 Am, and 238 Pu, but also in view of high requests to the α-spectrometric specimen purity, the multistage and laborious chemical procedures to separate 241 Am from plutonium radionuclides and other elements (with a thorough control of each separation stage) are needed

  16. Development of online, continuous heavy metals detection and monitoring sensors based on microfluidic plasma reactors

    Science.gov (United States)

    Abdul-Majeed, Wameath Sh

    This research is dedicated to develop a fully integrated system for heavy metals determination in water samples based on micro fluidic plasma atomizers. Several configurations of dielectric barrier discharge (DBD) atomizer are designed, fabricated and tested toward this target. Finally, a combination of annular and rectangular DBD atomizers has been utilized to develop a scheme for heavy metals determination. The present thesis has combined both theoretical and experimental investigations to fulfil the requirements. Several mathematical studies are implemented to explore the optimal design parameters for best system performance. On the other hand, expanded experimental explorations are conducted to assess the proposed operational approaches. The experiments were designed according to a central composite rotatable design; hence, an empirical model has been produced for each studied case. Moreover, several statistical approaches are adopted to analyse the system performance and to deduce the optimal operational parameters.. The introduction of the examined analyte to the plasma atomizer has been achieved by applying chemical schemes, where the element in the sample has been derivitized by using different kinds of reducing agents to produce vapour species (e.g. hydrides) for a group of nine elements examined in this research individually and simultaneously. Moreover, other derivatization schemes based on photochemical vapour generation assisted by ultrasound irradiation are also investigated. Generally speaking, the detection limits achieved in this research for the examined set of elements (by applying hydroborate scheme) are found to be acceptable in accordance with the standard limits in drinking water. The results of copper compared with the data from other technologies in the literature, showed a competitive detection limit obtained from applying the developed scheme, with an advantage of conducting simultaneous, fully automated, insitu, online- real time

  17. Proton-sensing transistor systems for detecting ion leakage from plasma membranes under chemical stimuli.

    Science.gov (United States)

    Imaizumi, Yuki; Goda, Tatsuro; Schaffhauser, Daniel F; Okada, Jun-Ichi; Matsumoto, Akira; Miyahara, Yuji

    2017-03-01

    The membrane integrity of live cells is routinely evaluated for cytotoxicity induced by chemical or physical stimuli. Recent progress in bioengineering means that high-quality toxicity validation is required. Here, we report a pH-sensitive transistor system developed for the continuous monitoring of ion leakage from cell membranes upon challenge by toxic compounds. Temporal changes in pH were generated with high reproducibility via periodic flushing of HepG2 cells on a gate insulator of a proton-sensitive field-effect transistor with isotonic buffer solutions with/without NH 4 Cl. The pH transients at the point of NH 4 Cl addition/withdrawal originated from the free permeation of NH 3 across the semi-permeable plasma membranes, and the proton sponge effect produced by the ammonia equilibrium. Irreversible attenuation of the pH transient was observed when the cells were subjected to a membrane-toxic reagent. Experiments and simulations proved that the decrease in the pH transient was proportional to the area of the ion-permeable pores on the damaged plasma membranes. The pH signal was correlated with the degree of hemolysis produced by the model reagents. The pH assay was sensitive to the formation of molecularly sized pores that were otherwise not measurable via detection of the leakage of hemoglobin, because the hydrodynamic radius of hemoglobin was greater than 3.1nm in the hemolysis assay. The pH transient was not disturbed by inherent ion-transporter activity. The ISFET assay was applied to a wide variety of cell types. The system presented here is fast, sensitive, practical and scalable, and will be useful for validating cytotoxins and nanomaterials. The plasma membrane toxicity and hemolysis are widely and routinely evaluated in biomaterials science and biomedical engineering. Despite the recent development of a variety of methods/materials for efficient gene/drug delivery systems to the cytosol, the methodologies for safety validation remain unchanged in

  18. Methodology of analysis of very weak acids by isotachophoresis with electrospray-ionization mass-spectrometric detection: Anionic electrolyte systems for the medium-alkaline pH range

    Czech Academy of Sciences Publication Activity Database

    Malá, Zdeňka; Gebauer, Petr

    2017-01-01

    Roč. 998, JAN (2017), s. 67-74 ISSN 0003-2670 R&D Projects: GA ČR(CZ) GA16-09135S Institutional support: RVO:68081715 Keywords : capillary isotachophoresis * ESI-MS detection * medium-alkaline pH Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 4.950, year: 2016

  19. Electrolyte system strategies for anionic isotachophoresis with electrosprayionization mass-spectrometric detection. 3. The ITP spacer technique in moving-boundary systems and configurations with two self-maintained ITP subsystems

    Czech Academy of Sciences Publication Activity Database

    Gebauer, Petr; Malá, Zdeňka; Boček, Petr

    2014-01-01

    Roč. 35, č. 5 (2014), s. 746-754 ISSN 0173-0835 R&D Project s: GA ČR(CZ) GA13-05762S Keywords : electrolyte systems * ESI-MS detection * moving-boundary electrophoresis * spacers * ITP Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.028, year: 2014

  20. High-Throughput Analysis of Plasma Hybrid Markers for Early Detection of Cancers

    Directory of Open Access Journals (Sweden)

    Jung-hyun Rho

    2014-01-01

    Full Text Available Biomarkers for the early detection of cancer in the general population have to perform with high sensitivity and specificity in order to prevent the costs associated with over-diagnosis. There are only a few current tissue or blood markers that are recommended for generalized cancer screening. Despite the recognition that combinations of multiple biomarkers will likely improve their utility, biomarker panels are usually limited to a single class of molecules. Tissues and body fluids including plasma and serum contain not only proteins, DNA and microRNAs that are differentially expressed in cancers but further cancer specific information might be gleaned by comparing different classes of biomolecules. For example, the level of a certain microRNA might be related to the level of a particular protein in a cancer specific manner. Proteins might have cancer-specific post-translational modifications (e.g., phosphorylation or glycosylation or lead to the generation of autoantibodies. Most currently approved biomarkers are glycoproteins. Autoantibodies can be produced as a host’s early surveillance response to cancer-specific proteins in pre-symptomatic and pre-diagnostic stages of cancer. Thus, measurement of the level of a protein, the level of its glycosylation or phosphorylation and whether autoantibodies are produced to it can yield multi-dimensional information on each protein. We consider specific proteins that show consistent cancer-specific changes in two or three of these measurements to be “hybrid markers”. We hypothesize these markers will suffer less variation between different individuals since one component can act to “standardize” the other measurement. As a proof of principle, a 180 plasma sample set consisting of 120 cases (60 colon cancers and 60 adenomas and 60 controls were analyzed using our high-density antibody array for changes in their protein, IgG-complex and sialyl-Lewis A (SLeA modified proteins. At p < 0

  1. Determination of lithium and potassium in uranium oxide powders and pellets by Flame Atomic Emission Spectrometric method

    International Nuclear Information System (INIS)

    Jat, J.R.; Balaji Rao, Y.; Prasada Rao, G.; Prahlad, B.

    2012-01-01

    The present paper describes a method developed at Control Laboratory, NFC which includes prior separation of lithium and potassium from uranium matrix before their measurements. Solvent extraction, using Tri-n-Butyl Phosphate (TBP) in CCI 4 followed by Tri-n-Octyl Phosphine Oxide (TOPO) in CCI 4 , is employed for prior separation of Li and K. The resultant aqueous solution was analyzed by Flame-Atomic Emission Spectrometric (AES) method. Solvent extraction conditions are optimized for measurement of Li and K in the same aliquot. Experimental conditions such as instrument calibration, flame condition, fuel flow, sample flow rate through nebulizer, burner height etc. are also optimized. Under the optimal condition the detection limits achieved for lithium is 0.02 ppm and 0.2 ppm for potassium. A RSD of ± 3 % for Li at 0.05 ppm and ± 4% for K at 1 ppm level has been achieved in this method. The results of lithium in the sample are compared with the values obtained by Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). Similarly, values of potassium are compared with Flame-Atomic Absorption Spectrometry (Flame-AAS) technique. The comparisons are in good agreement. The above method is simple, sensitive, reproducible and can be used for measurement of lithium and potassium in UO 2 powder and pellets on regular basis

  2. Internal standardization in atomic-emission spectrometry using inductively coupled plasma

    International Nuclear Information System (INIS)

    Moore, G.L.

    1985-01-01

    The principle of internal standardization has been used in quantitative analytical emission spectroscopy since 1925 to minimize the errors arising from fluctuations in sample preparation, excitation-source conditions, and detection parameters. Although modern spectroscopic excitation sources are far more stable and electronic detection methods are more precise than before, the system for the introduction of the sample in spectrometric analysis using inductively coupled plasma (ICP) introduces significant errors, and internal standardization can still play a useful role in improving the overall precision of the analytical results. The criteria for the selection of the elements to be used as internal standards in arc and spark spectrographic analysis apply to a much lesser extent in ICP-spectrometric analysis. Internal standardization is recommended for use in routine ICP-simultaneous spectrometric analysis to improve its accuracy and precision and to provide a monitor for the reassurance of the analyst. However, the selection of an unsuitable reference element can result in misuse of the principle of internal standardization and, although internal standardization can be applied when a sequential monochromator is used, the main sources of error will not be minimized

  3. Plasma Biomarkers for Detecting Hodgkin's Lymphoma in HIV Patients

    Energy Technology Data Exchange (ETDEWEB)

    Varnum, Susan M.; Webb-Robertson, Bobbie-Jo M.; Hessol, Nancey; Smith, Richard D.; Zangar, Richard C.

    2011-12-16

    The lifespan of AIDS patients has increased as a result of aggressive antiretroviral therapy, and the incidences of the AIDS-defining cancers, Hodgkin's lymphoma and Kaposi sarcoma, are declining, Still, the increased longevity of AIDS patients is now associated with increased incidence of other cancers, including Hodgkin's lymphoma (HL). In order to determine if we could identify biomarkers for the early detection of HL, we undertook an accurate mass and elution time tag proteomics analysis of individual plasma samples from AIDS patients without HL (n=14) and with HL (n=22). This analysis identified 33 proteins, included C-reactive protein and three serum amyloid proteins, that were statistically (p<0.05) altered by at least 1.5-fold between the two groups. At least three of these proteins have previously been reported to be altered in the blood of HL patients. Ingenuity Pathway Analysis software identified 'inflammatory response' and 'cancer' as the top two, biological functions commonly associated with these proteins. The clear association of these proteins with cancer and inflammation suggests that they are truly associated with HL and that they would be useful in the detection of this disease.

  4. Moderate plasma treatment enhances the quality of optically detected magnetic resonance signals of nitrogen-vacancy centres in nanodiamonds

    Science.gov (United States)

    Sotoma, Shingo; Igarashi, Ryuji; Shirakawa, Masahiro

    2016-05-01

    We demonstrate that a moderate plasma treatment increases the quality of optically detected magnetic resonance (ODMR) signals from negatively charged nitrogen-vacancy centres in nanodiamonds (NDs). We measured the statistics of the ODMR spectra of 50-nm-size NDs before and after plasma treatment. We then evaluated each ODMR spectrum in terms of fluorescence and ODMR intensities, line width and signal-to-noise (SN) ratio. Our results showed that plasma treatment for more than 10 min contributes to higher-quality ODMR signals, i.e. signals that are brighter, stronger, sharper and have a higher SN ratio. We showed that such signal improvement is due to alteration of the surface chemical states of the NDs by the plasma treatment. Our study contributes to the advancement of biosensing applications using ODMR of NDs.

  5. Moessbauer spectrometric data acquisition based on FPGA

    International Nuclear Information System (INIS)

    Zhang Yuan; Li Shimin; Chen Nan; Zhu Jingbo; Xia Yuanfu

    2008-01-01

    FPGA(Field Programmable Gate Array) is a programmable device with strong logical function and timing control ability. It is extremely potent in acquiring and processing timing signals. By replacing the traditional used SCM (Single-Chip Microcomputer) with FPGA, counting speed of Moessbauer spectrometric data acquisition can be improved markedly with significantly decreased size of the spectrometer. The counter, RAM and RS-232 communication of the module are developed on Altera Cyclone series chip EP1C6T144C8 with Quartus II. EP1C6T144C8 has 5980 logical units accompanied by 92160 bits of memory space. It is so powerful that all needs in data acquisition of the Moessbauer spectrometer can be perfectly satisfied while allowing modifications in functions and parameters. (authors)

  6. Mass Spectrometric Analysis of Synthetic Organic Pigments.

    Science.gov (United States)

    Sugaya, Naeko; Takahashi, Mitsuko; Sakurai, Katsumi; Tanaka, Nobuko; Okubo, Ichiro; Kawakami, Tsuyoshi

    2018-04-18

    Though synthetic organic colorants are used in various applications nowadays, there is the concern that impurities by-produced during the manufacturing and degradation products in some of these colorants are persistent organic pollutants and carcinogens. Thus, it is important to identify the synthetic organic colorants in various products, such as commercial paints, ink, cosmetics, food, textile, and plastics. Dyes, which are soluble in water and other solvents, could be analyzed by chromatographic methods. In contrast, it is difficult to analyze synthetic organic pigments by these methods because of their insolubility. This review is an overview of mass spectrometric analysis of synthetic organic pigments by various ionization methods. We highlight a recent study of textile samples by atmospheric pressure solid analysis probe MS. Furthermore, the mass spectral features of synthetic organic pigments and their separation from other components such as paint media and plasticizers are discussed.

  7. Determination of phenyl-N-methylcarbamates and their hydrolysis products in water, using solid-phase extraction and reversed-phase liquid chromatography with UV and electrospray mass spectrometric detection

    International Nuclear Information System (INIS)

    El Atrache, L.L.; Sabbah, S.

    2003-01-01

    In this study, eight phenyl-N-methylcarbamates (PNMCs) were considered. Reversed-phase LC was set up for UV and mass spectrometry (MS) detection mode. Gradient elution was used, and the mobile phase was composed of acetonitrile and water. UV-vis was performed at 220 nm. The method was tested with different reversed-phase columns. Comparison between chromatographic parameters: retention time (t R ), resolution (R S ), and selectivity (α) was established. Hydrolysis kinetics of three of the PNMCs were reported. The major hydrolysis products were determined by LC-UV, and the effect of pH on hydrolysis was also studied. Also, chromatographic separation of a mixture of PNMCs and four of their hydrolysis products was carried out. The preconcentration of 12 studied solutes was realized by solid-phase extraction. C18 extraction cartridges of 1 g were used to extract solutes from a 100 mL volume of tap and surface water spiked at 10 μg/L. The recoveries were, respectively, between 68-86% and 62-83% with relative a standard deviation of less than 11%. Limits of detection (LODs) and limits of quantitation (LOQs) ranged, respectively, from 1-4 μg/L and from 4-10 μg/L. Since standard UV detection does not provide adequate selectivity for water samples, an electrospray (ES)-MS instrument equipped with a triple quadrupole mass filter was used. MS data acquisition was performed by a time-scheduled, selected-ion monitoring (SIM) program. Limits of quantitation gave values between 0.1-0.5 μg/L. (author)

  8. Quantitative determination of the dopamine agonist lisuride in plasma using high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Wolthers, B G; Verhagen Kamerbeek, W D; van Beusekom, C M; Elshof, F; de Ruyter Buitenhuis, A W; Brunt, E P; Lakke, J P

    1993-12-08

    An HPLC method for the determination of lisuride hydrogen maleate in plasma is described. After addition of ergotamine tartrate as internal standard, plasma is extracted with diethyl ether. Following evaporation of the solvent and redissolving in methanol the extract is injected on a silica HPLC column and lisuride is monitored by fluorescence detection using an excitation wavelength of 322 nm and an emission wavelength of 405 nm. The method is sufficiently accurate and precise with a detection limit of 20 pg/ml lisuride in plasma. The usefulness of the method is demonstrated by measurements of lisuride levels after oral intake of a 0.6 mg dose of the drug by a healthy male volunteer, showing a peak level of 1266 pg/ml, 45 min after intake.

  9. Non-invasive aneuploidy detection using free fetal DNA and RNA in maternal plasma: recent progress and future possibilities.

    NARCIS (Netherlands)

    Go, A.T.; Vugt, J.M.G. van; Oudejans, C.B.

    2011-01-01

    BACKGROUND: Cell-free fetal DNA (cff DNA) and RNA can be detected in maternal plasma and used for non-invasive prenatal diagnostics. Recent technical advances have led to a drastic change in the clinical applicability and potential uses of free fetal DNA and RNA. This review summarizes the latest

  10. Transversely Excited Atmospheric CO2 Laser-Induced Plasma Spectroscopy for the Detection of Heavy Metals in Soil

    Science.gov (United States)

    Khumaeni, A.; Sugito, H.; Setia Budi, W.; Yoyo Wardaya, A.

    2018-01-01

    A rapid detection of heavy metals in soil was presented by the metal-assisted gas plasma method using specific characteristics of a pulsed, transversely excited atmospheric (TEA) CO2 laser. The soil particles were placed in a hole made of acrylic plate. The sample was covered by a to prevent the soil particles from being blown off. The mesh also functioned to initiate a luminous plasma. When a TEA CO2 laser (1500 mJ, 200 ns) was focused on the soil sample, passing through the metal mesh, some of the laser energy was used to generate the gas plasma on the mesh surface, and the remaining laser energy was employed to ablate the soil particles. The fine, ablated soil particles moved into the gas plasma region to be dissociated and excited. Using this technique, analysis can be made with reduced sample pretreatment, and therefore a rapid analysis can be performed efficiently. The results proved that the signal to noise ratio (S/N) of the emission spectral lines is much better for the case of the present method (mesh method) compared to the case of standard laser-induced breakdown spectroscopy using the pellet method. Rapid detection of heavy metal elements in soil has been successfully carried out. The detection limits of Cu and Hg in soil were estimated to be 3 and 10 mg/kg, respectively. The present method has good potential for rapid and sensitive detection of heavy metals in soil samples.

  11. Automated detection and analysis of particle beams in laser-plasma accelerator simulations

    International Nuclear Information System (INIS)

    Ushizima, Daniela Mayumi; Geddes, C.G.; Cormier-Michel, E.; Bethel, E. Wes; Jacobsen, J.; Prabhat; Ruebel, O.; Weber, G.; Hamann, B.

    2010-01-01

    scientific data mining is increasingly considered. In plasma simulations, Bagherjeiran et al. presented a comprehensive report on applying graph-based techniques for orbit classification. They used the KAM classifier to label points and components in single and multiple orbits. Love et al. conducted an image space analysis of coherent structures in plasma simulations. They used a number of segmentation and region-growing techniques to isolate regions of interest in orbit plots. Both approaches analyzed particle accelerator data, targeting the system dynamics in terms of particle orbits. However, they did not address particle dynamics as a function of time or inspected the behavior of bunches of particles. Ruebel et al. addressed the visual analysis of massive laser wakefield acceleration (LWFA) simulation data using interactive procedures to query the data. Sophisticated visualization tools were provided to inspect the data manually. Ruebel et al. have integrated these tools to the visualization and analysis system VisIt, in addition to utilizing efficient data management based on HDF5, H5Part, and the index/query tool FastBit. In Ruebel et al. proposed automatic beam path analysis using a suite of methods to classify particles in simulation data and to analyze their temporal evolution. To enable researchers to accurately define particle beams, the method computes a set of measures based on the path of particles relative to the distance of the particles to a beam. To achieve good performance, this framework uses an analysis pipeline designed to quickly reduce the amount of data that needs to be considered in the actual path distance computation. As part of this process, region-growing methods are utilized to detect particle bunches at single time steps. Efficient data reduction is essential to enable automated analysis of large data sets as described in the next section, where data reduction methods are steered to the particular requirements of our clustering analysis

  12. Mirion--a software package for automatic processing of mass spectrometric images.

    Science.gov (United States)

    Paschke, C; Leisner, A; Hester, A; Maass, K; Guenther, S; Bouschen, W; Spengler, B

    2013-08-01

    Mass spectrometric imaging (MSI) techniques are of growing interest for the Life Sciences. In recent years, the development of new instruments employing ion sources that are tailored for spatial scanning allowed the acquisition of large data sets. A subsequent data processing, however, is still a bottleneck in the analytical process, as a manual data interpretation is impossible within a reasonable time frame. The transformation of mass spectrometric data into spatial distribution images of detected compounds turned out to be the most appropriate method to visualize the results of such scans, as humans are able to interpret images faster and easier than plain numbers. Image generation, thus, is a time-consuming and complex yet very efficient task. The free software package "Mirion," presented in this paper, allows the handling and analysis of data sets acquired by mass spectrometry imaging. Mirion can be used for image processing of MSI data obtained from many different sources, as it uses the HUPO-PSI-based standard data format imzML, which is implemented in the proprietary software of most of the mass spectrometer companies. Different graphical representations of the recorded data are available. Furthermore, automatic calculation and overlay of mass spectrometric images promotes direct comparison of different analytes for data evaluation. The program also includes tools for image processing and image analysis.

  13. Detection of Independent Associations of Plasma Lipidomic Parameters with Insulin Sensitivity Indices Using Data Mining Methodology.

    Directory of Open Access Journals (Sweden)

    Steffi Kopprasch

    Full Text Available Glucolipotoxicity is a major pathophysiological mechanism in the development of insulin resistance and type 2 diabetes mellitus (T2D. We aimed to detect subtle changes in the circulating lipid profile by shotgun lipidomics analyses and to associate them with four different insulin sensitivity indices.The cross-sectional study comprised 90 men with a broad range of insulin sensitivity including normal glucose tolerance (NGT, n = 33, impaired glucose tolerance (IGT, n = 32 and newly detected T2D (n = 25. Prior to oral glucose challenge plasma was obtained and quantitatively analyzed for 198 lipid molecular species from 13 different lipid classes including triacylglycerls (TAGs, phosphatidylcholine plasmalogen/ether (PC O-s, sphingomyelins (SMs, and lysophosphatidylcholines (LPCs. To identify a lipidomic signature of individual insulin sensitivity we applied three data mining approaches, namely least absolute shrinkage and selection operator (LASSO, Support Vector Regression (SVR and Random Forests (RF for the following insulin sensitivity indices: homeostasis model of insulin resistance (HOMA-IR, glucose insulin sensitivity index (GSI, insulin sensitivity index (ISI, and disposition index (DI. The LASSO procedure offers a high prediction accuracy and and an easier interpretability than SVR and RF.After LASSO selection, the plasma lipidome explained 3% (DI to maximal 53% (HOMA-IR variability of the sensitivity indexes. Among the lipid species with the highest positive LASSO regression coefficient were TAG 54:2 (HOMA-IR, PC O- 32:0 (GSI, and SM 40:3:1 (ISI. The highest negative regression coefficient was obtained for LPC 22:5 (HOMA-IR, TAG 51:1 (GSI, and TAG 58:6 (ISI.Although a substantial part of lipid molecular species showed a significant correlation with insulin sensitivity indices we were able to identify a limited number of lipid metabolites of particular importance based on the LASSO approach. These few selected lipids with the closest

  14. Monoclonal anti-human factor VII antibodies. Detection in plasma of a second protein antigenically and genetically related to factor VII.

    OpenAIRE

    Broze, G J; Hickman, S; Miletich, J P

    1985-01-01

    Several murine monoclonal anti-human Factor VII antibodies were produced using hybridoma technology. Two noncompetitive monoclonal antibodies were used to examine by Western blotting the Factor VII cross-reactive material (CRM) in normal human plasma and three commercially available congenitally Factor VII-deficient plasmas, and to construct a facile "sandwich" immunoassay for plasma Factor VII. A second, previously undescribed, form of Factor VII CRM was detected in human plasma, which on We...

  15. Energy dispersive X-Ray fluorescence spectrometric study of ...

    African Journals Online (AJOL)

    Energy dispersive X-Ray fluorescence spectrometric study of compositional differences in trace elements in dried Moringa oleifera leaves grown in two different agro-ecological locations in Ebonyi State, Nigeria.

  16. Gas Chromatography-Mass Spectrometric Analysis and Insecticidal ...

    African Journals Online (AJOL)

    HP

    Original Research Article. Gas Chromatography-Mass Spectrometric Analysis and ... into a natural fumigant/insecticide for the control of stored product insects. Keywords: Mallotus ..... stability as well as reduce cost. ACKNOWLEDGEMENT.

  17. Gas Chromatography-Mass Spectrometric Analysis of Nematicidal ...

    African Journals Online (AJOL)

    Gas Chromatography-Mass Spectrometric Analysis of Nematicidal Essential Oil of Valeriana ... Tropical Journal of Pharmaceutical Research ... have a potential to be developed to natural nematicides for the control of cereal cyst nematodes.

  18. Gas Chromatography-Mass Spectrometric Analysis and Insecticidal ...

    African Journals Online (AJOL)

    Tropical Journal of Pharmaceutical Research ... apelta aerial parts was analyzed by gas chromatography/mass spectrometric (GC/MS) to determine its composition. ... into a natural fumigant/insecticide for the control of stored product insects.

  19. Detection of HIV-1 p24 Gag in plasma by a nanoparticle-based bio-barcode-amplification method.

    Science.gov (United States)

    Kim, Eun-Young; Stanton, Jennifer; Korber, Bette T M; Krebs, Kendall; Bogdan, Derek; Kunstman, Kevin; Wu, Samuel; Phair, John P; Mirkin, Chad A; Wolinsky, Steven M

    2008-06-01

    Detection of HIV-1 in patients is limited by the sensitivity and selectivity of available tests. The nanotechnology-based bio-barcode-amplification method offers an innovative approach to detect specific HIV-1 antigens from diverse HIV-1 subtypes. We evaluated the efficacy of this protein-detection method in detecting HIV-1 in men enrolled in the Chicago component of the Multicenter AIDS Cohort Study (MACS). The method relies on magnetic microparticles with antibodies that specifically bind the HIV-1 p24 Gag protein and nanoparticles that are encoded with DNA and antibodies that can sandwich the target protein captured by the microparticle-bound antibodies. The aggregate sandwich structures are magnetically separated from solution, and treated to remove the conjugated barcode DNA. The DNA barcodes (hundreds per target) were identified by a nanoparticle-based detection method that does not rely on PCR. Of 112 plasma samples from HIV-1-infected subjects, 111 were positive for HIV-1 p24 Gag protein (range: 0.11-71.5 ng/ml of plasma) by the bio-barcode-amplification method. HIV-1 p24 Gag protein was detected in only 23 out of 112 men by the conventional ELISA. A total of 34 uninfected subjects were negative by both tests. Thus, the specificity of the bio-barcode-amplification method was 100% and the sensitivity 99%. The bio-barcode-amplification method detected HIV-1 p24 Gag protein in plasma from all study subjects with less than 200 CD4(+) T cells/microl of plasma (100%) and 19 out of 20 (95%) HIV-1-infected men who had less than 50 copies/ml of plasma of HIV-1 RNA. In a separate group of 60 diverse international isolates, representative of clades A, B, C and D and circulating recombinant forms CRF01_AE and CRF02_AG, the bio-barcode-amplification method identified the presence of virus correctly. The bio-barcode-amplification method was superior to the conventional ELISA assay for the detection of HIV-1 p24 Gag protein in plasma with a breadth of coverage for diverse

  20. Comprehensive solid-phase extraction of multitudinous bioactive peptides from equine plasma and urine for doping detection.

    Science.gov (United States)

    Guan, Fuyu; Robinson, Mary A

    2017-09-08

    The ability to analyze biological samples for multitudinous exogenous peptides with a single analytical method is desired for doping control in horse racing. The key to achieving this goal is the capability of extracting all target peptides from the sample matrix. In the present study, theory of mixed-mode solid-phase extraction (SPE) of peptides from plasma is described, and a generic mixed-mode SPE procedure has been developed for recovering multitudinous exogenous peptides with remarkable sequence diversity, from equine plasma and urine in a single procedure. Both the theory and the developed SPE procedure have led to the development of a novel analytical method for comprehensive detection of multitudinous bioactive peptides in equine plasma and urine using liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS). Thirty nine bioactive peptides were extracted with strong anion-exchange mixed-mode SPE sorbent, separated on a reversed-phase C 18 column and detected by HRMS and data-dependent tandem mass spectrometry. The limit of detection (LOD) was 10-50 pg mL -1 in plasma for most of the peptides and 100 pg mL -1 for the remaining. For urine, LOD was 20-400 pg mL -1 for most of the peptides and 1-4 ng mL -1 for the others. In vitro degradation of the peptides in equine plasma and urine was examined at ambient temperature; the peptides except those with a D-amino acid at position 2 were unstable not only in plasma but also in urine. The developed method was successful in analysis of plasma and urine samples from horses administered dermorphin. Additionally, dermorphin metabolites were identified in the absence of reference standards. The developed SPE procedure and LC-HRMS method can theoretically detect virtually all peptides present at a sufficient concentration in a sample. New peptides can be readily included in the method to be detected without method re-development. The developed method also generates such data that can be

  1. Endogenous Plasma Peptide Detection and Identification in the Rat by a Combination of Fractionation Methods and Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Fabrice Bertile

    2007-01-01

    Full Text Available Mass spectrometry-based analyses are essential tools in the field of biomarker research. However, detection and characterization of plasma low abundance and/or low molecular weight peptides is challenged by the presence of highly abundant proteins, salts and lipids. Numerous strategies have already been tested to reduce the complexity of plasma samples. The aim of this study was to enrich the low molecular weight fraction of rat plasma. To this end, we developed and compared simple protocols based on membrane filtration, solid phase extraction, and a combination of both. As assessed by UV absorbance, an albumin depletion 99% was obtained. The multistep fractionation strategy (including reverse phase HPLC allowed detection, in a reproducible manner (CV [1] 30%–35%, of more than 450 peaks below 3000 Da by MALDI-TOF/MS. A MALDI-TOF/MS-determined LOD as low as 1 fmol/μL was obtained, thus allowing nanoLC-Chip/ MS/MS identification of spiked peptides representing ∼10–6% of total proteins, by weight. Signal peptide recovery ranged between 5%–100% according to the spiked peptide considered. Tens of peptide sequence tags from endogenous plasma peptides were also obtained and high confidence identifications of low abundance fibrinopeptide A and B are reported here to show the efficiency of the protocol. It is concluded that the fractionation protocol presented would be of particular interest for future differential (high throughput analyses of the plasma low molecular weight fraction.

  2. Detection of lung cancer using plasma protein profiling by matrix-assisted laser desorption/ionization mass spectrometry.

    Science.gov (United States)

    Shevchenko, Valeriy E; Arnotskaya, Natalia E; Zaridze, David G

    2010-01-01

    There are no satisfactory plasma biomarkers which are available for the early detection and monitoring of lung cancer, one of the most frequent cancers worldwide. The aim of this study is to explore the application of matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-ToF MS) to plasma proteomic patterns to distinguish lung cancer patients from healthy individuals. The EDTA plasma samples have been pre-fractionated using magnetic bead kits functionalized with weak cation exchange coatings. We compiled MS protein profiles for 90 patients with squamous cell carcinomas (SCC) and compared them with profiles from 187 healthy controls. The MALDI-ToF spectra were analyzed statistically using ClinProTools bioinformatics software. Depending on the sample used, up to 441 peaks/spectrum could be detected in a mass range of 1000-20,000 Da; 33 of these proteins had statistically differential expression levels between SCC and control plasma (P 90%) in external validation test. These results suggest that plasma MALDI-ToF MS protein profiling can distinguish patients with SCC and also from healthy individuals with relatively high sensitivity and specificity and that MALDI- ToF MS is a potential tool for the screening of lung cancer.

  3. Enhanced sensing of dengue virus DNA detection using O{sub 2} plasma treated-silicon nanowire based electrical biosensor

    Energy Technology Data Exchange (ETDEWEB)

    Rahman, S.F.A., E-mail: siti_fatimah0410@yahoo.com [Institute of Advanced Technology, Universiti Putra Malaysia, 43400, UPM, Serdang, Selangor (Malaysia); Yusof, N.A., E-mail: azahy@upm.edu.my [Institute of Advanced Technology, Universiti Putra Malaysia, 43400, UPM, Serdang, Selangor (Malaysia); Chemistry Department, Faculty of Science, Universiti Putra Malaysia, 43400, UPM, Serdang, Selangor (Malaysia); Hashim, U. [Institute of Nano Electronic Engineering, Universiti Malaysia Perlis, 01000, Kangar, Perlis (Malaysia); Hushiarian, R. [La Trobe Institute for Molecular Science, La Trobe University, Victoria, 3086 (Australia); Nuzaihan, M.N.M. [Institute of Nano Electronic Engineering, Universiti Malaysia Perlis, 01000, Kangar, Perlis (Malaysia); Hamidon, M.N. [Institute of Advanced Technology, Universiti Putra Malaysia, 43400, UPM, Serdang, Selangor (Malaysia); Zawawi, R.M. [Chemistry Department, Faculty of Science, Universiti Putra Malaysia, 43400, UPM, Serdang, Selangor (Malaysia); Fathil, M.F.M. [Institute of Nano Electronic Engineering, Universiti Malaysia Perlis, 01000, Kangar, Perlis (Malaysia)

    2016-10-26

    Dengue Virus (DENV) has become one of the most serious arthropod-borne viral diseases, causing death globally. The existing methods for DENV detection suffer from the late stage treatment due to antibodies-based detection which is feasible only after five days following the onset of the illness. Here, we demonstrated the highly effective molecular electronic based detection utilizing silicon nanowire (SiNW) integrated with standard complementary metal-oxide-semiconductor (CMOS) process as a sensing device for detecting deoxyribonucleic acid (DNA) related to DENV in an early stage diagnosis. To transform the fabricated devices as a functional sensing element, three-step procedure consist of SiNW surface modification, DNA immobilization and DNA hybridization were employed. The detection principle works by detecting the changes in current of SiNW which bridge the source and drain terminal to sense the immobilization of probe DNA and their hybridization with target DNA. The oxygen (O{sub 2}) plasma was proposed as an effective strategy for increasing the binding amounts of target DNA by modified the SiNW surface. It was found that the detection limit of the optimized O{sub 2} plasma treated-SiNW device could be reduced to 1.985 × 10{sup −14} M with a linear detection range of the sequence-specific DNA from 1.0 × 10{sup −9} M to 1.0 × 10{sup −13} M. In addition, the developed biosensor device was able to discriminate between complementary, single mismatch and non-complementary DNA sequences. This highly sensitive assay was then applied to the detection of reverse transcription-polymerase chain reaction (RT-PCR) product of DENV-DNA, making it as a potential method for disease diagnosis through electrical biosensor. - Highlights: • Molecular electronic detection of Dengue Virus (DENV) DNA using SiNW biosensor is presented. • Oxygen plasma surface treatment as an enhancer technique for device sensitivity is highlighted. • The limit of detection (Lo

  4. Enhanced sensing of dengue virus DNA detection using O_2 plasma treated-silicon nanowire based electrical biosensor

    International Nuclear Information System (INIS)

    Rahman, S.F.A.; Yusof, N.A.; Hashim, U.; Hushiarian, R.; Nuzaihan, M.N.M.; Hamidon, M.N.; Zawawi, R.M.; Fathil, M.F.M.

    2016-01-01

    Dengue Virus (DENV) has become one of the most serious arthropod-borne viral diseases, causing death globally. The existing methods for DENV detection suffer from the late stage treatment due to antibodies-based detection which is feasible only after five days following the onset of the illness. Here, we demonstrated the highly effective molecular electronic based detection utilizing silicon nanowire (SiNW) integrated with standard complementary metal-oxide-semiconductor (CMOS) process as a sensing device for detecting deoxyribonucleic acid (DNA) related to DENV in an early stage diagnosis. To transform the fabricated devices as a functional sensing element, three-step procedure consist of SiNW surface modification, DNA immobilization and DNA hybridization were employed. The detection principle works by detecting the changes in current of SiNW which bridge the source and drain terminal to sense the immobilization of probe DNA and their hybridization with target DNA. The oxygen (O_2) plasma was proposed as an effective strategy for increasing the binding amounts of target DNA by modified the SiNW surface. It was found that the detection limit of the optimized O_2 plasma treated-SiNW device could be reduced to 1.985 × 10"−"1"4 M with a linear detection range of the sequence-specific DNA from 1.0 × 10"−"9 M to 1.0 × 10"−"1"3 M. In addition, the developed biosensor device was able to discriminate between complementary, single mismatch and non-complementary DNA sequences. This highly sensitive assay was then applied to the detection of reverse transcription-polymerase chain reaction (RT-PCR) product of DENV-DNA, making it as a potential method for disease diagnosis through electrical biosensor. - Highlights: • Molecular electronic detection of Dengue Virus (DENV) DNA using SiNW biosensor is presented. • Oxygen plasma surface treatment as an enhancer technique for device sensitivity is highlighted. • The limit of detection (LoD) as low as 1.985

  5. Rapid, Sensitive and Validated Ultra-Performance Liquid Chromatography/Mass Spectrometric Method for the Determination of Fenofibric Acid and its Application to Human Pharmacokinetic Study

    Directory of Open Access Journals (Sweden)

    Sunil K. Dubey

    2010-01-01

    Full Text Available The first, rapid and sensitive ultra performance liquid chromatography mass spectrometric method for the determination of fenofibric acid, the active metabolite of fenofibrate, a lipid regulating agent, in human EDTA plasma has been developed and validated using fenofibric d6 acid as internal standard and Waters LC-MS/MS. Negative ions of fenofibric acid and fenofibric d6 acid were detected in multiple reaction-monitoring (MRM mode. The method was validated over a concentration range of 0.176 μg/mL to 19.837 μg/mL (r ≥ 0.99. It took only 1.5 minute to analyse a sample. Intra- and inter-run precision of fenofibric acid assay at four concentrations ranged from 0.5% to 4.3% with accuracy varied from 93.1 to 108.1% indicating good precision and accuracy. Analytical recoveries of fenofibric acid and internal standard in plasma were less than 90%. This method was successfully applied for evaluation of pharmacokinetics of fenofibric acid after a single oral dose of 145 mg fenofibrate to 10 Indian healthy volunteers

  6. An evaluation of inductively coupled plasma optical emission spectrometry using electrothermal atomisation sample introduction and photographic plate detection

    International Nuclear Information System (INIS)

    Khathing, D.T.; Pickford, C.J.

    1984-05-01

    A photographic radiation measurement approach has been used with an inductively coupled plasma source to evaluate and tabulate the more prominent optical emission lines of 66 elements. Compared with the more common sample introduction technique using nebulisation, increased sensitivity for multielement analysis of small samples was achieved by using a simple graphite electrothermal atomisation system. This was constructed to serve as a dual purpose atomiser ie both for Atomic Absorption and for Inductively Coupled Plasma Emission spectroscopy. The system offers the advantage of a wide multi-elemental coverage, but sensitivities achieved with photographic detection are poorer than those obtained photoelectrically. (author)

  7. The detection of ovulation with a two-hour radioimmunoassay for human plasma luteinizing hormone using the Centria Analyzer

    International Nuclear Information System (INIS)

    Schwarz, S.

    1980-01-01

    We describe a rapid (2-h) radioimmunoassay for human plasma luteinizing hormone which utilizes the reagents from a commercially available kit. Standardization of the assay was achieved using plasma standards instead of a buffer system and the Centria radioimmunoassay centrifugal analyzer which allowed simultaneous initiation and termination of reactions in all assay tubes. The specificity, precision, and accuracy of the assay were equal to or better than the conventional 24-h assay. Since this assay is designed to detect the mid-cycle surge of luteinizing hormone, its decreased sensitivity was small price to pay for the speed with which a result could be obtained. (orig.) [de

  8. Radio spectrometric survey of un-surveyed areas in Syria

    International Nuclear Information System (INIS)

    Aissa, M.; Al-Hent, R; Jubeli, Y.

