检索结果-南通市图书馆

A Validated Liquid Chromatography-Mass spectrometry Method for the Detection and Quantification of Oxidative Metabolites of 2,2',4,4'-Tetrabromodiphenyl Ether in Rat Hepatic Microsomes

引用

American Journal of Analytical Chemistry 2011年第3期2卷 352-362页

作者： sarah Catherine Moffatt Patrick Robert Edwards andrás szeitz stelvio Mario Bandiera 不详

In the present study, we developed and validated an analytical method using ultra performance liquid chromatography-mass spectrometry (UPLC/Ms) for the quantitative determination of 2,2',4,4'-tetrabromodiphenyl ether (BDE-47) metabolism by rat hepatic microsomes. BDE-47 is a brominated flame retardant that was widely used in a variety of consumer products and has subsequently been identified as a ubiquitous environmental contaminant. Hydroxy-bromodiphenyl ethers (OH-BDEs) were isolated from rat hepatic microsomes by liquid-liquid extraction. Chromatographic separation was achieved by UPLC on a C18 column with gradient elution using a mobile phase consisting of methanol and water, each containing 0.1% formic acid, at a flow rate of 0.2 mL/min. Detection and quantification were performed using a mass spectrometer in single ion recording mode with negative electrospray ionization. The UPLC/Ms method was validated for linearity, limit of quantification (LOQ), accuracy, precision and recovery. The weighted calibration curves (1/X2) were linear over a concentration range of 5 - 250 nM with LOQ values between 5 nM and 50 nM for the individual OH-BDEs. Intra- and inter- day accuracy (%DEV) and precision (%RsD) values ranged from –11.7% to 9.5% and 5.9% to 16.5%, respectively. Recovery values of 70% to 90% were obtained for all OH-BDEs. The validated method allowed us to successfully analyze metabolite formation following incubation of BDE-47 with hepatic microsomes prepared from phenobarbital-treated rats. Results demonstrate that the UPLC/Ms method has sufficient sensitivity and reproducibility to fully characterize the in vitro metabolism of BDE-47 and possibly other PBDEs.

关键词： BDE-47 Hepatic Metabolism Polybrominated Diphenyl Ethers Rat Hepatic Microsomes Ultra Performance Liquid Chromatography-Mass spectrometry

来源：

维普期刊数据库评论

在线全文

维普期刊数据库

学校读者我要写书评

暂无评论

A Validated Enantioselective Assay for the Determination of Ibuprofen in Human Plasma Using Ultra Performance Liquid Chromatography with Tandem Mass spectrometry (UPLC-Ms/Ms)

引用

American Journal of Analytical Chemistry 2010年第2期1卷 47-58页

作者： andrás szeitz andrea Nicole Edginton Henry Tao Peng Bob Cheung Kenneth Wayne Riggs 不详

A modified ultra performance liquid chromatography-tandem mass spectrometry (UPLC-Ms/Ms) method was developed and validated for the quantitation of ibuprofen enantiomers in human plasma. Ibuprofen and flurbiprofen (internal standard) were extracted from human plasma at acidic pH, using a single-step liquid-liquid extraction with methyl-tert-butyl ether. The enantiomers of ibuprofen and flurbiprofen were derivatized to yield the corresponding diastereomers. Chromatographic separation was achieved using a phenyl column with a run time of 20 min. (R)- and (s)-ibuprofen were quantitated at the multiple reaction monitoring (MRM) transition of m/z 360.2 ? 232.1, and (R)- and (s)-flurbiprofen were monitored at the MRM transition of m/z 398.3 ? 270.1. The method was validated for accuracy, precision, linearity, range, limit of quantitation (LOQ), limit of detection (LOD), selectivity, absolute recovery, matrix effect, dilution integrity, and evaluation of carry-over. Accuracy for (R)-ibuprofen ranged between –11.8% and 11.2%, and for (s)-ibuprofen between –8.6% and –0.3%. Precision for (R)-ibuprofen was ≤ 11.2%, and for (s)-ibuprofen ≤ 7.0%. The calibration curves were weighted (1/X2, n = 7) and were linear with r2 for (R)-ibuprofen ≥ 0.988 and for (s)-ibuprofen ≥ 0.990. The range of the method was 50 to 5000 ng/mL with the LOQ of 50 ng/mL, and LOD of 1 ng/mL, for (R)- and (s)-ibuprofen requiring 100 μL of sample. The method was applied successfully to a pharmacokinetic study with the administration of a single oral dose of ibuprofen capsules to human subjects.

