Analysis of flumequine enantiomers in rat plasma by UFLC-ESI-MS/MS

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• 作者：Zhao-Hong Hu ; Yang-Guang Wang ; Huo-Xi Jin ; Xiao-Kun Ouyang and Wei-Jian Wu
• 刊名：Chirality
• 出版年：2016
• 出版时间：November 2016
• 年：2016
• 卷：28
• 期：11
• 页码：737-743
• 全文大小：375K
• ISSN：1520-636X

文摘

In this study the analysis and confirmation of flumequine enantiomers in rat plasma by ultra-fast liquid chromatography coupled with electron spray ionization mass spectrometry (using propranolol as an internal standard [IS]) was developed and validated. Plasma samples were prepared by liquid–liquid extraction using methyl tert-butyl ether as the extraction solvent. Direct resolution of the R- and S-isomers was performed on a CHIRALCEL OJ-RH column (4.6 × 150 mm, 5 μm) using acetonitrile / 0.1% formic acid / 1 mM ammonium acetate as the mobile phase. Detection was operated by electron spray ionization in the selected ion monitoring and positive ion mode. The target ions at m/z 262.1 and m/z 260.1 were selected for the quantification of the enantiomers and IS, respectively. The linear range was 0.5–500 ng/mL. The precisions (coefficient of variation, CV%) and recoveries were 1.43–8.68 and 94.24–106.76%, respectively. The lowest quantitation limit for both enantiomers is 0.5 ng/mL, which is sensitive enough to be applied to sample analysis in other related studies.