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  1 / 17958 MEDLINE  
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[PMID]:29446276
[Au] Autor:Yudina TV; Fedorova NE; Larkina MV; Egorchenkova OE; Rogacheva CK
[Ti] Título:[Determination of residual amounts of chlorothalonil in peaches: problems of gas chromatographic identification with the use of electron capture detector].
[So] Source:Gig Sanit;95(11):1108-12, 2016.
[Is] ISSN:0016-9900
[Cp] País de publicação:Russia (Federation)
[La] Idioma:rus
[Ab] Resumo:In the work there are presented results of studies on the validation of the gas chromatographic (GC) methodfor the determination of chlorothalonil residue amounts in peaches with the use of electron capture detector (ECD). For the analytical control there was selected such stone fruit crop as the peach, referring to the crops, the most contaminated with residue amounts ofpesticides. There was justified the necessity of the inclusion in the procedure of the detection of the method of confirmation, based on mass spectrometry detection (MSD) (the type of ionization - electron impact). The significant source of the obtaining of incorrect data in the identification with the use of ECD of ions are shown to be phthalates, visualized in the chromatogram as intense and/or broad peaks. Mass spectra of compounds of the class ofphthalates are characterized by the dominant peak of the ion with the value of (mass/ charge) 149, just on this peak the detection of low molecular weight phthalates occurs in various matrices, on the spectrum there are also recorded typical ions corresponding to fragments of radical residues. The combination of the use of various types of the detection allows to prove that the revealed response (detector signal) is caused just by the analyte, but not the impurities, and optionally to optimize chromatographic conditions towards to the obtaining reliable results. The lower limit of the quantitation of chlorothalonil in peach fruits accounts for 0.01 mg/kg, determined with a signal/noise ratio of 10. The range of measured concentrations is volatile between 0.01-0.1 mg/kg, recovery rate of chlorothalonil from samples of peaches, established according to results of the analysis of model samples with the introduction of the substance in four points along the detection range, was 84-102%, the SD value of the repeatability varies in the range of 2.0-5.8%.
[Mh] Termos MeSH primário: Contaminação de Alimentos/análise
Cromatografia Gasosa-Espectrometria de Massas/métodos
Nitrilos/análise
Prunus persica/química
[Mh] Termos MeSH secundário: Fungicidas Industriais/análise
Seres Humanos
Limite de Detecção
Resíduos de Praguicidas/análise
Reprodutibilidade dos Testes
[Pt] Tipo de publicação:JOURNAL ARTICLE
[Nm] Nome de substância:
0 (Fungicides, Industrial); 0 (Nitriles); 0 (Pesticide Residues); J718M71A7A (tetrachloroisophthalonitrile)
[Em] Mês de entrada:1803
[Cu] Atualização por classe:180309
[Lr] Data última revisão:
180309
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:180216
[St] Status:MEDLINE


  2 / 17958 MEDLINE  
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[PMID]:29438379
[Au] Autor:Säll A; Corbee D; Vikström S; Ottosson F; Persson H; Waldemarson S
[Ad] Endereço:Department of Immunotechnology, Lund University, Lund, Sweden.
[Ti] Título:Advancing the immunoaffinity platform AFFIRM to targeted measurements of proteins in serum in the pg/ml range.
[So] Source:PLoS One;13(2):e0189116, 2018.
[Is] ISSN:1932-6203
[Cp] País de publicação:United States
[La] Idioma:eng
[Ab] Resumo:There is a great need for targeted protein assays with the capacity of sensitive measurements in complex samples such as plasma or serum, not the least for clinical purposes. Proteomics keeps generating hundreds of biomarker candidates that need to be transferred towards true clinical application through targeted verification studies and towards clinically applicable analysis formats. The immunoaffinity assay AFFIRM (AFFInity sRM) combines the sensitivity of recombinant single chain antibodies (scFv) for targeted protein enrichment with a specific mass spectrometry readout through selected reaction monitoring (SRM) in an automated workflow. Here we demonstrate a 100 times improved detection capacity of the assay down to pg/ml range through the use of oriented antibody immobilization to magnetic beads. This was achieved using biotin-tagged scFv coupled to streptavidin coated magnetic beads, or utilizing the FLAG tag for coupling to anti-FLAG antibody coated magnetic beads. An improved multiplexing capacity with an 11-plex setup was also demonstrated compared to a previous 3-plex setup, which is of great importance for the analysis of panels of biomarker targets.