    2002-11-01

    The values and distribution of the radioelements e U, e Th, % K and Ur units in the surface geological formations of the west and south sectors of Syrian region, were estimated using carbone gamma ray spectrometric survey. The radiometric maps were prepared, as well as, many geological profiles, cross sections studied in different locations and geochemical samples were analyzed by laboratory gamma ray spectrometry and by x-ray diffractometry, the results of the all sets were compared. In general, the survey shows, low radioelement concentrations in the area, especially on basic rocks (Jabal Al-arab, Hawran) south Syria, and on ultra basic rocks (ophiolitic complex) north-west Syria, but there are some separate anomalous spots were connected with phosphate rocks, detected on cretaceous and Palaeogene age. Some times we noticed high radioelement concentrations haloes associated with fractured zones were already arise from secondary uranium mineralization, as a result of solutions movement through fissures in carbonatic and/or chalk like limestone rocks. finally, the obtained concentrations, represent a background values which has no significant importance for uranium exploration point of view. (author)

  9. Detection, in real time, of metallic pollutants present in the industrial atmospheric effluents by inductively coupled plasma torch; Detection, en temps reel, d'elements metalliques presents dans les rejets atmospheriques industriels par torche a plasma a couplage inductif

    Energy Technology Data Exchange (ETDEWEB)

    Vacher, D.

    2001-12-15

    This work is devoted to the development of a process of detection in real time of metallic pollutants present in industrial atmospheric effluents. The method of measurement is the atomic spectrometry of emission coupled to an ICP torch (Inductively coupled Plasma). The technology of the fluidized beds is used as system of introduction of the metallic particles into the ICP torch, the interest of the principle of detection resting on the stamping from the usual procedure of calibration of the analytical system. The results are presented in two parts. The first relates to the diagnosis of plasmas formed with various mixtures of N{sub 2}/O{sub 2} which one corresponds to pure air, the second presents the setting process of detection in real time starting from the intensities ratios of the spectral lines of the metallic element with those of the plasma-producing element (argon or pure air) The study of the diagnosis of plasmas made up of mixtures N{sub 2}/O{sub 2} relates to the determination of the atomic excitation temperature from the spectral lines of the copper element and the evaluation of the thermal disequilibrium q Te/Th. This last is obtained by considering the mass enthalpy of various mixtures N{sub 2}/O{sub 2}. The existence of a small thermal disequilibrium is highlighted. The study of detection in real time by ICP torch, without calibration of the system, is based on three points: - spectroscopic data processing to determine the values of the intensities ratios of spectral lines; - the insertion of the intensities ratios and the characteristics of plasma (argon or pure air) into a calculation code of plasma composition; - the comparison of the mass flux values of the metallic pollutants, in real time, obtained by experiments with those resulting from the elutriation calculation, term which defines the phenomenon of entrainment of the particles out of the fluidized bed. The results made it possible to show the similarity of the analytical system response

  10. Gas Chromatographic Mass Spectrometric Determination of Myo-inositol in Humans Utilizing a Deuterated Internal Standard

    DEFF Research Database (Denmark)

    Andersen, Jan Rud; Larsen, Elfinn; Harbo, Helge

    1982-01-01

    The isotopic dilution technique was used for determining the content of myo-inositol in human urine, plasma and haemolysed erythrocyte samples. A deuterated myo-inositol, synthesized from inosose-2 by base-catalysed exchange of hydrogens by deuterium, followed by reduction of the inosose with 2H2......, was added as internal standard to the samples at an early stage in the analytical procedure. After separation and derivatization to the hexa-acetate, the gas chromatographic mass spectrometric analysis was carried out. A 25 m fused silica capillary column coated with methyl silicone was used, and the ions...... selected for monitoring were m/z 210 and m/z 214, which are characteristic and abundant fragment ions from unlabelled and hexadeuterated myo-inositolhexa-acetate, respectively. Calibration curves from water, urine, plasma and haemolysed erythrocytes show parallel, linear responses in the ratio between...

  11. Plasma erythropoietin by high-detectability immunoradiometric assay in untreated and treated patients with polycythaemia vera and essential thrombocythaemia

    Energy Technology Data Exchange (ETDEWEB)

    Carneskog, J.; Kutti, J.; Wadenvik, H. [Univ. of Goeteborg, Sahlgrenska Univ. Hospital, Dept. of Medicine, Haematology Section (Sweden); Lundberg, P.A.; Lindstedt, G. [Univ. of Goeteborg, Sahlgrenska Univ. Hospital, Dept. of Clinical Chemistry and Transfusion Medicine (Sweden)

    1998-12-31

    By using an immunoradiometric method with a stated detection limit of {<=}1 IU/l (stated normal reference limit in adults 3.7-16 IU/l) we determined EDTA-plasma erythropoietin (EPO) in 58 patients with polycythaemia vera (PV) and 49 patients with essential thrombocythaemia (ET). At the time of blood sampling, 20 of the PV patients were newly diagnosed and untreated, 23 were treated by phlebotomy only, and 30 also received myelosuppressive treatment (with 32P, hydroxyurea of alpha-interferon). Of the ET patients 24 were untreated and 28 received myelosuppressive therapy. For comparison plasma EPO was also determined in 10 patients with pseudopolycythaemia (PP). In this latter group the results for plasma EPO agreed well with the cited normal reference limits. The majority of untreated PV patients (12/20) had undetectable plasma EPO concentration, and the remainder all had values below the lower normal reference limit. Plasma EPO in PV was not significantly influenced by phlebotomy therapy. Twelve of the 24 untreated ET patients (50%) had plasma EPO values below the reference interval (undetectable in 2 patients). The mean EPO concentration was significantly lower in PV patients receiving phlebotomy therapy than in patients with untreated ET. In the total material of PV and ET treated with myelosuppressive agents the PV patients showed significantly lower values for EPO concentration than did patients with ET. The present results support the view that EPO measurements by high-detectability methods are diagnostically useful and should be included in the panel of new criteria for the diagnosis of PV. (au) 20 refs.

  12. An evaluation of saliva as an alternative to plasma for the detection of hepatitis C virus antibodies

    Directory of Open Access Journals (Sweden)

    Moorthy M

    2008-01-01

    Full Text Available Purpose: Seroepidemiological studies on the prevalence of Hepatitis C virus (HCV in India have been hampered by reluctance of subjects to provide blood samples for testing. We evaluated the use of saliva as an alternate specimen to blood for the detection of antibodies to HCV. Methods: Chronic liver disease (CLD patients attending the liver clinic were recruited for this study. A saliva and plasma sample (sample pair was collected from each patient included in the study. Saliva samples were collected using a commercially available collection device - OmniSal. Sample pairs were tested with an in-use ELISA for the detection of antibodies to HCV (HCV-Ab, with a minor modification in the manufacturer′s protocol while testing saliva. The cut-off absorbance value for declaring a sample as positive was determined by receiver operating curve (ROC analysis. HCV-Ab positivity in saliva was compared with that in plasma as well as with viral load in plasma and infecting genotype of the virus. Sensitivity, specificity, positive and negative predictive values, and correlation coefficients were calculated using Medcalc statistical software. Results: The optimal accuracy indices were: sensitivity-81.6%; specificity-92.5%; PPV-85.1% and NPV-90.5%. No correlation was found between salivary positivity and HCV viral load in plasma or infecting genotype. Conclusions: The accuracy indices indicate that the assay must be optimized further before it can be recommended for routine use in epidemiological surveys for HCV-Ab.

  13. Application value of Serum Hs-CRP, IL-6 and plasma FIB joint detection in COPD

    Directory of Open Access Journals (Sweden)

    Feng Ji

    2016-11-01

    .86%; Specificities were 80.46%, 83.91%, 79.31%; Accuracies were 93.10%, 95.40%, 94.83%. Conclusions: COPD illness evolution and severity could be reflected by serum hs-CRP, IL-6 and plasma FIB all in some extent, the joint detection could be a reference on prognostic evaluation.

  14. Anomaly disentanglement on the basis of automatic processing of the aerial gamma-spectrometric survey data

    International Nuclear Information System (INIS)

    Perlovskij, V.A.; Zaika, S.D.; Lomtadze, V.V.

    1976-01-01

    Automated processing airborne gamma spectrometric data has been introduced with the use of the BESM-4 computer. Discrimination of anomalies is effected using a variable interval 200-300 m within which maximum values in the general counting channel and their coordinates are found; reference points are detected too against which one can determine the excess and amplitude of the anomalies. The discriminated anomalies are fixed on printer and charts of anomalies are constructed. The charts and tables characterizing the anomaly help in the identification of its potentialities and hence underlie a decision to start ground works

  15. Validation and implementation of liquid chromatographic-mass spectrometric (LC-MS) methods for the quantification of tenofovir prodrugs.

    Science.gov (United States)

    Hummert, Pamela; Parsons, Teresa L; Ensign, Laura M; Hoang, Thuy; Marzinke, Mark A

    2018-04-15

    The nucleotide reverse transcriptase inhibitor tenofovir (TFV) is widely administered in a disoproxil prodrug form (tenofovir disoproxil fumarate, TDF) for HIV management and prevention. Recently, novel prodrugs tenofovir alafenamide fumarate (TAF) and hexadecyloxypropyl tenofovir (CMX157) have been pursued for HIV treatment while minimizing adverse effects associated with systemic TFV exposure. Dynamic and sensitive bioanalytical tools are required to characterize the pharmacokinetics of these prodrugs in systemic circulation. Two parallel methods have been developed, one to combinatorially quantify TAF and TFV, and a second method for CMX157 quantification, in plasma. K 2 EDTA plasma was spiked with TAF and TFV, or CMX157. Following the addition of isotopically labeled internal standards and sample extraction via solid phase extraction (TAF and TFV) or protein precipitation (CMX157), samples were subjected to liquid chromatographic-tandem mass spectrometric (LC-MS/MS) analysis. For TAF and TFV, separation occurred using a Zorbax Eclipse Plus C18 Narrow Bore RR, 2.1 × 50 mm, 3.5 μm column and analytes were detected on an API5000 mass analyzer; CMX157 was separated using a Kinetex C8, 2.1 × 50 mm, 2.6 μm column and quantified using an API4500 mass spectrometer. Methods were validated according to FDA Bioanalytical Method Validation guidelines. Analytical methods: were optimized for the multiplexed monitoring of TAF and TFV, and CMX157 in plasma. The lower limits of quantification (LLOQs) for TAF, TFV, and CMX157 were 0.03, 1.0, and 0.25 ng/mL, respectively. Calibration curves were generated via weighted linear regression of standards. Intra- and inter-assay precision and accuracy studies demonstrated %CVs ≤ 14.4% and %DEVs ≤ ± 7.95%, respectively. Stability and matrix effects studies were also performed. All results were acceptable and in accordance with the recommended guidelines for bioanalytical methods. Assays were also

  16. Magnetic spires for the detection of the position of the plasma column in a Tokamak (linear approximation); Espiras magneticas para la deteccion de la posicion de la columna de plasma en un Tokamak (aproximacion lineal)

    Energy Technology Data Exchange (ETDEWEB)

    Colunga S, S

    1990-07-15

    In this report the simplified analysis of a method to detect the movement of the plasma column of a tokamak in the vertical direction and of the biggest radius is given. The peculiar case of the Tokamak Novillo of the Plasma Physics Laboratory of the ININ is studied. (Author)

  17. Mass spectrometric detection of 27-hydroxycholesterol in breast cancer exosomes.

    Science.gov (United States)

    Roberg-Larsen, Hanne; Lund, Kaja; Seterdal, Kristina Erikstad; Solheim, Stian; Vehus, Tore; Solberg, Nina; Krauss, Stefan; Lundanes, Elsa; Wilson, Steven Ray

    2017-05-01

    Exosomes from cancer cells are rich sources of biomarkers and may contain elevated levels of lipids of diagnostic value. 27-Hydroxycholesterol (27-OHC) is associated with proliferation and metastasis in estrogen receptor positive (ER+) breast cancer. In this study, we investigated the levels of 27-OHC, and other sidechain-hydroxylated oxysterols in exosomes. To study both cytoplasmic and exosomal oxysterol samples of limited size, we have developed a capillary liquid chromatography-mass spectrometry platform that outperforms our previously published systems regarding chromatographic resolution, analysis time and sensitivity. In the analyzed samples, the quantified level of cytoplasmic 27-OHC using this platform fitted with mRNA levels of 27-OHC's corresponding enzyme, CYP27A1. We find clearly increased levels of 27-OHC in exosomes (i.e., enrichment) from an ER+ breast cancer cell line (MCF-7) compared to exosomes derived from an estrogen receptor (ER-) breast cancer cell line (MDA-MB-231) and other control exosomes (non-cancerous cell line (HEK293) and human pooled serum). The exosomal oxysterol profile did not reflect cytoplasmic oxysterol profiles in the cells of origin; cytoplasmic 27-OHC was low in ER+ MCF-7 cells while high in MDA-MB-231 cells. Other control cancer cells showed varied cytoplasmic oxysterol levels. Hence, exosome profiling in cancer cells might provide complementary information with the possibility of diagnostic value. Copyright © 2016 Elsevier Ltd. All rights reserved.

  18. Detection of artificially ripened mango using spectrometric analysis

    Science.gov (United States)

    Mithun, B. S.; Mondal, Milton; Vishwakarma, Harsh; Shinde, Sujit; Kimbahune, Sanjay

    2017-05-01

    Hyperspectral sensing has been proven to be useful to determine the quality of food in general. It has also been used to distinguish naturally and artificially ripened mangoes by analyzing the spectral signature. However the focus has been on improving the accuracy of classification after performing dimensionality reduction, optimum feature selection and using suitable learning algorithm on the complete visible and NIR spectrum range data, namely 350nm to 1050nm. In this paper we focus on, (i) the use of low wavelength resolution and low cost multispectral sensor to reliably identify artificially ripened mango by selectively using the spectral information so that classification accuracy is not hampered at the cost of low resolution spectral data and (ii) use of visible spectrum i.e. 390nm to 700 nm data to accurately discriminate artificially ripened mangoes. Our results show that on a low resolution spectral data, the use of logistic regression produces an accuracy of 98.83% and outperforms other methods like classification tree, random forest significantly. And this is achieved by analyzing only 36 spectral reflectance data points instead of the complete 216 data points available in visual and NIR range. Another interesting experimental observation is that we are able to achieve more than 98% classification accuracy by selecting only 15 irradiance values in the visible spectrum. Even the number of data needs to be collected using hyper-spectral or multi-spectral sensor can be reduced by a factor of 24 for classification with high degree of confidence

  19. The significance and robustness of a plasma free amino acid (PFAA) profile-based multiplex function for detecting lung cancer

    International Nuclear Information System (INIS)

    Shingyoji, Masato; Mitsushima, Toru; Yamakado, Minoru; Kimura, Hideki; Iizasa, Toshihiko; Higashiyama, Masahiko; Imamura, Fumio; Saruki, Nobuhiro; Imaizumi, Akira; Yamamoto, Hiroshi; Daimon, Takashi; Tochikubo, Osamu

    2013-01-01

    We have recently reported on the changes in plasma free amino acid (PFAA) profiles in lung cancer patients and the efficacy of a PFAA-based, multivariate discrimination index for the early detection of lung cancer. In this study, we aimed to verify the usefulness and robustness of PFAA profiling for detecting lung cancer using new test samples. Plasma samples were collected from 171 lung cancer patients and 3849 controls without apparent cancer. PFAA levels were measured by high-performance liquid chromatography (HPLC)–electrospray ionization (ESI)–mass spectrometry (MS). High reproducibility was observed for both the change in the PFAA profiles in the lung cancer patients and the discriminating performance for lung cancer patients compared to previously reported results. Furthermore, multivariate discriminating functions obtained in previous studies clearly distinguished the lung cancer patients from the controls based on the area under the receiver-operator characteristics curve (AUC of ROC = 0.731 ~ 0.806), strongly suggesting the robustness of the methodology for clinical use. Moreover, the results suggested that the combinatorial use of this classifier and tumor markers improves the clinical performance of tumor markers. These findings suggest that PFAA profiling, which involves a relatively simple plasma assay and imposes a low physical burden on subjects, has great potential for improving early detection of lung cancer

  20. Simultaneous detection of xenon and krypton in equine plasma by gas chromatography-tandem mass spectrometry for doping control.

    Science.gov (United States)

    Kwok, Wai Him; Choi, Timmy L S; So, Pui-Kin; Yao, Zhong-Ping; Wan, Terence S M

    2017-02-01

    Xenon can activate the hypoxia-inducible factors (HIFs). As such, it has been allegedly used in human sports for increasing erythropoiesis. Krypton, another noble gas with reported narcosis effect, can also be expected to be a potential and less expensive erythropoiesis stimulating agent. This has raised concern about the misuse of noble gases as doping agents in equine sports. The aim of the present study is to establish a method for the simultaneous detection of xenon and krypton in equine plasma for the purpose of doping control. Xenon- or krypton-fortified equine plasma samples were prepared according to reported protocols. The target noble gases were simultaneously detected by gas chromatography-triple quadrupole mass spectrometry using headspace injection. Three xenon isotopes at m/z 129, 131, and 132, and four krypton isotopes at m/z 82, 83, 84, and 86 were targeted in selected reaction monitoring mode (with the precursor ions and product ions at identical mass settings), allowing unambiguous identification of the target analytes. Limits of detection for xenon and krypton were about 19 pmol/mL and 98 pmol/mL, respectively. Precision for both analytes was less than 15%. The method has good specificity as background analyte signals were not observed in negative equine plasma samples (n = 73). Loss of analytes under different storage temperatures has also been evaluated. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  1. A neural network detection system for lower-hybrid cavities in electron plasma density measured by the FREJA satellite

    International Nuclear Information System (INIS)

    Waldemark, J.; Karlsson, Jan

    1995-03-01

    This paper presents a lower-hybrid cavity detection system, CDS, for measurements of electron plasma density on the FREJA satellite wave experiment. The system can reduce the amount of data to be analysed by as much as 96% and still retain more than 85% of the desired information. The CDS is a combination of a hybrid neural network, HNN and expert rules. The HNN is a Self Organizing Map, SOM, combined with a feed forward back propagation neural net, BP. The CDS can be controlled by the user to operate with various degrees of sensitivity. Maximum detection capability is as high as 95% with data reduction lowered to 85%. 10 refs

  2. Novel charge plasma based dielectric modulated impact ionization MOSFET as a biosensor for label-free detection

    Science.gov (United States)

    Chanda, Manash; Dey, Prithu; De, Swapnadip; Sarkar, Chandan Kumar

    2015-10-01

    In this paper a charge plasma based dielectric modulated impact ionization MOSFET (CP-DIMOSFET) has been proposed for the first time to ease the label free detection of biomolecules. The concept of CP-DIMOSFET is proposed and analyzed on basis of simulated data using SILVACO ATLAS. Low thermal budgeting and thin silicon layer without any dopant implantations make the proposed structure advantageous compared to the existing MOSFET based biosensors. The results show that the proposed device is capable to detect the presence of biomolecules. Simple fabrication schemes, miniaturization, high sensitivity, dominance of dielectric modulation make the proposed biosensor a promising one that could one day revolutionize the healthcare industry.

  3. Enhanced plasma wave detection of terahertz radiation using multiple high electron-mobility transistors connected in series

    KAUST Repository

    Elkhatib, Tamer A.; Kachorovskiǐ, Valentin Yu; Stillman, William J.; Veksler, Dmitry B.; Salama, Khaled N.; Zhang, Xicheng; Shur, Michael S.

    2010-01-01

    We report on enhanced room-temperature detection of terahertz radiation by several connected field-effect transistors. For this enhanced nonresonant detection, we have designed, fabricated, and tested plasmonic structures consisting of multiple InGaAs/GaAs pseudomorphic high electron-mobility transistors connected in series. Results show a 1.63-THz response that is directly proportional to the number of detecting transistors biased by a direct drain current at the same gate-to-source bias voltages. The responsivity in the saturation regime was found to be 170 V/W with the noise equivalent power in the range of 10-7 W/Hz0.5. The experimental data are in agreement with the detection mechanism based on the rectification of overdamped plasma waves excited by terahertz radiation in the transistor channel. © 2010 IEEE.

  4. Enhanced plasma wave detection of terahertz radiation using multiple high electron-mobility transistors connected in series

    KAUST Repository

    Elkhatib, Tamer A.

    2010-02-01

    We report on enhanced room-temperature detection of terahertz radiation by several connected field-effect transistors. For this enhanced nonresonant detection, we have designed, fabricated, and tested plasmonic structures consisting of multiple InGaAs/GaAs pseudomorphic high electron-mobility transistors connected in series. Results show a 1.63-THz response that is directly proportional to the number of detecting transistors biased by a direct drain current at the same gate-to-source bias voltages. The responsivity in the saturation regime was found to be 170 V/W with the noise equivalent power in the range of 10-7 W/Hz0.5. The experimental data are in agreement with the detection mechanism based on the rectification of overdamped plasma waves excited by terahertz radiation in the transistor channel. © 2010 IEEE.

  5. Development of gallium arsenide gamma spectrometric detector

    International Nuclear Information System (INIS)

    Kobayashi, T.; Kuru, I.

    1975-03-01

    GaAs semiconductor material has been considered to be a suitable material for gamma-ray spectrometer operating at room temperature since it has a wid-band gap, larger than that of silicon and germanium. The basic objective of this work is to develop a GaAs gamma-ray spectrometric detector which could be used for gamma spectrometric measurement of uranium and plutonium in nuclear fuel safeguards. Liquid phase epitaxial techniques using iron (Fe) as dopant have been developed in making high purity GaAs crystals suitable for gamma-ray spectrometer operating at room temperature. Concentration of Fe in the epitaxial crystal was controlled by initial growth temperature. The best quality epitaxial crystal was obtained under the following conditions: starting temperature is about 800degC, the proportion of Fe to Ga solvent is 1 to 300. Carrier concentration of epitaxial crystals grown distributed in the ranges of 10 12 cm -3 to 10 14 cm -3 at room temperature. The thickness of the crystals ranged from 38 μm to 120 μm. Au-GaAs surface barrier detector was made of epitaxial crystal. Some of the detector were encapsulated in a can with a 50 μm Be window by welding a can to the detector holder. The detector with high energy resolution and good charge collecting characteristics was selected by alpha spectrometry at room temperature. Energy resolution of the detector for gamma-rays up to about 200 keV was very good at room temperature operation. The best energy resolutions taken with a GaAs detector were 3 keV (fwhm) and 3.8 keV for 241 Am 59.6 keV and 57 Co 122 keV, respectively, at room temperature. In order to study the applicability of the detector for nuclear safeguards, the measurements of 235 U gamma-ray spectrum have been carried out at room temperature. It was clarified that the gamma-ray spectrum of enriched U sample could be measured in high resolution with GaAs detector at room temperature, and that the content of 235 U in enriched U sources could be determined by

  6. Plasma Panel Detectors for MIP Detection for the SLHC and a Test Chamber Design

    CERN Document Server

    Ball, Robert; Etzion, Erez; Friedman, Peter S; Levin, Daniel S; Moshe, Meny Ben; Weaverdyck, Curtis; Zhou, Bing

    2010-01-01

    Performance demands for high and super-high luminosity at the LHC (up to 10^35 cm^(-2) sec^(-1) after the 2017 shutdown) and at future colliders demand high resolution tracking detectors with very fast time response and excellent temporal and spatial resolution. We are investigating a new radiation detector technology based on Plasma Display Panels (PDP), the underlying engine of panel plasma television displays. The design and production of PDPs is supported by four decades of industrial development. Emerging from this television technology is the Plasma Panel Sensor (PPS), a novel variant of the micropattern radiation detector. The PPS is fundamentally an array of micro-Geiger plasma discharge cells operating in a non-ageing, hermetically sealed gas mixture . We report on the PPS development program, including design of a PPS Test Cell.

  7. Detection of cervical cancer biomarker patterns in blood plasma and urine by differential scanning calorimetry and mass spectrometry.

    Science.gov (United States)

    Garbett, Nichola C; Merchant, Michael L; Helm, C William; Jenson, Alfred B; Klein, Jon B; Chaires, Jonathan B

    2014-01-01

    Improved methods for the accurate identification of both the presence and severity of cervical intraepithelial neoplasia (CIN) and extent of spread of invasive carcinomas of the cervix (IC) are needed. Differential scanning calorimetry (DSC) has recently been shown to detect specific changes in the thermal behavior of blood plasma proteins in several diseases. This methodology is being explored to provide a complementary approach for screening of cervical disease. The present study evaluated the utility of DSC in differentiating between healthy controls, increasing severity of CIN and early and advanced IC. Significant discrimination was apparent relative to the extent of disease with no clear effect of demographic factors such as age, ethnicity, smoking status and parity. Of most clinical relevance, there was strong differentiation of CIN from healthy controls and IC, and amongst patients with IC between FIGO Stage I and advanced cancer. The observed disease-specific changes in DSC profiles (thermograms) were hypothesized to reflect differential expression of disease biomarkers that subsequently bound to and affected the thermal behavior of the most abundant plasma proteins. The effect of interacting biomarkers can be inferred from the modulation of thermograms but cannot be directly identified by DSC. To investigate the nature of the proposed interactions, mass spectrometry (MS) analyses were employed. Quantitative assessment of the low molecular weight protein fragments of plasma and urine samples revealed a small list of peptides whose abundance was correlated with the extent of cervical disease, with the most striking plasma peptidome data supporting the interactome theory of peptide portioning to abundant plasma proteins. The combined DSC and MS approach in this study was successful in identifying unique biomarker signatures for cervical cancer and demonstrated the utility of DSC plasma profiles as a complementary diagnostic tool to evaluate cervical cancer

  8. Detection of cervical cancer biomarker patterns in blood plasma and urine by differential scanning calorimetry and mass spectrometry.

    Directory of Open Access Journals (Sweden)

    Nichola C Garbett

    Full Text Available Improved methods for the accurate identification of both the presence and severity of cervical intraepithelial neoplasia (CIN and extent of spread of invasive carcinomas of the cervix (IC are needed. Differential scanning calorimetry (DSC has recently been shown to detect specific changes in the thermal behavior of blood plasma proteins in several diseases. This methodology is being explored to provide a complementary approach for screening of cervical disease. The present study evaluated the utility of DSC in differentiating between healthy controls, increasing severity of CIN and early and advanced IC. Significant discrimination was apparent relative to the extent of disease with no clear effect of demographic factors such as age, ethnicity, smoking status and parity. Of most clinical relevance, there was strong differentiation of CIN from healthy controls and IC, and amongst patients with IC between FIGO Stage I and advanced cancer. The observed disease-specific changes in DSC profiles (thermograms were hypothesized to reflect differential expression of disease biomarkers that subsequently bound to and affected the thermal behavior of the most abundant plasma proteins. The effect of interacting biomarkers can be inferred from the modulation of thermograms but cannot be directly identified by DSC. To investigate the nature of the proposed interactions, mass spectrometry (MS analyses were employed. Quantitative assessment of the low molecular weight protein fragments of plasma and urine samples revealed a small list of peptides whose abundance was correlated with the extent of cervical disease, with the most striking plasma peptidome data supporting the interactome theory of peptide portioning to abundant plasma proteins. The combined DSC and MS approach in this study was successful in identifying unique biomarker signatures for cervical cancer and demonstrated the utility of DSC plasma profiles as a complementary diagnostic tool to evaluate

  9. Toward sub-Kelvin resistive cooling and non destructive detection of trapped non-neutral electron plasma

    Science.gov (United States)

    Di Domizio, S.; Krasnický, D.; Lagomarsino, V.; Testera, G.; Vaccarone, R.; Zavatarelli, S.

    2015-01-01

    A resonant circuit tuned to a particular frequency of the motion of charged particles stored in a Penning trap and connected to a low noise amplifier allows, at the same time, cooling and non destructive detection of the particles. Its use is widely diffused when single or few particles are stored near the centre of a hyperbolic Penning trap. We present a consistent model that predicts the shape of the induced signal when the tuned circuit is used to detect and cool the axial motion of a cold non neutral plasma stored in an open-ended cylindrical Penning trap. The model correctly accounts for the not negligible axial plasma size. We show that the power spectrum of the signal measured across the tuned circuit provides information about the particle number and insights about the plasma temperature. We report on the design of a HEMT-based cryogenic amplifier working at 14.4 MHz and 4.2 K and the results of the noise measurements. We have measured a drain current noise in the range from 6 to 17 pA/√Hz, which corresponds to an increase of the tuned circuit equivalent temperature of at maximum 0.35 K. The cryogenic amplifier has a very low power consumption from few tens to few hundreds of μW corresponding to a drain current in the range 100-800 μ A. An additional contribution due to the gate noise has been identified when the drain current is below 300 μA above that value an upper limit of the increase of the equivalent tuned circuit temperature due to this contribution of 0.02 K has been obtained. These features make the tuned circuit connected to this amplifier a promising device for detecting and cooling the axial motion of an electron plasma when the Penning trap is mounted inside a dilution refrigerator.

  10. Alkylation of human serum albumin by sulfur mustard in vitro and in vivo : Mass spectrometric analysis of a cysteine adduct as a sensitive biomarker of exposure

    NARCIS (Netherlands)

    Noort, D.; Hulst, A.G.; Jong, L.P.A. de; Benschop, H.P.

    1999-01-01

    To develop a mass spectrometric assay for the detection of sulfur mustard adducts with human serum albumin, the following steps were performed: quantitation of the binding of the agent to the protein by using [14C] sulfur mustard and analysis of acidic and tryptic digests of albumin from blood after

  11. C-13 NMR spectroscopy of plasma reduces interference of hypertriglyceridemia in the H-1 NMR detection of malignancy

    International Nuclear Information System (INIS)

    Fossell, E.T.; Hall, F.M.; McDonagh, J.

    1991-01-01

    The authors have previously described the application of water-suppressed proton nuclear magnetic resonance (H-1 NMR) spectroscopy of plasma for detection of malignancy. Subsequently, hypertriglyceridemia has been identified as a source of false positive results. Here is described a confirmatory, adjunctive technique -analysis of the carbon-13 (C-13) NMR spectrum of plasma- which also identifies the presence of malignancy but is not sensitive to the plasma triglyceride level. Blinded plasma samples from 480 normal donors and 208 patients scheduled for breast biopsy were analyzed by water-suppressed H-1 and C-13 NMR spectroscopy. Triglyceride levels were also measured. Among the normal donors, there were 38 individuals with hypertriglyceridemia of whom 18 had results consistent with malignancy by H-1 NMR spectroscopy. However, the C-13 technique reduced the apparent H-1 false positive rate from 7.0 to 0.6 percent. Similarly, in the breast biopsy cohort, C-13 reduced the false positive rate from 2.8 to 0.9 percent. Furthermore, the accuracy of the combined H-1/C-13 test in this blinded study was greater than 96 percent in 208 patients studied. (author). 27 refs.; 5 figs.; 4 tabs

  12. Modeling, fabrication and plasma actuator coupling of flexible pressure sensors for flow separation detection and control in aeronautical applications

    International Nuclear Information System (INIS)

    Francioso, L; De Pascali, C; Siciliano, P; Pescini, E; De Giorgi, M G

    2016-01-01

    Preventing the flow separation could enhance the performance of propulsion systems and future civil aircraft. To this end, a fast detection of boundary layer separation is mandatory for a sustainable and successful application of active flow control devices, such as plasma actuators. The present work reports on the design, fabrication and functional tests of low-cost capacitive pressure sensors coupled with dielectric barrier discharge (DBD) plasma actuators to detect and then control flow separation. Finite element method (FEM) simulations were used to obtain information on the deflection and the stress distribution in different-shaped floating membranes. The sensor sensitivity as a function of the pressure load was also calculated by experimental tests. The results of the calibration of different capacitive pressure sensors are reported in this work, together with functional tests in a wind tunnel equipped with a curved wall plate on which a DBD plasma actuator was mounted to control the flow separation. The flow behavior was experimentally investigated by particle image velocimetry (PIV) measurements. Statistical and spectral analysis, applied to the output signals of the pressure sensor placed downstream of the profile leading edge, demonstrated that the sensor is able to discriminate different ionic wind velocity and turbulence conditions. The sensor sensitivity in the 0–100 Pa range was experimentally measured and it ranged between 0.0030 and 0.0046 pF Pa −1 for the best devices. (paper)

  13. Modeling, fabrication and plasma actuator coupling of flexible pressure sensors for flow separation detection and control in aeronautical applications

    Science.gov (United States)

    Francioso, L.; De Pascali, C.; Pescini, E.; De Giorgi, M. G.; Siciliano, P.

    2016-06-01

    Preventing the flow separation could enhance the performance of propulsion systems and future civil aircraft. To this end, a fast detection of boundary layer separation is mandatory for a sustainable and successful application of active flow control devices, such as plasma actuators. The present work reports on the design, fabrication and functional tests of low-cost capacitive pressure sensors coupled with dielectric barrier discharge (DBD) plasma actuators to detect and then control flow separation. Finite element method (FEM) simulations were used to obtain information on the deflection and the stress distribution in different-shaped floating membranes. The sensor sensitivity as a function of the pressure load was also calculated by experimental tests. The results of the calibration of different capacitive pressure sensors are reported in this work, together with functional tests in a wind tunnel equipped with a curved wall plate on which a DBD plasma actuator was mounted to control the flow separation. The flow behavior was experimentally investigated by particle image velocimetry (PIV) measurements. Statistical and spectral analysis, applied to the output signals of the pressure sensor placed downstream of the profile leading edge, demonstrated that the sensor is able to discriminate different ionic wind velocity and turbulence conditions. The sensor sensitivity in the 0-100 Pa range was experimentally measured and it ranged between 0.0030 and 0.0046 pF Pa-1 for the best devices.

  14. The design and construction of a scintillation pair spectrometer for the detection of {gamma}-rays in the energy range 2-20 MeV; Realisation d'un spectrometre a scintillations et a paires pour la detection des rayonnements {gamma} d'energie comprise entre 2 et 20 MeV

    Energy Technology Data Exchange (ETDEWEB)

    Longequeue, J P [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1958-07-15

    The scintillation pair spectrometer is designed to allow the measurement of the energy of {gamma} rays in the range 2 to 20 MeV. Such an instrument is chosen because of its main features: high energy resolution and ease of working. Against this, however, the efficiency is low. It was possible to tolerate this low efficiency because of the facts that the {gamma}-rays studied emanated from (p, {gamma}) reactions and that the two electrostatic acceleration available could provide beams of 500 {mu}A having energy maxima at 300 and 600 keV. We used the {gamma} rays produced by the reactions {sup 23}Na (p, {gamma}) {sup 24}Mg, {sup 19}F (p, {alpha} {gamma}) {sup 16}O and {sup 7}Li (p, {gamma}) {sup 8}Be as well as the {gamma} rays emitted by sources of RTh and of {sup 24}Na. Under these conditions the spectrometer attained a resolving power of 6,5 {+-} 0,5 per cent at 6,1 MeV and it was able to separate the 14,8 and 17,6 MeV lines produced by the reaction {sup 7}Li (p, {gamma}) {sup 8}Be. As well as this, the efficiency which varied from 2.10{sup -4} to 1,7.10{sup -3} between 2 and 20 MeV was well above the efficiencies already obtained with this type of instrument. (author) [French] Le spectrometre a scintillations et a paires presente dans cette these a pour but de mesurer l'energie des rayonnements {gamma} dans la bande de 2 a 20 MeV. Le choix d'un tel appareil est du a ses caracteristiques essentielles: bonne resolution en energie et maniabilite. Par contre, son efficacite est faible. Nous avons pu tolerer cette faible efficacite car les rayonnements {gamma} que nous avons etudies provenaient de reactions (p, {gamma}) et les deux accelerateurs electrostatiques dont nous disposions pouvaient fournir des faisceaux de 500 {mu}A avec des energies maximum de 300 et 600 keV. Nous avons utilise les rayonnements {gamma} produits par les reactions {sup 23}Na (p, {gamma}) {sup 24}Mg, {sup 19}F (p, {alpha} {gamma}) {sup 16}O et {sup 7}Li (p, {gamma}) {sup 8}Be ainsi que les

  15. Experimental characterization of the Clear-PEM scanner spectrometric performance

    Energy Technology Data Exchange (ETDEWEB)

    Bugalho, R; Carrico, B; Ferreira, C S; Frade, M; Ferreira, M; Moura, R; Ortigao, C; Pinheiro, J F; Rodrigues, P; Rolo, I; Silva, J C; Trindade, A; Varela, J [Laboratorio de Instrumentacao e Fisica Experimental de Particulas (LIP), Av. Elias Garcia 14-1, 1000-149 Lisboa (Portugal)], E-mail: frade@lip.pt

    2009-10-15

    In the framework of the Clear-PEM project for the construction of a high-resolution and high-specificity scanner for breast cancer imaging, a Positron Emission Mammography tomograph has been developed and installed at the Instituto Portugues de Oncologia do Porto hospital. The Clear-PEM scanner is mainly composed by two planar detector heads attached to a robotic arm, trigger/data acquisition electronics system and computing servers. The detector heads hold crystal matrices built from 2 x 2 x 20 mm{sup 3} LYSO:Ce crystals readout by Hamamatsu S8550 APD arrays. The APDs are optically coupled to both ends of the 6144 crystals in order to extract the DOI information for each detected event. Each one of 12288 APD's pixels is read and controlled by Application Specific Integrated Circuits water-cooled by an external cooling unit. The Clear-PEM frontend boards innovative design results in a unprecedented integration of the crystal matrices, APDs and ASICs, making Clear-PEM the PET scanner with the highest number of APD pixels ever integrated so far. In this paper, the scanner's main technical characteristics, calibration strategies and the first spectrometric performance evaluation in a clinical environment are presented. The first commissioning results show 99.7% active channels, which, after calibration, have inter-pixel and absolute gain distributions with dispersions of, respectively, 12.2% and 15.3%, demonstrating that despite the large number of channels, the system is uniform. The mean energy resolution at 511 keV is of 15.9%, with a 8.8% dispersion, and the mean C{sub DOI}{sup -1} is 5.9%/mm, with a 7.8% dispersion. The coincidence time resolution, at 511 keV, for a energy window between 400 and 600 keV, is 5.2 ns FWHM.

  16. Multiplexed microRNA detection using lanthanide-labeled DNA probes and laser ablation inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    de Bang, Thomas Christian; Shah, Pratik; Cho, Seok Keun

    2014-01-01

    coupled plasma mass spectrometry (LA-ICPMS). Three miRNAs from Arabidopsis thaliana were analyzed simultaneously with high specificity, and the sensitivity of the method was comparable to radioactive detection (low femtomol range). The perspective of the developed method is highly multiplexed......In the past decade, microRNAs (miRNAs) have drawn increasing attention due to their role in regulation of gene expression. Especially, their potential as biomarkers in disease diagnostics has motivated miRNA research, including the development of simple, accurate, and sensitive detection methods....... The narrow size range of miRNAs (20-24 nucleotides) combined with the chemical properties of conventional reporter tags has hampered the development of multiplexed miRNA assays. In this study, we have used lanthanide-labeled DNA probes for the detection of miRNAs on membranes using laser ablation inductively...

  17. Impact of low-temperature plasmas on Deinococcus radiodurans and biomolecules

    Science.gov (United States)

    Mogul, Rakesh; Bol'shakov, Alexander A.; Chan, Suzanne L.; Stevens, Ramsey M.; Khare, Bishun N.; Meyyappan, M.; Trent, Jonathan D.

