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LC-MS/MS法测定大鼠知母皂苷B-Ⅱ的血药浓度

Determination of timosaponin B-Ⅱ plasma concentration in rats by LC-MS /MS

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【作者】 陈宝婷冯怡林爱华刘奕明徐茹

【Author】 CHEN Bao-ting,Feng Yi,LIN Ai-hua,LIU Yi-ming,XU Ru(Guangdong Provincial Hospital of Chinese Medicine Afiliated,Guangzhou University of Chinese Medicine,Guangzhou 510120,China)

【机构】 广州中医药大学附属广东省中医院

【摘要】 目的建立LC-MS/MS法测定知母皂苷B-Ⅱ在大鼠血浆中的浓度。方法以人参皂苷Rg2为内标,血浆样品用固相萃取法处理,色谱柱为AgilentXDB-C8柱(2.1 mm×150 mm,5μm);流动相为乙腈-2 mmol·L-1乙酸铵(55∶45);流速250μL·min-1,用电喷雾离子化和负离子多离子反应监测(MRM)方式检测知母皂苷B-Ⅱ。结果该方法知母皂苷B-II的线性范围为3~3000ng·mL-1,LLOQ为3 ng·mL-1,批内、批间相对标准偏差均≤9.1%,提取回收率为(89.33±5.09)%~(96.85±6.62)%。结论该方法准确、灵敏、特异、简便,适用于血浆知母皂苷B-II浓度测定。

【Abstract】 Objective To establish a LC-MS /MS method for the determination of timosaponin B-Ⅱ in rat plasma.Methods Ginsenoside Rg2 was used as the internal standard.Plasma samples were pretreated by solid phase extraction.Chromatographic separation was carried out on Agilent XDB-C8column by isocratic elution with acetonitrile-2 mmol.L-1ammonium acetate(55 ∶ 45) with a flow rate of 250 μL.min-1.Timosaponin B-Ⅱ was detected by the negative electrospray ionization MS method in multiple reaction monitoring mode.Results The calibration curve of tmosaponin B-II in plasma was linear in the range of 3 3000 ng.mL-1,the lower limit of quantitation was 3 ng.mL-1,and inter-day and intra-day RSDs were less than 9.1%.The extract recovery was(89.33 ± 5.09) %-(96.85 ± 6.62) %.Conclusion This assay method is accurate,sensitive,and specific,which is suitable for the measurement of plasma timosaponin B-II concentration in rats.

【基金】 广东省科技计划基金资助项目(2009B080701023);广东省科技厅基金资助项目(2010B030700078);广东省自然科学基金资助项目(8151040701000014)
  • 【文献出处】 中国临床药理学杂志 ,The Chinese Journal of Clinical Pharmacology , 编辑部邮箱 ,2013年06期
  • 【分类号】R285
  • 【被引频次】3
  • 【下载频次】238
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