[Mh] Termos MeSH primário: Proteínas Sanguíneas/análise
Cromatografia de Afinidade/métodos
[Mh] Termos MeSH secundário: Seres Humanos
Limite de Detecção
Espectrometria de Massas em Tandem
[Pt] Tipo de publicação:JOURNAL ARTICLE; RESEARCH SUPPORT, NON-U.S. GOV'T
[Nm] Nome de substância:
0 (Blood Proteins)
[Em] Mês de entrada:1803
[Cu] Atualização por classe:180309
[Lr] Data última revisão:
180309
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:180214
[St] Status:MEDLINE
[do] DOI:10.1371/journal.pone.0189116


  3 / 17958 MEDLINE  
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[PMID]:29377915
[Au] Autor:VanInsberghe M; Zahn H; White AK; Petriv OI; Hansen CL
[Ad] Endereço:Michael Smith Laboratories, University of British Columbia, Vancouver, British Columbia, Canada.
[Ti] Título:Highly multiplexed single-cell quantitative PCR.
[So] Source:PLoS One;13(1):e0191601, 2018.
[Is] ISSN:1932-6203
[Cp] País de publicação:United States
[La] Idioma:eng
[Ab] Resumo:We present a microfluidic device for rapid gene expression profiling in single cells using multiplexed quantitative polymerase chain reaction (qPCR). This device integrates all processing steps, including cell isolation and lysis, complementary DNA synthesis, pre-amplification, sample splitting, and measurement in twenty separate qPCR reactions. Each of these steps is performed in parallel on up to 200 single cells per run. Experiments performed on dilutions of purified RNA establish assay linearity over a dynamic range of at least 104, a qPCR precision of 15%, and detection sensitivity down to a single cDNA molecule. We demonstrate the application of our device for rapid profiling of microRNA expression in single cells. Measurements performed on a panel of twenty miRNAs in two types of cells revealed clear cell-to-cell heterogeneity, with evidence of spontaneous differentiation manifested as distinct expression signatures. Highly multiplexed microfluidic RT-qPCR fills a gap in current capabilities for single-cell analysis, providing a rapid and cost-effective approach for profiling panels of marker genes, thereby complementing single-cell genomics methods that are best suited for global analysis and discovery. We expect this approach to enable new studies requiring fast, cost-effective, and precise measurements across hundreds of single cells.
[Mh] Termos MeSH primário: Reação em Cadeia da Polimerase Multiplex/métodos
[Mh] Termos MeSH secundário: Limite de Detecção
Microfluídica/instrumentação
[Pt] Tipo de publicação:JOURNAL ARTICLE; RESEARCH SUPPORT, NON-U.S. GOV'T
[Em] Mês de entrada:1803
[Cu] Atualização por classe:180309
[Lr] Data última revisão:
180309
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:180130
[St] Status:MEDLINE
[do] DOI:10.1371/journal.pone.0191601


  4 / 17958 MEDLINE  
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[PMID]:29264676
[Au] Autor:Faraji H; Helalizadeh M; Kordi MR
[Ad] Endereço:Department of Chemistry, Varamin-Pishva Branch, Islamic Azad University, Varamin, 338177489, Iran. hakimfaraji@yahoo.com.
[Ti] Título:Overcoming the challenges of conventional dispersive liquid-liquid microextraction: analysis of THMs in chlorinated swimming pools.
[So] Source:Anal Bioanal Chem;410(2):605-614, 2018 Jan.