    2003-01-01

    The effects of cold plasma on Deinococcus radiodurans, plasmid DNA, and model proteins were assessed using microbiological, spectrometric, and biochemical techniques. In low power O(2) plasma (approximately 25 W, approximately 45 mTorr, 90 min), D. radiodurans, a radiation-resistant bacterium, showed a 99.999% reduction in bioburden. In higher power O(2) plasma (100 W and 500 mTorr), the reduction rate increased about 10-fold and observation by atomic force microscopy showed significant damage to the cell. Damage to cellular lipids, proteins, and chromosome was indicated by losses of infrared spectroscopic peaks at 2930, 1651, 1538, and 1245 cm(-1), respectively. In vitro experiments show that O(2) plasmas induce DNA strand scissions and cross-linking as well as reduction of enzyme activity. The observed degradation and removal of biomolecules was power-dependent. Exposures to 200 W at 500 mTorr removed biomolecules to below detection limits in 60 s. Emission spectroscopy indicated that D. radiodurans cells were volatilized into CO(2), CO, N(2), and H(2)O, confirming that these plasmas were removing complex biological matter from surfaces. A CO(2) plasma was not as effective as the O(2) plasma, indicating the importance of plasma composition and the dominant role of chemical degradation. Together, these findings have implications for NASA planetary protection schemes and for the contamination of Mars.

  18. Failure to detect variant (CRM+) plasma thromboplastin antecedent (factor XI) molecules in hereditary plasma thromboplastin antecedent deficiency: a study of 125 patients of several ethnic backgrounds.

    Science.gov (United States)

    Saito, H; Ratnoff, O D; Bouma, B N; Seligsohn, U

    1985-12-01

    Plasma samples of 125 patients from 80 kindreds with hereditary plasma thromboplastin antecedent (PTA, factor XI) deficiency were tested by factor XI radioimmunoassay (RIA) and electroimmunoassay (EIA) in an attempt to detect variant molecules. Ninety-six patients (70 kindreds) were Jewish, and 29 (10 kindreds) were of other ethnic backgrounds, namely, Japanese, black American, Korean, Arab, Indian, and English. Seventy-eight patients were homozygotes, and 47 were heterozygotes. Both non-Jewish homozygotes and heterozygotes had lower factor XI activity than respective Jewish subjects. Twenty-eight homozygotes whose factor XI clotting activities (XI:C) were 1.5% to 13% had factor XI-related antigen (XI:RAG) levels less than 10% by EIA. In 72 homozygotes, including 22 patients who were also tested with EIA, XI:C was 2.9% +/- 3.0% (mean +/- SD) and XI:RAG tested by RIA, 2.9% +/- 3.0%. In 47 heterozygotes, XI:C and XI:RAG tested by RIA were 51.9% +/- 16.6% and 51.0% +/- 16.2%, respectively. Similar results were obtained when only unrelated patients (62 homozygotes and 27 heterozygotes) were analyzed. There was a highly significant correlation between XI:C and XI:RAG (RIA) in 38 homozygotes and 47 heterozygotes (r = 0.94, n = 85, P less than 0.001). Thus, we failed to identify functionally abnormal factor XI molecules (CRM+ variant) in these patients with hereditary factor XI deficiency.

  19. Detection of cholesterol-rich microdomains in the inner leaflet of the plasma membrane

    International Nuclear Information System (INIS)

    Hayashi, Masami; Shimada, Yukiko; Inomata, Mitsushi; Ohno-Iwashita, Yoshiko

    2006-01-01

    The C-terminal domain (D4) of perfringolysin O binds selectively to cholesterol in cholesterol-rich microdomains. To address the issue of whether cholesterol-rich microdomains exist in the inner leaflet of the plasma membrane, we expressed D4 as a fusion protein with EGFP in MEF cells. More than half of the EGFP-D4 expressed in stable cell clones was bound to membranes in raft fractions. Depletion of membrane cholesterol with β-cyclodextrin reduced the amount of EGFP-D4 localized in raft fractions, confirming EGFP-D4 binding to cholesterol-rich microdomains. Subfractionation of the raft fractions showed most of the EGFP-D4 bound to the plasma membrane rather than to intracellular membranes. Taken together, these results strongly suggest the existence of cholesterol-rich microdomains in the inner leaflet of the plasma membrane

  20. Simultaneous Power Deposition Detection of Two EC Beams with the BIS Analysis in Moving TCV Plasmas

    Science.gov (United States)

    Curchod, L.; Pochelon, A.; Decker, J.; Felici, F.; Goodman, T. P.; Moret, J.-M.; Paley, J. I.

    2009-11-01

    Modulation of power amplitude is a widespread to determine the radial absorption profile of externally launched power in fusion plasmas. There are many techniques to analyze the plasma response to such a modulation. The break-in-slope (BIS) analysis can draw an estimated power deposition profile for each power step up. In this paper, the BIS analysis is used to monitor the power deposition location of one or two EC power beams simultaneously in a non-stationary plasma being displaced vertically in the TCV tokamak vessel. Except from radial discrepancies, the results have high time resolution and compare well with simulations from the R2D2-C3PO-LUKE ray-tracing and Fokker-Planck code suite.

  1. Detection of the position and cross-section of a tokamak plasma with magnetic probes

    International Nuclear Information System (INIS)

    Aikawa, Hiroshi; Ogata, Atsushi; Suzuki, Yasuo

    1977-02-01

    The position and cross-sectional shape of a Tokamak plasma are obtained analytically from magnetic probe signals, taking into consideration the toroidal effect. Multipole moment analysis of the plasma current density, introducing the vertical asymmetry, shows the horizontal and vertical displacements and the elliptical deviation. The error in the measurement is estimated by means of the least square method. The observed error is proportional to the error of setting the probes, and inversely proportional to the square root of the number of probes. (auth.)

  2. Li-BES detection system for plasma turbulence measurements on the COMPASS tokamak

    Czech Academy of Sciences Publication Activity Database

    Berta, Miklós; Anda, G.; Bencze, A.; Dunai, D.; Háček, Pavel; Hron, Martin; Kovácsik, A.; Krbec, Jaroslav; Pánek, Radomír; Réfy, D.; Véres, G.; Weinzettl, Vladimír; Zoletnik, S.

    96-97, October (2015), s. 795-798 ISSN 0920-3796. [Symposium on Fusion Technology 2014(SOFT-28)/28./. San Sebastián, 29.09.2014-03.10.2014] R&D Projects: GA MŠk(CZ) LM2011021 Institutional support: RVO:61389021 Keywords : BES * plasma diagnostics * COMPASS tokamak * density fluctuations * plasma density profile Subject RIV: JF - Nuclear Energetics OBOR OECD: Nuclear related engineering Impact factor: 1.301, year: 2015 http://www.sciencedirect.com/science/article/pii/S0920379615300442

  3. Detection of light charged particles from plasma focus by CR-39

    Energy Technology Data Exchange (ETDEWEB)

    Antanasijevic, R.; Vukovic, J.; Popovic, S.; Popovic, M. (Belgrade Univ. (Yugoslavia). Inst. za Fiziku); Puric, J.; Cuk, M. (Faculty of Physical Science, Belgrade (Yugoslavia))

    1991-01-01

    An analysis of a deuteron (D{sup +}) beam, emitted from a plasma focus has been carried out, using a CR-39 plastic nuclear track detector. The CR-39 was pretreated using different processes to destroy the existing background before exposing it to the particles produced in the plasma focus. From measurements of the diameters of the tracks, the estimated energy of the D{sup +} ions is about 0.5 MeV. The total number of emitted D{sup +} ions was 10 particles/pulse. Some preliminary results on imaging etched CR-39 with an Atomic Force Microscope (NanoScope AFM) are also presented. (author).

  4. Detection of light charged particles from plasma focus by CR-39

    International Nuclear Information System (INIS)

    Antanasijevic, R.; Vukovic, J.; Popovic, S.; Popovic, M.

    1991-01-01

    An analysis of a deuteron (D + ) beam, emitted from a plasma focus has been carried out, using a CR-39 plastic nuclear track detector. The CR-39 was pretreated using different processes to destroy the existing background before exposing it to the particles produced in the plasma focus. From measurements of the diameters of the tracks, the estimated energy of the D + ions is about 0.5 MeV. The total number of emitted D + ions was 10 particles/pulse. Some preliminary results on imaging etched CR-39 with an Atomic Force Microscope (NanoScope AFM) are also presented. (author)

  5. Optimisation of the muon spectrometer from the detector ALICE used for the study of the quark and gluon plasma at LHC; Optimisation du spectrometre a muons du detecteur ALICE pour l'etude du plasma de quarks et de gluons au LHC

    Energy Technology Data Exchange (ETDEWEB)

    Guernane, R

    2001-01-01

    The ALICE experiment performed at the LHC will establish and study the phase transition from hadronic matter to a matter to a state of deconfined partons called Quark Gluon Plasma (QGP). The suppression of heavy flavour resonances (J{phi},{gamma}) is the most promising probe for diagnosing the formation and early stages of the QGP in ultrarelativistic heavy ion collisions. The complete spectrum of heavy quarkonia resonances, i.e. J/{phi}, {phi}', {gamma}, {gamma}' and {phi}' will be measured via their muonic decay in a forward spectrometer with a mass resolution sufficient to separate all states. It is composed of five tracking stations, each consisting of two Cathode Pad Chambers (CPC). In this work, we developed a prototype of CPC having the original feature of parallel charge read out from one segmented cathode. The geometry and operating parameters have been optimized for station 3. The expected multi-hit rate and multi-hit deconvolution have been evaluated with a complete detailed simulation and an efficient method to disentangle close hits has been proposed. The magnetic field effect on the intrinsic spatial resolution of the chambers has also been estimated. The simulated performance of the CPC's is confirmed by beam-test results obtained at CERN with prototypes. The measurement of dimuons is expected to be contaminated by beam-related background. The rate of beam-gas interactions is several orders of magnitude larger than the signal rate for p-p collisions which is the reference for further studies of p-A and A-A collisions. The ALICE Collaboration decided to equip the muon spectrometer with a level 0 trigger counter (V0) in order to validate the dimuon trigger signal in p-p mode. The various steps involved in designing the V0 scintillator hodoscope are presented in this thesis. (author)

  6. Gamma Spectrometric Determination of U, Th, K and Some Geochemical Applications

    International Nuclear Information System (INIS)

    Dodona, A.; Tashko, A.

    2001-01-01

    The application of 'in situ' gamma-spectrometric method (''infinite'' environment), made possible the simultanious determination of U, Th and K. 4 channel gamma-spectrometric analyser with NaI(TI) scintilation counter crystal detector (103 cm 3 φ=50x50mm) was used to determin U, Th(more than 1-2 ppm) and K (more than 1%) in laboratory conditions. The detector was inserted into a lead camera and calibrated for measurement geometry with vessel of ''Marineli'' type of a 17o cm 3 volume. The study of main factors, which influence in the gamma spectrometric measurements, (the technical, physical, geometrical and time parameters) has been carried out. International standards of U, Th, K and internal monitoring standard samples are used for the calibration. External analytical control has been realized by other radiometric and chemical methods. The detection limits ( 1 ppm Th, 2ppm U and 1% K) and the relative errors (17-20% for 1-10 ppm U, Th and 10-15% for more than 10 ppm U, Th and more than 1% K) guarantee a quantitative analysis that may be used successfully in the geochemical studies. Some geochemical applications, based on the content of Th, U and Th/U ratio in rocks samples that we have we have analyzed with this method, are shown in this paper. U, Th and their ratio are used as trace elements to indicate the differences between the acidic magmatic rocks of Albania (Th/U ratio=2-6 and>10). The bimodal character of Th/U scattering in ignimbrides and monzonites (Korabi zone) shows that in addition to the ''normal'' rocks, there are also some ones enriched with Th, So, the differential analysis of Th, U, and K may be used as geochemical exploration criteria for the radioactive and non-radioactive mineralization, such as REE (Rare Earth Elements), phospghorites, bauxites, placers etc. (authors)

  7. Detection of antibodies in blood plasma using bioluminescent sensor proteins and a smartphone

    NARCIS (Netherlands)

    Arts, R.; den Hartog, I.; Zijlema, S.E.; Thijssen, V.; van der Beelen, S.H.E.; Merkx, M.

    2016-01-01

    Antibody detection is of fundamental importance in many diagnostic and bioanalytical assays, yet current detection techniques tend to be laborious and/or expensive. We present a new sensor platform (LUMABS) based on bioluminescence resonance energy transfer (BRET) that allows detection of antibodies

  8. Mass spectrometric methods for studying nutrient mineral and trace element absorption and metabolism in humans using stable isotopes: a review

    International Nuclear Information System (INIS)

    Crews, H.M.; Eagles, J.; Mellon, F.A.; Luten, J.B.; McGaw, B.A.

    1994-01-01

    Mass spectrometric methods for determining stable isotopes of nutrient minerals and trace elements in human metabolic studies are described and discussed. The advantages and disadvantages of the techniques of electron ionization, fast atom bombardment, thermal ionization, and inductively coupled plasma and gas chromatography mass spectrometry are evaluated with reference to their accuracy, precision, sensitivity, and convenience, and the demands of human nutrition research. Examples of specific applications are described and the significance of current developments in mass spectrometry are discussed with reference to present and probable future research needs. (Author)

  9. [Determination of atracurium and laudanosine in dog plasma during cardiopulmonary bypass by high performance liquid chromatography with fluorometric detection].

    Science.gov (United States)

    Yang, Yingying; Chen, Mei; Kuang, Yushan; Ye, Liming; Zhang, Wensheng

    2013-06-01

    A high performance liquid chromatographic method coupled with fluorometric detection has been developed for the determination of atracurium and its major metabolite laudanosine in dog plasma. The separation of atracurium and laudanosine was performed on an Agilent Eclipse Plus C18 column, and the mobile phase consisted of 0.03 mol/L dipotassium hydrogen phosphate and acetonitrile (72: 28, v/v) at a flow rate of 1.0 mL/min. Verapamil was used as the internal standard. The sample was extracted by dichloromethane, concentrated and dissolved in the mobile phase. The detection is performed at 240 nm for excitation and 320 nm for emission. The results showed that the linear concentration ranges of the calibration curve were 25 - 5 000 microg/L for atracurium (r = 0.999 0), and 25 - 6 000 microg/L for laudanosine (r = 0.9984). The recoveries were 92.1% - 109.5%. The limits of detection were 3 microg/L for atracurium and 1 microg/L for laudanosine. The RSDs of intra-day and inter-day were less than 10%. The stability tests under various conditions have been performed. The method is specific, sensitive and accurate in the determination of atracurium and laudanosine, and also can be used for the pharmacokinetic investigations of atracurium and laudanosine in plasma.

  10. Compact quasi-monoenergetic photon sources from laser-plasma accelerators for nuclear detection and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Geddes, Cameron G.R., E-mail: cgrgeddes@lbl.gov; Rykovanov, Sergey; Matlis, Nicholas H.; Steinke, Sven; Vay, Jean-Luc; Esarey, Eric H.; Ludewigt, Bernhard; Nakamura, Kei; Quiter, Brian J.; Schroeder, Carl B.; Toth, Csaba; Leemans, Wim P.

    2015-05-01

    Near-monoenergetic photon sources at MeV energies offer improved sensitivity at greatly reduced dose for active interrogation, and new capabilities in treaty verification, nondestructive assay of spent nuclear fuel and emergency response. Thomson (also referred to as Compton) scattering sources are an established method to produce appropriate photon beams. Applications are however restricted by the size of the required high-energy electron linac, scattering (photon production) system, and shielding for disposal of the high energy electron beam. Laser-plasma accelerators (LPAs) produce GeV electron beams in centimeters, using the plasma wave driven by the radiation pressure of an intense laser. Recent LPA experiments are presented which have greatly improved beam quality and efficiency, rendering them appropriate for compact high-quality photon sources based on Thomson scattering. Designs for MeV photon sources utilizing the unique properties of LPAs are presented. It is shown that control of the scattering laser, including plasma guiding, can increase photon production efficiency. This reduces scattering laser size and/or electron beam current requirements to scale compatible with the LPA. Lastly, the plasma structure can decelerate the electron beam after photon production, reducing the size of shielding required for beam disposal. Together, these techniques provide a path to a compact photon source system.

  11. New enhanced sensitivity infrared laser spectroscopy techniques applied to reactive plasmas and trace gas detection

    NARCIS (Netherlands)

    Welzel, S.

    2009-01-01

    Infrared laser absorption spectroscopy (IRLAS) employing both tuneable diode and quantum cascade lasers (TDLs, QCLs) has been applied with both high sensitivity and high time resolution to plasma diagnostics and trace gas measurements. TDLAS combined with a conventional White type multiple pass cell

  12. No neuronal autoantibodies detected in plasma of patients with a bipolar I disorder

    NARCIS (Netherlands)

    Snijders, Gijsje; Titulaer, Maarten J.; Bergink, Veerle; Bastiaansen, Anna E.; Schreurs, Marco W.J.; Ophoff, Roel A.; Boks, Marco P.; Kahn, René S.; de Witte, Lot D.

    2018-01-01

    A subpopulation of patients with bipolar disorder type I (BD-I) might suffer from undiagnosed autoimmune encephalitis. We tested plasma of 104 BD-I patients with a current or recent manic episode in the past 2 years for the presence of neuronal autoantibodies using immunohistochemistry,

  13. A Comparative Study for Detection of EGFR Mutations in Plasma Cell-Free DNA in Korean Clinical Diagnostic Laboratories

    Directory of Open Access Journals (Sweden)

    Yoonjung Kim

    2018-01-01

    Full Text Available Liquid biopsies to genotype the epidermal growth factor receptor (EGFR for targeted therapy have been implemented in clinical decision-making in the field of lung cancer, but harmonization of detection methods is still scarce among clinical laboratories. We performed a pilot external quality assurance (EQA scheme to harmonize circulating tumor DNA testing among laboratories. For EQA, we created materials containing different levels of spiked cell-free DNA (cfDNA in normal plasma. The limit of detection (LOD of the cobas® EGFR Mutation Test v2 (Roche Molecular Systems was also evaluated. From November 2016 to June 2017, seven clinical diagnostic laboratories participated in the EQA program. The majority (98.94% of results obtained using the cobas assay and next-generation sequencing (NGS were acceptable. Quantitative results from the cobas assay were positively correlated with allele frequencies derived from digital droplet PCR measurements and showed good reproducibility among laboratories. The LOD of the cobas assay was 5~27 copies/mL for p.E746_A750del (exon 19 deletion, 35~70 copies/mL for p.L858R, 18~36 copies/mL for p.T790M, and 15~31 copies/mL for p.A767_V769dup (exon 20 insertion. Deep sequencing of materials (>100,000X depth of coverage resulted in detection of low-level targets present at frequencies of 0.06~0.13%. Our results indicate that the cobas assay is a reliable and rapid method for detecting EGFR mutations in plasma cfDNA. Careful interpretation is particularly important for p.T790M detection in the setting of relapse. Individual laboratories should optimize NGS performance to maximize clinical utility.

  14. Mass spectrometric investigation of vinyl-substituted organic boron compounds

    International Nuclear Information System (INIS)

    Tarielashvili, V.O.; Ordzhonikidze, K.G.; Parulava, L.P.; Vakhaniya, G.V.

    1992-01-01

    Mass spectrometric investigation of vinyl-substituted organic compounds was conducted. Ionization was performed by electron shock. Possibility of determining boron isotope content is all analyzed organic boron vinyl-substituted compounds by direct method is shown. This simplifies sufficiently and lowers the price of analysis, improves its accuracy and rapidity

  15. Spectrometric determination of ammonium-nitrogen with quinol in ...

    African Journals Online (AJOL)

    Quinol is proposed as a reagent for the spectrometric determination of ammonium-nitrogen (NH4+-N) in aqueous medium. Quinol forms a pink complex with ammonium salt in aqueous medium. Hydrogen peroxide is needed for colour accentuation. The quinol/ammonium charge transfer complex has absorption maximum ...

  16. Preparation and spectrometric identification of amide derivatives with antimalaric

    International Nuclear Information System (INIS)

    Ferreira, E.J.

    1987-01-01

    The structures of polymeric compounds using spectrometric analysis of infrared, ultraviolet and protonic magnetic resonance and 13 C nuclear magnetic resonance are studied. Some structural models are used such as antimalaric-sulfones and pyrimidinic derivatives, and non-polymeric derivatives of active compounds. A comparative analysis on structures less complexes is shown. (M.J.C.). Spectrums 186 p [pt

  17. Development of a PCR/LDR/capillary electrophoresis assay with potential for the detection of a beta-thalassemia fetal mutation in maternal plasma.

    Science.gov (United States)

    Yi, Ping; Chen, Zhuqin; Yu, Lili; Zheng, Yingru; Liu, Guodong; Xie, Haichang; Zhou, Yuanguo; Zheng, Xiuhui; Han, Jian; Li, Li

    2010-08-01

    Analysis of fetal DNA in maternal plasma has recently been introduced for non-invasive prenatal diagnosis. We have now investigated the feasibility of polymerase chain reaction (PCR)/ligase detection reaction (LDR)/capillary electrophoresis for the detection of fetal point mutations, such as the beta-thalassemia mutation, IVS2 654(C --> T), in maternal plasma DNA. The sensitivity of LDR/capillary electrophoresis was examined by quantifying the mutant PCR products in the presence of a vast excess of non-mutant competitor template, a situation that mimics the detection of rare fetal mutations in the presence of excess maternal DNA. PCR/LDR/capillary electrophoresis was applied to detect the mutation, IVS2 654(C --> T), in an experimental model at different sensitivity levels and from 10 maternal plasma samples. Our results demonstrated that this approach to detect a low abundance IVS2 654(C --> T) mutation achieved a sensitivity of approximately 1:10,000. The approach was applied to maternal plasma DNA to detect the paternally inherited fetal IVS2 654(C --> T) mutation, and the results were equivalent to those obtained by PCR/reverse dot blot of amniotic fluid cell DNA. PCR/LDR/capillary electrophoresis has a very high sensitivity that can distinguish low abundance single nucleotide differences and can detect paternally inherited fetal point mutations in maternal plasma.

  18. Bead Injection Extraction Chromatography using High-capacity Lab-on-Valve as a Front End to Inductively Coupled Plasma Mass Spectrometry for Rapid Urine Radiobioassay

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2013-01-01

    A novel bead injection (BI) extraction chromatographic microflow system exploiting high-capacity lab-on-valve (LOV) platform coupled with inductively coupled plasma mass spectrometric detection is developed for rapid and automated determination of plutonium in human urine. A microconduit (1 m......L) incorporated within the LOV processing unit is loaded on-line with a metered amount of disposable extraction chromatographic resin (up to 330 mg of TEVA) through programmable beads transport. Selective capture and purification of plutonium onto the resin beads is then performed by pressure driven flow after...

  19. Determination of actinides by alpha spectrometric methods

    International Nuclear Information System (INIS)

    Galanda, D.

    2011-01-01

    defined attributes of mass activities of radionuclides in oyster mushroom's sporocarps compared to their sub-base. We used two methods to separate the monitored radionuclides in a radiochemical analyse. The first of them was an extraction fluid - fluid with Aliquat-336 to separate Pu and TOPO to separate Am. The second method was a proceeding modified by us and utilizing principles of an extraction chromatography with TRU Resin and DGA Resin sorbents made by Eichrom Company. An effectivity and a suitability of both applied methods were monitored following the attributes of radiochemical extractions used in tracer's radionuclides 242 Pu a 243 Am in this particular type of environmental samples. The reliability of the modified methodology, in accordance to selected criteria for validation of analytical method, was proved by comparison of both above mentioned methods. material delivered from IAEA, which presented a soil sample with code identification Soil IAEA-375. The obtained values of mass activities of 239 + 240 Pu, 239 Pu and 241 Am used in reference material, demonstrated a conformity with IAEA values, whereby we fulfilled one of the significant conditions of validate process. At the end of this thesis we applied the modified method of extraction chromatography with UTEVA Resin sorbent to define mass activities of uranium on soil and water samples where we monitored attributes of radiochemical extractions of 232 U tracer's radionuclide as the criteria of utilizability. The reliability of our modified method was verified by participation in international interlaboratory comparative proficiency tests and our results were in accordance with results of the reference laboratory. It means also a fulfilment of notable standard of the validate process. The results of all realized experimentations of radionuclides separation whether by extraction fluid - fluid or by extraction chromatography were determined by alpha-spectrometric measurements. (author)

  20. Quantitation of Pyrrole-Imidazole Polyamide in Rat Plasma by High-Performance Liquid Chromatography Coupled with UV Detection

    Directory of Open Access Journals (Sweden)

    Tomonori Kamei

    2012-01-01

    Full Text Available A simple and robust method using high-performance liquid chromatography with UV detection was developed and validated for the determination of six pyrrole-imidazole (PI polyamides (HN.49, TGF-β1f, TGF-β1t, HN.50f, HN.50t, and LOX-1 in rat plasma. After the plasma proteins were precipitated with methanol containing phenacetin as an internal standard, the analytes were separated on a Luna C18 (2 (5 μm, 4.6×150 mm. Calibration curves were linear over the range of 0.5 to 200 μg/mL for HN.49, 0.25 to 200 μg/mL for TGF-β1f, TGF-β1t, HN.50t, and LOX-1, 1 to 200 μg/mL for HN.50f in rat plasma. The inter- and intraday precision were below 15%, and the accuracy was within 15% at the quality controls. The validated method was successfully applied to sample analysis for the pharmacokinetic study.

  1. 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.

  2. The Plasma Focus Technology Applied to the Detection of Hydrogenated Substances

    International Nuclear Information System (INIS)

    Ramos, R.; Moreno, C.; Gonzalez, J.; Clausse, A

    2003-01-01

    The feasibility study of an industrial application of thermonuclear pulsors is presented.An experiment was conducted to detect hydrogenated substances using PF technology.The detection system is composed by two neutron detectors operated simultaneously on every shot.The first detector is used to register the PF neutron yield in each shot; whereas the other one was designed to detect neutrons scattered by the blanket.We obtained the detector sensitivity charts as a function of the position in space and frontal area of the substance to be detected

  3. Abrupt changes in neon discharge plasma detected via the optogalvanic effect

    Energy Technology Data Exchange (ETDEWEB)

    Han, Xianming L., E-mail: xhan@butler.edu [Dept. of Physics and Astronomy, Butler University, Indianapolis, IN 46208 (United States); Blosser, Michael C. [Dept. of Physics and Astronomy, Butler University, Indianapolis, IN 46208 (United States); Misra, Prabhakar [Dept. of Physics and Astronomy, Howard University, Washington DC 20059 (United States); Chandran, Haridass [Dept. of Physical Science, Belfry School, Belfry, KY 41514 (United States)

    2012-10-30

    When a laser is tuned between two excited energy levels of a gas in a Direct Current discharge lamp, the discharge current will experience a temporary disturbance lasting tens or hundreds of microseconds known as the optogalvanic effect. We have carried out extensive studies of optogalvanic effects in neon discharge plasmas for transitions at 621.7 nm, 630.5 nm, 638.3 nm, 650.7 nm and 659.9 nm. A nonlinear least-squares Monte Carlo technique has been used to determine the relevant amplitude coefficients, decay rates and the instrumental time constant. We discovered an abrupt change in the neon discharge plasma at a discharge current of about 6 mA.

  4. Detection of hemophilia A carriers by use of frozen plasma samples

    International Nuclear Information System (INIS)

    Yang, H.C.; Hardin, J.; Vaudreuil, C.

    1978-01-01

    The efficacy of using promptly frozen plasma samples in the diagnosis of the carrier state for hemophilia A was evaluated by simultaneous measurement of factor VIII activity and antigen in 20 normal women and 20 obligate carriers. Factor VIII antigen was measured by two methods, electroimmunoassay and immunoradiometric assay. When the factor VIII activity and antigen data were evaluated by regression analysis, 94% of the carriers were correctly identified at the 95% confidence level

  5. Towards real-time detection and tracking of spatio-temporal features: Blob-filaments in fusion plasma

    International Nuclear Information System (INIS)

    Wu, Lingfei; Wu, Kesheng; Sim, Alex; Churchill, Michael; Choi, Jong Youl

    2016-01-01

    A novel algorithm and implementation of real-time identification and tracking of blob-filaments in fusion reactor data is presented. Similar spatio-temporal features are important in many other applications, for example, ignition kernels in combustion and tumor cells in a medical image. This work presents an approach for extracting these features by dividing the overall task into three steps: local identification of feature cells, grouping feature cells into extended feature, and tracking movement of feature through overlapping in space. Through our extensive work in parallelization, we demonstrate that this approach can effectively make use of a large number of compute nodes to detect and track blob-filaments in real time in fusion plasma. Here, on a set of 30GB fusion simulation data, we observed linear speedup on 1024 processes and completed blob detection in less than three milliseconds using Edison, a Cray XC30 system at NERSC.

  6. Conformational changes of plasma fibronectin detected upon adsorption to solid substrates: A spin-label study

    International Nuclear Information System (INIS)

    Narasimhan, C.; Lai, Chingsan

    1989-01-01

    Changes in local environment of the free sulfhydryl groups in plasma fibronectin upon adsorption of the protein to polystyrene beads have been examined by electron spin resonance (ESR) spin-label spectroscopy. The two free sulfhydryl groups per subunit of plasma fibronectin were modified chemically with an [ 15 N, 2 H]maleimide spin-label. For soluble fibronectin, both free sulfhydryl groups shown to be in confined environments as evidenced from the labeled protein exhibiting a strongly immobilized ESR spectrum as described previously using [ 14 N, 1 H]maleimide spin-labels. When the labeled protein was adsorbed to the beads, half of the strongly immobilized component was found to convert into a weakly immobilized component, a result indicating that one of the two labeled sites becomes exposed and exhibits a fast tumbling motion. Experiments conducted using various spin-labeled fibronectin fragments suggest that the newly exposed labeled site is located between the DNA-binding and the cell-binding regions of the molecule. The data obtained indicate that, upon adsorption to polystyrene beads, plasma fibronectin undergoes a conformational change through which the buried free sulfhydryl group near the cell-binding region of the molecule is exposed. This observation may have important implications regarding the expression of cell adhesive properties of the fibronectin molecule

  7. How mass spectrometric approaches applied to bacterial identification have revolutionized the study of human gut microbiota.

    Science.gov (United States)

    Grégory, Dubourg; Chaudet, Hervé; Lagier, Jean-Christophe; Raoult, Didier

    2018-03-01

    Describing the human hut gut microbiota is one the most exciting challenges of the 21 st century. Currently, high-throughput sequencing methods are considered as the gold standard for this purpose, however, they suffer from several drawbacks, including their inability to detect minority populations. The advent of mass-spectrometric (MS) approaches to identify cultured bacteria in clinical microbiology enabled the creation of the culturomics approach, which aims to establish a comprehensive repertoire of cultured prokaryotes from human specimens using extensive culture conditions. Areas covered: This review first underlines how mass spectrometric approaches have revolutionized clinical microbiology. It then highlights the contribution of MS-based methods to culturomics studies, paying particular attention to the extension of the human gut microbiota repertoire through the discovery of new bacterial species. Expert commentary: MS-based approaches have enabled cultivation methods to be resuscitated to study the human gut microbiota and thus to fill in the blanks left by high-throughput sequencing methods in terms of culturing minority populations. Continued efforts to recover new taxa using culture methods, combined with their rapid implementation in genomic databases, would allow for an exhaustive analysis of the gut microbiota through the use of a comprehensive approach.

  8. Assessment of current mass spectrometric workflows for the quantification of low abundant proteins and phosphorylation sites

    Directory of Open Access Journals (Sweden)

    Manuel Bauer

    2015-12-01

    Full Text Available The data described here provide a systematic performance evaluation of popular data-dependent (DDA and independent (DIA mass spectrometric (MS workflows currently used in quantitative proteomics. We assessed the limits of identification, quantification and detection for each method by analyzing a dilution series of 20 unmodified and 10 phosphorylated synthetic heavy labeled reference peptides, respectively, covering six orders of magnitude in peptide concentration with and without a complex human cell digest background. We found that all methods performed very similarly in the absence of background proteins, however, when analyzing whole cell lysates, targeted methods were at least 5–10 times more sensitive than directed or DDA methods. In particular, higher stage fragmentation (MS3 of the neutral loss peak using a linear ion trap increased dynamic quantification range of some phosphopeptides up to 100-fold. We illustrate the power of this targeted MS3 approach for phosphopeptide monitoring by successfully quantifying 9 phosphorylation sites of the kinetochore and spindle assembly checkpoint component Mad1 over different cell cycle states from non-enriched pull-down samples. The data are associated to the research article ‘Evaluation of data-dependent and data-independent mass spectrometric workflows for sensitive quantification of proteins and phosphorylation sites׳ (Bauer et al., 2014 [1]. The mass spectrometry and the analysis dataset have been deposited to the ProteomeXchange Consortium (http://proteomecentral.proteomexchange.org via the PRIDE partner repository with the dataset identifier PXD000964.

  9. Determination of total and unbound warfarin and warfarin alcohols in human plasma by high performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Lomonaco, Tommaso; Ghimenti, Silvia; Piga, Isabella; Onor, Massimo; Melai, Bernardo; Fuoco, Roger; Di Francesco, Fabio

    2013-11-01

    Two analytical procedures are presented for the determination of the total content and unbound fraction of both warfarin and warfarin alcohols in human plasma. Chromatographic separation was carried out in isocratic conditions at 25°C on a C-18 reversed-phase column with a mobile phase consisting of a 70% buffer phosphate 25mM at pH=7, 25% methanol and 5% acetonitrile at a flow rate of 1.2mL/min. Fluorescence detection was performed at 390nm (excitation wavelength 310nm). Neither method showed any detectable interference or matrix effect. Inter-day recovery of the total warfarin and warfarin alcohols at a concentration level of 1000ng/mL was 89±3% and 73±3%, respectively, whereas for their unbound fraction (at a concentration level of 10ng/mL) was 66±8% and 90±7%, respectively. The intra- and inter-day precision (assessed as relative standard deviation) was alcohols, respectively. The methods were successfully applied to a pooled plasma sample obtained from 69 patients undergoing warfarin therapy. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. Plasma Free Amino Acid Profiling of Five Types of Cancer Patients and Its Application for Early Detection

    Science.gov (United States)

    Miyagi, Yohei; Higashiyama, Masahiko; Gochi, Akira; Akaike, Makoto; Ishikawa, Takashi; Miura, Takeshi; Saruki, Nobuhiro; Bando, Etsuro; Kimura, Hideki; Imamura, Fumio; Moriyama, Masatoshi; Ikeda, Ichiro; Chiba, Akihiko; Oshita, Fumihiro; Imaizumi, Akira; Yamamoto, Hiroshi; Miyano, Hiroshi; Horimoto, Katsuhisa; Tochikubo, Osamu; Mitsushima, Toru; Yamakado, Minoru; Okamoto, Naoyuki

    2011-01-01

    Background Recently, rapid advances have been made in metabolomics-based, easy-to-use early cancer detection methods using blood samples. Among metabolites, profiling of plasma free amino acids (PFAAs) is a promising approach because PFAAs link all organ systems and have important roles in metabolism. Furthermore, PFAA profiles are known to be influenced by specific diseases, including cancers. Therefore, the purpose of the present study was to determine the characteristics of the PFAA profiles in cancer patients and the possibility of using this information for early detection. Methods and Findings Plasma samples were collected from approximately 200 patients from multiple institutes, each diagnosed with one of the following five types of cancer: lung, gastric, colorectal, breast, or prostate cancer. Patients were compared to gender- and age- matched controls also used in this study. The PFAA levels were measured using high-performance liquid chromatography (HPLC)–electrospray ionization (ESI)–mass spectrometry (MS). Univariate analysis revealed significant differences in the PFAA profiles between the controls and the patients with any of the five types of cancer listed above, even those with asymptomatic early-stage disease. Furthermore, multivariate analysis clearly discriminated the cancer patients from the controls in terms of the area under the receiver-operator characteristics curve (AUC of ROC >0.75 for each cancer), regardless of cancer stage. Because this study was designed as case-control study, further investigations, including model construction and validation using cohorts with larger sample sizes, are necessary to determine the usefulness of PFAA profiling. Conclusions These findings suggest that PFAA profiling has great potential for improving cancer screening and diagnosis and understanding disease pathogenesis. PFAA profiles can also be used to determine various disease diagnoses from a single blood sample, which involves a relatively simple

  11. Plasma free amino acid profiling of five types of cancer patients and its application for early detection.

    Directory of Open Access Journals (Sweden)

    Yohei Miyagi

    Full Text Available BACKGROUND: Recently, rapid advances have been made in metabolomics-based, easy-to-use early cancer detection methods using blood samples. Among metabolites, profiling of plasma free amino acids (PFAAs is a promising approach because PFAAs link all organ systems and have important roles in metabolism. Furthermore, PFAA profiles are known to be influenced by specific diseases, including cancers. Therefore, the purpose of the present study was to determine the characteristics of the PFAA profiles in cancer patients and the possibility of using this information for early detection. METHODS AND FINDINGS: Plasma samples were collected from approximately 200 patients from multiple institutes, each diagnosed with one of the following five types of cancer: lung, gastric, colorectal, breast, or prostate cancer. Patients were compared to gender- and age- matched controls also used in this study. The PFAA levels were measured using high-performance liquid chromatography (HPLC-electrospray ionization (ESI-mass spectrometry (MS. Univariate analysis revealed significant differences in the PFAA profiles between the controls and the patients with any of the five types of cancer listed above, even those with asymptomatic early-stage disease. Furthermore, multivariate analysis clearly discriminated the cancer patients from the controls in terms of the area under the receiver-operator characteristics curve (AUC of ROC >0.75 for each cancer, regardless of cancer stage. Because this study was designed as case-control study, further investigations, including model construction and validation using cohorts with larger sample sizes, are necessary to determine the usefulness of PFAA profiling. CONCLUSIONS: These findings suggest that PFAA profiling has great potential for improving cancer screening and diagnosis and understanding disease pathogenesis. PFAA profiles can also be used to determine various disease diagnoses from a single blood sample, which involves a

  12. Simultaneous determination of sulpiride and mebeverine by HPLC method using fluorescence detection: application to real human plasma

    Directory of Open Access Journals (Sweden)

    Walash Mohamed I

    2012-02-01

    Full Text Available Abstract A new simple, rapid and sensitive reversed-phase liquid chromatographic method was developed and validated for the simultaneous determination of sulpiride (SUL and mebeverine Hydrochloride (MEB in the presence of their impurities and degradation products. The separation of these compounds was achieved within 6 min on a 250 mm, 4.6 mm i.d., 5 m particle size Waters®-C18 column using isocractic mobile phase containing a mixture of acetonitrile and 0.01 M dihydrogenphosphate buffer (45:55 at pH = 4.0. The analysis was performed at a flow rate of 1.0 mL/min with fluorescence-detection at excitation 300 nm and emission at 365 nm. The concentration-response relationship was linear over a concentration range of 10- 100 ng/mL for both MEB and SUL with a limit of detection 0.73 ng/mL and 0.85 ng/mL for MEB and SUL respectively. The proposed method was successfully applied for the analysis of both MEB and SUL in bulk with average recoveries of 100.22 ± 0.757% and 99.96 ± 0.625% respectively, and in commercial tablets with average recoveries of 100.04 ± 0.93% and 100.03 ± 0.376% for MEB and SUL respectively. The proposed method was successfully applied to the determination of MEB metabolite (veratic acid in real plasma simultaneously with SUL. The mean% recoveries (n = 3 for both MEB metabolite (veratic acid and SUL were 100.36 ± 2.92 and 99.06 ± 2.11 for spiked human plasma respectively. For real human plasma, the mean% recoveries (n = 3 were and respectively.

  13. Evaluation of silicon-chemiluminescence monitoring as a novel method for atomic fluorine determination and end point detection in plasma etch systems

    NARCIS (Netherlands)

    Zijlstra, P.A.; Beenakker, C.I.M.