关键词： Ibuprofen Enantiomers UPLC-Ms/Ms Human Plasma Method Validation Pharmacokinetics

来源：

维普期刊数据库评论

在线全文

维普期刊数据库

学校读者我要写书评

暂无评论

An Ultra-High Performance Liquid Chromatography-Tandem Mass spectrometry Method for the Quantification of Vancomycin Requiring Only 2 μL of Rabbit serum

引用

American Journal of Analytical Chemistry 2017年第9期8卷 553-563页

作者： Veronika schmitt andras szeitz Tara L.Klassen Urs O.Hafeli Faculty of Pharmaceutical sciences The University of British ColumbiaVancouverCanada

A highly sensitive ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-Ms/Ms) method was developed for the quantification of vancomycin (VAN) in low volumes of rabbit serum. For each analysis, 2 μL rabbit serum was precipitated with methanol that contained the internal standard teicoplanin (TEI). The supernatant was transferred into a 384 well-plate, diluted with water, covered with a pierceable silicone mat and 5 μL was analyzed in positive ionization mode. The UHPLC-Ms/Ms consisted of an Agilent 1290 Infinity UHPLC system connected to an AB sciex QTrap®5500 hybrid linear ion-trap triple quadrupole mass spectrometer equipped with a Turbo spray source. Chromatographic separation was achieved using a Waters Acquity UPLC BEH C18 (1.7 μm, 2.1 mm × 100 mm) column, a VanGuard (1.7 μm, 2.1 × 5 mm) guard column and a mobile phase of water and methanol both containing 5 mM ammonium acetate with 0.1% formic acid. VAN was quantified with multiple reaction monitoring using the transitions of m/z 725.5/144.2, and TEI was monitored at m/z 940.6/316.4. The accuracy, precision, linearity, range and lower limit of quantification (LLOQ) were determined. The accuracy was ≤9.93% and the precision was ≤10.6%. The range was established as 0.1 to 40 μg·mL-1. The LLOQ was 0.1 μg·mL-1 VAN requiring 2 μL of sample with an accuracy of -20.2% and precision of 8.39%. The method was applied successfully to determine the VAN concentrations in rabbit serum after the i.v. administration of VAN via implanted ear catheters.

关键词： Ultra-High Performance Liquid Chromatography-Tandem Mass spectrometry Vancomycin Rabbit serum Pharmacokinetics

来源：

维普期刊数据库评论

在线全文

维普期刊数据库

学校读者我要写书评

暂无评论

欢迎您,

建议与咨询留下您的常用邮箱和电话号码，以便我们向您反馈解决方案和替代方法

时间限定

文献类型

馆藏选择

核心期刊

语言

文献类型

帮助

文字说明：

检索规则说明：

检索范例：

分类表

所选分类

限定检索结果

文献类型

馆藏范围

日期分布

学科分类号

主题

机构

作者

语言

在线全文

在线全文

在线全文

请选择保存的检索档案：

请选择收藏分类：

通借通还

欢迎您,

建议与咨询 留下您的常用邮箱和电话号码，以便我们向您反馈解决方案和替代方法

时间限定

文献类型

馆藏选择

核心期刊

语言

文献类型

帮助

文字说明：

检索规则说明：

检索范例：

分类表

所选分类

限定检索结果

文献类型

馆藏范围

日期分布

学科分类号

主题

机构

作者

语言

在线全文

在线全文

在线全文

请选择保存的检索档案： 新增检索档案 确定 取消

请选择收藏分类： 新增自定义分类 确定 取消

通借通还

建议与咨询留下您的常用邮箱和电话号码，以便我们向您反馈解决方案和替代方法

请选择保存的检索档案：

请选择收藏分类：