[Is] ISSN:1618-2650
[Cp] País de publicação:Germany
[La] Idioma:eng
[Ab] Resumo:A rapid, simple, and sensitive approach to the analysis of trihalomethanes (THMs) in swimming pool water samples has been developed. The main goal of this study was to overcome or to improve the shortcomings of conventional dispersive liquid-liquid microextraction (DLLME) and to maximize the realization of green analytical chemistry principles. The method involves a simple vortex-assisted microextraction step, in the absence of the dispersive solvent, followed by salting-out effect for the elimination of the centrifugation step. A bell-shaped device and a solidifiable solvent were used to simplify the extraction solvent collection after phase separation. Optimization of the independent variables was performed by using chemometric methods in three steps. The method was statistically validated based on authentic guidance documents. The completion time for extraction was less than 8 min, and the limits of detection were in the range between 4 and 72 ng L . Using this method, good linearity and precision were achieved. The results of THMs determination in different real samples showed that in some cases the concentration of total THMs was more than threshold values of THMs determined by accredited healthcare organizations. This method indicated satisfactory analytical figures of merit. Graphical Abstract A novel green microextraction technique for overcoming the challenges of conventional DLLME. The proposed procedure complies with the principles of green/sustainable analytical chemistry, comprising decreasing the sample size, making easy automation of the process, reducing organic waste, diminishing energy consumption, replacing toxic reagents with safer reagents, and enhancing operator safety.
[Mh] Termos MeSH primário: Microextração em Fase Líquida/métodos
Piscinas
Trialometanos/análise
Poluentes Químicos da Água/análise
[Mh] Termos MeSH secundário: Halogenação
Limite de Detecção
Solventes
Trialometanos/isolamento & purificação
Água/análise
Poluentes Químicos da Água/isolamento & purificação
[Pt] Tipo de publicação:JOURNAL ARTICLE; VALIDATION STUDIES
[Nm] Nome de substância:
0 (Solvents); 0 (Trihalomethanes); 0 (Water Pollutants, Chemical); 059QF0KO0R (Water)
[Em] Mês de entrada:1803
[Cu] Atualização por classe:180309
[Lr] Data última revisão:
180309
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:171222
[St] Status:MEDLINE
[do] DOI:10.1007/s00216-017-0762-3


  5 / 17958 MEDLINE  
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[PMID]:29214539
[Au] Autor:Barroso PJ; Martín J; Santos JL; Aparicio I; Alonso E
[Ad] Endereço:Department of Analytical Chemistry, Escuela Politécnica Superior, University of Seville, C/ Virgen de África 7, 41011, Seville, Spain.
[Ti] Título:Analytical method for the evaluation of the outdoor air contamination by emerging pollutants using tree leaves as bioindicators.
[So] Source:Anal Bioanal Chem;410(2):417-428, 2018 Jan.
[Is] ISSN:1618-2650
[Cp] País de publicação:Germany
[La] Idioma:eng
[Ab] Resumo:In this work, an analytical method, based on sonication-assisted extraction, clean-up by dispersive solid-phase extraction and determination by liquid chromatography-tandem mass spectrometry, has been developed and validated for the simultaneous determination of 15 emerging pollutants in leaves from four ornamental tree species. Target compounds include perfluorinated organic compounds, plasticizers, surfactants, brominated flame retardant, and preservatives. The method was optimized using Box-Behnken statistical experimental design with response surface methodology and validated in terms of recovery, accuracy, precision, and method detection and quantification limits. Quantification of target compounds was carried out using matrix-matched calibration curves. The highest recoveries were achieved for the perfluorinated organic compounds (mean values up to 87%) and preservatives (up to 88%). The lowest recoveries were achieved for plasticizers (51%) and brominated flame retardant (63%). Method detection and quantification limits were in the ranges 0.01-0.09 ng/g dry matter (dm) and 0.02-0.30 ng/g dm, respectively, for most of the target compounds. The method was successfully applied to the determination of the target compounds on leaves from four tree species used as urban ornamental trees (Citrus aurantium, Celtis australis, Platanus hispanica, and Jacaranda mimosifolia). Graphical abstract Analytical method for the biomonitorization of emerging pollutants in outdoor air.