    1981-01-01

    Optical methods for the detection of atomic fluorine in plasma etch systems are discussed and an experimental comparison is made between detection by optical emission and by a novel method based on the chemiluminescence from solid silicon in the presence of atomic fluorine. Although both methods

  14. Mass spectrometric analysis of EPO IEF-PAGE interfering substances in nitrile examination gloves.

    Science.gov (United States)

    Reichel, Christian

    2012-10-01

    Direct detection of doping with recombinant erythropoietins (rhEPO) is accomplished by isoelectric focusing (IEF) or sodium dodecylsulfate (SDS) polyacrylamide gel electrophoresis (PAGE). In a recent publication, Lasne et al. (Electrophoresis 2011, 32, 1444) showed that improper use of nitrile examination gloves during sample collection, sample preparation, and IEF-PAGE may lead to distorted or absent EPO IEF-profiles. In order to clarify which substances are responsible for this observation, a mass spectrometric study on water extractable compounds found in nitrile gloves was performed. Several substance classes were shown to be present, among them polyethylene glycols (PEG), anionic and nonionic surfactants, as well as alcohol ethoxylates and plasticizers. It could be demonstrated that alkylbenzenesulfonates, the main category of detectable anionic detergents, and among them sodium dodecylbenzenesulfonate (SDBS) and its homologs, are the prime reason for the interference of nitrile gloves with EPO IEF-PAGE. Copyright © 2012 John Wiley & Sons, Ltd.

  15. Levelling Airborne and Ground Gamma-Ray Spectrometric Data to Assist Uranium Exploration

    Energy Technology Data Exchange (ETDEWEB)

    Matolin, M., E-mail: matolin@natur.cuni.cz [Charles University, Prague (Czech Republic); Minty, B. [Geoscience Australia, Canberra (Australia)

    2014-05-15

    Geophysical methods can be used for mapping in both 2 and 3 dimensions, as well as the direct detection of ore bodies. The gamma-ray spectrometric method is an efficient method for the regional assessment of uranium potential and the detection of surface mineralization. However, the full potential of the method can only be realized when the data are adequately standardized. Examples of this standardization at both regional and local scales are dealt in this paper. At a regional scale, it is shown how the levelling of airborne gamma-ray spectrometry data over Australia increases the value of the resulting data, and on a local scale a geometrical correction for ground gamma-ray spectrometry in shallow holes that improves the accuracy of measurements is introduced. (author)

  16. Profiling of tryptophan-related plasma indoles in patients with carcinoid tumors by automated, on-line, solid-phase extraction and HPLC with fluorescence detection.

    Science.gov (United States)

    Kema, I P; Meijer, W G; Meiborg, G; Ooms, B; Willemse, P H; de Vries, E G

    2001-10-01

    Profiling of the plasma indoles tryptophan, 5-hydroxytryptophan (5-HTP), serotonin, and 5-hydroxyindoleacetic acid (5-HIAA) is useful in the diagnosis and follow-up of patients with carcinoid tumors. We describe an automated method for the profiling of these indoles in protein-containing matrices as well as the plasma indole concentrations in healthy controls and patients with carcinoid tumors. Plasma, cerebrospinal fluid, and tissue homogenates were prepurified by automated on-line solid-phase extraction (SPE) in Hysphere Resin SH SPE cartridges containing strong hydrophobic polystyrene resin. Analytes were eluted from the SPE cartridge by column switching. Subsequent separation and detection were performed by reversed-phase HPLC combined with fluorometric detection in a total cycle time of 20 min. We obtained samples from 14 healthy controls and 17 patients with metastasized midgut carcinoid tumors for plasma indole analysis. In the patient group, urinary excretion of 5-HIAA and serotonin was compared with concentrations of plasma indoles. Within- and between-series CVs for indoles in platelet-rich plasma were 0.6-6.2% and 3.7-12%, respectively. Results for platelet-rich plasma serotonin compared favorably with those obtained by single-component analysis. Plasma 5-HIAA, but not 5-HTP was detectable in 8 of 17 patients with carcinoid tumors. In the patient group, platelet-rich plasma total tryptophan correlated negatively with platelet-rich plasma serotonin (P = 0.021; r = -0.56), urinary 5-HIAA (P = 0.003; r = -0.68), and urinary serotonin (P manual, single-component analyses.

  17. Detection of Viral RNA in Tissues following Plasma Clearance from an Ebola Virus Infected Patient.

    Directory of Open Access Journals (Sweden)

    Mirella Biava

    2017-01-01

    Full Text Available An unprecedented Ebola virus (EBOV epidemic occurred in 2013-2016 in West Africa. Over this time the epidemic exponentially grew and moved to Europe and North America, with several imported cases and many Health Care Workers (HCW infected. Better understanding of EBOV infection patterns in different body compartments is mandatory to develop new countermeasures, as well as to fully comprehend the pathways of human-to-human transmission. We have longitudinally explored the persistence of EBOV-specific negative sense genomic RNA (neg-RNA and the presence of positive sense RNA (pos-RNA, including both replication intermediate (antigenomic-RNA and messenger RNA (mRNA molecules, in the upper and lower respiratory tract, as compared to plasma, in a HCW infected with EBOV in Sierra Leone, who was hospitalized in the high isolation facility of the National Institute for Infectious Diseases "Lazzaro Spallanzani" (INMI, Rome, Italy. We observed persistence of pos-RNA and neg-RNAs in longitudinally collected specimens of the lower respiratory tract, even after viral clearance from plasma, suggesting possible local replication. The purpose of the present study is to enhance the knowledge on the biological features of EBOV that can contribute to the human-to-human transmissibility and to develop effective intervention strategies. However, further investigation is needed in order to better understand the clinical meaning of viral replication and shedding in the respiratory tract.

  18. Detection of EGFR mutations in plasma and biopsies from non-small cell lung cancer patients by allele-specific PCR assays

    DEFF Research Database (Denmark)

    Weber, Britta; Meldgaard, Peter; Hager, Henrik

    2014-01-01

    samples with allele-specific PCR assays. METHODS: Pairs of the diagnostic biopsy and plasma obtained just prior to start of erlotinib treatment were collected from 199 patients with adenocarcinoma of non-small-cell lung cancer. DNA from both sample types was isolated and examined for the presence...... of mutations in exons 18-21 of the EGFR gene, employing the cobas(®) EGFR Tissue Test and cobas(®) EGFR Blood Test (in development, Roche Molecular Systems, Inc., CA, USA). RESULTS: Test results were obtained in all 199 (100%) plasma samples and 196/199 (98%) of the biopsies. EGFR-activating mutations were...... identified in 24/199 (12%) plasma samples and 28/196 (14%) biopsy samples, and 17/196 (9%) matched pairs contained the same mutation. Six EGFR mutations were present only in plasma samples but not in the biopsy samples. The overall concordance of the EGFR gene mutations detected in plasma and biopsy tissue...

  19. Mass spectrometric diagnosis of an atmospheric pressure helium microplasma jet

    International Nuclear Information System (INIS)

    McKay, K; Oh, J-S; Walsh, J L; Bradley, J W

    2013-01-01

    Ambient molecular beam mass spectrometry (MBMS) has been used to study how different capillary widths (530 µm and 2.4 mm) and excitation waveforms (continuous wave kHz and pulsed dc) affect the ionic composition of atmospheric pressure plasma jets. It is shown from time-averaged ion intensities that reducing the width of the jet capillary results in a significant increase in the variety of both positive and negative ions detected within the discharge. We discuss this in terms of changes in flow velocity and the onset of turbulence within the plasma plume. Changing the mode of excitation had little effect on the ionic species detected from the microplasma jet; however, there was a notable shift in dominance towards higher mass ions when operated in a continuous wave kHz mode. The temporal evolution of the ions within the microplasma jet was observed for both excitation sources, operated at 5 and 15 kHz. Positive ions were created during periods correlated with the positive and negative peaks in discharge current, while negative ions were predominantly created at times when the discharge current peak was negative. This phenomenon was independent of the driving waveform. For pulsed dc excitation, considerably fewer positive ions were created in periods related to the negative current peaks, especially at higher frequencies. We propose a simple explanation for these processes based on ideas of streamer propagation and the influence of self-induced electric fields in the plasma plume. (paper)

  20. A new method for detection of the electron temperature in laser-plasma short wave cut off of stimulated Raman scattering spectrum

    International Nuclear Information System (INIS)

    Zhang Jiatai

    1994-01-01

    From the theory of stimulated Raman scattering (SRS) three wave interaction, a new method of detecting the electron temperature in laser-plasma is obtained. SRS spectrum obtained from Shenguang No. 12 Nd-laser experiments are analysed. Using the wave length of short wave cut off of SRS, the electron temperature in corona plasma region is calculated consistently. These results agree reasonable with X-ray spectrum experiments

  1. Detection and quantification of serum or plasma HCV RNA: mini review of commercially available assays.

    Science.gov (United States)

    Le Guillou-Guillemette, Helene; Lunel-Fabiani, Francoise

    2009-01-01

    The treatment schedule (combination of compounds, doses, and duration) and the virological follow-up for management of antiviral treatment in patients chronically infected by HCV is now well standardized, but to ensure good monitoring of the treated patients, physicians need rapid, reproducible, and sensitive molecular virological tools with a wide range of detection and quantification of HCV RNA in blood samples. Several assays for detection and/or quantification of HCV RNA are currently commercially available. Here, all these assays are detailed, and a brief description of each step of the assay is provided. They are divided into two categories by method: those based on signal amplification and those based on target amplification. These two categories are then divided into qualitative, quantitative, and quantitative detection assays. The real-time reverse-transcription polymerase chain reaction (RT-PCR)-based assays are the most promising strategy in the HCV virological area.

  2. The Stool DNA Test is More Accurate than the Plasma Septin 9 Test in Detecting Colorectal Neoplasia

    Science.gov (United States)

    Ahlquist, David A.; Taylor, William R.; Mahoney, Douglas W.; Zou, Hongzhi; Domanico, Michael; Thibodeau, Stephen N.; Boardman, Lisa A.; Berger, Barry M.; Lidgard, Graham P.

    2014-01-01

    Background & Aims Several noninvasive tests have been developed for colorectal cancer (CRC) screening. We compared the sensitivities of a multi-marker test for stool DNA (sDNA) and a plasma test for methylated Septin 9 (SEPT9) in identifying patients with large adenomas or CRC. Methods We analyzed paired stool and plasma samples from 30 patients with CRC and 22 with large adenomas from Mayo Clinic archives. Stool (n=46) and plasma (n=49) samples from age- and sex-matched patients with normal colonoscopy results were used as controls. The sDNA test is an assay for methylated BMP3, NDRG4, vimentin, and TFPI2; mutant KRAS; the β-actin gene, and quantity of hemoglobin (by the porphyrin method). It was performed blindly at Exact Sciences (Madison WI); the test for SEPT9 was performed at ARUP Laboratories (Salt Lake City UT). Results were considered positive based on the manufacturer's specificity cutoff values of 90% and 89%, respectively. Results The sDNA test detected adenomas (median 2 cm, range 1–5 cm) with 82% sensitivity (95% confidence interval [CI], 60%–95%); SEPT9 had 14% sensitivity (95% CI, 3%–35%; P=.0001). The sDNA test identified patients with CRC with 87% sensitivity (95% CI, 69%–96%); SEPT9 had 60% sensitivity (95% CI, 41%–77%; P=.046). The sDNA test identified patients with stage I–III CRC with 91% sensitivity (95% CI, 71%–99%); SEPT9 had 50% sensitivity (95% CI, 28%–72%; P=.013); for stage IV CRC, sensitivity values were 75% (95% CI, 35%–97%) and 88% (95% CI, 47%–100%), respectively (P=.56). False-positive rates were 7% for the sDNA test and 27% for SEPT9. Conclusions Based on analyses of paired samples, the sDNA test detects non-metastatic CRC and large adenomas with significantly greater levels of sensitivity than the SEPT9 test. These findings might be used to modify approaches for CRC prevention and early detection. PMID:22019796

  3. A detection method of negative pionlike particles from a H2 gas discharge plasma

    International Nuclear Information System (INIS)

    Uramoto, Joshin.

    1996-02-01

    The negative pionlike particles π - penetrate a metal (or insulator) plate if positive ions produced secondarily by H - ions, diffuse to the back of the plate. Thus, the π - particles are not detected by a usual beam collector of mass analyzer using a metal plate. In order to detect the π - particles, we must interrupt the diffusion of the positive ions to the back of the beam collector while the π - particles are confined inside the beam collector and changed into a multiplied electron current. (author)

  4. Longitudinal Bank for Serum, Plasma and DNA for Detection of Biomarkers

    Energy Technology Data Exchange (ETDEWEB)

    Ward, David C. [Nevada Cancer Institute, Las Vegas, NV (United States)

    2009-01-31

    With the support of this DOE appropriation, NVCI has established a biorepository for serum, plasma, DNA and urine specimens. Over 2,500 patients have been consented which is over 90% of all new patients seen at NVCI. The specimens have been coded, centrifuged, aliquoted and frozen at -80°C in a rapid manner so that they are all processed in less than 1 hour from the acquisition. There are over 28,000 aliquoted, coded tubes in our inventory. Specimens from 200 control volunteer subjects without any history of cancer also have been banked. The patient specimens are encoded and the demographics and therapeutic treatments are linked to the Oncore software. This computer program catalogues the specimens and provides a rapid conduit between the biorepository and the NVCI electronic medical record.

  5. Seminal plasma as a source of prostate cancer peptide biomarker candidates for detection of indolent and advanced disease.

    Directory of Open Access Journals (Sweden)

    Jochen Neuhaus

    Full Text Available BACKGROUND: Extensive prostate specific antigen screening for prostate cancer generates a high number of unnecessary biopsies and over-treatment due to insufficient differentiation between indolent and aggressive tumours. We hypothesized that seminal plasma is a robust source of novel prostate cancer (PCa biomarkers with the potential to improve primary diagnosis of and to distinguish advanced from indolent disease. METHODOLOGY/PRINCIPAL FINDINGS: In an open-label case/control study 125 patients (70 PCa, 21 benign prostate hyperplasia, 25 chronic prostatitis, 9 healthy controls were enrolled in 3 centres. Biomarker panels a for PCa diagnosis (comparison of PCa patients versus benign controls and b for advanced disease (comparison of patients with post surgery Gleason score 7 were sought. Independent cohorts were used for proteomic biomarker discovery and testing the performance of the identified biomarker profiles. Seminal plasma was profiled using capillary electrophoresis mass spectrometry. Pre-analytical stability and analytical precision of the proteome analysis were determined. Support vector machine learning was used for classification. Stepwise application of two biomarker signatures with 21 and 5 biomarkers provided 83% sensitivity and 67% specificity for PCa detection in a test set of samples. A panel of 11 biomarkers for advanced disease discriminated between patients with Gleason score 7 and organ-confined (plasma represents a robust source of potential peptide makers

  6. A review on the mass spectrometric studies of americium: Present status and future perspective.

    Science.gov (United States)

    Aggarwal, Suresh Kumar

    2018-01-01

    The manuscript reviews the various mass spectrometric techniques for analysis and chemical studies of Americium. These methods include thermal ionization mass spectrometry (TIMS), and inductively coupled plasma source mass spectrometry (ICPMS) for the determination of Am isotope ratios and concentration in nuclear fuel samples of interest in nuclear technology, and in complex biological and environmental samples. Ultra-sensitive mass spectrometric techniques of resonance-ionization mass spectrometry (RIMS), and accelerator-based mass spectrometry (AMS) are also discussed. The novel applications of electrospray ionization mass spectrometry (ESIMS) to understand the solution chemistry of Am and other actinides are presented. These studies are important in view of the world-wide efforts to develop novel complexing agents to separate lanthanides and minor actinides (Am, Np, and Cm) for partitioning and transmutation of minor actinides from the point of view of nuclear waste management. These mass spectrometry experiments are also of great interest to examine the covalent character of actinides with increasing atomic number. Studies on gas-phase chemistry of Am and its oxides with Knudsen effusion mass spectrometry (KEMS), Fourier-transform ion cyclotron resonance mass spectrometry (FTICR-MS), and laser-based experiments with reflectron time-of-flight mass spectrometer (R-ToF) are highlighted. These studies are important to understand the fundamental chemistry of 5f electrons in actinides. Requirement of certified isotopic reference materials of Am to improve the accuracy of experimental nuclear data (e.g., the half-life of 243 Am) is emphasized. © 2016 Wiley Periodicals, Inc. Mass Spec Rev. © 2016 Wiley Periodicals, Inc.

  7. Simple Hydrogen Plasma Doping Process of Amorphous Indium Gallium Zinc Oxide-Based Phototransistors for Visible Light Detection.

    Science.gov (United States)

    Kang, Byung Ha; Kim, Won-Gi; Chung, Jusung; Lee, Jin Hyeok; Kim, Hyun Jae

    2018-02-28

    A homojunction-structured amorphous indium gallium zinc oxide (a-IGZO) phototransistor that can detect visible light is reported. The key element of this technology is an absorption layer composed of hydrogen-doped a-IGZO. This absorption layer is fabricated by simple hydrogen plasma doping, and subgap states are induced by increasing the amount of hydrogen impurities. These subgap states, which lead to a higher number of photoexcited carriers and aggravate the instability under negative bias illumination stress, enabled the detection of a wide range of visible light (400-700 nm). The optimal condition of the hydrogen-doped absorption layer (HAL) is fabricated at a hydrogen partial pressure ratio of 2%. As a result, the optimized a-IGZO phototransistor with the HAL exhibits a high photoresponsivity of 1932.6 A/W, a photosensitivity of 3.85 × 10 6 , and a detectivity of 6.93 × 10 11 Jones under 635 nm light illumination.

  8. Development of a double-antibody radioimmunoassay for detecting ovarian tumor-associated antigen fraction OCA in plasma

    International Nuclear Information System (INIS)

    Knauf, S.; Urbach, G.I.

    1978-01-01

    Ovarian tumor-associated antigen isolated from human tumor tissue was shown to have a different mobility from that of carcinoembryonic antigen (CEA) in both acrylamide gel electrophoresis and immunoelectrophoresis in agarose. The ovarian tumor antigen is composed of six species with different electrophoretic mobility in acrylamide gel electrophoresis. Three of these species were detected in Sephadex G-100 ovarian fraction OCA (from the void volume peak) and the other three species of lower apparent molecular weight were detected in fraction OCD (from the second peak). Fractions OCA and OCD did not share common antigenic determinants as determined by immunodiffusion. CEA was shown to share antigenic determinants with both OCA and OCD. A double-antibody radioimmunoassay capable of detecting nanogram quantities of plasma OCA was developed. In a preliminary study of ovarian cancer patients, OCA appeared to be a more sensitive marker for ovarian cancer than CEA. There was virtually no correlation (r 2 = 0.1) between OCA and CEA levels in these patients, as determined by radioimmunoassay

  9. System for Gamma an X rays fluorescence spectrometric

    International Nuclear Information System (INIS)

    Alonso Abad, D.; Arista Romeu, E.; Bolanos Perez, L. and others

    1997-01-01

    A system for spectrometry of gamma or fluorescence X rays is presented. It sis composed by a Si(Li) semiconductors detector, a charge sensitive preamplifier, a high voltage power supply, a spectrometric amplifier and a monolithic 1024 channels multichannel analyzers or an IBM compatible 4096 channels add - on- card multichannel analyzer. The system can be configured as a 1024 or 4096 channels gamma or fluorescent X rays spectrometer

  10. Electrospray Ionization Mass Spectrometric Analysis of Highly Reactive Glycosyl Halides

    Directory of Open Access Journals (Sweden)

    Lajos Kovács

    2012-07-01

    Full Text Available Highly reactive glycosyl chlorides and bromides have been analysed by a routine mass spectrometric method using electrospray ionization and lithium salt adduct-forming agents in anhydrous acetonitrile solution, providing salient lithiated molecular ions [M+Li]+, [2M+Li]+ etc. The role of other adduct-forming salts has also been evaluated. The lithium salt method is useful for accurate mass determination of these highly sensitive compounds.

  11. Gamma spectrometric system based on the personal computer Pravetz-83

    International Nuclear Information System (INIS)

    Yanakiev, K; Grigorov, T.; Vuchkov, M.

    1985-01-01

    A gamma spectrometric system based on a personal microcomputer Pravets-85 is described. The analog modules are NIM standard. ADC data are stored in the memory of the computer via a DMA channel and a real-time data processing is possible. The results from a series of tests indicate that the performance of the system is comparable with that of comercially avalable computerized spectrometers Ortec and Canberra

  12. Neutron activation and mass spectrometric measurement of /sup 129/I

    International Nuclear Information System (INIS)

    Strebin, R.S. Jr.; Brauer, F.P.; Kaye, J.H.; Rapids, M.S.; Stoffels, J.J.

    1987-11-01

    An integrated procedure has been developed for measurement of /sup 129/I by neutron activation analysis and mass spectrometry. An iodine isolation procedure previously used for neutron activation has been modified to provide separated iodine suitable for mass spectrometric measurement as well. Agreement between both methods has been achieved within error limits. The measurement limit by each method is about 10/sup 7/ atoms (2 fg) of /sup 129/I. 13 refs,. 4 figs., 1 tab

  13. Non-leaky vesiculation of large unilamellar vesicles (LUV) induced by plasma high density lipoproteins (HDL): Detection by HPLC

    International Nuclear Information System (INIS)

    Tischler, U.; Rueckert, D.S.; Schubert, R.; Jaroni, H.W.; Schmidt, K.H.

    1989-01-01

    Interaction of large unilamellar phosphatidylcholine vesicles (LUV, 75nm) and plasma high density lipoproteins (HDL) resulted in a non-leaky vesiculation of LUV. This vesiculation was detected by a HPLC-system consisting of a combination of three TSK-gel columns (6000PW, 5000PW, 3000SW). With increasing incubation time liposomal [ 14 C]PC, entrapped [ 3 H]inulin, and apoprotein of HDL origin decreased. The decrease was accompanied by a formation of new particles, consisting of liposomal PC and apoprotein. These particles also enclosed [3H]inulin, reflecting a hydrophilic inner space. The formation of the particles reached a maximum after one day of incubation. Retention time was 21 minutes for LUV, 28 minutes for the new particles, and 36 minutes for HDL. In vesicles with membranes consisting of phosphatidylcholine and 30% cholesterol no interactions were observed

  14. Mass Spectrometric Calibration of Controlled Fluoroform Leak Rate Devices Technique and Uncertainty Analysis

    CERN Document Server

    Balsley, S D; Laduca, C A

    2003-01-01

    Controlled leak rate devices of fluoroform on the order of 10 sup - sup 8 atm centre dot cc sec sup - sup 1 at 25 C are used to calibrate QC-1 War Reserve neutron tube exhaust stations for leak detection sensitivity. Close-out calibration of these tritium-contaminated devices is provided by the Gas Dynamics and Mass Spectrometry Laboratory, Organization 14406, which is a tritium analytical facility. The mass spectrometric technique used for the measurement is discussed, as is the first principals calculation (pressure, volume, temperature and time). The uncertainty of the measurement is largely driven by contributing factors in the determination of P, V and T. The expanded uncertainty of the leak rate measurement is shown to be 4.42%, with a coverage factor of 3 (k=3).

  15. Anomalies from aerial spectrometric and total count radiometric surveys in the southeastern United States

    International Nuclear Information System (INIS)

    Lee, C.H.; Lawton, D.E.

    1978-01-01

    Aerial radiometric reconnaissance surveys are conducted because of their cost, time, and manpower savings compared to surface studies. Two types of aerial surveys are being flown in the southeastern United States: total count gamma-ray surveys for the Coastal Plains Regional Commission and the US Geological Survey, and differential gamma-ray spectrometric surveys for the US Department of Energy. Anomalous radioactivity detected during aerial surveys is related to higher concentrations of naturally occurring uranium, or to cultural activities, natural causes, or mapping errors which simulate real uranium anomalies. Each anomaly should be ground checked; however, several types of anomalies may be eliminated by evaluation of the aerial data in the office if field time is limited

  16. Circular viral DNA detection and junction sequence analysis from PBMC of SHIV-infected cynomolgus monkeys with undetectable virus plasma RNA

    International Nuclear Information System (INIS)

    Cara, Andrea; Maggiorella, Maria Teresa; Bona, Roberta; Sernicola, Leonardo; Baroncelli, Silvia; Negri, Donatella R.M.; Leone, Pasqualina; Fagrouch, Zahra; Heeney, Jonathan; Titti, Fausto; Cafaro, Aurelio; Ensoli, Barbara

    2004-01-01

    Extrachromosomal forms of human immunodeficiency virus (HIV)-1 can be detected in peripheral blood mononuclear cell (PBMC) from HIV-infected patients in the absence of detectable viral replication and are thought to be a sign of active but cryptic virus replication. No information, however, are available on whether these forms are also present in animal models for acquired immunodeficiency syndrome (AIDS) and on their relation with other methods of detection of virus replication. To this aim, a polymerase chain reaction (PCR) approach was used to detect and analyze unintegrated circular 2-LTR-containing forms in PBMC of simian human immunodeficiency virus (SHIV)89.6P infected cynomolgus monkeys with RNA levels ranging between 1.8x10 6 and less than 50 copies/ml of plasma. 2-LTR forms were detected in 96.5% of monkeys' samples above 50 copies/ml of plasma, whereas they were present in 75.8% of monkeys' samples below 50 copies/ml of plasma. Persistence of unintegrated viral DNA in monkeys with undetectable plasma RNA could indicate either stability in non-dividing cells or ongoing low levels of viral replication in dividing cells

  17. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    Energy Technology Data Exchange (ETDEWEB)

    Herrero Latorre, C., E-mail: carlos.herrero@usc.es [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain); Alvarez Mendez, J.; Barciela Garcia, J.; Garcia Martin, S.; Pena Crecente, R.M. [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain)

    2012-10-24

    Highlights: Black-Right-Pointing-Pointer The use of CNTs as sorbent for metal species in solid phase extraction has been described. Black-Right-Pointing-Pointer Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. Black-Right-Pointing-Pointer Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes - due to their high adsorption and desorption capacities - have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

  18. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    International Nuclear Information System (INIS)

    Herrero Latorre, C.; Álvarez Méndez, J.; Barciela García, J.; García Martín, S.; Peña Crecente, R.M.

    2012-01-01

    Highlights: ► The use of CNTs as sorbent for metal species in solid phase extraction has been described. ► Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. ► Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes – due to their high adsorption and desorption capacities – have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

  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. Quantitative determination of famotidine in human maternal plasma, umbilical cord plasma and urine using high-performance liquid chromatography - mass spectrometry

    Science.gov (United States)

    Wang, Xiaoming; Rytting, Erik; Abdelrahman, Doaa R.; Nanovskaya, Tatiana N.; Hankins, Gary D.V.; Ahmed, Mahmoud S.

    2013-01-01

    The liquid chromatography with electrospray ionization mass spectrometry for the quantitative determination of famotidine in human urine, maternal and umbilical cord plasma was developed and validated. The plasma samples were alkalized with ammonium hydroxide and extracted twice with ethyl acetate. The extraction recovery of famotidine in maternal and umbilical cord plasma ranged from 53% to 64% and 72% to 79%, respectively. Urine samples were directly diluted with the initial mobile phase then injected into the HPLC system. Chromatographic separation of famotidine was achieved by using a Phenomenex Synergi™ Hydro-RP™ column with a gradient elution of acetonitrile and 10 mM ammonium acetate aqueous solution (pH 8.3, adjusted with ammonium hydroxide). Mass Spectrometric detection of famotidine was set in the positive mode and used a selected ion monitoring method. Carbon-13-labeled famotidine was used as internal standard. The calibration curves were linear (r2> 0.99) in the concentration ranges of 0.631-252 ng/mL for umbilical and maternal plasma samples, and of 0.075-30.0 μg/mL for urine samples. The relative deviation of method was less than 14% for intra- and inter-day assays, and the accuracy ranged between 93% and 110%. The matrix effect of famotidine in human urine, maternal and umbilical cord plasma is less than 17%. PMID:23401067

  1. Vitamin D analysis in plasma by high performance liquid chromatography (HPLC) with C30 reversed phase column and UV detection - easy and acetonitrile-free

    DEFF Research Database (Denmark)

    Hymøller, Lone; Jensen, Søren Krogh

    2011-01-01

    Two physiologically important forms of vitamin D exist: vitamin D2 and vitamin D3, which by liver based hydroxylase enzymes are converted to 25-hydroxyvitamin D2 and 25-hydroxyvitamin D3, respectively. These hydroxylated metabolites of vitamin D are measured in plasma to assess the vtamin D status...... detection at 265nm for quantifying vitamin D2, vitamin D3, 25-hydroxyvitamin D2, and 25-hydroxyvitamin D3. The method proved versatile with respect to plasma lipid content, sample amount, and plasma concentration of the vitamin D metabolites as it was tested using plasma from six different species: cattle...... material® 972 “Vitamin D in human serum” from the National Institute of Standards and Technology (NIST) (Gaithersburg, USA) the results for 25-hydroxyvitamin D2 and 25-hydroxyvitamin D3 concentrations were within the boundaries provided by NIST, reflected by Z-scores between 0.1 and 0.9....

  2. Simple measurement of isepamicin, a new aminoglycoside antibiotic, in guinea pig and human plasma, using high-performance liquid chromatography with ultraviolet detection

    International Nuclear Information System (INIS)

    Dionisotti, S.; Bamonte, F.; Scaglione, F.; Ongini, E.

    1991-01-01

    Isepamicin, the 1-N-(S-alpha-hydroxy-beta-aminopropionyl) derivative of gentamicin B, is a new aminoglycoside antibiotic, which not only has most of the properties of amikacin but also is effective against several amikacin-resistant strains of bacteria. The drug was assayed in guinea-pig and human plasma with a high-performance liquid chromatographic procedure using precolumn derivatization with 1-fluoro-2,4-dinitrobenzene and ultraviolet detection. Linearity was established over the range 0.5-40 micrograms/ml using 50 microliters of plasma. Accuracy has a mean relative error of less than 3% and precision a mean coefficient of variation of 5%. Isepamicin was determined without interference from plasma constituents or other drugs commonly prescribed during aminoglycoside therapy. This procedure correlates well with radioimmunoassay and can be used either in experimental studies or therapeutic monitoring of plasma levels

  3. Spectrometric devices of itinerant radiometric laboratory

    International Nuclear Information System (INIS)

    Dolgirev, E.I.; Moroz, G.L.; Shchedrin, D.A.

    1978-01-01

    Scintillation gamma-spectrometer is described designed for mobile radiometric laboratory for individual monitoring of internal γ-radiation of members of the general population and service personnel as well as for analysis of the isotopic composition of radiocontaminants in the environment. Description and technical features of device are given. The detection unit consists of detectors made on the basis of NaI(Tl) monocrystals 63 x 63 mm in size. The unit permits measurement of various levels of gamma-emitting nuclides throughout the body and in the thyroid and lungs of man. Provision is made for measuring samples with high specific activities (more than 10 -5 Cu/g) and for examining individuals having high levels of incorporated radionuclides

  4. Plasma TIMP-1 and CEA in detection of primary colorectal cancer: a prospective, population based study of 4509 high-risk individuals

    DEFF Research Database (Denmark)

    Nielsen, Hans J; Brünner, Nils; Jørgensen, Lars Nannestad

    2011-01-01

    . Individuals (n = 4509) referred for large bowel endoscopy due to symptoms of CRC were prospectively included. Baseline data and concurrent diseases were recorded. The primary endpoint was detection of CRC and findings at examinations were recorded using International Classification of Diseases-10 codes....... This prospective validation study supports the use of the combination of plasma TIMP-1 and CEA protein measurements as a potential aid in early detection of CRC and specifically of CC....

  5. Clinical significance of detection of plasma β-amyloid protein (β-AP) levels in patients with senile dementia

    International Nuclear Information System (INIS)

    Yu Binwei; Xu Shangao; Lu Zhifeng; Wang Weihua; Mao Xiaohua; Zhou Chaohua

    2007-01-01

    Objective: To explore the value of determination of plasma β-AP levels in the diagnosis and monitoring of Alzheimer's disease (AD). Methods: Plasma β-AP levels were weasured with RIA in 43 patients with AD and 58 controls, as well as in 8 AD patients after a course of cerebrolysin treatment. Results: The plasma β-AP levels in the AD patients were significance higher those in controls (P<0.01). The plasma β-AP levels were especially higher in the severe eases, however, the plasma β-AP levels in some late AD patients dropped again, even lower than those in the controls. The plasma β-AP levels in the 8 AD patients decreased significantly after treatment with cerebrolysin. Conclusion: The plasma β-AP is a biochemical maker of AD. Dynamic examnation of plasma β-AP levels is valuable in assessing the progression and prognosis of the disease. (authors)

  6. Simultaneous determination of albumin and low-molecular-mass thiols in plasma by HPLC with UV detection.

    Science.gov (United States)

    Borowczyk, Kamila; Wyszczelska-Rokiel, Monika; Kubalczyk, Paweł; Głowacki, Rafał

    2015-02-15

    In this paper, we describe a simple and robust HPLC based method for determination of total low- and high-molecular-mass thiols, protein S-linked thiols and reduced albumin in plasma. The method is based on derivatization of analytes with 2-chloro-1-methylquinolinium tetrafluoroborate, separation and quantification by reversed-phase liquid chromatography followed by UV detection. Disulfides were converted to their thiol counterparts by reductive cleavage with tris(2-carboxyethyl)phosphine. Linearity in detector response for total thiols was observed over the range of 1-40 μmol L(-1) for Hcy and glutathione (GSH), 5-100 μmol L(-1) for Cys-Gly, 20-300 μmol L(-1) for Cys and 3.1-37.5 μmol L(-1) (0.2-2.4gL(-1)) for human serum albumin (HSA). For the protein S-bound forms these values were as follows: 0.5-30 μmol L(-1) for Hcy and GSH, 2.5-60 μmol L(-1) for Cys-Gly and 5-200 μmol L(-1) for Cys. The LOQs for total HSA, Cys, Hcy, Cys-Gly and GSH were 0.5, 0.2, 0.4, 0.3 and 0.4 μmol L(-1), respectively. The estimated validation parameters for all analytes are more than sufficient to allow the analytical method to be used for monitoring of the total and protein bound thiols as well as redox status of HSA in plasma. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Performance Evaluation of NIPT in Detection of Chromosomal Copy Number Variants Using Low-Coverage Whole-Genome Sequencing of Plasma DNA

    DEFF Research Database (Denmark)

    Liu, Hongtai; Gao, Ya; Hu, Zhiyang

    2016-01-01

    , including 33 CNVs samples and 886 normal samples from September 1, 2011 to May 31, 2013, were enrolled in this study. The samples were randomly rearranged and blindly sequenced by low-coverage (about 7M reads) whole-genome sequencing of plasma DNA. Fetal CNVs were detected by Fetal Copy-number Analysis...

  8. Flow injection on-line dilution for multi-element determination in human urine with detection by inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald; Gammelgaard, Bente

    2001-01-01

    A simple flow injection on-line dilution procedure with detection by inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of copper, zinc, arsenic, lead, selenium, nickel and molybdenum in human urine. Matrix effects were minimized by employing a dilution factor...

  9. Validation of a method for the determination of zolpidem in human plasma using LC with fluorescence detection.

    Science.gov (United States)

    Ring, P R; Bostick, J M

    2000-04-01

    A sensitive and selective high-performance liquid chromatography (HPLC) method was developed for the determination of zolpidem in human plasma. Zolpidem and the internal standard (trazodone) were extracted from human plasma that had been made basic. The basic sample was loaded onto a conditioned Bond Elut C18 cartridge, rinsed with water and eluted with methanol. Forty microliters were then injected onto the LC system. Separation was achieved on a C18 column (150 x 4.6 mm, 5 microm) with a mobile phase composed of acetonitrile:50 mM potassium phosphate monobasic at pH 6.0 (4:6, v/v). Detection was by fluorescence, with excitation at 254 nm and emission at 400 nm. The retention times of zolpidem and internal standard were approximately 4.7 and 5.3 min, respectively. The LC run time was 8 min. The assay was linear in concentration range 1-400 ng/ml for zolpidem in human plasma. The analysis of quality control samples for zolpidem (3, 30, and 300 ng/ml) demonstrated excellent precision with relative standard deviations (RSD) of 3.7, 4.6, and 3.0%, respectively (n = 18). The method was accurate with all intraday (n = 6) and overall (n = 18) mean concentrations within 5.8% from nominal at all quality control sample concentrations. This method was also performed using a Gilson Aspec XL automated sample processor and autoinjector. The samples were manually fortified with internal standard and made basic. The aspec then performed the solid phase extraction and made injections of the samples onto the LC system. Using the automated procedure for analysis, quality control samples for zolpidem (3, 30, and 300 ng/ml) demonstrated acceptable precision with RSD values of 9.0, 4.9, and 5.1%, respectively (n = 12). The method was accurate with all intracurve (n = 4) and overall (n = 12) mean values being less than 10.8% from nominal at all quality control sample concentrations.

  10. Gamma spectrometric methods for measuring plutonium

    International Nuclear Information System (INIS)

    Gunnink, R.

    1978-01-01

    Nondestructive analyses of plutonium can be made by detecting and measuring the gamma rays emitted by a sample. Although qualitative and semiquantitative assays can be performed with relative ease, only recently have methods been developed, using computer analysis techniques, that provide quantitative results. This paper reviews some new techniques developed for measuring plutonium. The features of plutonium gamma-ray spectra are reviewed and some of the computer methods used for spectrum analysis are discussed. The discussion includes a description of a powerful computer method of unfolding complex peak multiplets that uses the standard linear least-squares techniques of data analysis. This computer method is based on the generation of response profiles for the isotopes composing a plutonium sample and requires a description of the peak positions, relative intensities, and line shapes. The principles that plutonium isotopic measurements are based on are also developed, followed by illustrations of the measurement procedures as applied to the quantitative analysis of plutonium liquid and solid samples

  11. Rational utilisation of a spectrometer detector for leaks; Utilisation rationnelle d'un spectrometre detecteur de fuites

    Energy Technology Data Exchange (ETDEWEB)

    Geller, R [Commissariat a l' Energie Atomique, Saclay(France). Centre d' Etudes Nucleaires

    1954-07-01

    In this following article, we expose the general problem of the leakage in a vacuum installation. We consider the principles of the detection in general and study especially the conditions of detection by an helium spectrometer. We deduce practical conclusions as for the branching of this last and to its application in the most current cases. (author) [French] Dans l'article qui suit, nous exposons le probleme general des fuites dans une installation a vide. Nous y envisageons les principes de la detection en general et etudions particulierement les conditions de detection par spectrometre a helium. Noue tirons des conclusions pratiques quant au branchement de ce dernier et a son application dans les cas les plus courants. (auteur)

  12. Particle desorption mass spectrometric surface characterization

    International Nuclear Information System (INIS)

    Summers, W.R.

