Development of a sensitive and rapid method for quantitation of (S)-(-)- and (R)-(+)-metoprolol in human plasma by chiral LC–ESI–MS/MS

查看全文 作　　者：Primal [1,2]Sharma;Pritesh [2]Contractor;Swati [2]Guttikar;Daxesh [1]P.Patel;Pranav [1]S.Shrivastav

机构地区：[1]Department of Chemistry, School of Sciences, Gujarat University;[2]Bioanalytical Research Department, Veeda Clinical Research

出　　处：《Journal of Pharmaceutical Analysis》索引2014年第4卷第1期,共17页

摘　　要：A selective, sensitive and high throughput liquid chromatography-tandem mass spectrometry(LC–ESI–MS/MS) method has been developed for separation and quantification of metoprolol enantiomers on a chiral Lux Amylose-2(250 mm 4.6 mm, 5 mm) column. Solid phase extraction of(S)-()- and(R)-(t)-metoprolol and rac-metoprolol-d6 as an internal standard(IS)was achieved on Lichrosep DVB HL cartridges employing 200 mL human plasma. Both the analytes were chromatographically separated with a resolution factor of 2.24 using 15 mM ammonium acetate in water, pH 5.0 and 0.1%(v/v) diethyl amine in acetonitrile(50:50, v/v) as the mobile phase within 7.0 min. The precursor-product ion transitions for the enantiomers and IS were monitored in the multiple reaction monitoring and positive ionization mode. The method was validated over the concentration range of 0.500–500 ng/mL for both the enantiomers. Matrix effect was assessed by post-column analyte infusion experiment and the mean extraction recovery was greater than 94.0% for both the enantiomers at all quality control levels. The stability of analytes was evaluated in plasma and whole blood under different storage conditions. The method was successfully applied to a clinical study in 14 healthy volunteers after oral administration of200 mg metoprolol tablet under fasting conditions. The assay reproducibility is shown by reanalysis of 68 incurred samples. The suitability of the developed method was assessed in comparison 关键词：美多心安人血浆手性对映异构体多反应监测敏感色谱分离液相色谱

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Development of a sensitive and rapid method for quantitation of (S)-(-)- and (R)-(+)-metoprolol in human plasma by chiral LC–ESI–MS/MS

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