[Mh] Termos MeSH primário: Poluentes Atmosféricos/análise
Fluorcarbonetos/análise
Folhas de Planta/química
Extração em Fase Sólida/métodos
Espectrometria de Massas em Tandem/métodos
Árvores/química
[Mh] Termos MeSH secundário: Poluição do Ar/análise
Cromatografia Líquida de Alta Pressão/métodos
Citrus/química
Biomarcadores Ambientais
Retardadores de Chama/análise
Limite de Detecção
Plastificantes/análise
Sonicação/métodos
Tensoativos/análise
Ulmaceae/química
[Pt] Tipo de publicação:EVALUATION STUDIES; JOURNAL ARTICLE
[Nm] Nome de substância:
0 (Air Pollutants); 0 (Environmental Biomarkers); 0 (Flame Retardants); 0 (Fluorocarbons); 0 (Plasticizers); 0 (Surface-Active Agents)
[Em] Mês de entrada:1803
[Cu] Atualização por classe:180309
[Lr] Data última revisão:
180309
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:171208
[St] Status:MEDLINE
[do] DOI:10.1007/s00216-017-0733-8


  6 / 17958 MEDLINE  
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[PMID]:29214538
[Au] Autor:Akbarzade S; Chamsaz M; Rounaghi GH; Ghorbani M
[Ad] Endereço:Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Mashhad, Iran.
[Ti] Título:Zero valent Fe-reduced graphene oxide quantum dots as a novel magnetic dispersive solid phase microextraction sorbent for extraction of organophosphorus pesticides in real water and fruit juice samples prior to analysis by gas chromatography-mass spectrometry.
[So] Source:Anal Bioanal Chem;410(2):429-439, 2018 Jan.
[Is] ISSN:1618-2650
[Cp] País de publicação:Germany
[La] Idioma:eng
[Ab] Resumo:A selective and sensitive magnetic dispersive solid-phase microextraction (MDSPME) coupled with gas chromatography-mass spectrometry was developed for extraction and determination of organophosphorus pesticides (Sevin, Fenitrothion, Malathion, Parathion, and Diazinon) in fruit juice and real water samples. Zero valent Fe-reduced graphene oxide quantum dots (rGOQDs@ Fe) as a new and effective sorbent were prepared and applied for extraction of organophosphorus pesticides using MDSPME method. In order to study the performance of this new sorbent, the ability of rGOQDs@ Fe was compared with graphene oxide and magnetic graphene oxide nanocomposite by recovery experiments of the organophosphorus pesticides. Several affecting parameters in the microextraction procedure, including pH of donor phase, donor phase volume, stirring rate, extraction time, and desorption conditions such as the type and volume of solvents and desorption time were thoroughly investigated and optimized. Under the optimal conditions, the method showed a wide linear dynamic range with R-square between 0.9959 and 0.9991. The limit of detections, the intraday and interday relative standard deviations (n = 5) were less than 0.07 ngmL , 4.7, and 8.6%, respectively. The method was successfully applied for extraction and determination of organophosphorus pesticides in real water samples (well, river and tap water) and fruit juice samples (apple and grape juice). The obtained relative recoveries were in the range of 82.9%-113.2% with RSD percentages of less than 5.8% for all the real samples.
[Mh] Termos MeSH primário: Sucos de Frutas e Vegetais/análise
Grafite/química
Compostos Organofosforados/análise
Praguicidas/análise
Microextração em Fase Sólida/métodos
Poluentes Químicos da Água/análise
Água/análise
[Mh] Termos MeSH secundário: Cromatografia Gasosa-Espectrometria de Massas/métodos
Ferro/química
Limite de Detecção
Compostos Organofosforados/isolamento & purificação
Oxirredução
Óxidos/química
Praguicidas/isolamento & purificação
Pontos Quânticos/química
Poluentes Químicos da Água/isolamento & purificação
[Pt] Tipo de publicação:JOURNAL ARTICLE; VALIDATION STUDIES
[Nm] Nome de substância:
0 (Organophosphorus Compounds); 0 (Oxides); 0 (Pesticides); 0 (Water Pollutants, Chemical); 059QF0KO0R (Water); 7782-42-5 (Graphite); E1UOL152H7 (Iron)
[Em] Mês de entrada:1803
[Cu] Atualização por classe:180309
[Lr] Data última revisão:
180309
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:171208
[St] Status:MEDLINE
[do] DOI:10.1007/s00216-017-0732-9


  7 / 17958 MEDLINE  
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[PMID]:29214535
[Au] Autor:Mijangos L; Ziarrusta H; Olivares M; Zuloaga O; Möder M; Etxebarria N; Prieto A
[Ad] Endereço:Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080, Bilbao, Spain.