    1986-01-01

    The feasibility of utilizing 252 Cf-Particle Desorption Mass Spectrometry (PDMS) to characterize the surface region of solid samples has been evaluated. The PDMS experiment was adapted to an ultrahigh vacuum (UHV) environment and was configured so as to allow the analysis of thick as well as thin samples. This apparatus included an in situ sputter cleaning/depth profiling facility. The mass resolution was variable from 300 to 200 at 133 daltons by changing the drift length from 27 cm to 20 cm. Desorbed ions were focused by using either a dual grid assembly or an einzel lens. The overall instrumental transmission efficiency with the einzel lens operative was approximately 50%. The applicability of 252 Cf-PDMS to samples that were thick and insulating was demonstrated in the analysis of geological specimens. Pollucite, Microcline, Amblygonite, and Lepidolite were analyzed without complications associated with sample thickness or charge accumulation. Substitution occurring between the alkali metals in the environment was observed by PDMS and was corroborated by SIMS, XPS, and EMP analyses. The analysis of NBM SRM glasses addressed the suitability of combining the PDMS technique was sputter etching. This application demonstrated the ability of this technique to sense changes in the chemical environment brought about by sputter cleaning. The analysis of these samples also allowed the estimation of detection limits for lithium, rubidium, and cesium in a glass matrix as 300 ppm, 400 ppm, and 400 ppm, respectively. Sputter depth profiling combined with 252 Cf-PDMS analysis of an aluminum layer on a silicon substrate established the utility of the PDMS technique in surface characterization

  13. Mass spectrometric analysis of simple hydrogen compounds; Analyse de composes hydrogenes simples au spectrometre de masse

    Energy Technology Data Exchange (ETDEWEB)

    Nief, C; Botter, R [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

    1960-07-01

    A uranium furnace is inserted in the gas inlet line of a mass spectrometer between the leak and the source. The line is fed with simple hydrogen compounds (H{sub 2}O, NH{sub 3}, H{sub 2}S) which are in this way reduced to hydrogen gas. Memory effects are largely avoided by heating the sample line to 90 deg. C. The speed of the isotopic analysis is only slightly less than that of hydrogen gas itself; the accuracy is better due to the reduction of fractionating effects in the leak. For the absolute measurements of deuterium in water, the presence of H{sub 3}{sup +} is a problem. Water samples, prepared by mixing an unknown light water sample with different amounts of heavy water, are equilibrated with hydrogen sulphide and analysis of the two phases of each sample enables the zero of the concentration scale to be determined from the point of intersection of the two curves obtained by plotting mixture composition against the observed isotope ratio in the two phases. The whole experiment can be carried out in the apparatus described which analyses hydrogen in H{sub 2}S and H{sub 2}O in the same way. (author) [French] Un four a uranium est insere dans la ligne d'introduction de gaz d'un spectrometre de masse entre la fuite et la source. La ligne est alimentee par des composes hydrogenes simples (H{sub 2}O, NH{sub 3}, H{sub 2}S) qui sont de cette facon transformes en hydrogene gazeux. On evite dans une large mesure les effets de memoire en chauffant la ligne de l'echantillon jusqu'a 90 deg. C. La vitesse de l'analyse isotopique est seulement legerement inferieure a celle de l'hydrogene gazeux lui-meme; la precision est meilleure du fait de la reduction des effets de fractionnement dans la fuite. Pour les mesures absolues du deuterium dans l'eau, la presence de H{sub 3}{sup +} pose un probleme. Les echantillons d'eau, prepares en melangeant un echantillon inconnu d'eau legere a differentes quantites d'eau lourde, sont equilibres par de l'hydrogene sulfure et l'analyse de

  14. Challenges and recent advances in mass spectrometric imaging of neurotransmitters

    Science.gov (United States)

    Gemperline, Erin; Chen, Bingming; Li, Lingjun

    2014-01-01

    Mass spectrometric imaging (MSI) is a powerful tool that grants the ability to investigate a broad mass range of molecules, from small molecules to large proteins, by creating detailed distribution maps of selected compounds. To date, MSI has demonstrated its versatility in the study of neurotransmitters and neuropeptides of different classes toward investigation of neurobiological functions and diseases. These studies have provided significant insight in neurobiology over the years and current technical advances are facilitating further improvements in this field. neurotransmitters, focusing specifically on the challenges and recent Herein, we advances of MSI of neurotransmitters. PMID:24568355

  15. Mass spectrometric study of Nd2S3 vaporization

    International Nuclear Information System (INIS)

    Fenochka, B.V.

    1987-01-01

    The authors conduct a mass-spectrometric study of neodymium(III) sulfide vaporization. The chemical composition of the samples was stoichiometric and the samples were vaporized from tantalum effusion cells. When the vapor over Nd 2 S 3 is ionized by electrons the mass spectra shows monovalent cations of Nd, S, NdS, and NdO. The enthalpy of vaporization if Nd atoms from Nd 2 S 3 at average experimental temperatures and the standard enthalpy of reaction is shown. Also presented is the enthalpy of vaporization of NdS molecules from Nd 2 S 3 at average experimental temperatures and the standard enthalpy of reaction

  16. Gamma spectrometric analyses of environmental samples at PINSTECH

    International Nuclear Information System (INIS)

    Faruq, M.U.; Parveen, N.; Ahmed, B.; Aziz, A.

    1979-01-01

    Gamma spectrometric analyses of air and other environmental samples from PINSTECH were carried out. Air particulate samples were analyzed by a Ge(Li) detector on a computer-based multichannel analyzer. Other environmental samples were analyzed by a Na(T1) scintillation detector spectrometer and a multichannel analyzer with manual analysis. Concentration of radionuclides in the media was determined and the sources of their production were identified. Age of the fall out was estimated from the ratios of the fission products. (authors)

  17. Mass spectrometric investigation of fluorated europium. beta. -diketonates. [Electrons

    Energy Technology Data Exchange (ETDEWEB)

    Khomenko, V.S.; Lozinskij, M.O.; Fialkov, Yu.A.; Rasshinina, T.A.; Suboch, V.P. (AN Belorusskoj SSR, Minsk. Inst. Fiziki; AN Ukrainskoj SSR, Kiev. Inst. Organicheskoj Khimii)

    Ternary complexes of europium with two organic ligands - fluorated ..beta..-diketone and organic base - in the aqueous phase at electron shock are investigated; regroupings that take place in them are established. Mass-spectrometric investigation has shown that complexes with ..beta..-diketones, containing in oxygen atom in a fluorated radical, eliminate stable molecules of difluorophosgen, CoF/sub 2/. For the complexes studied under the above conditions the Co molecule elimination is also typical which is accompanied by the formation of ions with a metal-carbon bond.

  18. Mass spectrometric investigation of fluorated europium β-diketonates

    International Nuclear Information System (INIS)

    Khomenko, V.S.; Lozinskij, M.O.; Fialkov, Yu.A.; Rasshinina, T.A.; Suboch, V.P.; AN Ukrainskoj SSR, Kiev. Inst. Organicheskoj Khimii)

    1983-01-01

    Ternary complexes of europium with two organic lidands - fluorated β-diketone and organic base - in the aqueous phase at electron shock are investigated; regroupings that take place in them are established. Mass-spectrometric investigation has shown that complexes with β-diketones, containing in oxygen atom in a fluorated radical, eliminate stable molecules of difluorophosgen, CoF 2 . For the complexes studied under the above conditions the Co molecule elimination is also typical which is accompanied by the formation of ions with a metal-carbon bond

  19. Thermogravimetric-quadrupole mass-spectrometric analysis of geochemical samples.

    Science.gov (United States)

    Gibson, E. K., Jr.; Johnson, S. M.

    1972-01-01

    Thermogravimetric-quadrupole mass-spectrometric-analysis techniques can be used to study a wide variety of problems involving decomposition processes and identification of released volatile components. A recording vacuum thermoanalyzer has been coupled with a quadrupole mass spectrometer. The rapid scan capabilities of the quadrupole mass spectrometer are used to identify the gaseous components released. The capability of the thermogravimetric-quadrupole mass spectrometer to provide analytical data for identification of the released volatile components, for determination of their sequence of release and for correlation of thermal-decomposition studies is illustrated by an analysis of the Orgueil carbonaceous chondrite.

  20. Determination of uranium enrichment by using gamma-spectrometric methods

    International Nuclear Information System (INIS)

    Kutnyj, D.V.; Telegin, Yu.N.; Odejchuk, N.P.; Mikhailov, V.A.; Tovkanets, V.E.

    2009-01-01

    By using commercial analysis programs MGAU (LLNL, USA) and FRAM (LANL, USA) the summary error of gamma-spectrometric uranium enrichment measurements was investigated. Uranium samples with enrichments of 0,71; 4,46 and 20,1 % were measured. The coaxial high purity germanium detector (type GC) and the planar germanium detector (type LEGe) were used as gamma-radiation detectors. It was shown that experimental equipment and mathematical software available in NSC KIPT allow us to measure uranium enrichment by nondestructive method with accuracy of not worse than 2%.

  1. Detection of microbial translocation in HIV and SIV infection using the Limulus amebocyte lysate assay is masked by serum and plasma.

    Directory of Open Access Journals (Sweden)

    Ashwin Balagopal

    Full Text Available Microbial translocation (MT is thought to be a major contributor to the pathogenesis of HIV-related immune activation, and circulating lipopolysaccharide (LPS from gram-negative bacteria is the principle measurement of this process. However, related research has been impeded by inconsistent LPS test results.Specimens were obtained from HIV-infected adults enrolled in the PEARLS study (ACTG A5175 and HIV-HCV co-infected participants enrolled in a study of liver disease staging using MRI elastography. Pig-tailed macaque specimens were obtained from SIV-infected and -uninfected animals. Samples were tested for LPS using the LAL assay with diazo-coupling modifications to improve sensitive detection.When exogenous LPS was added to macaque plasma, >25% inhibition of LPS detection was found in 10/10 (100% samples at 20% plasma concentration compared to control; in contrast 5/10 (50% samples at 2% plasma concentration (p = 0.07 and 0/10 (0% at 0.1% plasma concentration (p = 0.004 showed >25% inhibition of LPS detection. Similarly, when LPS was added to human serum, >25% inhibition of LPS detection was found in 5/12 (42% of samples at 2% serum concentration compared to control, while 0/12 (0% of samples in 0.1% serum showed >25% inhibition of LPS detection (p = 0.07. Likewise, LPS detection in human sera without exogenous LPS was improved by dilution: LPS was detected in 2/12 (17% human samples in 2% serum, ranging from 3,436-4,736 pg/mL, compared to 9/12 (75% samples in 0.1% serum, ranging from 123 pg/mL -60,131 pg/mL (p = 0.016. In a separate validation cohort of HIV-HCV co-infected participants sampled at two different times on the same day, LPS measured in 0.2% plasma and with diazo-coupling was closely correlated between the first and second samples (R = 0.66, p<0.05.Undiluted serum and plasma mask LPS detection. The extent of MT may be substantially underestimated.

  2. Plasma container

    International Nuclear Information System (INIS)

    Ebisawa, Katsuyuki.

    1985-01-01

    Purpose: To enable to easily detect that the thickness of material to be abraded is reduced to an allowable limit from the outerside of the plasma container even during usual operation in a plasma vessel for a thermonuclear device. Constitution: A labelled material is disposed to the inside or rear face of constituent members of a plasma container undergoing the irradiation of plasma particles. A limiter plate to be abraded in the plasma container is composed of an armour member and heat removing plate, in which the armour member is made of graphite and heat-removing plate is made of copper. If the armour member is continuously abraded under the effect of sputtering due to plasma particles, silicon nitride embedded so far in the graphite at last appears on the surface of the limiter plate to undergo the impact shocks of the plasma particles. Accordingly, abrasion of the limiter material can be detected by a detector comprising gas chromatography and it can easily be detected from the outside of the plasma content even during normal operation. (Horiuchi, T.)

  3. Proteomic-Biostatistic Integrated Approach for Finding the Underlying Molecular Determinants of Hypertension in Human Plasma.

    Science.gov (United States)

    Gajjala, Prathibha R; Jankowski, Vera; Heinze, Georg; Bilo, Grzegorz; Zanchetti, Alberto; Noels, Heidi; Liehn, Elisa; Perco, Paul; Schulz, Anna; Delles, Christian; Kork, Felix; Biessen, Erik; Narkiewicz, Krzysztof; Kawecka-Jaszcz, Kalina; Floege, Juergen; Soranna, Davide; Zidek, Walter; Jankowski, Joachim

    2017-08-01

    Despite advancements in lowering blood pressure, the best approach to lower it remains controversial because of the lack of information on the molecular basis of hypertension. We, therefore, performed plasma proteomics of plasma from patients with hypertension to identify molecular determinants detectable in these subjects but not in controls and vice versa. Plasma samples from hypertensive subjects (cases; n=118) and controls (n=85) from the InGenious HyperCare cohort were used for this study and performed mass spectrometric analysis. Using biostatistical methods, plasma peptides specific for hypertension were identified, and a model was developed using least absolute shrinkage and selection operator logistic regression. The underlying peptides were identified and sequenced off-line using matrix-assisted laser desorption ionization orbitrap mass spectrometry. By comparison of the molecular composition of the plasma samples, 27 molecular determinants were identified differently expressed in cases from controls. Seventy percent of the molecular determinants selected were found to occur less likely in hypertensive patients. In cross-validation, the overall R 2 was 0.434, and the area under the curve was 0.891 with 95% confidence interval 0.8482 to 0.9349, P hypertensive patients were found to be -2.007±0.3568 and 3.383±0.2643, respectively, P hypertensives and normotensives. The identified molecular determinants may be the starting point for further studies to clarify the molecular causes of hypertension. © 2017 American Heart Association, Inc.

  4. Unsuccessful Detection of Plant MicroRNAs in Beer, Extra Virgin Olive Oil and Human Plasma After an Acute Ingestion of Extra Virgin Olive Oil.

    Science.gov (United States)

    Micó, Victor; Martín, Roberto; Lasunción, Miguel A; Ordovás, Jose M; Daimiel, Lidia

    2016-03-01

    The recent description of the presence of exogenous plant microRNAs from rice in human plasma had profound implications for the interpretation of microRNAs function in human health. If validated, these results suggest that food should not be considered only as a macronutrient and micronutrient supplier but it could also be a way of genomic interchange between kingdoms. Subsequently, several studies have tried to replicate these results in rice and other plant foods and most of them have failed to find plant microRNAs in human plasma. In this scenario, we aimed to detect plant microRNAs in beer and extra virgin olive oil (EVOO)--two plant-derived liquid products frequently consumed in Spain--as well as in human plasma after an acute ingestion of EVOO. Our hypothesis was that microRNAs present in beer and EVOO raw material could survive manufacturing processes, be part of these liquid products, be absorbed by human gut and circulate in human plasma. To test this hypothesis, we first optimized the microRNA extraction protocol to extract microRNAs from beer and EVOO, and then tried to detect microRNAs in those samples and in plasma samples of healthy volunteers after an acute ingestion of EVOO.

  5. Detection and quantitation of twenty-seven cytokines, chemokines and growth factors pre- and post-high abundance protein depletion in human plasma

    Directory of Open Access Journals (Sweden)

    Seong-Beom Ahn

    2014-06-01

    Full Text Available Cytokines, chemokines and growth factors (CCGFs in human plasma are analyzed for identification of biomarkers. However concentrations of CCGFs are very low; it is difficult to identify and quantify low abundance proteins in the presence of the high abundance proteins (HAPs unless HAPs are removed prior to analysis. However, there is a concern that the low abundance proteins such as CCGFs may also be removed during the HAP depletion process. In this study, we have examined whether or not depletion of the HAPs enhances detection of the CCGFs by immuno-assays. Top 14 HAPs were depleted from 10 healthy volunteers’ plasma using MARS-14 immuno-depletion column and a total of 27 CCGFs were analyzed by bead-based multiplexed immuno-assay. All 27 CCGFs were detected in neat plasma (NP, 25 were detected in flow through fraction (FT and 21 were detected in bound protein (BP fraction. Concentrations of 22 CCGFs were significantly higher in NP compared to FT and BP. Only one CCGF had higher concentration in FT compared to NP. The remaining 2 CCGFs were not different between NP and FT. It was counter-productive for the detection of 24 CCGFs after HAP removal, primarily due to post-depletion protein precipitation and/or re-suspension of pellets.

  6. Sensitivity of the activated partial thromboplastin time, the dilute Russell's viper venom time, and the kaolin clotting time for the detection of the lupus anticoagulant: a direct comparison using plasma dilutions.

    Science.gov (United States)

    Martin, B A; Branch, D W; Rodgers, G M

    1996-01-01

    Increasing dilutions of lupus anticoagulant (LA) plasmas from twelve patients were used to directly compare the sensitivity of four tests for LA. The tests evaluated were the modified Bell and Alton activated partial thromboplastin time (APTT), an APTT using a commercially prepared partial thromboplastin (Platelin LS APTT), a modified dilute Russell's viper venom time (DRVVT), and a modified kaolin clotting time (KCT). LAs were detected in all twelve plasmas by each of three tests and eleven of twelve plasmas in a fourth test when undiluted patient plasma was used. Repeating the tests after diluting the LA plasmas with normal platelet-free plasma (PFP) showed that the KCT was the most sensitive test for LA, detecting eleven of twelve LAs at a dilution of 10% patient plasma and ten of twelve LAs at a dilution of 5% patient plasma. The modified Bell and Alton APTT and the modified DRVVT had similar sensitivities at a patient plasma concentration of 10%, detecting seven of twelve and eight of twelve LAs, respectively. The Platelin LS APTT detected only four of twelve LAs at a patient plasma concentration of 10%. Our results indicate that the modified KCT is a sensitive method for the detection of LAs. The modified Bell and Alton APTT and the DRVVT were less sensitive.

  7. Human herpesvirus infections of the central nervous system: laboratory diagnosis based on DNA detection by nested PCR in plasma and cerebrospinal fluid samples.

    Science.gov (United States)

    Rimério, Carla Aparecida Tavares; De Oliveira, Renato Souza; de Almeida Bonatelli, Murilo Queiroz; Nucci, Anamarli; Costa, Sandra Cecília Botelho; Bonon, Sandra Helena Alves

    2015-04-01

    Infections of the central nervous systems (CNS) present a diagnostic problem for which an accurate laboratory diagnosis is essential. Invasive practices, such as cerebral biopsy, have been replaced by obtaining a polymerase chain reaction (PCR) diagnosis using cerebral spinal fluid (CSF) as a reference method. Tests on DNA extracted from plasma are noninvasive, thus avoiding all of the collateral effects and patient risks associated with CSF collection. This study aimed to determine whether plasma can replace CSF in nested PCR analysis for the detection of CNS human herpesvirus (HHV) diseases by analysing the proportion of patients whose CSF nested PCR results were positive for CNS HHV who also had the same organism identified by plasma nested PCR. In this study, CSF DNA was used as the "gold standard," and nested PCR was performed on both types of samples. Fifty-two patients with symptoms of nervous system infection were submitted to CSF and blood collection. For the eight HHV, one positive DNA result-in plasma and/or CSF nested PCR-was considered an active HHV infection, whereas the occurrence of two or more HHVs in the same sample was considered a coinfection. HHV infections were positively detected in 27/52 (51.9%) of the CSF and in 32/52 (61.5%) of the plasma, difference not significant, thus nested PCR can be performed on plasma instead of CSF. In conclusion, this findings suggest that plasma as a useful material for the diagnosis of cases where there is any difficulty to perform a CSF puncture. © 2015 Wiley Periodicals, Inc.

  8. Rapid determination of telmisartan in human plasma by HPLC using a monolithic column with fluorescence detection and its application to a bioequivalence study.

    Science.gov (United States)

    Zhang, He; Jiang, Yunyun; Wen, Jun; Zhou, Tingting; Fan, Guorong; Wu, Yutian

    2009-11-01

    A rapid HPLC method using a monolithic column with fluorescence detection has been developed for determination of telmisartan in human plasma. Sample preparation was done by protein precipitation with acetonitrile and naproxen was used as IS. The compounds were detected by fluorescence detection, using an excitation wavelength of 300 nm and emission wavelength of 385 nm. Calibration curves of telmisartan were linear in the range of 1-200 ng/mL. The assay was high throughput, sensitive and precise, and it was successfully applied to a bioequivalence study of two formulations of telmisartan.

  9. Determination of Four Anti-epileptic Drugs in Plasma Using Ultra Performance Liquid Chromatography with Mass Detection Technique.

    Science.gov (United States)

    Hassib, Sonia T; Hashem, Hanaa M A; Mahrouse, Marianne A; Mostafa, Eman A

    2018-04-10

    Status epilepticus (SE) is considered the second most frequent neurologic emergency. Its therapeutic management is performed using sequential anti-epileptic drug regimens. Diazepam (DIA), midazolam (MID), phenytoin (PHT) and phenobarbital (PB) are four drugs of different classes used sequentially in the management of SE. A sensitive, selective, accurate and precise method was developed and validated for simultaneous determination of the four anti-epileptic drugs in human plasma. Their separation and quantification were achieved using ultra performance liquid chromatography (UPLC) with mass detection using carbamazepine as internal standard (IS). For the first three drugs and IS, UPLC-MS/MS with electrospray ionization working in multiple reaction monitoring mode was used at the following transitions: m/z 285→193 for DIA, m/z 326→291 for MID, m/z 253→182 for PHT and m/z 237→194, 237→192 for IS. For the fourth drug (PB), molecular ion peak of PB [M+H] + at m/z 233 was used for its quantitation. The method was linear over concentration ranges of 5-500 ng/ml for DIA and MID and 0.25-20 μg/ml for PHT and PB, respectively. Bio-analytical validation of the developed method was carried out according to European Medicines Agency guidelines. The developed method can be applied for routine drug analysis, therapeutic drug monitoring and bioequivalence studies. This article is protected by copyright. All rights reserved.

  10. Determination of itopride hydrochloride in human plasma by RP-HPLC with fluorescence detection and its use in bioequivalence study.

    Science.gov (United States)

    Ma, Jing; Yuan, Li-Hua; Ding, Mei-Juan; Zhang, Jun; Zhang, Qing; Xu, Qun-Wei; Zhou, Xue-Min

    2009-03-01

    A sensitive, selective and simple method using a precipitation of protein with 10% perchloric acid, followed by high-performance liquid chromatography (HPLC) with fluorescence detection was developed for the determination of itopride hydrochloride in human plasma, using levofloxacin as the internal standard (IS). Chromatographic separation was obtained within 7.0 min using a reverse phase Hypersil BDS C(18) (250 mm x 4.6 mm, 5 microm) column and an isocratic mobile phase, constituting of a mixture of 0.1 mol/l ammonium acetate-methanol (30:70, v/v) flowing at 1.1 ml/min. The excitation and emission wavelengths were set at 304 and 344 nm, respectively. The method was validated over the concentration range of 5 ng/ml to 1000.0 ng/ml. The lower limit of quantitation (LLOQ) was 5 ng/ml. The extractive recovery of itopride hydrochloride from the biological matrix was more than 80.77%. The intra-day accuracy of the drug containing serum samples was more than 82.94% with a precision of 2.81-4.37%. The inter-day accuracy was 82.91% or more, with a precision of 6.89-9.54%. The limit we have used (70-143%) is based on the local regulatory authority (SFDA). The developed method was validated and successfully applied to bioequivalence studies of itopride hydrochloride in healthy male volunteers.

  11. Real-time breath analysis with active capillary plasma ionization-ambient mass spectrometry.

    Science.gov (United States)

    Bregy, Lukas; Sinues, Pablo Martinez-Lozano; Nudnova, Maryia M; Zenobi, Renato

    2014-06-01

    On-line analysis of exhaled human breath is a growing area in analytical science, for applications such as fast and non-invasive medical diagnosis and monitoring. In this work, we present a novel approach based on ambient ionization of compounds in breath and subsequent real-time mass spectrometric analysis. We introduce a plasma ionization source for this purpose, which has no need for additional gases, is very small, and is easily interfaced with virtually any commercial atmospheric pressure ionization mass spectrometer (API-MS) without major modifications. If an API-MS instrument exists in a laboratory, the cost to implement this technology is only around [Formula: see text]500, far less than the investment for a specialized mass spectrometric system designed for volatile organic compounds (VOCs) analysis. In this proof-of-principle study we were able to measure mass spectra of exhaled human breath and found these to be comparable to spectra obtained with other electrospray-based methods. We detected over 100 VOCs, including relevant metabolites like fatty acids, with molecular weights extending up to 340 Da. In addition, we were able to monitor the time-dependent evolution of the peaks and show the enhancement of the metabolism after a meal. We conclude that this approach may complement current methods to analyze breath or other types of vapors, offering an affordable option to upgrade any pre-existing API-MS to a real-time breath analyzer.

  12. Rapid Preparation of a Plasma Membrane Fraction: Western Blot Detection of Translocated Glucose Transporter 4 from Plasma Membrane of Muscle and Adipose Cells and Tissues.

    Science.gov (United States)

    Yamamoto, Norio; Yamashita, Yoko; Yoshioka, Yasukiyo; Nishiumi, Shin; Ashida, Hitoshi

    2016-08-01

    Membrane proteins account for 70% to 80% of all pharmaceutical targets, indicating their clinical relevance and underscoring the importance of identifying differentially expressed membrane proteins that reflect distinct disease properties. The translocation of proteins from the bulk of the cytosol to the plasma membrane is a critical step in the transfer of information from membrane-embedded receptors or transporters to the cell interior. To understand how membrane proteins work, it is important to separate the membrane fraction of cells. This unit provides a protocol for rapidly obtaining plasma membrane fractions for western blot analysis. © 2016 by John Wiley & Sons, Inc. Copyright © 2016 John Wiley & Sons, Inc.

  13. Spectrometric properties and radiation damage of BGO crystals

    Science.gov (United States)

    Kim, Gen C.; Gasanov, Eldar M.

    1997-07-01

    Spectrometric properties, such as light output, energy resolution BGO crystals before and after (superscript 60)Co gamma-ray (dose 10(superscript 4) - 10(superscript 6) R) and neutron irradiation (fluence 10(superscript 14) cm(superscript -2)) are investigated. Condition for degradation of spectrometric properties and their recovering after irradiation are studied. The energy spectrum of the photons emitted from BGO crystals irradiated with neutron fluence contains the long living background peak which is caused by self-irradiation with radioactive isotopes produced in the crystals. The defect production was studied in crystals under the high dose gamma-irradiation with (superscript 60)Co isotope. It was found that after doses above 10(superscript 8) R the color center at 365 nm and doses higher than 10(superscript 9) R a wide absorption band in the region of 300 - 350 nm occur. Comparison of these results with those of reactor irradiation has shown that under the high dose gamma-irradiation the structure defect production takes place.

  14. In situ probing of cholesterol in astrocytes at the single-cell level using laser desorption ionization mass spectrometric imaging with colloidal silver.

    Science.gov (United States)

    Perdian, D C; Cha, Sangwon; Oh, Jisun; Sakaguchi, Donald S; Yeung, Edward S; Lee, Young Jin

    2010-04-30

    Mass spectrometric imaging has been utilized to localize individual astrocytes and to obtain cholesterol populations at the single-cell level in laser desorption ionization (LDI) with colloidal silver. The silver ion adduct of membrane-bound cholesterol was monitored to detect individual cells. Good correlation between mass spectrometric and optical images at different cell densities indicates the ability to perform single-cell studies of cholesterol abundance. The feasibility of quantification is confirmed by the agreement between the LDI-MS ion signals and the results from a traditional enzymatic fluorometric assay. We propose that this approach could be an effective tool to study chemical populations at the cellular level. Published in 2010 by John Wiley & Sons, Ltd.

  15. Factors influencing cerebrospinal fluid and plasma HIV-1 RNA detection rate in patients with and without opportunistic neurological disease during the HAART era

    Directory of Open Access Journals (Sweden)

    Aleixo Agdemir W

    2007-12-01

    Full Text Available Abstract Background In the central nervous system, HIV replication can occur relatively independent of systemic infection, and intrathecal replication of HIV-1 has been observed in patients with HIV-related and opportunistic neurological diseases. The clinical usefulness of HIV-1 RNA detection in the cerebrospinal fluid (CSF of patients with opportunistic neurological diseases, or the effect of opportunistic diseases on CSF HIV levels in patients under HAART has not been well defined. We quantified CSF and plasma viral load in HIV-infected patients with and without different active opportunistic neurological diseases, determined the characteristics that led to a higher detection rate of HIV RNA in CSF, and compared these two compartments. Methods A prospective study was conducted on 90 HIV-infected patients submitted to lumbar puncture as part of a work-up for suspected neurological disease. Seventy-one patients had active neurological diseases while the remaining 19 did not. Results HIV-1 RNA was quantified in 90 CSF and 70 plasma samples. The HIV-1 RNA detection rate in CSF was higher in patients with neurological diseases, in those with a CD4 count lower than 200 cells/mm3, and in those not receiving antiretroviral therapy, as well as in patients with detectable plasma HIV-1 RNA. Median viral load was lower in CSF than in plasma in the total population, in patients without neurological diseases, and in patients with toxoplasmic encephalitis, while no significant difference between the two compartments was observed for patients with cryptococcal meningitis and HIV-associated dementia. CSF viral load was lower in patients with cryptococcal meningitis and neurotoxoplasmosis under HAART than in those not receiving HAART. Conclusion Detection of HIV-1 RNA in CSF was more frequent in patients with neurological disease, a CD4 count lower than 200 cells/mm3 and detectable plasma HIV-1. Median HIV-1 RNA levels were generally lower in CSF than in

  16. Treatment of infants with congenital toxoplasmosis: tolerability and plasma concentrations of sulfadiazine and pyrimethamine

    DEFF Research Database (Denmark)

    Schmidt, Dorte Remmer; Høgh, Birthe; Andersen, O

    2006-01-01

    A-antibodies on 3 mm blood spots collected from phenylketonuria [PKU cards (Guthrie cards)]. Toxoplasma-infected children received 3 months continuous treatment with 50–100 mg/kg per day sulfadiazine in two separate administrations and 1 mg/kg per day pyrimethamine after a 1-day loading dose of 2 mg/kg, and folinic...... acid 7.5 mg was administered twice weekly. Blood cell counts and body weight were recorded during follow-up. The plasma concentrations of pyrimethamine and sulfadiazine were analysed in a subgroup of seven children, using high performance liquid chromatography with ultraviolet and mass spectrometric...... detection. Of 48 infants, 41 completed the treatment without change in schedule. Six infants had neutrophil counts below 0.5×109/l, and one infant had an elevated bilirubin value. Twenty-nine children were tested by a series of neutrophil counts during treatment. The neutrophil count was 0.5×109/l or lower...

  17. Exploratory Study of Total and Free Prednisolone Plasma Exposure and Cushingoid Appearance, Quality of Life and Biochemical Toxicity in Adult Male Kidney Transplant Recipients

    DEFF Research Database (Denmark)

    Bergmann, Troels K; Isbel, Nicole M; Ostini, Remo

    2015-01-01

    relationships between prednisolone exposure and adverse effects. METHODS: Male kidney transplant recipients were recruited for serial blood sampling and assessment of glucocorticoid-related adverse effects including dyslipidaemia, abnormal body fat distribution, Cushingoid appearance and impaired quality...... of life. Total and free prednisolone plasma concentrations were determined using ultra-high-performance liquid chromatography with tandem mass spectrometric detection. Prednisolone exposure was estimated using a limited sampling strategy. RESULTS: Fifty-six patients were recruited. Patients had a mean age...... of 54 years and median time post-transplantation of 75 months. Median prednisolone dose was 5 mg. Mean area under the plasma concentration-time curve was 2390 nmol h/L (±580) (SD) and 175 nmol h/L (±78) for total and free prednisolone, respectively. Waist to upper arm circumference ratio was positively...

  18. Development of a gas-cylinder-free plasma desorption/ionization system for on-site detection of chemical warfare agents.

    Science.gov (United States)

    Iwai, Takahiro; Kakegawa, Ken; Aida, Mari; Nagashima, Hisayuki; Nagoya, Tomoki; Kanamori-Kataoka, Mieko; Miyahara, Hidekazu; Seto, Yasuo; Okino, Akitoshi

    2015-06-02

    A gas-cylinder-free plasma desorption/ionization system was developed to realize a mobile on-site analytical device for detection of chemical warfare agents (CWAs). In this system, the plasma source was directly connected to the inlet of a mass spectrometer. The plasma can be generated with ambient air, which is drawn into the discharge region by negative pressure in the mass spectrometer. High-power density pulsed plasma of 100 kW could be generated by using a microhollow cathode and a laboratory-built high-intensity pulsed power supply (pulse width: 10-20 μs; repetition frequency: 50 Hz). CWAs were desorbed and protonated in the enclosed space adjacent to the plasma source. Protonated sample molecules were introduced to the mass spectrometer by airflow through the discharge region. To evaluate the analytical performance of this device, helium and air plasma were directly irradiated to CWAs in the gas-cylinder-free plasma desorption/ionization system and the protonated molecules were analyzed by using an ion-trap mass spectrometer. A blister agent (nitrogen mustard 3) and nerve gases [cyclohexylsarin (GF), tabun (GA), and O-ethyl S-2-N,N-diisopropylaminoethyl methylphosphonothiolate (VX)] in solution in n-hexane were applied to the Teflon rod and used as test samples, after solvent evaporation. As a result, protonated molecules of CWAs were successfully observed as the characteristic ion peaks at m/z 204, 181, 163, and 268, respectively. In air plasma, the limits of detection were estimated to be 22, 20, 4.8, and 1.0 pmol, respectively, which were lower than those obtained with helium plasma. To achieve quantitative analysis, calibration curves were made by using CWA stimulant dipinacolyl methylphosphonate as an internal standard; straight correlation lines (R(2) = 0.9998) of the peak intensity ratios (target per internal standard) were obtained. Remarkably, GA and GF gave protonated dimer ions, and the ratios of the protonated dimer ions to the protonated

  19. Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography-ultraviolet detection to determination of opium alkaloids in human plasma.

    Science.gov (United States)

    Ahmadi-Jouibari, Toraj; Fattahi, Nazir; Shamsipur, Mojtaba; Pirsaheb, Meghdad

    2013-11-01

    A novel, simple, rapid and sensitive dispersive liquid-liquid microextraction method based on the solidification of floating organic drop (DLLME-SFO) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was used to determine opium alkaloids in human plasma. During the extraction procedure, plasma protein was precipitated by using a mixture of zinc sulfate solution and acetonitrile. Some effective parameters on extraction were studied and optimized. Under the optimum conditions (extraction solvent: 30.0 μl 1-undecanol; disperser solvent: 470 μl acetone; pH: 9; salt addition: 1%(w/v) NaCl and extraction time: 0.5 min), calibration curves are linear in the range of 1.5-1000 μgl(-1) and limit of detections (LODs) are in the range of 0.5-5 μgl(-1). The relative standard deviations (RSDs) for 100 μgl(-1) of morphine and codeine, 10.0 μgl(-1) of papaverine and 20.0 μgl(-1) of noscapine in diluted human plasma are in the range of 4.3-7.4% (n=5). Finally, the method was successfully applied in the determination of opium alkaloids in the actual human plasma samples. The relative recoveries of plasma samples spiked with alkaloids are 88-110.5%. The obtained results show that DLLME-SFO combined with HPLC-UV is a fast and simple method for the determination of opium alkaloids in human plasma. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Preparation of magnetic ODS-PAN thin-films for microextraction of quetiapine and clozapine in plasma and urine samples followed by HPLC-UV detection.

    Science.gov (United States)

    Li, Dan; Zou, Juan; Cai, Pei-Shan; Xiong, Chao-Mei; Ruan, Jin-Lan

    2016-06-05

    In this study, conventional thin-film microextraction (TFME) was endowed with magnetic by introducing superparamagnetic SiO2@Fe3O4 nanoparticles in thin-films. Novel magnetic octadecylsilane (ODS)-polyacrylonitrile (PAN) thin-films were prepared by spraying, and used for the microextraction of quetiapine and clozapine in plasma and urine samples, followed by the detection of HPLC-UV. The influencing factors on the extraction efficiency of magnetic ODS-PAN TFME, including pH, extraction time, desorption solvent, desorption time, and ion strength were investigated systematically. Under the optimal conditions, both analytes showed good linearity over ranges of 0.070-9.000μgmL(-1) and 0.012-9.000μgmL(-1) in plasma and urine samples, respectively, with correlation coefficients (R(2)) above 0.9990. Limits of detection (LODs) for quetiapine in plasma and urine samples were 0.013 and 0.003μgmL(-1), respectively. LODs for clozapine in plasma and urine samples were 0.015 and 0.003μgmL(-1), respectively. The relative standard deviations (RSDs) for quetiapine and clozapine were less than 9.23%. After the validation, the protocol was successfully applied for the determination of quetiapine and clozapine in patients' plasma and urine samples with satisfactory recoveries between 99-110%. The proposed magnetic ODS-PAN TFME was very simple, fast and easy to handle. It showed high potential as a powerful pretreatment technology for routine therapeutic drug monitoring (TDM) in plasma and urine samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. A newly validated high-performance liquid chromatography method with diode array ultraviolet detection for analysis of the antimalarial drug primaquine in the blood plasma.

    Science.gov (United States)

    Carmo, Ana Paula Barbosa do; Borborema, Manoella; Ribeiro, Stephan; De-Oliveira, Ana Cecilia Xavier; Paumgartten, Francisco Jose Roma; Moreira, Davyson de Lima

    2017-01-01

    Primaquine (PQ) diphosphate is an 8-aminoquinoline antimalarial drug with unique therapeutic properties. It is the only drug that prevents relapses of Plasmodium vivax or Plasmodium ovale infections. In this study, a fast, sensitive, cost-effective, and robust method for the extraction and high-performance liquid chromatography with diode array ultraviolet detection (HPLC-DAD-UV ) analysis of PQ in the blood plasma was developed and validated. After plasma protein precipitation, PQ was obtained by liquid-liquid extraction and analyzed by HPLC-DAD-UV with a modified-silica cyanopropyl column (250mm × 4.6mm i.d. × 5μm) as the stationary phase and a mixture of acetonitrile and 10mM ammonium acetate buffer (pH = 3.80) (45:55) as the mobile phase. The flow rate was 1.0mL·min-1, the oven temperature was 50OC, and absorbance was measured at 264nm. The method was validated for linearity, intra-day and inter-day precision, accuracy, recovery, and robustness. The detection (LOD) and quantification (LOQ) limits were 1.0 and 3.5ng·mL-1, respectively. The method was used to analyze the plasma of female DBA-2 mice treated with 20mg.kg-1 (oral) PQ diphosphate. By combining a simple, low-cost extraction procedure with a sensitive, precise, accurate, and robust method, it was possible to analyze PQ in small volumes of plasma. The new method presents lower LOD and LOQ limits and requires a shorter analysis time and smaller plasma volumes than those of previously reported HPLC methods with DAD-UV detection. The new validated method is suitable for kinetic studies of PQ in small rodents, including mouse models for the study of malaria.

  2. A newly validated high-performance liquid chromatography method with diode array ultraviolet detection for analysis of the antimalarial drug primaquine in the blood plasma

    Directory of Open Access Journals (Sweden)

    Ana Paula Barbosa do Carmo

    Full Text Available Abstract INTRODUCTION: Primaquine (PQ diphosphate is an 8-aminoquinoline antimalarial drug with unique therapeutic properties. It is the only drug that prevents relapses of Plasmodium vivax or Plasmodium ovale infections. In this study, a fast, sensitive, cost-effective, and robust method for the extraction and high-performance liquid chromatography with diode array ultraviolet detection (HPLC-DAD-UV analysis of PQ in the blood plasma was developed and validated. METHODS: After plasma protein precipitation, PQ was obtained by liquid-liquid extraction and analyzed by HPLC-DAD-UV with a modified-silica cyanopropyl column (250mm × 4.6mm i.d. × 5μm as the stationary phase and a mixture of acetonitrile and 10mM ammonium acetate buffer (pH = 3.80 (45:55 as the mobile phase. The flow rate was 1.0mL·min-1, the oven temperature was 50OC, and absorbance was measured at 264nm. The method was validated for linearity, intra-day and inter-day precision, accuracy, recovery, and robustness. The detection (LOD and quantification (LOQ limits were 1.0 and 3.5ng·mL-1, respectively. The method was used to analyze the plasma of female DBA-2 mice treated with 20mg.kg-1 (oral PQ diphosphate. RESULTS: By combining a simple, low-cost extraction procedure with a sensitive, precise, accurate, and robust method, it was possible to analyze PQ in small volumes of plasma. The new method presents lower LOD and LOQ limits and requires a shorter analysis time and smaller plasma volumes than those of previously reported HPLC methods with DAD-UV detection. CONCLUSIONS: The new validated method is suitable for kinetic studies of PQ in small rodents, including mouse models for the study of malaria.

  3. Loading of deuterium and helium by Pilot-PSI plasma and their detection by in-situ LIBS

    NARCIS (Netherlands)

    Piip, K.; van der Meiden, H. J.; Bystrov, K.; Hämarik, L.; Karhunen, J.; Aints, M.; Laan, M.; Paris, P.; Seemen, H.; Hakola, A.; Brezinsek, S.