[Ti] Título:Simultaneous determination of 41 multiclass organic pollutants in environmental waters by means of polyethersulfone microextraction followed by liquid chromatography-tandem mass spectrometry.
[So] Source:Anal Bioanal Chem;410(2):615-632, 2018 Jan.
[Is] ISSN:1618-2650
[Cp] País de publicação:Germany
[La] Idioma:eng
[Ab] Resumo:A new procedure using polyethersulfone (PES) microextraction followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis was developed in this work for the simultaneous determination of 41 multiclass priority and emerging organic pollutants including herbicides, hormones, personal care products, and pharmaceuticals, among others, in seawater, wastewater treatment plant (WWTP) effluents, and estuary samples. The optimization of the analysis included two different chromatographic columns and different variables (polarity, fragmentor voltage, collision energy, and collision cell accelerator) of the mass spectrometer. In the case of PES extraction, ion strength of the water, pH, addition of EDTA, and the amount of the polymeric material were thoroughly investigated. The developed procedure was compared with a previously validated one based on a standard solid-phase extraction (SPE). In contrast to the SPE protocol, the PES method allowed a cost-efficient extraction of complex aqueous samples with lower matrix effect from 120 mL of water sample. Satisfactory and comparable apparent recovery values (80-119 and 70-131%) and method quantification limits (MQLs, 0.4-26 and 0.2-23 ng/L) were obtained for PES and SPE procedures, respectively, regardless of the matrix. Repeatability values lower than 27% were obtained. Finally, the developed methods were applied to the analysis of real samples from the Basque Country and irbesartan, valsartan, acesulfame, and sucralose were the analytes most often detected at the highest concentrations (51-1096 ng/L). Graphical abstract Forty-one multiclass pollutant determination in environmental waters by means of PES/SPE-LC-MS/MS.
[Mh] Termos MeSH primário: Herbicidas/análise
Hormônios/análise
Preparações Farmacêuticas/análise
Polímeros/química
Extração em Fase Sólida/métodos
Sulfonas/química
Espectrometria de Massas em Tandem/métodos
Poluentes Químicos da Água/análise
[Mh] Termos MeSH secundário: Cromatografia Líquida/métodos
Estuários
Limite de Detecção
Água do Mar/análise
Águas Residuais/análise
[Pt] Tipo de publicação:JOURNAL ARTICLE; VALIDATION STUDIES
[Nm] Nome de substância:
0 (Herbicides); 0 (Hormones); 0 (Pharmaceutical Preparations); 0 (Polymers); 0 (Sulfones); 0 (Waste Water); 0 (Water Pollutants, Chemical); 25667-42-9 (polyether sulfone)
[Em] Mês de entrada:1803
[Cu] Atualização por classe:180309
[Lr] Data última revisão:
180309
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:171208
[St] Status:MEDLINE
[do] DOI:10.1007/s00216-017-0763-2


  8 / 17958 MEDLINE  
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[PMID]:29184992
[Au] Autor:Le T; Zhang Z; Wu J; Shi H; Cao X
[Ad] Endereço:College of Life Science, Chongqing Normal University, Chongqing, 401331, China. hnxylt@163.com.
[Ti] Título:A fluorescent immunochromatographic strip test using a quantum dot-antibody probe for rapid and quantitative detection of 1-aminohydantoin in edible animal tissues.
[So] Source:Anal Bioanal Chem;410(2):565-572, 2018 Jan.