    2017-01-01

    Laser-induced breakdown spectroscopy (LIBS) is a promising method for quantifying the fuel content of the plasma-facing components of ITER both in between plasma discharges (in-situ) and after maintenance operations. The aim of the present study is to test the applicability of in-situ LIBS for

  4. QUANTITATIVE-DETERMINATION OF THE DOPAMINE AGONIST LISURIDE IN PLASMA USING HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY WITH FLUORESCENCE DETECTION

    NARCIS (Netherlands)

    WOLTHERS, BG; KAMERBEEK, WDJV; VANBEUSEKOM, CM; ELSHOF, F; BUITENHUIS, AWD; BRUNT, EPR; LAKKE, JPWF

    1993-01-01

    An HPLC method for the determination of lisuride hydrogen maleate in plasma is described. After addition of ergotamine tartrate as internal standard, plasma is extracted with diethyl ether. Following evaporation of the solvent and redissolving in methanol the extract is injected on a silica HPLC

  5. A simple and sensitive HPLC method for analysis of imipramine in human plasma with UV detection and liquid-liquid extraction: Application in bioequivalence studies.

    Science.gov (United States)

    Rezazadeh, Mahboubeh; Emami, Jaber

    2016-01-01

    High-performance liquid chromatography (HPLC) methods employing ultraviolet (UV) detector are not sufficiently sensitive to measure the low plasma concentrations following single oral dose of imipramine. Therefore, in the present study a simple, rapid and yet sensitive HPLC method with UV detection was developed and validated for quantitation of imipramine in human plasma samples. An efficient liquid-liquid extraction (LLE) of imipramine from plasma with the mixture of hexane/isoamyl alcohol (98:2) and back extraction of the drug in acidic medium concomitant with evaporation of organic phase allowed the use of UV detector to conveniently measure plasma levels of this compound as low level as 3 ng/ml. Separation was achieved on a μ-Bondapak C18 HPLC column using sodium hydrogen phosphate solution (0.01 M)/acetonitrile (60/40 v/v) at pH 3.5 ± 0.1 at 1.5 ml/min. Trimipramine was used as the internal standard for analysis of plasma samples. The retention times for imipramine and trimipramine were 4.3 and 5.2 min, respectively. Calibration curve was linear in the range of 3-40 ng/ml using human plasma with the average extraction recovery of 85 ± 5%. Imipramine was found to be stable in plasma samples with no evidence of degradation during three freeze-thaw cycles and three months storage at -70°C. The current validated method was finally applied in bioequivalence studies of two different imipramine products according to a standard two-way crossover design with a two weeks washout period.

  6. The potential of organic (electrospray- and atmospheric pressure chemical ionisation) mass spectrometric techniques coupled to liquid-phase separation for speciation analysis.

    Science.gov (United States)

    Rosenberg, Erwin

    2003-06-06

    The use of mass spectrometry based on atmospheric pressure ionisation techniques (atmospheric pressure chemical ionisation, APCI, and electrospray ionisation, ESI) for speciation analysis is reviewed with emphasis on the literature published in and after 1999. This report accounts for the increasing interest that atmospheric pressure ionisation techniques, and in particular ESI, have found in the past years for qualitative and quantitative speciation analysis. In contrast to element-selective detectors, organic mass spectrometric techniques provide information on the intact metal species which can be used for the identification of unknown species (particularly with MS-MS detection) or the confirmation of the actual presence of species in a given sample. Due to the complexity of real samples, it is inevitable in all but the simplest cases to couple atmospheric pressure MS detection to a separation technique. Separation in the liquid phase (capillary electrophoresis or liquid chromatography in reversed phase, ion chromatographic or size-exclusion mode) is particularly suitable since the available techniques cover a very wide range of analyte polarities and molecular mass. Moreover, derivatisation can normally be avoided in liquid-phase separation. Particularly in complex environmental or biological samples, separation in one dimension is not sufficient for obtaining adequate resolution for all relevant species. In this case, multi-dimensional separation, based on orthogonal separation techniques, has proven successful. ESI-MS is also often used in parallel with inductively coupled plasma MS detection. This review is structured in two parts. In the first, the fundamentals of atmospheric pressure ionisation techniques are briefly reviewed. The second part of the review discusses recent applications including redox species, use of ESI-MS for structural elucidation of metal complexes, characterisation and quantification of small organometallic species with relevance to

  7. Detection of x-rays emitted from a plasma focus device with energy of 2.8 KJ, and its applications in plasma diagnostic and radiography

    International Nuclear Information System (INIS)

    AL-Hawat, Sh.; Akel, M.

    2011-06-01

    The local plasma focus device was modified by replacing the old capacitors (25μF,20 kV ,1.43μH ) and the open spark gap by new capacitors with (25μF,20 kV ,200 nH ) and a new closed spark gap, so instead of a current of 50 kA as a maximum value we obtained a maximum current about 120 kA. The modified device is capable now to generate x-rays, which was confirmed by taking some radiographies for metallic pieces, electronic elements and others . In addition to that some diagnostics were carried out on the device using Ohm voltage divider to record voltage curves, Rogovskii coil for measuring the current, and five channel diodes to evaluate the temporal evolution of x-rays generated in the device working on argon vs. pressure and voltage. The generation of the soft x-ray emission in a low energy 2.8 kJ plasma focus device operated with argon using a detector of five PIN-Si BPX-65 diodes filtered with different foils of Mylar, Al and Cu. Spectral analysis using the recorded x-ray signals ratio method shows that there are two components in the x-ray emissions: one arising from the focused argon plasma with temperature of 2.5 keV and the other arising from the electron beam activity on copper anode, where the second component is predominant in most of investigated experiments due to the used of solid anode. Numerical experiments were carried out using five phases radiative Lee model RADPF5.15d-dd with N 2 , O 2 , Ar, Ne gases on plasma focus device AECS PF1-2 (or PF SY1-2) for its characterization and soft x-ray optimization. (author)

  8. Analysis of 6-mercaptopurine in human plasma with a high-performance liquid chromatographic method including post-column derivatization and fluorimetric detection.

    Science.gov (United States)

    Jonkers, R E; Oosterhuis, B; ten Berge, R J; van Boxtel, C J

    1982-12-10

    A relatively simple assay with improved reliability and sensitivity for measuring levels of 6-mercaptopurine in human plasma is presented. After extraction of the compound and the added internal standard with phenyl mercury acetate, samples were separated by ion-pair reversed-phase high-performance liquid chromatography. On-line the analytes were oxidized to fluorescent products and detected in a flow-fluorimeter. The within-day coefficient of variation was 3.8% at a concentration of 25 ng/ml. The lower detection limit was 2 ng/ml when 1.0 ml of plasma was used. Mercaptopurine concentration versus time curves of two subjects after a single oral dose of azathioprine are shown.

  9. Spectrometric and Voltammetric Analysis of Urease – Nickel Nanoelectrode as an Electrochemical Sensor

    Directory of Open Access Journals (Sweden)

    Rene Kizek

    2007-07-01

    Full Text Available Urease is the enzyme catalyzing the hydrolysis of urea into carbon dioxide andammonia. This enzyme is substrate-specific, which means that the enzyme catalyzes thehydrolysis of urea only. This feature is a basic diagnostic criterion used in thedetermination of many bacteria species. Most of the methods utilized for detection ofurease are based on analysis of its enzyme activity – the hydrolysis of urea. The aim of thiswork was to detect urease indirectly by spectrometric method and directly by voltammetricmethods. As spectrometric method we used is called indophenol assay. The sensitivity ofdetection itself is not sufficient to analyse the samples without pre-concentration steps.Therefore we utilized adsorptive transfer stripping technique coupled with differential pulse voltammetry to detect urease. The influence of accumulation time, pH of supporting electrolyte and concentration of urease on the enzyme peak height was investigated. Under the optimized experimental conditions (0.2 M acetate buffer pH 4.6 and accumulation time of 120 s the detection limit of urease evaluated as 3 S/N was 200 ng/ml. The activity of urease enzyme depends on the presence of nickel. Thus the influence of nickel(II ions on electrochemical response of the enzyme was studied. Based on the results obtained the interaction of nickel(II ions and urease can be determined using electrochemical methods. Therefore we prepared Ni nanoelectrodes to measure urease. The Ni nanoelectrodes was analysed after the template dissolution by scanning electron microscopy. The results shown vertically aligned Ni nanopillars almost covered the electrode surface, whereas the defect places are minor and insignificant in comparison with total electrode surface. We were able to not only detect urease itself but also to distinguish its native and denatured form.

  10. Sensitivity of whole-body CT and MRI versus projection radiography in the detection of osteolyses in patients with monoclonal plasma cell disease

    Energy Technology Data Exchange (ETDEWEB)

    Wolf, Maya B., E-mail: m.mueller-wolf@dkfz.de [Department of Diagnostic and Interventional Radiology, University Hospital Heidelberg, Im Neuenheimer Feld 110, 69120 Heidelberg Germany (Germany); Department of Radiology, German Cancer Research Center (Dkfz), Im Neuenheimer Feld 280, 69120 Heidelberg (Germany); Murray, Fritz, E-mail: fritz.murray@hotmail.de [Department of Diagnostic and Interventional Radiology, University Hospital Heidelberg, Im Neuenheimer Feld 110, 69120 Heidelberg Germany (Germany); Kilk, Kerstin, E-mail: k_fechtner@hotmail.com [Department of Diagnostic and Interventional Radiology, University Hospital Heidelberg, Im Neuenheimer Feld 110, 69120 Heidelberg Germany (Germany); Hillengass, Jens, E-mail: jens.hillengass@med.uni-heidelberg.de [Department of Haematology, Oncology, Rheumatology, University Hospital Heidelberg, Im Neuenheimer Feld 410, 69120 Heidelberg (Germany); Delorme, Stefan, E-mail: s.delorme@dkfz-heidelberg.de [Department of Radiology, German Cancer Research Center (Dkfz), Im Neuenheimer Feld 280, 69120 Heidelberg (Germany); Heiss, Christiane, E-mail: c.heiss@dkfz-heidelberg.de [Department of Biostatistics, German Cancer Research Center (Dkfz), Im Neuenheimer Feld 280, 69120 Heidelberg (Germany); Neben, Kai, E-mail: k.neben@klinikum-mittelbaden.de [Department of Haematology, Oncology, Rheumatology, University Hospital Heidelberg, Im Neuenheimer Feld 410, 69120 Heidelberg (Germany); Goldschmidt, Hartmut, E-mail: hartmut.goldschmidt@med.uni-heidelberg.de [Department of Haematology, Oncology, Rheumatology, University Hospital Heidelberg and National Center for Tumour Diseases, Im Neuenheimer Feld 410, 69120 Heidelberg (Germany); Kauczor, Hans-Ulrich, E-mail: hu.kauczor@med.uni-heidelberg.de [Department of Diagnostic and Interventional Radiology, University Hospital Heidelberg, Im Neuenheimer Feld 110, 69120 Heidelberg Germany (Germany); and others

    2014-07-15

    Purpose: To compare sensitivity of whole-body Computed Tomography (wb-CT) and whole-body Magnetic Resonance Imaging (wb-MRI) with Projection Radiography (PR) regarding each method's ability to detect osteolyses in patients with monoclonal plasma cell disease. Patients and methods: The bone status of 171 patients was evaluated. All patients presented with multiple myeloma (MM) of all stages, monoclonal gammopathy of unknown significance (MGUS) or solitary plasmacytoma. Two groups were formed. Group A consisted of 52 patients (26 females, 26 males) with an average age of 62 years (range, 45–89 years) who received, both, PR and wb-CT as part of their diagnostic work-up. Group B comprised 119 patients (58 females, 61 males) averaging 57 years of age (range, 20–80 years) who received, both, PR and wb-MRI. Two experienced radiologists were blinded regarding the disease status and assessed the number and location of osteolyses in consensus. A distinction was made between axial and extra-axial lesions. Results: In group A, wb-CT revealed osteolyses in 12 patients (23%) that were not detected in PR. CT was superior in detecting lesions in patients with osteopenia and osteoporosis. Compared with PR, wb-CT was significantly more sensitive in detecting osteolyses than PR (p < 0.001). This was particularly true for axial lesions. Additionally, CT revealed clinically relevant incidental findings in 33 patients (63%). In group B, wb-MRI revealed lesions in 19 patients (16%) that were not detected in PR. All lesions detected by PR were also detected by wb-MRI and wb-CT. Wb-MRI and wb-CT are each superior to PR in detecting axial lesions. Conclusion: Wb-CT can detect 23% more focal lesions than PR, especially in the axial skeleton. Therefore, this imaging method should be preferred over PR in the diagnostic work-up and staging of patients with monoclonal plasma cell disease.

  11. The theoretical study of full spectrum analysis method for airborne gamma-ray spectrometric data

    International Nuclear Information System (INIS)

    Ni Weichong

    2011-01-01

    Spectra of airborne gamma-ray spectrometry was found to be the synthesis of spectral components of radioelement sources by analyzing the constitution of radioactive sources for airborne gamma-ray spectrometric survey and establishing the models of gamma-ray measurement. The mathematical equation for analysising airborne gamma-ray full spectrometric data can be expressed into matrix and related expansions were developed for the mineral resources exploration, environmental radiation measurement, nuclear emergency monitoring, and so on. Theoretical study showed that the atmospheric radon could be directly computed by airborne gamma-ray spectrometric data with full spectrum analysis without the use of the accessional upward-looking detectors. (authors)

  12. Protein Detection Using the Multiplexed Proximity Extension Assay (PEA) from Plasma and Vaginal Fluid Applied to the Indicating FTA Elute Micro Card™

    Science.gov (United States)

    Berggrund, Malin; Ekman, Daniel; Gustavsson, Inger; Sundfeldt, Karin; Olovsson, Matts; Enroth, Stefan; Gyllensten, Ulf

    2016-01-01

    The indicating FTA elute micro card™ has been developed to collect and stabilize the nucleic acid in biological samples and is widely used in human and veterinary medicine and other disciplines. This card is not recommended for protein analyses, since surface treatment may denature proteins. We studied the ability to analyse proteins in human plasma and vaginal fluid as applied to the indicating FTA elute micro card™ using the sensitive proximity extension assay (PEA). Among 92 proteins in the Proseek Multiplex Oncology Iv2 panel, 87 were above the limit of detection (LOD) in liquid plasma and 56 among 92 above LOD in plasma applied to FTA cards. Washing and protein elution protocols were compared to identify an optimal method. Liquid-based cytology samples showed a lower number of proteins above LOD than FTA cards with vaginal fluid samples applied. Our results demonstrate that samples applied to the indicating FTA elute micro card™ are amendable to protein analyses, given that a sensitive protein detection assay is used. The results imply that biological samples applied to FTA cards can be used for DNA, RNA and protein detection. PMID:28936257

  13. Protein Detection Using the Multiplexed Proximity Extension Assay (PEA from Plasma and Vaginal Fluid Applied to the Indicating FTA Elute Micro Card™

    Directory of Open Access Journals (Sweden)

    Malin Berggrund

    2016-01-01

    Full Text Available The indicating FTA elute micro card™ has been developed to collect and stabilize the nucleic acid in biological samples and is widely used in human and veterinary medicine and other disciplines. This card is not recommended for protein analyses, since surface treatment may denature proteins. We studied the ability to analyse proteins in human plasma and vaginal fluid as applied to the indicating FTA elute micro card™ using the sensitive proximity extension assay (PEA. Among 92 proteins in the Proseek Multiplex Oncology Iv2 panel, 87 were above the limit of detection (LOD in liquid plasma and 56 among 92 above LOD in plasma applied to FTA cards. Washing and protein elution protocols were compared to identify an optimal method. Liquid-based cytology samples showed a lower number of proteins above LOD than FTA cards with vaginal fluid samples applied. Our results demonstrate that samples applied to the indicating FTA elute micro card™ are amendable to protein analyses, given that a sensitive protein detection assay is used. The results imply that biological samples applied to FTA cards can be used for DNA, RNA and protein detection.

  14. Protein Detection Using the Multiplexed Proximity Extension Assay (PEA) from Plasma and Vaginal Fluid Applied to the Indicating FTA Elute Micro Card™.

    Science.gov (United States)

    Berggrund, Malin; Ekman, Daniel; Gustavsson, Inger; Sundfeldt, Karin; Olovsson, Matts; Enroth, Stefan; Gyllensten, Ulf

    2016-01-01

    The indicating FTA elute micro card™ has been developed to collect and stabilize the nucleic acid in biological samples and is widely used in human and veterinary medicine and other disciplines. This card is not recommended for protein analyses, since surface treatment may denature proteins. We studied the ability to analyse proteins in human plasma and vaginal fluid as applied to the indicating FTA elute micro card™ using the sensitive proximity extension assay (PEA). Among 92 proteins in the Proseek Multiplex Oncology Iv2 panel, 87 were above the limit of detection (LOD) in liquid plasma and 56 among 92 above LOD in plasma applied to FTA cards. Washing and protein elution protocols were compared to identify an optimal method. Liquid-based cytology samples showed a lower number of proteins above LOD than FTA cards with vaginal fluid samples applied. Our results demonstrate that samples applied to the indicating FTA elute micro card™ are amendable to protein analyses, given that a sensitive protein detection assay is used. The results imply that biological samples applied to FTA cards can be used for DNA, RNA and protein detection.

  15. Tungsten oxide coatings deposited by plasma spray using powder and solution precursor for detection of nitrogen dioxide gas

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Chao, E-mail: zhangc@yzu.edu.cn [College of Mechanical Engineering, Yangzhou University, Yangzhou 225127 (China); Wang, Jie [College of Mechanical Engineering, Yangzhou University, Yangzhou 225127 (China); Geng, Xin [College of Mechanical Engineering, Yangzhou University, Yangzhou 225127 (China); College of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou 225002 (China)

    2016-05-25

    Increasing attention has been paid on preparation methods for resistive-type gas sensors based on semiconductor metal oxides. In this work, tungsten oxide (WO{sub 3}) coatings were prepared on alumina substrates and used as gas sensitive layers. The coatings were deposited by atmospheric plasma spray using powder, solution precursor, or a combination of both. Tungsten oxide powder through a powder port and ammonium tungstate aqueous solution through a liquid port were injected into plasma stream respectively or together to deposit WO{sub 3} coatings. Phase structures in the coatings were characterized by X-ray diffraction analyzer. The field-emission scanning electron microscopy images confirmed that the coatings were in microstructure, nanostructure or micro-nanostructure. The sensing properties of the sensors based on the coatings exposed to 1 ppm nitrogen dioxide gas were characterized in a home-made instrument. Sensing properties of the coatings were compared and discussed. The influences of gas humidity and working temperature on the sensor responses were further studied. - Highlights: • Porous gas sensitive coatings were deposited by plasma spray using powder and solution precursor. • Crystallized WO{sub 3} were obtained through hybrid plasma spray plus a pre-conditioned step. • Plasma power had an important influence on coating microstructure. • The particle size of atmospheric plasma-sprayed microstructured coating was stable. • Solution precursor plasma-sprayed WO{sub 3} coatings had nanostructure and showed good responses to 1 ppm NO{sub 2}.

  16. Vapor generation – atomic spectrometric techniques. Expanding frontiers through specific-species preconcentration. A review

    International Nuclear Information System (INIS)

    Gil, Raúl A.; Pacheco, Pablo H.; Cerutti, Soledad; Martinez, Luis D.

    2015-01-01

    This article reviews 120 articles found in SCOPUS and specific Journal cites corresponding to the terms ‘preconcentration’; ‘speciation’; ‘vapor generation techniques’ and ‘atomic spectrometry techniques’ in the last 5 years. - Highlights: • Recent advances in vapor generation and atomic spectrometry were reviewed. • Species-specific preconcentration strategies after and before VG were discussed. • New preconcentration and speciation analysis were evaluated within this framework. - Abstract: We review recent progress in preconcentration strategies associated to vapor generation techniques coupled to atomic spectrometric (VGT-AS) for specific chemical species detection. This discussion focuses on the central role of different preconcentration approaches, both before and after VG process. The former was based on the classical solid phase and liquid–liquid extraction procedures which, aided by automation and miniaturization strategies, have strengthened the role of VGT-AS in several research fields including environmental, clinical, and others. We then examine some of the new vapor trapping strategies (atom-trapping, hydride trapping, cryotrapping) that entail improvements in selectivity through interference elimination, but also they allow reaching ultra-low detection limits for a large number of chemical species generated in conventional VG systems, including complete separation of several species of the same element. This review covers more than 100 bibliographic references from 2009 up to date, found in SCOPUS database and in individual searches in specific journals. We finally conclude by giving some outlook on future directions of this field

  17. Vapor generation – atomic spectrometric techniques. Expanding frontiers through specific-species preconcentration. A review

    Energy Technology Data Exchange (ETDEWEB)

    Gil, Raúl A.; Pacheco, Pablo H.; Cerutti, Soledad [Área de Química Analítica, Facultad de Química Bioquímica y Farmacia, Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Instituto de Química de San Luis, INQUISAL, Centro Científico-Tecnológico de San Luis (CCT-San Luis), Consejo Nacional de Investigaciones Científicas y Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Martinez, Luis D., E-mail: ldm@unsl.edu.ar [Área de Química Analítica, Facultad de Química Bioquímica y Farmacia, Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Instituto de Química de San Luis, INQUISAL, Centro Científico-Tecnológico de San Luis (CCT-San Luis), Consejo Nacional de Investigaciones Científicas y Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina)

    2015-05-22

    This article reviews 120 articles found in SCOPUS and specific Journal cites corresponding to the terms ‘preconcentration’; ‘speciation’; ‘vapor generation techniques’ and ‘atomic spectrometry techniques’ in the last 5 years. - Highlights: • Recent advances in vapor generation and atomic spectrometry were reviewed. • Species-specific preconcentration strategies after and before VG were discussed. • New preconcentration and speciation analysis were evaluated within this framework. - Abstract: We review recent progress in preconcentration strategies associated to vapor generation techniques coupled to atomic spectrometric (VGT-AS) for specific chemical species detection. This discussion focuses on the central role of different preconcentration approaches, both before and after VG process. The former was based on the classical solid phase and liquid–liquid extraction procedures which, aided by automation and miniaturization strategies, have strengthened the role of VGT-AS in several research fields including environmental, clinical, and others. We then examine some of the new vapor trapping strategies (atom-trapping, hydride trapping, cryotrapping) that entail improvements in selectivity through interference elimination, but also they allow reaching ultra-low detection limits for a large number of chemical species generated in conventional VG systems, including complete separation of several species of the same element. This review covers more than 100 bibliographic references from 2009 up to date, found in SCOPUS database and in individual searches in specific journals. We finally conclude by giving some outlook on future directions of this field.

  18. Targeted selected reaction monitoring mass spectrometric immunoassay for insulin-like growth factor 1.

    Directory of Open Access Journals (Sweden)

    Eric E Niederkofler

    Full Text Available Insulin-like growth factor 1 (IGF1 is an important biomarker of human growth disorders that is routinely analyzed in clinical laboratories. Mass spectrometry-based workflows offer a viable alternative to standard IGF1 immunoassays, which utilize various pre-analytical preparation strategies. In this work we developed an assay that incorporates a novel sample preparation method for dissociating IGF1 from its binding proteins. The workflow also includes an immunoaffinity step using antibody-derivatized pipette tips, followed by elution, trypsin digestion, and LC-MS/MS separation and detection of the signature peptides in a selected reaction monitoring (SRM mode. The resulting quantitative mass spectrometric immunoassay (MSIA exhibited good linearity in the range of 1 to 1,500 ng/mL IGF1, intra- and inter-assay precision with CVs of less than 10%, and lowest limits of detection of 1 ng/mL. The linearity and recovery characteristics of the assay were also established, and the new method compared to a commercially available immunoassay using a large cohort of human serum samples. The IGF1 SRM MSIA is well suited for use in clinical laboratories.

  19. Spectroscopic and Spectrometric Methods Used for the Screening of Certain Herbal Food Supplements Suspected of Adulteration.

    Science.gov (United States)

    Mateescu, Cristina; Popescu, Anca Mihaela; Radu, Gabriel Lucian; Onisei, Tatiana; Raducanu, Adina Elena

    2017-06-01

    Purpose: This study was carried out in order to find a reliable method for the fast detection of adulterated herbal food supplements with sexual enhancement claims. As some herbal products are advertised as "all natural", their "efficiency" is often increased by addition of active pharmaceutical ingredients such as PDE-5 inhibitors, which can be a real health threat for the consumer. Methodes: Adulterants, potentially present in 50 herbal food supplements with sexual improvement claims, were detected using 2 spectroscopic methods - Raman and Fourier Transform Infrared - known for reliability, reproductibility, and an easy sample preparation. GC-MS technique was used to confirm the potential adulterants spectra. Results: About 22% (11 out of 50 samples) of herbal food supplements with sexual enhancement claims analyzed by spectroscopic and spectrometric methods proved to be "enriched" with active pharmaceutical compounds such as: sildenafil and two of its analogues, tadalafil and phenolphthalein. The occurence of phenolphthalein could be the reason for the non-relevant results obtained by FTIR method in some samples. 91% of the adulterated herbal food supplements were originating from China. Conclusion: The results of this screening highlighted the necessity for an accurate analysis of all alleged herbal aphrodisiacs on the Romanian market. This is a first such a screening analysis carried out on herbal food supplements with sexual enhancement claims.

  20. Synoptic view of the different domains of application of airborne radiometric and spectrometric surveys in egypt

    International Nuclear Information System (INIS)

    Fouad, K.M.

    1998-01-01

    Airborne radiometric survey has been applied for more than three decades in egypt. Experience gained from the acquired data over different geological environments has revealed the importance of this geophysical tool in: 1. disclosure of anomalies of potential uranium deposits, 2. geological mapping, 3. environmental monitoring of natural radiometric background around nuclear facilities, as well as the detection of nuclear fallout resulting from local or foreign nuclear activities. The advent of recording of the discriminated gamma ray energies in the airborne 256-channel spectrometer has eventually resulted in the quantitative detection of uranium, thorium, and potassium and their elemental ratios in the rocks. This has greatly widened the scope of geophysical and geochemical application. When this type is coupled with airborne magnetometry, the geological and structural configuration is appreciably revealed in three dimensions. The important role played by the statistical method of analysis is also shown. Case histories from the eastern desert, and sinai peninsula, are exhibited to help manifest the wide variety of applications of radiometric and spectrometric surveys

  1. Mass spectrometric study of vaporization of cesium tellurate and tellurite

    International Nuclear Information System (INIS)

    Semenov, G.A.; Fokina, L.A.; Mouldagalieva, R.A.

    1994-01-01

    The process of vaporization of cesium tellurate and tellurite was studied by the Knudsen effusion method with a mass spectrometric analysis of the vapor composition. The thermal dissociation of Cs 2 TeO 4 to Cs 2 TeO 3 and the congruent vaporization of Cs 2 TeO 3 were established. Thermodynamic functions for gaseous Cs 2 TeO 3 have been calculated. The standard enthalpy of sublimation Δ s H (298.15)=268.1±13.0 kJ mol -1 was determined by the 2nd and 3rd laws of thermodynamics. The enthalpy of formation Δ f H (298.15)=-725.1±13.0 kJ mol -1 for gaseous Cs 2 TeO 3 and the enthalpy of atomization Δ at H (298.15)=1841.3±15.0 kJ mol -1 have been computed. ((orig.))

  2. 5th colloquium on atomic spectrometric trace analysis

    International Nuclear Information System (INIS)

    Welz, B.

    1989-01-01

    This book deals with apparatus, use-oriented and theoretical aspects of trace analysis and spectroscopy. General articles are concerned with the analysis of environmentally relevant samples; a comparison of modern spectroscopic techniques, the coupling of hydride production, chromatography and spectrometry; chemical modifiers for graphite tube furnace atomic absorption spectroscopy (AAS), and possible applications of flow injection to atomic spectrometric trace analysis - one of the outstanding subjects of the colloquium. About one quarter of the 85 contributions deals with new techniques including flow injection. Other priority subjects are the theory and application of graphite tube furnace AAS, and a comparison between different dissolution methods and direct solid analysis. Medicine and toxicology, analysis of biological materials and environmentally relevant samples are in the foreground of use-oriented papers. (orig./BBR) [de

  3. Modern spectrometric methods for the analysis of labelled compounds

    International Nuclear Information System (INIS)

    Kaspersen, F.M.; Funke, C.W.; Wagenaars, G.N.; Jacobs, P.L.

    1988-01-01

    A proper analysis of chemical compounds should give information about the chemical identity (not only the structure but also enantiomeric form), the chemical purity and chemical composition (e.g. giving information about counter-ions, solvents of crystallization). For labelled compounds information is also needed about isotopic purity (defined as the % of isotope present in the compound), the position/distribution of the isotope in the molecule and degree of labelling/specific activity. In the past ten years the possibilities for spectrometric analyses of labelled compounds have increased enormously and this chapter will give an overview of these methods with the exception of (radio)chromatography that will be dealt with in another chapter. (author)

  4. Validation of a stability-indicating spectrometric method for the determination of sulfacetamide sodium in pure form and ophthalmic preparations

    Directory of Open Access Journals (Sweden)

    Sofia Ahmed

    2017-01-01

    Full Text Available Introduction: Sulfacetamide sodium is a widely used sulfonamide for ophthalmic infections. Objective: A number of analytical methods have been reported for the analysis of sulfacetamide but they lack the ability to determine both the active drug and its major degradation product, sulfanilamide, simultaneously in a sample. Materials and Methods: In the present study a simple, rapid and economical stability-indicating UV spectrometric method has been validated for the simultaneous assay of sulfacetamide sodium and sulfanilamide in pure form and in ophthalmic preparations. Results: The method has been found to be accurate (recovery 100.03 ±0.589% and precise (RSD 0.587% with detectable and quantifiable limits of 1.67×10–6 M (0.04 mg% and 5.07×10–6 M (0.13 mg%, respectively for the assay of pure sulfacetamide sodium. The method is also found to be accurate and precise to small changes in wavelength, pH and buffer concentration as well as to forced degradation. The study further includes the validation of the method for the assay of pure sulfanilamide in solution, which has been found to be accurate, precise and robust. Conclusion: The results indicate that the proposed two-component spectrometric method is stability-indicating and can be used for the simultaneous assay of both sulfacetamide sodium and sulfanilamide in synthetic mixtures and degraded solutions.

  5. A gas/liquid chromatographic-mass spectrometric method for the rapid screening of 250 pesticides in aqueous matrices

    Energy Technology Data Exchange (ETDEWEB)

    Chandramouli, B.; Harvan, D.; Brittain, S.; Hass, R. [Eno River Labs, LLC. Durham, NC (United States)

    2004-09-15

    Pesticide residues in food present a potentially serious and significant cause for concern. Many pesticides have been associated with significant health effects to the nervous and endocrine systems and some have been deemed carcinogenic. There are many well-established techniques for pesticide analysis. However, commercial pesticide methods have traditionally only been available for specific pesticide families, such as chlorinated pesticides or herbicides, and at detection limits ranging from 0.05 ppb to 1 ppm in aqueous matrices. Techniques that can quickly screen for the presence/absence of pesticide residues in food matrices are critical in ensuring the safety of food and water. This paper outlines a combined Gas Chromatographic-High Resolution Mass Spectrometric (GC-HRMS) and Liquid Chromatographic Tandem Mass Spectrometric (LC-MS/MS) screening assay for 250 pesticides that was developed for use in water, and soda samples at screening levels ranging from 0.1-5 ppb. The pesticides selected have been identified by the European Union as being of concern and the target of possible legislation. The list encompasses a variety of pesticide classes and compound groupings.

  6. In situ monitoring of molecular changes during cell differentiation processes in marine macroalgae through mass spectrometric imaging.

    Science.gov (United States)

    Kessler, Ralf W; Crecelius, Anna C; Schubert, Ulrich S; Wichard, Thomas

    2017-08-01

    Matrix-assisted laser desorption/ionization mass spectrometric imaging (MALDI-MSI) was employed to discriminate between cell differentiation processes in macroalgae. One of the key developmental processes in the algal life cycle is the production of germ cells (gametes and zoids). The gametogenesis of the marine green macroalga Ulva mutabilis (Chlorophyta) was monitored by metabolomic snapshots of the surface, when blade cells differentiate synchronously into gametangia and giving rise to gametes. To establish MSI for macroalgae, dimethylsulfoniopropionate (DMSP), a known algal osmolyte, was determined. MSI of the surface of U. mutabilis followed by chemometric data analysis revealed dynamic metabolomic changes during cell differentiation. DMSP and a total of 55 specific molecular biomarkers, which could be assigned to important stages of the gametogenesis, were detected. Our research contributes to the understanding of molecular mechanisms underlying macroalgal cell differentiation. Graphical abstract Molecular changes during cell differentiation of the marine macroalga Ulva were visualized by matrix assisted laser desorption/ionization mass spectrometric imaging (MALDI-MSI).

  7. Detection and differentiation of 22kDa and 20kDa Growth Hormone proteoforms in human plasma by LC-MS/MS

    DEFF Research Database (Denmark)

    Sanmartín, Gerard Such; Bache, N.; Bosch, J.

    2015-01-01

    Human growth hormone (GH) is suspected to be widely and illegally used in sport to improve athletes' performance. For the detection of GH abuse, blood samples are screened for abnormal ratios between the 22 and 20kDa GH proteoforms that demonstrate the administration of the synthetic hormone....... Current detection methods are based on classical immunoassays as they provide sufficient sensitivity for the detection of GH proteoforms. These antibody based methods, however, suffer from unclear selectivity and potential cross-reactivity towards similar proteins. For unambiguous GH detection, we report...... a Mass Spectrometry ImmunoAssay (MSIA) that first enriches GH from plasma with an antibody of relatively low specificity, and subsequently quantifies the 22 and 20kDa proteoforms by Selected Reaction Monitoring (SRM) LC-MS/MS analysis. This method proved superior to an antibody-free strategy based on GH...

  8. Liquid chromatographic-tandem mass spectrometric assay for ...

    African Journals Online (AJOL)

    for simultaneous quantitation of tofacitinib, cabozantinib ... The method was validated with regard to its limits of .... quantitative determination of TOF alone was .... prepared in human plasma only. Blank plasma/urine samples were similarly ...

  9. Determination of fluspirilene in human plasma by liquid chromatography-tandem mass spectrometry with electrospray ionisation.

    Science.gov (United States)

    Swart, K J; Sutherland, F C; van Essen, G H; Hundt, H K; Hundt, A F

    1998-12-18

    An ultra-sensitive method for the determination of fluspirilene in plasma was established, using high-performance liquid chromatographic separation with tandem mass spectrometric detection. The samples were extracted with hexane/isoamyl alcohol, separated on a Phenomenex Luna C18 5 mu 150 x 2.1 mm column with a mobile phase consisting of methanol-water-acetic acid (600:400:1) at a flow-rate of 0.3 ml/min. Detection was achieved by a Finnigan Matt mass spectrometer (LCQ) at unit resolution in full scan mode scanning the product ion spectrum from m/z 130-500 and monitoring the transition of the protonated molecular ion at m/z 476.2, to the sum of the largest product ions m/z 371, 342 and 274 (MS-MS). Electrospray ionisation was used for ion production. The mean recovery for fluspirilene was 90% with a lower limit of quantification of 21.50 pg/ml using 1 ml plasma for extraction. This is the first chromatographic method described for the determination of fluspirilene in plasma that is accurate and sensitive enough to be used in pharmacokinetic studies.

  10. Determination of linsidomine in human plasma by tandem LC-MS with ESI.

    Science.gov (United States)

    Sutherland, F C; de Jager, A D; Swart, K J; Hundt, H K; Scanes, T; Hundt, A F

    2000-04-01

    A sensitive method for the determination of linsidomine in plasma was developed, using high-performance liquid chromatographic (HPLC) separation with tandem mass spectrometric detection. Linsidomine was derivatised with propyl chloroformate and extracted with tert-butyl methyl ether/1,2-dichloroethane (55:45, v/v), back-extracted into HCl (0.01 M) followed by alkalinisation and back-extraction into ether; the final ether extract evaporated, reconstituted in mobile phase and then separated on a Phenomenex Luna C18 (2) 5 micron 2.1 x 150 mm column with a mobile phase consisting of methanol water formic acid (98/100%) (400:600:0.05, v/v/v) at a flow-rate of 0.4 ml min(-1). Detection was achieved by a Finnigan MAT mass spectrometer (LCQ) at unit resolution in the selected reaction monitoring (SRM) mode monitoring the transition of the protonated molecular ion m/z 257.0 to the product ion m/z 86.0. The mean recovery for linsidomine was 51% with a lower limit of quantification of 0.70 ng/ml using 1 ml plasma for extraction. This LC-MS/MS method for the determination of linsidomine in human plasma allows for better specificity and a higher sample throughput than the traditional LC-UV methods. It also demonstrates the profound effect that the composition of acidic modifiers and matrix constituents can have on the electrospray ionisation (ESI) of the analyte.

  11. Detection of drugs of abuse in exhaled breath using a device for rapid collection: comparison with plasma, urine and self-reporting in 47 drug users.

    Science.gov (United States)

    Beck, Olof; Stephanson, Niclas; Sandqvist, Sören; Franck, Johan

    2013-06-01

    Exhaled breath has recently been identified as a matrix for the detection of drugs of abuse. This work aims to further document this application using a new and simple collection device in patients following recovery from acute intoxication. Breath, plasma and urine samples were collected from 47 patients (38 males, age range 25-74) together with interview data. Analysis of breath and plasma samples was done by liquid chromatography-mass spectrometry methods. Urine was screened using immunochemical reagents and positive findings confirmed with liquid chromatography-mass spectrometry methods. The 12 analytes investigated were: methadone, amphetamine, methamphetamine, 6-acetylmorphine, morphine, benzoylecgonine, cocaine, diazepam, oxazepam, alprazolam, buprenorphine and tetrahydrocannabinol. In all 47 cases, recent intake of an abused substance prior to admission was reported, but in one case the substance (ketobemidone) was not investigated. In 40 of the remaining cases (87%) breath analysis gave a positive finding of any of the substances that were part of the analytical investigation. Identifications were based on correct chromatographic retention time and product ion ratios obtained in selected reaction monitoring mode. In general, data from breath, plasma, urine and self-reporting were in good agreement, but in 23% of the cases substances were detected that had not been self-reported. All substances covered were detected in a number of breath samples. Considering that breath sampling was often done about 24 h after intake, the detection rate was considered to be high for most substances. Analytes with low detection rates were benzodiazepines, and a further increase in analytical sensitivity is needed to overcome this. This study further supports use of exhaled breath as a new matrix in clinical toxicology.

  12. Enhancement of laser-induced breakdown spectroscopy (LIBS) Detection limit using a low-pressure and short-pulse laser-induced plasma process.

    Science.gov (United States)

    Wang, Zhen Zhen; Deguchi, Yoshihiro; Kuwahara, Masakazu; Yan, Jun Jie; Liu, Ji Ping

    2013-11-01

    Laser-induced breakdown spectroscopy (LIBS) technology is an appealing technique compared with many other types of elemental analysis because of the fast response, high sensitivity, real-time, and noncontact features. One of the challenging targets of LIBS is the enhancement of the detection limit. In this study, the detection limit of gas-phase LIBS analysis has been improved by controlling the pressure and laser pulse width. In order to verify this method, low-pressure gas plasma was induced using nanosecond and picosecond lasers. The method was applied to the detection of Hg. The emission intensity ratio of the Hg atom to NO (IHg/INO) was analyzed to evaluate the LIBS detection limit because the NO emission (interference signal) was formed during the plasma generation and cooling process of N2 and O2 in the air. It was demonstrated that the enhancement of IHg/INO arose by decreasing the pressure to a few kilopascals, and the IHg/INO of the picosecond breakdown was always much higher than that of the nanosecond breakdown at low buffer gas pressure. Enhancement of IHg/INO increased more than 10 times at 700 Pa using picosecond laser with 35 ps pulse width. The detection limit was enhanced to 0.03 ppm (parts per million). We also saw that the spectra from the center and edge parts of plasma showed different features. Comparing the central spectra with the edge spectra, IHg/INO of the edge spectra was higher than that of the central spectra using the picosecond laser breakdown process.

  13. Mass spectrometric identification of isoforms of PR proteins in xylem sap of fungus-infected tomato

    NARCIS (Netherlands)

    Rep, Martijn; Dekker, Henk L.; Vossen, Jack H.; de Boer, Albert D.; Houterman, Petra M.; Speijer, Dave; Back, Jaap W.; de Koster, Chris G.; Cornelissen, Ben J. C.

    2002-01-01

    The protein content of tomato (Lycopersicon esculentum) xylem sap was found to change dramatically upon infection with the vascular wilt fungus Fusarium oxysporum. Peptide mass fingerprinting and mass spectrometric sequencing were used to identify the most abundant proteins appearing during

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

    Science.gov (United States)

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

    2016-02-01

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

  15. Simultaneous determination of phenytoin, carbamazepine, and 10,11-carbamazepine epoxide in human plasma by high-performance liquid chromatography with ultraviolet detection.

    Science.gov (United States)

    Bhatti, M M; Hanson, G D; Schultz, L

    1998-03-01

    The Bioanalytical Chemistry Department at the Madison facility of Covance Laboratories, has developed and validated a simple and sensitive method for the simultaneous determination of phenytoin (PHT), carbamazepine (CBZ) and 10,11-carbamazepine epoxide (CBZ-E) in human plasma by high-performance liquid chromatography with 10,11 dihydrocarbamazepine as the internal standard. Acetonitrile was added to plasma samples containing PHT, CBZ and CBZ-E to precipitate the plasma proteins. After centrifugation, the acetonitrile supernatant was transferred to a clean tube and evaporated under N2. The dried sample extract was reconstituted in 0.4 ml of mobile phase and injected for analysis by high-performance liquid chromatography. Separation was achieved on a Spherisorb ODS2 analytical column with a mobile phase of 18:18:70 acetonitrile:methanol:potassium phosphate buffer. Detection was at 210 nm using an ultraviolet detector. The mean retention times of CBZ-E, PHT and CBZ were 5.8, 9.9 and 11.8 min, respectively. Peak height ratios were fit to a least squares linear regression algorithm with a 1/(concentration)2 weighting. The method produces acceptable linearity, precision and accuracy to a minimum concentration of 0.050 micrograms ml-1 in human plasma. It is also simple and convenient, with no observable matrix interferences.

  16. Review of procedures involving separation and preconcentration for the determination of cadmium using spectrometric techniques

    International Nuclear Information System (INIS)

    Ferreira, Sergio L.C.; Andrade, Jailson B. de; Korn, Maria das Gracas A.; Pereira, Madson de G.; Lemos, Valfredo A.; Santos, Walter N.L. dos; Rodrigues, Frederico de Medeiros; Souza, Anderson S.; Ferreira, Hadla S.; Silva, Erik G.P. da

    2007-01-01

    Spectrometric techniques for the analysis of trace cadmium have developed rapidly due to the increasing need for accurate measurements at extremely low levels of this element in diverse matrices. This review covers separation and preconcentration procedures, such as electrochemical deposition, precipitation, coprecipitation, solid phase extraction, liquid-liquid extraction (LLE) and cloud point extraction (CPE), and consider the features of the their application with several spectrometric techniques

  17. Development of homologous radioimmunoassays for equine growth hormone and equine prolactin and their application to the detection of circulating levels of hormone in horse plasma

    Energy Technology Data Exchange (ETDEWEB)

    Cahill, C.M.; Hayden, T.J. [University Coll., Dublin (Ireland); Ven der Kolk, H. [Rijksuniversiteit Utrecht (Netherlands); Goode, J.A. [Agricultural Research Council, Cambridge (United Kingdom). Inst. of Animal Physiology

    1994-12-31

    Highly purified and well-characterized preparations of equine prolactin and growth hormone from equine pituitary glands were employed to set up highly sensitive and specific homologous radioimmunoassays (RIA) for the measurement of hormone in horse plasma. The limit of sensitivity of the GH RIA was 1.2 ng/ml with mean intra -and inter- assay coefficients of variation (CV) of 6.6 and 10%, respectively. The sensitivity of the equine prolactin (ePRL) RIA was 0.5 ng/ml with mean intra and inter-assay CV of 9.1 and 15.6%, respectively. Dose-response curves of a crude pituitary gland extract and plasma samples collected from a mare and foal were parallel to the standards and the PRL RIA was clinically validated by administration of thyrotropin-releasing hormone (TRH). Plasma samples taken at 15 min intervals over 24 h from lactating mares gave 24 h mean GH values in the range 5.5 to 7.95 ng/ml. Large intermittent elevations of GH activity were detected. The mean 24 h PRL concentrations were between 3.2-10.4 ng/ml in the lactating animals, with higher concentrations earlier in lactation. Long episodic bursts of PRL were detected. (authors). 48 refs., 9 figs.

  18. Novel liquid chromatography method based on linear weighted regression for the fast determination of isoprostane isomers in plasma samples using sensitive tandem mass spectrometry detection.

    Science.gov (United States)

    Aszyk, Justyna; Kot, Jacek; Tkachenko, Yurii; Woźniak, Michał; Bogucka-Kocka, Anna; Kot-Wasik, Agata

    2017-04-15

    A simple, fast, sensitive and accurate methodology based on a LLE followed by liquid chromatography-tandem mass spectrometry for simultaneous determination of four regioisomers (8-iso prostaglandin F 2α , 8-iso-15(R)-prostaglandin F 2α , 11β-prostaglandin F 2α , 15(R)-prostaglandin F 2α ) in routine analysis of human plasma samples was developed. Isoprostanes are stable products of arachidonic acid peroxidation and are regarded as the most reliable markers of oxidative stress in vivo. Validation of method was performed by evaluation of the key analytical parameters such as: matrix effect, analytical curve, trueness, precision, limits of detection and limits of quantification. As a homoscedasticity was not met for analytical data, weighted linear regression was applied in order to improve the accuracy at the lower end points of calibration curve. The detection limits (LODs) ranged from 1.0 to 2.1pg/mL. For plasma samples spiked with the isoprostanes at the level of 50pg/mL, intra-and interday repeatability ranged from 2.1 to 3.5% and 0.1 to 5.1%, respectively. The applicability of the proposed approach has been verified by monitoring of isoprostane isomers level in plasma samples collected from young patients (n=8) subjected to hyperbaric hyperoxia (100% oxygen at 280kPa(a) for 30min) in a multiplace hyperbaric chamber. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Development of homologous radioimmunoassays for equine growth hormone and equine prolactin and their application to the detection of circulating levels of hormone in horse plasma

    International Nuclear Information System (INIS)

    Cahill, C.M.; Hayden, T.J.; Ven der Kolk, H.; Goode, J.A.

    1994-01-01

    Highly purified and well-characterized preparations of equine prolactin and growth hormone from equine pituitary glands were employed to set up highly sensitive and specific homologous radioimmunoassays (RIA) for the measurement of hormone in horse plasma. The limit of sensitivity of the GH RIA was 1.2 ng/ml with mean intra -and inter- assay coefficients of variation (CV) of 6.6 and 10%, respectively. The sensitivity of the equine prolactin (ePRL) RIA was 0.5 ng/ml with mean intra and inter-assay CV of 9.1 and 15.6%, respectively. Dose-response curves of a crude pituitary gland extract and plasma samples collected from a mare and foal were parallel to the standards and the PRL RIA was clinically validated by administration of thyrotropin-releasing hormone (TRH). Plasma samples taken at 15 min intervals over 24 h from lactating mares gave 24 h mean GH values in the range 5.5 to 7.95 ng/ml. Large intermittent elevations of GH activity were detected. The mean 24 h PRL concentrations were between 3.2-10.4 ng/ml in the lactating animals, with higher concentrations earlier in lactation. Long episodic bursts of PRL were detected. (authors). 48 refs., 9 figs

  20. Detection of lower hybrid waves in the scrape-off layer of tokamak plasmas with microwave backscattering

    International Nuclear Information System (INIS)

    Baek, S. G.; Shiraiwa, S.; Parker, R. R.; Bonoli, P. T.; Marmar, E. S.; Wallace, G. M.; Lau, C.; Dominguez, A.; Kramer, G. J.

    2014-01-01

    Microwave backscattering experiments have been performed on the Alcator C-Mod tokamak in order to investigate the propagation of lower hybrid (LH) waves in reactor-relevant, high-density plasmas. When the line-averaged density is raised above 1 × 10 20 m –3 , lower hybrid current drive efficiency is found to be lower than expected [Wallace et al., Phys. Plasmas 19, 062505 (2012)] and LH power is thought to be dissipated at the plasma edge. Using a single channel (60 GHz) ordinary-mode (O-mode) reflectometer system, we demonstrate radially localized LH wave measurements in the scrape-off layer of high density plasmas (n ¯ e  ≳ 0.9×10 20  m −3 ). Measured backscattered O-mode power varies depending on the magnetic field line mapping, suggesting the resonance cone propagation of LH waves. Backscattered power is also sensitive to variations in plasma density and the launched parallel refractive index of the LH waves. LH ray-tracing simulations have been carried out to interpret the observed variations. To understand the measured LH waves in regions not magnetically connected to the launcher, two hypotheses are examined. One is the weak single pass absorption and the other is scattering of LH waves by non-linear effects

  1. Ultra-trace monitoring of copper in environmental and biological samples by inductively coupled plasma atomic emission spectrometry after separation and preconcentration by using octadecyl silica membrane disks modified by a new schiff's base

    Directory of Open Access Journals (Sweden)

    Mohammad Reza Ganjali

    2004-04-01

    Full Text Available Ultra-trace amounts of Cu(II were separated and preconcentrated by solid phase extraction on octadecyl-bonded silica membrane disks modified with a new Schiff,s base (Bis- (2-Hydroxyacetophenone -2,2-dimethyl-1,3-propanediimine (SBTD followed by elution and inductively coupled plasma atomic emission spectrometric detection. The method was applied as a separation and detection method for copper(II in environmental and biological samples. Extraction efficiency and the influence of sample matrix, flow rate, pH, and type and minimum amount of stripping acid were investigated. The concentration factor and detection limit of the proposed method are 500 and 12.5 pg mL-1, respectively.

  2. Application and evaluation of the mass spectrometric isotope dilution technique in the determination of rare earths in geological materials

    International Nuclear Information System (INIS)

    Moraes, N.M.P. de.

    1988-01-01

    Establishment of the experimental procedures employed in the rare earth element determination of geological samples by mass spectrometric isotope dilution analysis is discussed in the present work. The procedures involve preparation and calibration of the isotope tracers isotope dilution, dissolution in a teflon pressure vessel, chemical separation and isotope analysis using a fully automated Micromass VG ISOTOPES model 354 thermal ionization mass spectrometer. For the initial chemical separation of total rare earths the cationic resin was employed and HC1 and HNO 3 acids as eluents. In the second step rare earths elements were separated into individual (La, Ce and Nd) and subgroups (Sm-Eu-Gd, Yb-Er-Dy) fractions using the same cationic resin and α-HIBA as eluent. Nine elements La, Ce, Nd, Sm, Eu, Gd, Dy, Er and Yb are determined by this method in the ''United States Geological Survey'' (USGS) standard samples GSP-1, AGV-1 and G-2, with an overall precision of +- 1 to 2% and an accuracy of 5%. The concentration of rare earth element determined in the standard sample PCC-1 showed that the total analytical blanks are in submicrogram levels. The concentration of rare earth elements in the same USGS standard samples were also determined by Instrumental neutron activation analysis, neutron activation analysis with chemical separation before irradiation and inductively coupled argon plasma spectroscopy. The chemical procedures employed for these methods are the same as that used for mass spectrometric isotope dilution. Based on the results obtained, each method was evaluated pointing out their merits and defects. The study clearly showed that the chemical procedure employed for all these techniques was satisfactory. (author) [pt

  3. Major constituent quantitative determination in uranium alloys by coupled plasma atomic emission spectrometry and X ray fluorescence wavelength dispersive spectrometry

    International Nuclear Information System (INIS)

    Oliveira, Luis Claudio de; Silva, Adriana Mascarenhas Martins da; Gomide, Ricardo Goncalves; Silva, Ieda de Souza

    2013-01-01

    A wavelength-dispersive X-ray fluorescence (WD-XRF) spectrometric method for determination of major constituents elements (Zr, Nb, Mo) in Uranium/Zirconium/Niobium and Uranium/Molybdenum alloy samples were developed. The methods use samples taken in the form of chips that were dissolved in hot nitric acid and precipitate particles melted with lithium tetraborate and dissolved in hot nitric acid and finally analyzed as a solution. Studies on the determination by inductively coupled plasma optic emission spectrometry (ICP OES) using matched matrix in calibration curve were developed. The same samples solution were analyzed in both methods. The limits of detection (LOD), linearity of the calibrations curves, recovery study, accuracy and precision of the both techniques were carried out. The results were compared. (author)

  4. A spectrometrical method to measure the deuterium content in 2H-enriched water

    International Nuclear Information System (INIS)

    Dumke, I.

    1980-04-01

    A test method and spectrometer has been developed for emission-spectrometrical measurement of the deuterium content in water enriched with deuterium. The water sample is melted into a previously evacuated glas tube and a gas discharge is excited in vapour over the cooled sample to adjust to a low vapour pressure with high frequency. The intensities of the H(α) and D(α) lines appearing in the spectrum determine the D-content. Both lines were resolved by a Fabry-Perot interferometer and geometrically separated fed to two photodetectors. The remaining spectrum is filtered off. Following electronic calculation of the signals, the measured value is indicated which has to be corrected by a standard curve. The relative measuring accuracy is about +-1% for enrichments of over 1% D and less than +-5% in the region of 0.3-1% D. The detection limit is about 0.03% D (sample amount: 50 μl, average of 5 samples). (orig./HP) [de

  5. Liquid chromatography/mass spectrometric determination of patulin in apple juice using atmospheric pressure photoionization.

    Science.gov (United States)

    Takino, Masahiko; Daishima, Shigeki; Nakahara, Taketoshi

    2003-01-01

    This paper describes a comparison between atmospheric pressure chemical ionization (APCI) and the recently introduced atmospheric pressure photoionization (APPI) technique for the liquid chromatography/mass spectrometric (LC/MS) determination of patulin in clear apple juice. A column switching technique for on-line extraction of clear apple juice was developed. The parameters investigated for the optimization of APPI were the ion source parameters fragmentor voltage, capillary voltage, and vaporizer temperature, and also mobile phase composition and flow rate. Furthermore, chemical noise and signal suppression of analyte signals due to sample matrix interference were investigated for both APCI and APPI. The results indicated that APPI provides lower chemical noise and signal suppression in comparison with APCI. The linear range for patulin in apple juice (correlation coefficient >0.999) was 0.2-100 ng mL(-1). Mean recoveries of patulin in three apple juices ranged from 94.5 to 103.2%, and the limit of detection (S/N = 3), repeatability and reproducibility were 1.03-1.50 ng mL(-1), 3.9-5.1% and 7.3-8.2%, respectively. The total analysis time was 10.0 min. Copyright 2003 John Wiley & Sons, Ltd.

  6. Resolution of a protein sequence ambiguity by X-ray crystallographic and mass spectrometric methods

    International Nuclear Information System (INIS)

    Keefe, L.J.; Lattman, E.E.; Wolkow, C.; Woods, A.; Chevrier, M.; Cotter, R.J.

    1992-01-01

    Ambiguities in amino acid sequences are a potential problem in X-ray crystallographic studies of proteins. Amino acid side chains often cannot be reliably identified from the electron density. Many protein crystal structures that are now being solved are simple variants of a known wild-type structure. Thus, cloning artifacts or other untoward events can readily lead to cases in which the proposed sequence is not correct. An example is presented showing that mass spectrometry provides an excellent tool for analyzing suspected errors. The X-ray crystal structure of an insertion mutant of Staphylococcal nuclease has been solved to 1.67 A resolution and refined to a crystallographic R value of 0.170. A single residue has been inserted in the C-terminal α helix. The inserted amino acid was believed to be an alanine residue, but the final electron density maps strongly indicated that a glycine had been inserted instead. To confirm the observations from the X-ray data, matrix-assisted laser desorption mass spectrometry was employed to verify the glycine insertion. This mass spectrometric technique has sufficient mass accuracy to detect the methyl group that distinguishes glycine from alanine and can be extended to the more common situation in which crystallographic measurements suggest a problem with the sequence, but cannot pinpoint its location or nature. (orig.)

  7. Resolution of a protein sequence ambiguity by X-ray crystallographic and mass spectrometric methods

    Energy Technology Data Exchange (ETDEWEB)

    Keefe, L.J.; Lattman, E.E. (Dept. of Biophysics and Biophysical Chemistry, Johns Hopkins Univ. School of Medicine, Baltimore, MD (United States)); Wolkow, C.; Woods, A.; Chevrier, M.; Cotter, R.J. (Middle Atlantic Mass Spectrometry Lab., Johns Hopkins Univ. School of Medicine, Baltimore, MD (United States))

    1992-04-01

    Ambiguities in amino acid sequences are a potential problem in X-ray crystallographic studies of proteins. Amino acid side chains often cannot be reliably identified from the electron density. Many protein crystal structures that are now being solved are simple variants of a known wild-type structure. Thus, cloning artifacts or other untoward events can readily lead to cases in which the proposed sequence is not correct. An example is presented showing that mass spectrometry provides an excellent tool for analyzing suspected errors. The X-ray crystal structure of an insertion mutant of Staphylococcal nuclease has been solved to 1.67 A resolution and refined to a crystallographic R value of 0.170. A single residue has been inserted in the C-terminal {alpha} helix. The inserted amino acid was believed to be an alanine residue, but the final electron density maps strongly indicated that a glycine had been inserted instead. To confirm the observations from the X-ray data, matrix-assisted laser desorption mass spectrometry was employed to verify the glycine insertion. This mass spectrometric technique has sufficient mass accuracy to detect the methyl group that distinguishes glycine from alanine and can be extended to the more common situation in which crystallographic measurements suggest a problem with the sequence, but cannot pinpoint its location or nature. (orig.).

  8. Column preconcentration and electrothermal atomic absorption spectrometric determination of rhodium in some food and standard samples.

    Science.gov (United States)

    Taher, Mohammad Ali; Pourmohammad, Fatemeh; Fazelirad, Hamid

    2015-12-01

    In the present work, an electrothermal atomic absorption spectrometric method has been developed for the determination of ultra-trace amounts of rhodium after adsorption of its 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol/tetraphenylborate ion associated complex at the surface of alumina. Several factors affecting the extraction efficiency such as the pH, type of eluent, sample and eluent flow rates, sorption capacity of alumina and sample volume were investigated and optimized. The relative standard deviation for eight measurements of 0.1 ng/mL of rhodium was ±6.3%. In this method, the detection limit was 0.003 ng/mL in the original solution. The sorption capacity of alumina and the linear range for Rh(III) were evaluated as 0.8 mg/g and 0.015-0.45 ng/mL in the original solution, respectively. The proposed method was successfully applied for the extraction and determination of rhodium content in some food and standard samples with high recovery values. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Mass Spectrometric Identification and Differentiation of Botulinum Neurotoxins through Toxin Proteomics.

    Science.gov (United States)

    Kalb, Suzanne R; Barr, John R

    2013-08-01

    Botulinum neurotoxins (BoNTs) cause the disease botulism, which can be lethal if untreated. There are seven known serotypes of BoNT, A-G, defined by their response to antisera. Many serotypes are distinguished into differing subtypes based on amino acid sequence and immunogenic properties, and some subtypes are further differentiated into toxin variants. Toxin characterization is important as different types of BoNT can respond differently to medical countermeasures for botulism, and characterization of the toxin can aid in epidemiologic and forensic investigations. Proteomic techniques have been established to determine the serotype, subtype, or toxin variant of BoNT. These techniques involve digestion of the toxin into peptides, tandem mass spectrometric (MS/MS) analysis of the peptides, and database searching to identify the BoNT protein. These techniques demonstrate the capability to detect BoNT and its neurotoxin-associated proteins, and differentiate the toxin from other toxins which are up to 99.9% identical in some cases. This differentiation can be accomplished from toxins present in a complex matrix such as stool, food, or bacterial cultures and no DNA is required.

  10. Mass Spectrometric Methodologies for Investigating the Metabolic Signatures of Parkinson's Disease: Current Progress and Future Perspectives.

    Science.gov (United States)

    Gill, Emily L; Koelmel, Jeremy P; Yost, Richard A; Okun, Michael S; Vedam-Mai, Vinata; Garrett, Timothy J

    2018-03-06

    Parkinson's disease (PD) is a neurodegenerative disorder resulting from the loss of dopaminergic neurons of the substantia nigra as well as degeneration of motor and nonmotor basal ganglia circuitries. Typically known for classical motor deficits (tremor, rigidity, bradykinesia), early stages of the disease are associated with a large nonmotor component (depression, anxiety, apathy, etc.). Currently, there are no definitive biomarkers of PD, and the measurement of dopamine metabolites does not allow for detection of prodromal PD nor does it aid in long-term monitoring of disease progression. Given that PD is increasingly recognized as complex and heterogeneous, involving several neurotransmitters and proteins, it is of importance that we advance interdisciplinary studies to further our knowledge of the molecular and cellular pathways that are affected in PD. This approach will possibly yield useful biomarkers for early diagnosis and may assist in the development of disease-modifying therapies. Here, we discuss preanalytical factors associated with metabolomics studies, summarize current mass spectrometric methodologies used to evaluate the metabolic signature of PD, and provide future perspectives of the rapidly developing field of MS in the context of PD.

  11. Treatment of infants with congenital toxoplasmosis: Tolerability and plasma concentrations of sulfadiazine and pyrimethamine

    DEFF Research Database (Denmark)

    Schmidt, D.R.; Høgh, B; Andersen, O

    2006-01-01

    The aim was to study the tolerability and plasma concentrations of pyrimethamine and sulfadiazine in children treated for congenital toxoplasmosis. Infants were diagnosed through the Danish Toxoplasma Neonatal Screening Programme, based on detection of toxoplasma-specific IgM- and/or IgA-antibodi......The aim was to study the tolerability and plasma concentrations of pyrimethamine and sulfadiazine in children treated for congenital toxoplasmosis. Infants were diagnosed through the Danish Toxoplasma Neonatal Screening Programme, based on detection of toxoplasma-specific IgM- and/or Ig...... spectrometric detection. Of 48 infants, 41 completed the treatment without change in schedule. Six infants had neutrophil counts below 0.5x10(9)/l, and one infant had an elevated bilirubin value. Twenty-nine children were tested by a series of neutrophil counts during treatment. The neutrophil count was ... efficacy is still a concern, since progression of eye lesions was observed in three eyes during the follow-up period. We concluded that the treatment was well tolerated in 86% (25/29) of the children. The drugs did not affect their weight gain. Drugs given in the recommended doses led to concentrations...

  12. A plasma needle generates nitric oxide

    International Nuclear Information System (INIS)

    Stoffels, E; Gonzalvo, Y Aranda; Whitmore, T D; Seymour, D L; Rees, J A

    2006-01-01

    Generation of nitric oxide (NO) by a plasma needle is studied by means of mass spectrometry. The plasma needle is an atmospheric glow generated by a radio-frequency excitation in a mixture of helium and air. This source is used for the treatment of living tissues, and nitric oxide may be one of the most important active agents in plasma therapy. Efficient NO generation is of particular importance in the treatment of cardiovascular diseases. Mass spectrometric measurements have been performed under various plasma conditions; gas composition in the plasma and conversion of feed gases (nitrogen and oxygen) into other species has been studied. Up to 30% of the N 2 and O 2 input is consumed in the discharge, and NO has been identified as the main conversion product

  13. Characterization of used lubricating oil by spectrometric techniques

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Andressa Moreira de, E-mail: andressa@ctaa.embrapa.br [Embrapa Agroindustria de Alimentos, Guaratiba, Rio de Janeiro, RJ (Brazil); Correa, Sergio Machado [Faculdade de Engenharia. Universidade do Estado do Rio de Janeiro (UERJ), Resende, RJ (Brazil); Silva, Glauco Correa da [Instituto de Engenharia Nuclear (IEN/CNEN-RJ), Rio de Janeiro, RJ (Brazil)

    2011-07-01

    Full text: The engine lubricating oil drags all kinds of impurities generated by wear of internal components. Thus, it is necessary to monitor the physical and chemical properties and concentration of metals in lubricants used to determine the appropriate time to replace them. Moreover, one can monitor the wear of the engines through the levels of metals in oils. To achieve these goals, some detection techniques such as Flame atomic absorption spectrometry (FAAS), Inductively coupled plasma optical emission spectrometry (ICP-OES) and X-ray fluorescence (XRF), have been widely used to determine metals in lubricating oils and also in other oil derivatives. Thus, some of these techniques were used in this study. Also the technique used was Gas chromatography mass spectrometry (GC / MS) for characterization of chromatographic profile of the engine lubricating oil after use. Through the technique of ICP-OES for method of United States Environmental Protection Agency (USEPA) METHOD 6010B - Inductively coupled plasma optical emission spectrometry was performed to characterize metals in lubricating oil motor, using equipment from ICP-OES Perkin-Elmer{sup R} OPTIMA 3000 ICP-Winlab and software, obtaining the following identification of metals: barium (Ba), calcium (Ca), lead (Pb), copper (Cu), Chromium (Cr), iron (Fe), magnesium (Mg), molybdenum (Mo) and zinc (Zn). Using the XRF technique, through the equipment EDFRX Shimadzu{sup R} model 800HS EDX, Rh tube, applied voltage of 50kV, amperage 100{mu}A, detector Si (Li) cooled with liquid nitrogen and collimator 10mm, we analyzed all the components comprised in the range of Ti to U and Na to SC, identified the following metals: calcium (Ca), zinc (Zn), iron (Fe), copper (Cu), molybdenum (Mo) and nickel (Ni). The characterization was performed by chromatographic methods: USEPA METHOD 5021A - Volatile organic compounds in various sample matrices using equilibrium headspace analysis, USEPA METHOD 8015B - Nonhalogenated Organics

  14. Characterization of used lubricating oil by spectrometric techniques

    International Nuclear Information System (INIS)

    Souza, Andressa Moreira de; Correa, Sergio Machado; Silva, Glauco Correa da

    2011-01-01

    Full text: The engine lubricating oil drags all kinds of impurities generated by wear of internal components. Thus, it is necessary to monitor the physical and chemical properties and concentration of metals in lubricants used to determine the appropriate time to replace them. Moreover, one can monitor the wear of the engines through the levels of metals in oils. To achieve these goals, some detection techniques such as Flame atomic absorption spectrometry (FAAS), Inductively coupled plasma optical emission spectrometry (ICP-OES) and X-ray fluorescence (XRF), have been widely used to determine metals in lubricating oils and also in other oil derivatives. Thus, some of these techniques were used in this study. Also the technique used was Gas chromatography mass spectrometry (GC / MS) for characterization of chromatographic profile of the engine lubricating oil after use. Through the technique of ICP-OES for method of United States Environmental Protection Agency (USEPA) METHOD 6010B - Inductively coupled plasma optical emission spectrometry was performed to characterize metals in lubricating oil motor, using equipment from ICP-OES Perkin-Elmer R OPTIMA 3000 ICP-Winlab and software, obtaining the following identification of metals: barium (Ba), calcium (Ca), lead (Pb), copper (Cu), Chromium (Cr), iron (Fe), magnesium (Mg), molybdenum (Mo) and zinc (Zn). Using the XRF technique, through the equipment EDFRX Shimadzu R model 800HS EDX, Rh tube, applied voltage of 50kV, amperage 100μA, detector Si (Li) cooled with liquid nitrogen and collimator 10mm, we analyzed all the components comprised in the range of Ti to U and Na to SC, identified the following metals: calcium (Ca), zinc (Zn), iron (Fe), copper (Cu), molybdenum (Mo) and nickel (Ni). The characterization was performed by chromatographic methods: USEPA METHOD 5021A - Volatile organic compounds in various sample matrices using equilibrium headspace analysis, USEPA METHOD 8015B - Nonhalogenated Organics Using GC

  15. Accuracy of recommended sampling and assay methods for the determination of plasma-free and urinary fractionated metanephrines in the diagnosis of pheochromocytoma and paraganglioma: a systematic review.

    Science.gov (United States)

    Därr, Roland; Kuhn, Matthias; Bode, Christoph; Bornstein, Stefan R; Pacak, Karel; Lenders, Jacques W M; Eisenhofer, Graeme

    2017-06-01

    To determine the accuracy of biochemical tests for the diagnosis of pheochromocytoma and paraganglioma. A search of the PubMed database was conducted for English-language articles published between October 1958 and December 2016 on the biochemical diagnosis of pheochromocytoma and paraganglioma using immunoassay methods or high-performance liquid chromatography with coulometric/electrochemical or tandem mass spectrometric detection for measurement of fractionated metanephrines in 24-h urine collections or plasma-free metanephrines obtained under seated or supine blood sampling conditions. Application of the Standards for Reporting of Diagnostic Studies Accuracy Group criteria yielded 23 suitable articles. Summary receiver operating characteristic analysis revealed sensitivities/specificities of 94/93% and 91/93% for measurement of plasma-free metanephrines and urinary fractionated metanephrines using high-performance liquid chromatography or immunoassay methods, respectively. Partial areas under the curve were 0.947 vs. 0.911. Irrespective of the analytical method, sensitivity was significantly higher for supine compared with seated sampling, 95 vs. 89% (p sampling compared with 24-h urine, 95 vs. 90% (p sampling, seated sampling, and urine. Test accuracy increased linearly from 90 to 93% for 24-h urine at prevalence rates of 0.0-1.0, decreased linearly from 94 to 89% for seated sampling and was constant at 95% for supine conditions. Current tests for the biochemical diagnosis of pheochromocytoma and paraganglioma show excellent diagnostic accuracy. Supine sampling conditions and measurement of plasma-free metanephrines using high-performance liquid chromatography with coulometric/electrochemical or tandem mass spectrometric detection provides the highest accuracy at all prevalence rates.

  16. Mass spectrometric protein characterization in proteome analysis using GELoader tip micro-columns packed with various chromatographic material

    International Nuclear Information System (INIS)

    Larsen, M.R.

    2001-01-01

    In the early 90'ies mass spectrometry (MS) was introduced as a tool for identifying proteins in protein sequence databases. Since then it has become an integrated tool in protein characterization and is today routinely used to identify proteins separated by gel electrophoresis. A two-tiered mass spectrometric protein identification strategy has recently been proposed. In the first strategy peptide mass maps obtained from the protein of interest are compared with theoretically derived peptide mass maps from proteins in protein sequence databases. If the protein cannot be identified by this strategy, tandem mass spectrometric sequencing is used to generate enough sequence data to identify the protein in protein sequence databases or expressed sequence tag (EST) databases. However, the above strategies primarily identify a protein relatively to the DNA sequence, in which no information about e.g. post-translational modifications (PTMs) is stored. PTMs are known to modify the function, location, solubility and activity of proteins in the cell, and they are therefore very important for understanding living cells. More than 200 different PTMs are known, of which glycosylation, phosphorylation and proteolytic processing are the most common ones. Mass spectrometric analysis of PTMs on gel-separated proteins requires a higher amount of protein than for identification only. In addition, higher sequence coverage from the peptide mass maps or pre-purification of the modified peptides prior to MS analysis, is necessary for detection of putative modified peptides. In this study a multi-tiered strategy, in which GELoader tip micro-columns packed with increasingly more hydrophobic chromatographic material are used in combination with mass spectrometry, is described. The ultimate aim was to gain increased sequence coverage from peptide mixtures derived from gel-separated proteins, in order to locate modified peptides. Graphite powder is described as an alternative to traditional

  17. Development of a immunochromatographic test with avidin-biotin for the detection of antibodies against antigen e of hepatitis B in human plasma

    International Nuclear Information System (INIS)

    Mainet Gonzalez, Damian; Palenzuela Gardon, Daniel O; Diaz Argudin, Tamara

    2007-01-01

    The disappearance of antigen e of hepatitis B in the presence of the plasmatic antibodies against antigen e may indicate a satisfactory therapeutic response in patients with chronic hepatitis B. The immuno-chromatographic test carried out in the diagnosis of diseases use different antibody combinations and may employ the avidin or streptavidin-biotin technology to develop a rapid immuno-chromatographic test for the detection of antibodies anti-antigen e in the plasma. They were detected in the laboratory by means of two fast immuno-chromatographic tests when using in one of them the avidin-biotin technology. These tests are carried out with a one-step competitive inhibition format and amplified or not with avidin-biotin. Monoclonal antibodies against antigen e obtained by cellular hybridization were used. Forty-six plasmatic samples classified as positive and negative to the anti-antigen antibodies were evaluated with a reference immunochromatographic test Advanced QualityTM. The possible expiry time of the biological reagents forming part of these tests were studied with accelerated thermal-stability experiments. The possible interference in the plasma of some of the biochemical compounds used in these trials was analyzed. Four murine monoclonal antibodies anti-antigen e were obtained and only one of them was used in these immunochromatographic tests with an anti-antigen polyclonal antibody conjugated with gold. Both tests and their stable biological reagents discriminated the positive and negative samples to the antibodies anti-antigen e, as well as the commercial test. There was no interference in the biochemical compounds studied in these tests. Both immuno-chromatographic tests made in the laboratory are useful to detect antibodies anti-antigen e in the plasma. The avidin-biotin increased the analytical sensitivity of this type of fast immuno-chromatographic test without altering its performance features. (Author)

  18. Noninvasive Digital Detection of Fetal DNA in Plasma of 4-Week-Pregnant Women following In Vitro Fertilization and Embryo Transfer.

    Directory of Open Access Journals (Sweden)

    Bedri Karakas

    Full Text Available The discovery of cell-free fetal DNA (cfDNA circulating in the maternal blood has provided new opportunities for noninvasive prenatal diagnosis (NIPD. However, the extremely low levels of cfDNA within a high background of the maternal DNA in maternal circulation necessitate highly sensitive molecular techniques for its reliable use in NIPD. In this proof of principle study, we evaluated the earliest possible detection of cfDNA in the maternal plasma by a bead-based emulsion PCR technology known as BEAMing (beads, emulsion, amplification, magnetics. Blood samples were collected from in vitro fertilization (IVF patients at 2 to 6 weeks following embryo transfer (i.e., 4 to 8 week pregnancies and plasma DNA was extracted. The genomic regions of both X and Y chromosome-specific sequences (AMELX and AMELY were concurrently amplified in two sequential PCRs; first by conventional PCR then by BEAMing. The positive beads either for AMELX or AMELY gene sequences were counted by a flow cytometer. Our results showed that the pregnancies yielding boys had significantly higher plasma AMELY gene fractions (0.512 ± 0.221 than the ones yielding girls (0.028 ± 0.003 or non-pregnant women (0.020 ± 0.005, P= 0.0059. Here, we clearly demonstrated that the BEAMing technique is capable of reliably detecting cfDNA in the blood circulation of 4-week-pregnant women, which is only two weeks after the embryo transfer. BEAMing technique can also be used to early detect fetal DNA alterations in other pregnancy-associated disorders.

  19. Asymmetrical flow field-flow fractionation coupled with multiple detections: A complementary approach in the characterization of egg yolk plasma.

    Science.gov (United States)

    Dou, Haiyang; Li, Yueqiu; Choi, Jaeyeong; Huo, Shuying; Ding, Liang; Shen, Shigang; Lee, Seungho

    2016-09-23

    The capability of asymmetrical flow field-flow fractionation (AF4) coupled with UV/VIS, multiangle light scattering (MALS) and quasi-elastic light scattering (QELS) (AF4-UV-MALS-QELS) for separation and characterization of egg yolk plasma was evaluated. The accuracy of hydrodynamic radius (Rh) obtained from QELS and AF4 theory (using both simplified and full expression of AF4 retention equations) was discussed. The conformation of low density lipoprotein (LDL) and its aggregates in egg yolk plasma was discussed based on the ratio of radius of gyration (Rg) to Rh together with the results from bio-transmission electron microscopy (Bio-TEM). The results indicate that the full retention equation is more relevant than simplified version for the Rh determination at high cross flow rate. The Rh from online QELS is reliable only at a specific range of sample concentration. The effect of programmed cross flow rate (linear and exponential decay) on the analysis of egg yolk plasma was also investigated. It was found that the use of an exponentially decaying cross flow rate not only reduces the AF4 analysis time of the egg yolk plasma, but also provides better resolution than the use of either a constant or linearly decaying cross flow rate. A combination of an exponentially decaying cross flow AF4-UV-MALS-QELS and the utilization of full retention equation was proved to be a useful method for the separation and characterization of egg yolk plasma. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Determination of low concentrations of iron, arsenic, selenium, cadmium, and other trace elements in natural samples using an octopole collision/reaction cell equipped quadrupole-inductively coupled plasma mass spectrometer.

    Science.gov (United States)

    Dial, Angela R; Misra, Sambuddha; Landing, William M

    2015-04-30

    Accurate determination of trace metals has many applications in environmental and life sciences, such as constraining the cycling of essential micronutrients in biological production and employing trace metals as tracers for anthropogenic pollution. Analysis of elements such as Fe, As, Se, and Cd is challenged by the formation of polyatomic mass spectrometric interferences, which are overcome in this study. We utilized an Octopole Collision/Reaction Cell (CRC)-equipped Quadrupole-Inductively Coupled Plasma Mass Spectrometer for the rapid analysis of small volume samples (~250 μL) in a variety of matrices containing HNO3 and/or HCl. Efficient elimination of polyatomic interferences was demonstrated by the use of the CRC in Reaction Mode (RM; H2 gas) and in Collision-Reaction Mode (CRM; H2 and He gas), in addition to hot plasma (RF power 1500 W) and cool plasma (600 W) conditions. It was found that cool plasma conditions with RM achieved the greatest signal sensitivity while maintaining low detection limits (i.e. (56) Fe in 0.44 M HNO3 has a sensitivity of 160,000 counts per second (cps)-per-1 µg L(-1) and a limit of detection (LoD) of 0.86 ng L(-1) ). The average external precision was ≤ ~10% for minor (≤10 µg L(-1) ) elements measured in a 1:100 dilution of NIST 1643e and for iron in rainwater samples under all instrumental operating conditions. An improved method has been demonstrated for the rapid multi-element analysis of trace metals that are challenged by polyatomic mass spectrometric interferences, with a focus on (56) Fe, (75) As, (78) Se and (111) Cd. This method can contribute to aqueous environmental geochemistry and chemical oceanography, as well as other fields such as forensic chemistry, agriculture, food chemistry, and pharmaceutical sciences. Copyright © 2015 John Wiley & Sons, Ltd.

  1. Use of oxidative and reducing vapor generation for reducing the detection limits of iodine in biological samples by inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Vtorushina, Eh.A.; Saprykin, A.I.; Knapp, G.