[Is] ISSN:1618-2650
[Cp] País de publicação:Germany
[La] Idioma:eng
[Ab] Resumo:A rapid, simple, and sensitive fluorescent immunochromatographic strip test (ICST) based on quantum dots (QDs) has been developed to detect 1-aminohydantoin (AHD), a major metabolite of nitrofurantoin in animal tissues. To achieve this, QD-labeled antibody conjugates, which consist of CdSe/ZnS QDs and monoclonal antibodies, were prepared by an activated ester method. Under optimal conditions, with the nitrophenyl derivative of AHD as the target, the ICST had a linear range from 0.1 to 100 ng/mL, with a correlation coefficient of 0.9656 and a 50% inhibitory concentration of 4.51 ng/mL. The limit of detection was 0.14 ng/g, which was below the minimum required performance limit of 1 µg/kg for AHD established by the European Commission. The recoveries for AHD ranged from 81.5% to 108.2%, with coefficients of variation below 13%, based on intraday and interday analysis. Furthermore, for AHD in real samples, the ICST showed high reliability and high correlation with liquid chromatography-tandem mass spectrometry (correlation coefficient of 0.9916). To the best of our knowledge, this is the first report of a novel and sensitive method based on a fluorescent ICST to detect AHD below the minimum required performance limit. The ICST demonstrated high reliability, and could be ideally suited for rapid, simple, and on-site screening of AHD contamination in animal tissues. Graphical abstract A rapid, simple, and sensitive fluorescent immunochromatographic strip test that is based on quantum dots was developed to detect 1-aminohydantoin (AHD), a major metabolite of nitrofurantoin in animal tissues. 2-NBA 2-nitrobenzaldehyde, NP nitrophenyl.
[Mh] Termos MeSH primário: Anticorpos Imobilizados/química
Análise de Alimentos/métodos
Contaminação de Alimentos/análise
Hidantoínas/análise
Imunocromatografia/instrumentação
Pontos Quânticos/química
Fitas Reagentes/análise
[Mh] Termos MeSH secundário: Animais
Anticorpos Monoclonais/química
Desenho de Equipamento
Peixes
Fluorescência
Imunocromatografia/métodos
Limite de Detecção
Reprodutibilidade dos Testes
[Pt] Tipo de publicação:EVALUATION STUDIES; JOURNAL ARTICLE
[Nm] Nome de substância:
0 (1-aminohydantoin); 0 (Antibodies, Immobilized); 0 (Antibodies, Monoclonal); 0 (Hydantoins); 0 (Reagent Strips)
[Em] Mês de entrada:1803
[Cu] Atualização por classe:180309
[Lr] Data última revisão:
180309
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:171130
[St] Status:MEDLINE
[do] DOI:10.1007/s00216-017-0756-1


  9 / 17958 MEDLINE  
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[PMID]:28455844
[Au] Autor:Keshet U; Alon T; Fialkov AB; Amirav A
[Ad] Endereço:School of Chemistry, Tel Aviv University, Tel Aviv, 69978, Israel.
[Ti] Título:Open Probe fast GC-MS - combining ambient sampling ultra-fast separation and in-vacuum ionization for real-time analysis.
[So] Source:J Mass Spectrom;52(7):417-426, 2017 Jul.
[Is] ISSN:1096-9888
[Cp] País de publicação:England
[La] Idioma:eng
[Ab] Resumo:An Open Probe inlet was combined with a low thermal mass ultra-fast gas chromatograph (GC), in-vacuum electron ionization ion source and a mass spectrometer (MS) of GC-MS for obtaining real-time analysis with separation. The Open Probe enables ambient sampling via sample vaporization in an oven that is open to room air, and the ultra-fast GC provides ~30-s separation, while if no separation is required, it can act as a transfer line with 2 to 3-s sample transfer time. Sample analysis is as simple as touching the sample, pushing the sample holder into the Open Probe oven and obtaining the results in 30 s. The Open Probe fast GC was mounted on a standard Agilent 7890 GC that was coupled with an Agilent 5977A MS. Open Probe fast GC-MS provides real-time analysis combined with GC separation and library identification, and it uses the low-cost MS of GC-MS. The operation of Open Probe fast GC-MS is demonstrated in the 30-s separation and 50-s full analysis cycle time of tetrahydrocannabinol and cannabinol in Cannabis flower, sub 1-min analysis of trace trinitrotoluene transferred from a finger onto a glass surface, vitamin E in canola oil, sterols in olive oil, polybrominated flame retardants in plastics, alprazolam in Xanax drug pill and free fatty acids and cholesterol in human blood. The extrapolated limit of detection for pyrene is <1 fg, but the concentration is too high and the software noise calculation is untrustworthy. The broad range of compounds amenable for analysis is demonstrated in the analysis of reserpine. The possible use with alternate standard GC-MS and Open Probe fast GC-MS is demonstrated in the analysis of heroin in its street drug powder. The use of Open Probe with the fast GC acting as a transfer line is demonstrated in <10-s analysis without separation of ibuprofen and estradiol. Copyright © 2017 John Wiley & Sons, Ltd.
[Mh] Termos MeSH primário: Cromatografia Gasosa-Espectrometria de Massas/instrumentação
Cromatografia Gasosa-Espectrometria de Massas/métodos
Compostos Orgânicos/análise
[Mh] Termos MeSH secundário: Ionização do Ar
Seres Humanos
Limite de Detecção
Preparações Farmacêuticas/análise
Preparações Farmacêuticas/química
Drogas Ilícitas/análise
Drogas Ilícitas/química
Vácuo
[Pt] Tipo de publicação:JOURNAL ARTICLE
[Nm] Nome de substância:
0 (Organic Chemicals); 0 (Pharmaceutical Preparations); 0 (Street Drugs)
[Em] Mês de entrada:1803
[Cu] Atualização por classe:180309
[Lr] Data última revisão:
180309
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:170430
[St] Status:MEDLINE
[do] DOI:10.1002/jms.3941


  10 / 17958 MEDLINE  
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[PMID]:29441912
[Au] Autor:Wu JX; Zhang G; Song M; Liu M; Liang JL; Xu JL; Shang F; Qi P
[Ti] Título:Determination of gamithromycin in an injection by ultra-performance liquid chromatography-tandem quadrupole-time-of-flight mass spectrometry.
[So] Source:Pharmazie;71(7):378-381, 2016 Jul 07.
[Is] ISSN:0031-7144
[Cp] País de publicação:Germany
[La] Idioma:eng
[Ab] Resumo:In this study, a sensitive and precise method was developed for the determination of gamithromycin in an injection using ultra-performance liquid chromatography-tandem quadrupole-time-of-flight mass spectrometry (UPLC-QTOF-MS) and the results were compared with a similar analysis for the ion fragments of gamithromycin in MS/ MS. The sample was dissolved in methanol then filtered and separated on a C18 column using acetonitrile-0.1% formic acid (containing 2 mmol/L ammonium acetate) as the mobile phase. The flow rate was 0.4 mL/min and the column temperature was 40 °C. The mass spectrometry conditions were electrospray ionization (ESI) operated in positive ion full scan mode and quantified using external calibration. Subsequently, ion fragments of the MS/MS were compared and analyzed. The linear range was 10 ∼ 200 µg/L with a correlation coefficient of 0.9992. The limit of detection (LOD) was 0.77 µg/L and the limit of quantitation (LOQ) was 2.55 µg/L. The average recoveries of the intra-assay were 98.8%-105.6% with a relative standard deviation ranging from 1.79% to 2.38% and the inter-assay were 89.3%-110.7% with a relative standard deviation ranging from 4.93% to 6.27%. After the comparative analysis of the fragments with a Molecular Structure Correlator, the score of the total matching degree reached 83.19 and the scores of each ion fragment matching degree were all greater than 90, which supplied the basis for the confirmation of gamithromycin. The results indicated that the method was simple, sensitive and precise and could be applied in the determination of gamithromycin in real samples.
[Mh] Termos MeSH primário: Antibacterianos/análise
Macrolídeos/análise
[Mh] Termos MeSH secundário: Cromatografia Líquida de Alta Pressão
Indicadores e Reagentes
Limite de Detecção
Padrões de Referência
Reprodutibilidade dos Testes
Espectrometria de Massas por Ionização por Electrospray
Espectrometria de Massas em Tandem
[Pt] Tipo de publicação:JOURNAL ARTICLE; RESEARCH SUPPORT, NON-U.S. GOV'T
[Nm] Nome de substância:
0 (Anti-Bacterial Agents); 0 (Indicators and Reagents); 0 (Macrolides); ZE856183S0 (gamithromycin)
[Em] Mês de entrada:1803
[Cu] Atualização por classe:180308
[Lr] Data última revisão:
180308
[Sb] Subgrupo de revista:IM
[Da] Data de entrada para processamento:180215
[St] Status:MEDLINE
[do] DOI:10.1691/ph.2016.6004



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