    2009-01-01

    Procedures of microwave combustion in an oxygen flow and microwave acid decomposition of biological samples were optimized for the subsequent determination of iodine. A new method was proposed for the generation of molecular iodine from periodate iona using hydrogen peroxide as a reductant. Procedures were developed for determining iodine in biological samples by inductively coupled plasma atomic emission spectrometry (ICP-AES) using oxidative and reducing vapor generation; these allowed the detection limit for iodine to be lowered by 3-4 orders of magnitude. The developed procedures were used to analyze certified reference materials of milk (Skim Milk Powder BCR 150) and seaweed (Sea Lettuce BCR 279) and a Supradyn vitamin complex

  2. Study of natural diamond detector spectrometric properties under neutron irradiation

    CERN Document Server

    Alekseyev, A B; Kaschuck, Y; Krasilnikov, A; Portnov, D; Tugarinov, S

    2002-01-01

    Natural diamond detector (NDD) performance was studied up to a neutron fluence of 10 sup 1 sup 5 neutron/cm sup 2. The variations of the NDD spectrometric response to incident alpha-particles from sup 2 sup 4 sup 1 Am source after exposure to fast neutron fluences up to 3x10 sup 1 sup 6 n/cm sup 2 were examined. No significant variations up to the level of 10 sup 1 sup 4 n/cm sup 2 were observed. Degradation of charge collection efficiency at higher fluences is reported. No remarkable increase of the NDD leakage current and count rate change had been observed up to a neutron fluence of 3x10 sup 1 sup 6 n/cm sup 2. The charge collection efficiency variations of neutron irradiated diamond spectrometer were studied ex situ under gamma-rays, beta-radiation and visible light excitation. Charge collection efficiency restoration up to 75% level and the NDD performance stabilization by extrinsic low-intensity visible light (550 nm

  3. Functional proteomics with new mass spectrometric and bioinformatics tools

    International Nuclear Information System (INIS)

    Kesners, P.W.A.

    2001-01-01

    A comprehensive range of mass spectrometric tools is required to investigate todays life science applications and a strong focus is on addressing the needs of functional proteomics. Application examples are given showing the streamlined process of protein identification from low femtomole amounts of digests. Sample preparation is achieved with a convertible robot for automated 2D gel picking, and MALDI target dispensing. MALDI-TOF or ESI-MS subsequent to enzymatic digestion. A choice of mass spectrometers including Q-q-TOF with multipass capability, MALDI-MS/MS with unsegmented PSD, Ion Trap and FT-MS are discussed for their respective strengths and applications. Bioinformatics software that allows both database work and novel peptide mass spectra interpretation is reviewed. The automated database searching uses either entire digest LC-MS n ESI Ion Trap data or MALDI MS and MS/MS spectra. It is shown how post translational modifications are interactively uncovered and de-novo sequencing of peptides is facilitated

  4. Determination of iodine to compliment mass spectrometric measurements

    International Nuclear Information System (INIS)

    Hohorst, F.A.

    1994-11-01

    The dose of iodine-129 to facility personnel and the general public as a result of past, present, and future activities at DOE sites is of continuing interest, WINCO received about 160 samples annually in a variety of natural matrices, including snow, milk, thyroid tissue, and sagebrush, in which iodine-129 is determined in order to evaluate this dose, Currently, total iodine and the isotopic ratio of iodine-127 to iodine-129 are determined by mass spectrometry. These two measurements determine the concentration of iodine-129 in each sample, These measurements require at least 16 h of mass spectrometer operator time for each sample. A variety of methods are available which concentrate and determine small quantities of iodine. Although useful, these approaches would increase both time and cost. The objective of this effort was to determine total iodine by an alternative method in order to decrease the load on mass spectrometry by 25 to 50%. The preparation of each sample for mass spectrometric analysis involves a common step--collection of iodide on an ion exchange bed. This was the focal point of the effort since the results would be applicable to all samples

  5. Surface acoustic wave nebulization facilitating lipid mass spectrometric analysis.

    Science.gov (United States)

    Yoon, Sung Hwan; Huang, Yue; Edgar, J Scott; Ting, Ying S; Heron, Scott R; Kao, Yuchieh; Li, Yanyan; Masselon, Christophe D; Ernst, Robert K; Goodlett, David R

    2012-08-07

    Surface acoustic wave nebulization (SAWN) is a novel method to transfer nonvolatile analytes directly from the aqueous phase to the gas phase for mass spectrometric analysis. The lower ion energetics of SAWN and its planar nature make it appealing for analytically challenging lipid samples. This challenge is a result of their amphipathic nature, labile nature, and tendency to form aggregates, which readily precipitate clogging capillaries used for electrospray ionization (ESI). Here, we report the use of SAWN to characterize the complex glycolipid, lipid A, which serves as the membrane anchor component of lipopolysaccharide (LPS) and has a pronounced tendency to clog nano-ESI capillaries. We also show that unlike ESI SAWN is capable of ionizing labile phospholipids without fragmentation. Lastly, we compare the ease of use of SAWN to the more conventional infusion-based ESI methods and demonstrate the ability to generate higher order tandem mass spectral data of lipid A for automated structure assignment using our previously reported hierarchical tandem mass spectrometry (HiTMS) algorithm. The ease of generating SAWN-MS(n) data combined with HiTMS interpretation offers the potential for high throughput lipid A structure analysis.

  6. Oscillatory processes in plasma

    International Nuclear Information System (INIS)

    Gallin, E.

    1980-01-01

    The oscillatory process play an important part in plasma evolution, In hot plasma in particular, the interactions between the oscillation modes are preponderant in relation to the binary collisions between particles. The nonlineary interactions between collective plasma oscillations can generate, in this case, a non-balanced steady state of plasma (steady turbulence). The paper elucidates some aspects of the oscillatory phenomena which contribute to the plasma state evolution, especially of hot plasma. A major part of the paper is devoted to the study of parametric instabilities in plasma and their role in increasing the temperature of plasma components (electrons, ions). Both parametric instabilities in plasma in the vicinity of thermodynamic balance and parametric processes is steady turbulent plasma are analysed - in relation to additional heating of hot plasma. An important result of the thesis refers to the drowing-up of a non-lineary interaction model between the oscillation modes in turbulent plasma, being responsible for the electromagnetic radiation in hot plasma. On the basis of the model suggested in the paper the existence of a low frequency radiative mode in hot plasma in a turbulent state, can be demonstrated. Its frequency could be even lower than plasma frequency in the field of long waves be even lower than plasma frequency in the field of long waves. Such a radiative mode was detected experimentally in focussed plasma installations. (author)

  7. Simultaneous analysis of amphetamine-type stimulants in plasma by solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Mariotti, Kristiane de Cássia; Schuh, Roselena S; Ferranti, Priscila; Ortiz, Rafael S; Souza, Daniele Z; Pechansky, Flavio; Froehlich, Pedro E; Limberger, Renata P

    2014-09-01

    Brazil is considered one of the countries with the highest number of amphetamine-type stimulant (ATS) users worldwide, mainly diethylpropion (DIE) and fenproporex (FEN). The use of ATS is mostly linked to diverted prescription stimulants and this misuse is widely associated with (ab)use by drivers. A validated method was developed for the simultaneous analysis of amphetamine (AMP), DIE and FEN in plasma samples employing direct immersion-solid-phase microextraction, and gas chromatographic/mass spectrometric analysis. Trichloroacetic acid 10% was used for plasma deproteinization. In situ derivatization with propylchloroformate was employed. The linear range of the method covered from 5.0 to 100 ng/mL. The detection limits were 1.0 (AMP), 1.5 (DIE) and 2.0 ng/mL (FEN). The accuracy assessment of the control samples was within 85.58-108.33% of the target plasma concentrations. Recoveries ranged from 46.35 to 84.46% and precision was <15% of the value of relative standard deviation. This method is appropriate for screening and confirmation in plasma forensic toxicology analyses of these basic drugs. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  8. A Plasma Based OES-CRDS Dual-mode Portable Spectrometer for Trace Element Detection: Emission and Ringdown Measurements of Mercury

    Science.gov (United States)

    Sahay, Peeyush; Scherrer, Susan; Wang, Chuji

    2012-10-01

    Design and development of a plasma based optical emission spectroscopy-cavity ringdown spectroscopy (OES-CRDS) dual-mode portable spectrometer for in situ monitoring of trace elements is described. A microwave plasma torch (MPT) has been utilized, which serves both as an atomization and excitation source for the two modes, viz. OES and CRDS, of the spectrometer. Operation of both modes of the instrument is demonstrated with initial measurements of elemental mercury (Hg). A detection limit of 44 ng mL-1 for Hg at 253.65 nm was determined with the emission mode of the instrument. Severe radiation trapping of 253.65 nm line hampers the measurement of Hg in higher concentration region (> 50 μg ml-1). Therefore, a different wavelength, 365.01 nm, is suggested to measure Hg in that region. Ringdown measurements of the metastable 6s6p ^3P0 state of Hg in the plasma using a 404.65 nm palm size diode laser was conducted to demonstrate the CRDS mode of the instrument. Along with being portable, dual-mode, and self-calibrated, the instrument is capable of measuring a wide range of concentration ranging from sub ng mL-1 to several μg ml-1 for a number of elements.

  9. Development and validation of analytical method for Naftopidil in human plasma by LC–MS/MS

    Directory of Open Access Journals (Sweden)

    Pritam S. Jain

    2015-09-01

    Full Text Available A highly sensitive and simple high-performance liquid chromatographic–tandem mass spectrometric (LC–MS-MS assay is developed and validated for the quantification of Naftopidil in human plasma. Naftopidil is extracted from human plasma by methyl tertiary butyl ether and analyzed using a reversed-phase gradient elution on a discovery C 18 5 μ (50 × 4.6 column. A methanol: 2 mM ammonium formate (90:10 as mobile phase, is used and detection was performed by MS using electrospray ionization in positive mode. Propranolol is used as the internal standard. The lower limits of quantification are 0.495 ng/mL. The calibration curves are linear over the concentration range of 0.495–200.577 ng/mL of plasma for each analyte. This novel LC–MS-MS method shows satisfactory accuracy and precision and is sufficiently sensitive for the performance of pharmacokinetic studies in humans.

  10. GAE detection for mass measurement for plasma density control. JET article 14 contract no 950104. Final report

    International Nuclear Information System (INIS)

    Lister, J.B.; Ridder, G. de; Villard, L.

    1997-01-01

    In view of the interest in obtaining a direct mass measurement in JET D-T plasmas, ultimately for D/T ratio control, the CRPP has performed numerical simulation work to verify the underlying method. The work undertaken is described and the conclusions are presented. The use of the GAE in JET is concluded to be less interesting than initially hoped. The reasons are discussed. Such a method, however, provide useful additional information. (author) figs., tabs., 5 refs

  11. Investigation of the effect of plasma albumin levels on regorafenib-induced hepatotoxicity using a validated liquid chromatography-tandem mass spectrometry method.

    Science.gov (United States)

    Pang, Yi Yun; Tan, Yeong Lan; Ho, Han Kiat

    2017-09-01

    Regorafenib is an oral multikinase inhibitor indicated for metastatic colorectal cancer and gastrointestinal stromal tumour. Due to its extensive plasma protein binding and low calculated hepatic extraction ratio, the hepatotoxicity observed with usage of the drug may be related to its plasma exposure. To investigate the highly dynamic free:bound drug concentration for regorafenib in the plasma, a bioanalytical liquid chromatography-tandem mass spectrometric assay was developed and validated in human plasma. The concentration range of the assay was 2-1000ng/mL. Sample preparation was via protein precipitation using acetonitrile with sorafenib as the internal standard. The supernatant was injected into an ultra-performance liquid chromatographic system coupled to a triple quadrupole mass spectrometer. The analytes were separated on an AQUITY UPLC BEH C 18 column (120Å, 1.7μm, 2.1mm×50mm) and eluted with a gradient elution system. The ions were detected in multiple reaction monitoring mode. The linearity, lower limit of quantification, intra-day and inter-day precision and accuracy conformed to FDA guidelines. The validated method was successfully applied to determine the effect of albumin levels in plasma on the extent of protein binding of regorafenib. The results indicated that physiologically-relevant levels of albumin were found to have no significant effect on the extent of protein binding of regorafenib, hence imposing minimal effect on drug disposition. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. 2DB: a Proteomics database for storage, analysis, presentation, and retrieval of information from mass spectrometric experiments.

    Science.gov (United States)

    Allmer, Jens; Kuhlgert, Sebastian; Hippler, Michael

    2008-07-07

    The amount of information stemming from proteomics experiments involving (multi dimensional) separation techniques, mass spectrometric analysis, and computational analysis is ever-increasing. Data from such an experimental workflow needs to be captured, related and analyzed. Biological experiments within this scope produce heterogenic data ranging from pictures of one or two-dimensional protein maps and spectra recorded by tandem mass spectrometry to text-based identifications made by algorithms which analyze these spectra. Additionally, peptide and corresponding protein information needs to be displayed. In order to handle the large amount of data from computational processing of mass spectrometric experiments, automatic import scripts are available and the necessity for manual input to the database has been minimized. Information is in a generic format which abstracts from specific software tools typically used in such an experimental workflow. The software is therefore capable of storing and cross analysing results from many algorithms. A novel feature and a focus of this database is to facilitate protein identification by using peptides identified from mass spectrometry and link this information directly to respective protein maps. Additionally, our application employs spectral counting for quantitative presentation of the data. All information can be linked to hot spots on images to place the results into an experimental context. A summary of identified proteins, containing all relevant information per hot spot, is automatically generated, usually upon either a change in the underlying protein models or due to newly imported identifications. The supporting information for this report can be accessed in multiple ways using the user interface provided by the application. We present a proteomics database which aims to greatly reduce evaluation time of results from mass spectrometric experiments and enhance result quality by allowing consistent data handling

  13. 2DB: a Proteomics database for storage, analysis, presentation, and retrieval of information from mass spectrometric experiments

    Directory of Open Access Journals (Sweden)

    Hippler Michael

    2008-07-01

    Full Text Available Abstract Background The amount of information stemming from proteomics experiments involving (multi dimensional separation techniques, mass spectrometric analysis, and computational analysis is ever-increasing. Data from such an experimental workflow needs to be captured, related and analyzed. Biological experiments within this scope produce heterogenic data ranging from pictures of one or two-dimensional protein maps and spectra recorded by tandem mass spectrometry to text-based identifications made by algorithms which analyze these spectra. Additionally, peptide and corresponding protein information needs to be displayed. Results In order to handle the large amount of data from computational processing of mass spectrometric experiments, automatic import scripts are available and the necessity for manual input to the database has been minimized. Information is in a generic format which abstracts from specific software tools typically used in such an experimental workflow. The software is therefore capable of storing and cross analysing results from many algorithms. A novel feature and a focus of this database is to facilitate protein identification by using peptides identified from mass spectrometry and link this information directly to respective protein maps. Additionally, our application employs spectral counting for quantitative presentation of the data. All information can be linked to hot spots on images to place the results into an experimental context. A summary of identified proteins, containing all relevant information per hot spot, is automatically generated, usually upon either a change in the underlying protein models or due to newly imported identifications. The supporting information for this report can be accessed in multiple ways using the user interface provided by the application. Conclusion We present a proteomics database which aims to greatly reduce evaluation time of results from mass spectrometric experiments and enhance

  14. Determination of rifampicin in human plasma by high-performance liquid chromatography coupled with ultraviolet detection after automatized solid-liquid extraction.

    Science.gov (United States)

    Louveau, B; Fernandez, C; Zahr, N; Sauvageon-Martre, H; Maslanka, P; Faure, P; Mourah, S; Goldwirt, L

    2016-12-01

    A precise and accurate high-performance liquid chromatography (HPLC) quantification method of rifampicin in human plasma was developed and validated using ultraviolet detection after an automatized solid-phase extraction. The method was validated with respect to selectivity, extraction recovery, linearity, intra- and inter-day precision, accuracy, lower limit of quantification and stability. Chromatographic separation was performed on a Chromolith RP 8 column using a mixture of 0.05 m acetate buffer pH 5.7-acetonitrile (35:65, v/v) as mobile phase. The compounds were detected at a wavelength of 335 nm with a lower limit of quantification of 0.05 mg/L in human plasma. Retention times for rifampicin and 6,7-dimethyl-2,3-di(2-pyridyl) quinoxaline used as internal standard were respectively 3.77 and 4.81 min. This robust and exact method was successfully applied in routine for therapeutic drug monitoring in patients treated with rifampicin. Copyright © 2016 John Wiley & Sons, Ltd.

  15. Multielement detection limits and sample nebulization efficiencies of an improved ultrasonic nebulizer and a conventional pneumatic nebulizer in inductively coupled plasma-atomic emission spectrometry

    International Nuclear Information System (INIS)

    Olson, K.W.; Haas, W.J. Jr.; Fassel, V.A.

    1977-01-01

    Two important aspects of the analytical performance of a newly developed ultrasonic nebulizer and a specially designed pneumatic nebulizer have been compared for use in inductively coupled plasma--atomic emission spectroscopy (ICP-AES). The ultrasonic nebulizer, when combined with a conventional aerosol desolvation apparatus, provided an order of magnitude or more improvement in simultaneous multielement detection limits as compared to those obtained when the pneumatic nebulizer was used either with or without desolvation. Application of a novel method for direct measurement of the overall efficiency of nebulization to the two systems showed that an approximately tenfold greater rate of sample delivery to the plasma torch was primarily responsible for the superior detection limits afforded by the ultrasonic nebulizer. A unique feature of the ultrasonic nebulizer described is the protection against chemical attack which is achieved by completely enclosing the transducer in an acoustically coupled borosilicate glass cylinder. Direct sample introduction, convenient sample change, and rapid cleanout are other important characteristics of the system which make it an attractive alternate to pneumatic nebulizer systems

  16. High-performance Liquid Chromatographic Ultraviolet Detection of Nilotinib in Human Plasma from Patients with Chronic Myelogenous Leukemia, and Comparison with Liquid Chromatography-Tandem Mass Spectrometry.

    Science.gov (United States)

    Nakahara, Ryosuke; Satho, Yuhki; Itoh, Hiroki

    2016-11-01

    A method for determining nilotinib concentration in human plasma is proposed using high-performance liquid chromatography and ultraviolet detection. Nilotinib and the internal standard dasatinib were separated using a mobile phase of 0.5% Na 2 PO 4 H 2 O (pH 2.5)-acetonitrile-methanol (55:25:20, v/v/v) on a Capcell Pak C18 MG II column (250 × 4.6 mm) at a flow rate of 1.0 ml/min, and ultraviolet measurement at 250 nm. The calibration curve exhibited linearity over the nilotinib concentration range of 50-2,500 ng/ml at 250 nm, with relative standard deviations (n = 5) of 7.1%, 2.5%, and 2.9% for 250, 1,500, and 2,500 ng/ml, respectively. The detection limit for nilotinib was 5 ng/ml due to three blank determinations (ρ = 3). This method was successfully applied to assaying nilotinib in human plasma samples from patients with chronic myelogenous leukemia. In addition, we compared the results with those measured by liquid chromatography-tandem mass spectrometry (LC-MS/MS) at BML, Inc. (a commercial laboratory). A strong correlation was observed between the nilotinib concentrations measured by our high-performance liquid chromatographic method and those obtained by LC/MS-MS (r 2 = 0.988, P < 0.01). © 2016 Wiley Periodicals, Inc.

  17. Determination of gabapentin in human plasma by capillary electrophoresis-laser induced fluorescence detection with and without solid-phase extraction

    International Nuclear Information System (INIS)

    Cao, L.; Liang, S.; Tan, X.; Meng, J.

    2012-01-01

    We have developed two methods for the quantitation of gabapentin in human plasma. They are based on capillary electrophoresis with laser-induced fluorescence detection (CE-LIF) with and without solid-phase extraction (SPE) and the derivatizing reagent 5-(4,6-dichlorotriazinyl)amino fluoresencin. The conditions for derivatization, separation and extraction were investigated in detail, and the optimal labeling conditions include a temperature of 40 0 C, a reaction time of 30 min, and the use of a borate buffer of pH 9.0 as the reaction medium. A borate buffer of pH 9.2 served as a background electrolyte for CE separations. The CE-LIF and SPE-CE-LIF methods have linear ranges of 5-200 nmol L -1 and 0.2-10 nmol L -1 , respectively, and the limits of detection are 0.5 and 0.02 nmol L -1 , respectively. The SPE-CE-LIF method was successfully applied to the determination of gabapentin in blood plasma samples. (author)

  18. Superparamagnetic graphene oxide-based dispersive-solid phase extraction for preconcentration and determination of tamsulosin hydrochloride in human plasma by high performance liquid chromatography-ultraviolet detection.

    Science.gov (United States)

    Pashaei, Yaser; Ghorbani-Bidkorbeh, Fatemeh; Shekarchi, Maryam

    2017-05-26

    In the present study, superparamagnetic graphene oxide-Fe 3 O 4 nanocomposites were successfully prepared by a modified impregnation method (MGO mi ) and their application as a sorbent in the magnetic-dispersive solid phase extraction (M-dSPE) mode to the preconcentration and determination of tamsulosin hydrochloride (TMS) in human plasma was investigated by coupling with high performance liquid chromatography-ultraviolet detection (HPLC-UV). The structure, morphology and magnetic properties of the prepared nanocomposites were characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and vibrating sample magnetometry (VSM). Some factors affecting the extraction efficiency, including the pH value, amount of sorbent, extraction time, elution solvent and its volume, and desorption time were studied and optimized. Magnetic nanocomposites plasma extraction of TMS following HPLC analyses showed a linear calibration curve in the range of 0.5-50.0ngmL -1 with an acceptable correlation coefficient (R 2 =0.9988). The method was sensitive, with a low limit of detection (0.17ngmL -1 ) and quantification (0.48ngmL -1 ). Inter- and intra-day precision expressed as relative standard deviation (n=3) and the preconcentration factor, were found to be 5.6-7.2%, 2.9-4.2% and 10, respectively. Good recoveries (98.1-101.4%) with low relative standard deviations (4.2-5.0%) indicated that the matrices under consideration do not significantly affect the extraction process. Due to its high precision and accuracy, the developed method may be a HPLC-UV alternative with M-dSPE for bioequivalence analysis of TMS in human plasma. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. High-performance liquid chromatography with time-programmed fluorescence detection for the quantification of Levofloxacin in human plasma and cerebrospinal fluid in adults with tuberculous meningitis.

    Science.gov (United States)

    Van Toi, Pham; Pouplin, Thomas; Tho, Nguyen Duc Khanh; Phuong, Pham Nguyen; Chau, Tran Thi Hong; Thuong Thuong, Nguyen Thuy; Heemskerk, Dorothee; Hien, Tran Tinh; Thwaites, Guy E

    2017-09-01

    An accurate and reliable high-performance liquid chromatography with time-programmed fluorescence detection was developed and validated to measure levofloxacin in human plasma and cerebrospinal fluid (CSF). After solid phase extraction process using Evolute ® ABN 96 fixed well plate; levofloxacin and internal standard-enoxacin were separated using a mobile phase consisting of phosphate buffer 10mM with 0.025% triethylamine pH 3.0 - acetonitrile (88:12, v/v) on a Purosphere RP-8e column (5μm, 125×4.0mm) at a flow rate of 1.2mL/min at 35°C. The excitation/emission wavelengths were set to 269/400nm and 294/500nm, for enoxacin and levofloxacin, respectively. The method was linear over the concentration range of 0.02 to 20.0μg/mL with a limit of detection of 0.01μg/mL. The relative standard deviation of intra-assay and inter-assay precision for levofloxacin at four quality controls concentrations (0.02, 0.06, 3.0 and 15.0μg/mL) were less than 7% and the accuracies ranged from 96.75% to 101.9% in plasma, and from 93.00% to 98.67% in CSF. The validated method was successfully applied to quantify levofloxacin in a considerable quantity of plasma (826) and CSF (477) samples collected from 232 tuberculous meningitis patients, and the preliminary intensive pharmacokinetics analysis from 14 tuberculous meningitis patients in Vietnam is described in this paper. Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.

  20. A system design of gamma-ray spectrometric data processing for gold prospecting

    International Nuclear Information System (INIS)

    Yin Xueqin; Cheng Xuchu; Fang Lianxi; Huang Zuofeng.

    1992-01-01

    Based on different correlation between gamma-ray spectrometric data and gold grade in different types of gold deposits, it is necessary and possible to establish a mathematical model of gamma-ray spectrometric data processing for predicting specific gold deposits. A system design of gamma-ray spectrometric data processing for prospecting gold deposits has been worked out according to the mathematical method and procedure of data processing. The prediction effectiveness of commonly used multiple linear regression analysis is always not ideal but regression accuracy will be evidently increased after pre-processing of the calculated weight, deviation and favorability on gamma-ray spectrometric data. This system can establish more than ten models at the same time which enable users to have more choice. Tree structure and Chinese menu prompting are adopted in this system which can be utilized separately, sub-systems at different levels can be also individually operated. It can be transplanted to data processing of other similar geological deposit models (including non-gamma ray spectrometric data). The system is rapid, accurate, simple, convenient and flexible in use, more practical and easily popularized

  1. The use of car-borne gamma-ray spectrometric survey in a basin

    International Nuclear Information System (INIS)

    Liu Tengyao; Lu Shili; Luo Zongquan.

    1985-01-01

    This paper describes the geological results in a basin in the Inner Mongolia which were obtained by using our newly-developed and assembled car-borne gamma-ray spectrometric system. Combined with the work of regional geology and remote sensing, five relatively favourable uranium zones were located within the working area. The field procedures of car-borne gamma-ray spectrometry for less rigid regions is discussed. The gamma-ray spectrometric profiling is mainly used for regional reconnaissance. In the case of enhanced anomalious radioactivity the profiling with varying directions is adopted and the data are plotted on scale 1:50000 topographic map. It is suggested that the car-borne gamma-ray spectrometric system can be calibrated both by the pads specified for portable spectrometers and by testing site when the calibration facility for the car-borne gamma-ray spectrometric system is not available. The effect of rainfall on car-borne gamma-ray spectrometric survey and the simplified field qualitative determination of U-Ra disequilibrium are also briefly discussed

  2. Specific high-performance liquid chromatographic assay with ultraviolet detection for the determination of 1-(2-chloroethyl)-3-sarcosinamide-1-nitrosourea in plasma.

    Science.gov (United States)

    Supko, J G; Phillips, L R; Malspeis, L

    1996-03-03

    .1 micrograms/ml, exhibited R.S.D. values ranging from 1.3 to 4.7%. Thermospray-ionization MS detection was used to definitively establish the specificity of the method. The sensitivity of the assay was shown by application to be more than adequate for characterizing the plasma pharmacokinetics of SarCNU in mice.

  3. Accurate quantification of sphingosine-1-phosphate in normal and Fabry disease plasma, cells and tissues by LC-MS/MS with (13)C-encoded natural S1P as internal standard.

    Science.gov (United States)

    Mirzaian, Mina; Wisse, Patrick; Ferraz, Maria J; Marques, André R A; Gabriel, Tanit L; van Roomen, Cindy P A A; Ottenhoff, Roelof; van Eijk, Marco; Codée, Jeroen D C; van der Marel, Gijsbert A; Overkleeft, Herman S; Aerts, Johannes M

    2016-08-01

    We developed a mass spectrometric procedure to quantify sphingosine-1-phosphate (S1P) in biological materials. The use of newly synthesized (13)C5 C18-S1P and commercial C17-S1P as internal standards rendered very similar results with respect to linearity, limit of detection and limit of quantitation. Caution is warranted with determination of plasma S1P levels. Earlier it was reported that S1P is elevated in plasma of Fabry disease patients. We investigated this with the improved quantification. No clear conclusion could be drawn for patient plasma samples given the lack of uniformity of blood collection and plasma preparation. To still obtain insight, plasma and tissues were identically collected from α-galactosidase A deficient Fabry mice and matched control animals. No significant difference was observed in plasma S1P levels. A significant 2.3 fold increase was observed in kidney of Fabry mice, but not in liver and heart. Comparative analysis of S1P in cultured fibroblasts from normal subjects and classically affected Fabry disease males revealed no significant difference. In conclusion, accurate quantification of S1P in biological materials is feasible by mass spectrometry using the internal standards (13)C5 C18-S1P or C17-S1P. Significant local increases of S1P in the kidney might occur in Fabry disease as suggested by the mouse model. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Atomic absorption spectrometric determination of mineral elements in mammalian bones

    International Nuclear Information System (INIS)

    Udoh, Anthony P.

    2000-01-01

    The phosphorus content of the major bones of male and female selected mammals was determined using the yellow vanadomolybdate colorimetric method. For each animal, the bone with the highest phosphorus content was used as pilot sample. Varying concentrations of strontium were added to solutions of the ashed pilot samples to minimize phosphorus interference in the determination of calcium and magnesium using flame atomic absorption spectrophotometry operated on the air-acetylene mode. At least 6,000 ppm (0.6%) of strontium was required to give optimum results for calcium. The amount of magnesium obtained from the analysis was not affected by the addition of strontium. With the incorporation of strontium in the sample solution, all elements of interest can be determined in the same sample solution. Based on this, a procedure is proposed for the determination of calcium and other elements in bones. Average recoveries of spiked calcium and magnesium were 97.85% and 98.16%, respectively at the 95% confidence level. The coefficients of variation obtained for replicate determinations using one of the samples were 0.00% for calcium, lead and sodium, 2.93% for magnesium, 3.27% for iron and 3.92% for zinc at the concentration levels found in that sample. Results from the proposed procedure compared well with those from classical chemical methods at the 95% confidence level. It is evident that calcium phosphorus, magnesium and sodium which are the most abundant elements in the bones are distributed in varying amounts both in the different types of bones and different animal species, although the general trend is Ca > P > Na > Mg for each bone considered. The calcium - phosphorus ratio is generally 3:1. The work set out to propose an atomic absorption spectrometric method for the multi-element analysis of mammalian bones with a single sample preparation and to study the distribution pattern of these elements in the bones. (Author)

  5. Interpretation of Spectrometric Measurements of Active Geostationary Satellites

    Science.gov (United States)

    Bedard, D.; Wade, G.

    2014-09-01

    Over 5000 visible near-infrared (VNIR) spectrometric measurements of active geostationary satellites have been collected with the National Research Council (NRC) 1.8m Plaskett telescope located at the Dominion Astrophysical Observatory (DAO) in Victoria, Canada. The objective of this ongoing experiment is to study how reflectance spectroscopy can be used to reliably identify specific material types on the surface of artificial Earth-orbiting objects. Active geostationary satellites were selected as the main subjects for this experiment since their orientation is stable and can be estimated to a high-level of confidence throughout a night of observation. Furthermore, for most geostationary satellites, there is a wide variety of sources that can provide some level of information as to their external surface composition. Notwithstanding the high number of measurements that have been collected to date, it was assumed that the experimenters would have a much greater success rate in material identification given the choice experimental subjects. To date, only the presence of aluminum has been confidently identified in some of the reflectance spectra that have been collected. Two additional material types, namely photovoltaic cells and polyimide film, the first layer of multi-layer insulation (MLI), have also been possibly identified. However uncertainties in the reduced spectral measurements prevent any definitive conclusion with respect to these materials at this time. The surprising lack of results with respect to material identification have forced the experimenters to use other data interpretation methods to characterize the spectral scattering characteristics of the studied satellites. The results from this study have already led to improvements in the ways that reflectance spectra from spacecraft are collected and analysed. Equally important, the data interpretation techniques elaborated over the course of this experiment will also serve to increase the body of

  6. Elemental speciation via high-performance liquid chromatography combined with inductively coupled plasma atomic emission spectroscopic detection: application of a direct injection nebulizer

    International Nuclear Information System (INIS)

    LaFreniere, K.E; Fassel, V.A.; Eckels, D.E.

    1987-01-01

    An evaluation is presented of a direct injection nebulizer (DIN) interfaced to a high-performance liquid chromatograph (HPLC) with inductively coupled plasma atomic emission spectroscopic (ICP-AES) detection for simultaneous multielement speciation. The limits of detection (LODs) obtained with the DIN interface in the HPLC mode were found to be comparable to those obtained by continuous-flow sample introduction into the ICP, or inferior by up to only a factor of 4. In addition, the DIN allowed for the direct injection into the ICP of a variety of common HPLC solvents (up to 100% methanol, acetonitrile, methyl isobutyl ketone, pyridine, and water). The HPLC-DIN-ICP-AES system was compared to other HPLC-atomic spectroscopic detection techniques and was found to offer substantial improvement over the alternative on-line, detection methods in terms of LODs. Representative applications of the HPLC-DIN-ICP-AES system to the elemental speciation of coal process streams, shale oil, solvent refined coal, and crude oil are presented

  7. Detection of left ventricular enlargement and impaired systolic function with plasma N-terminal pro brain natriuretic peptide concentrations

    DEFF Research Database (Denmark)

    Grønning, Bjørn Aaris; Nilsson, Jens C.; Søndergaard, Lars

    2002-01-01

    overlap in the range of plasma levels between healthy subjects and subjects with heart failure. We hypothesized that imprecision of the reference method (ie, the echocardiographic evaluation of left ventricular [LV] function) may have affected results from those earlier studies. We therefore wanted...... to investigate the diagnostic potential of NT-proBNP with magnetic resonance imaging as the reference method for the cardiac measurements. METHODS: Forty-eight patients with stable symptomatic heart failure in New York Heart Association functional classifications II to IV were examined once with blood samples...

  8. Catalyst-free „click” functionalization of polymer brushes preserves antifouling properties enabling detection in blood plasma

    Czech Academy of Sciences Publication Activity Database

    Parrillo, Viviana; de los Santos Pereira, Andres; Riedel, Tomáš; Rodriguez-Emmenegger, C.

    2017-01-01

    Roč. 971, 8 June (2017), s. 78-87 ISSN 0003-2670 R&D Projects: GA ČR(CZ) GJ15-09368Y; GA MŠk(CZ) LQ1604; GA MŠk(CZ) ED1.1.00/02.0109 Grant - others:OPPK(XE) CZ.2.16/3.1.00/21545 Program:OPPK Institutional support: RVO:61389013 Keywords : affinity optical biosensors * blood plasma * fouling Subject RIV: CD - Macromolecular Chemistry OBOR OECD: Polymer science Impact factor: 4.950, year: 2016

  9. Rydberg gas theory of a glow discharge plasma: I. Application to the electrical behaviour of a fast flowing glow discharge plasma.

    Science.gov (United States)

    Mason, Rod S; Mitchell, David J; Dickinson, Paul M

    2010-04-21

    Current-voltage (I-V) curves have been measured, independent of the main discharge, for electricity passing through the steady state fast flowing 'afterglow' plasma of a low power dc glow discharge in Ar. Voltage profiles along the axial line of conduction have been mapped using fixed probes and potentiometry, and the mass spectra of cations emerging from the downstream sampling Cone, also acting as a probe anode, were recorded simultaneously. Floating double probe experiments were also carried out. The electrical behavior is consistent with the well established I-V characteristics of such discharges, but does not comply with classical plasma theory predictions. The plasma decays along the line of conduction, with a lifetime of approximately 1 ms, despite carrying a steady state current, and its potential is below that of the large surface area anode voltage; a situation which cannot exist in the presence of a conventional free ion-electron plasma, unless the electron temperature is super cold. Currents, large by comparison with the main discharge current, and independent of it, are induced to flow through the downstream plasma, from the Anode (acting as a cathode) to the anodic ion exit Cone, induced by electron impact ionisation at the anode, but without necessarily increasing the plasma density. It appears to be conducted by direct charge transfer between a part of the anode surface (acting as cathode to the auxiliary circuit) and the plasma, without secondary electron emission or heating, which suggests the direct involvement of Rydberg atom intermediates. The reaction energy defect (= the work function of the electrode surface) fits with the plasma potential threshold observed for the cathodic reaction to occur. A true free ion-electron plasma is readily detected by the observation of cations at the anode surface, when induced at the downstream anode, at high bias voltages, by the electron impact ionisation in the boundary region. In contrast to the classical

  10. Mass Spectrometric Investigation of Silicon Extremely Enriched in (28)Si: From (28)SiF4 (Gas Phase IRMS) to (28)Si Crystals (MC-ICP-MS).

    Science.gov (United States)

    Pramann, Axel; Rienitz, Olaf

    2016-06-07

    A new generation of silicon crystals even further enriched in (28)Si (x((28)Si) > 0.999 98 mol/mol), recently produced by companies and institutes in Russia within the framework of a project initiated by PTB, were investigated with respect to their isotopic composition and molar mass M(Si). A modified isotope dilution mass spectrometric (IDMS) method treating the silicon as the matrix containing a so-called virtual element (VE) existing of the isotopes (29)Si and (30)Si solely and high resolution multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) were applied in combination. This method succeeds also when examining the new materials holding merely trace amounts of (29)Si (x((29)Si) ≈ 5 × 10(-6) mol/mol) and (30)Si (x((30)Si) ≈ 7 × 10(-7) mol/mol) extremely difficult to detect with lowest uncertainty. However, there is a need for validating the enrichment in (28)Si already in the precursor material of the final crystals, silicon tetrafluoride (SiF4) gas prior to crystal production. For that purpose, the isotopic composition of selected SiF4 samples was determined using a multicollector magnetic sector field gas-phase isotope ratio mass spectrometer. Contaminations of SiF4 by natural silicon due to storing and during the isotope ratio mass spectrometry (IRMS) measurements were observed and quantified. The respective MC-ICP-MS measurements of the corresponding crystal samples show-in contrast-several advantages compared to gas phase IRMS. M(Si) of the new crystals were determined to some extent with uncertainties urel(M) < 1 × 10(-9). This study presents a clear dependence of the uncertainty urel(M(Si)) on the degree of enrichment in (28)Si. This leads to a reduction of urel(M(Si)) during the past decade by almost 3 orders of magnitude and thus further reduces the uncertainty of the Avogadro constant NA which is one of the preconditions for the redefinition of the SI unit kilogram.

  11. Automated colorimetric in situ hybridization (CISH) detection of immunoglobulin (Ig) light chain mRNA expression in plasma cell (PC) dyscrasias and non-Hodgkin lymphoma.

    Science.gov (United States)

    Beck, Rose C; Tubbs, Raymond R; Hussein, Mohamad; Pettay, James; Hsi, Eric D

    2003-03-01

    Immunohistochemistry (IHC) is frequently used to detect plasma cell (PC) or B cell monoclonality in histologic sections, but its interpretation is often confounded by background staining. We evaluated a new automated method for colorimetric in situ hybridization (CISH) detection of clonality in PC dyscrasias and small B cell lymphomas. Cases of PC dyscrasia included multiple myeloma (MM; 31 cases), plasmacytoma (seven cases), or amyloidosis (one case), while cases of lymphoma included small lymphocytic (three cases), marginal zone (four cases), lymphoplasmacytic (three cases), and mantle cell lymphomas (three cases). Tissue sections were stained for kappa and lambda light chains by IHC and for light chain mRNA by automated CISH using haptenated probes. Twenty-eight of 31 MM cases had detectable light chain restriction by IHC. Thirty of 31 MM cases demonstrated light chain restriction by CISH, including 2 cases with uninterpretable IHC and one case of nonsecretory myeloma, which was negative for light chains by IHC. Seven of 7 plasmacytoma cases had detectable light chain restriction by CISH, including one case of nonsecretory plasmacytoma in which IHC was noninformative. Automated CISH demonstrated monoclonality in 9 of 13 cases of B cell non-Hodgkin lymphoma and had a slightly higher sensitivity than IHC (6 of 13 cases), especially in cases of lymphoplasmacytic and marginal zone lymphoma. Overall, there were no discrepancies in light chain restriction results between IHC, CISH, or serum paraprotein analysis. Automated CISH is useful in detecting light chain expression in paraffin sections and appeared superior to IHC for light chain detection in PC dyscrasias and B cell non-Hodgkin lymphomas, predominantly due to lack of background staining.

  12. Low-activity spectrometric gamma-ray logging technique for delineation of coal/rock interfaces in dry blast holes

    International Nuclear Information System (INIS)

    Asfahani, J.; Borsaru, M.

    2007-01-01

    A low-activity spectrometric gamma-ray logging technique is proposed in this paper as a sensitive tool for the delineation of coal/rock interfaces in dry blast holes. The advantages and superiority of this technique over traditional micro-density non-spectrometric gamma-ray tools are demonstrated

  13. Stability and linearity control of spectrometric channels of the Cherenkov counters using controllable units

    International Nuclear Information System (INIS)