摘要
目的建立UPLC-MS/MS测定大鼠血浆中柴胡皂苷B2、B4,并对柴胡皂苷B2、B4静脉给药后的药动学进行研究。方法以柴胡皂苷F为内标,采用UPLC BEH C_(18)(2.1 mm×50 mm,1.7μm)柱,柱温为40℃。流动相为乙腈-0.1%甲酸水溶液,梯度洗脱,流速为0.4mL·min^(-1),洗脱时间为4min,使用氮气作为去溶剂化气体(800L·h^(-1))和锥形气体(50 L·h^(-1))。MRM模式对柴胡皂苷B2 m/z 825.4→617.5、柴胡皂苷B4 m/z 957.6→649.6和柴胡皂苷F(内标)m/z 973.7→119.0进行定量分析。大鼠血浆用乙腈沉淀法去除蛋白。结果在5～5 000 ng·mL^(-1)内,大鼠血浆中柴胡皂苷B2、B4线性良好(r>0.995),定量下限为5ng·mL^(-1)。柴胡皂苷B2日内精密度RSD<12%,日间精密度RSD<15%。柴胡皂苷B4日内精密度RSD<14%,日间精密度RSD<15%。柴胡皂苷B2、B4的准确度范围为89.3%～110.2%。结论该分析方法灵敏、快速、选择性良好,并成功应用于柴胡皂苷B2、B4静脉给药后的大鼠药动学研究。
OBJECTIVE To establish a UPLC-MS/MS method for the determination of saikosaponin B2 and B4 in rat plasma. The pharmacokinetics of saikosaponin B2 and B4 after intravenous administration in rats were studied. METHODS Saikosaponin F was used as internal standard, UPLC BEH C18(2.1 mm×50 mm, 1.7μm) column was used and the column temperature was set at 40 ℃. The mobile phase was consisted of acetonitrile and water(containing 0.1% formic acid), gradient elution with the flow rate of 0.4 mL·min-1 for 4 min. Nitrogen was used as desolvation gas(800 L·h-1) and cone gas(50 L·h-1). MRM was used to quantitatively analyze saikosaponin B2 m/z 825.4→617.5, saikosaponin B4 m/z 957.6→ 649.6 and saikosaponin F(internal standard) m/z 973.7→119.0. Rat plasma samples were treated by acetonitrile precipitation to remove protein. RESULTS In the range of 5-5 000 ng·mL-1, the concentrations of saikosaponin B2 and B4 in rat plasma showed good linear relation ship(r>0.995), with the lower limit of quantification of 5 ng mL-1. Saikosaponin B2 had an intra-day RSD<12% and inter-day RSD<15%. Saikosaponin B4 had an intra-day RSD<14%, inter-day RSD<15%. The accuracy of saikosaponin B2 and B4 ranged from 89.3% to 110.2%. CONCLUSION The method is sensitive, rapid and selective, and successfully applied to the pharmacokinetics study of saikosaponin B2 and B4 after intravenous administration.
作者
李剑波
谢明华
LI Jianbo;XIE Minghua(Yuhang Branch, Second Affiliated Hospital of Zhejiang University, Hangzhou 311000, China)
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2019年第3期317-321,共5页
Chinese Journal of Modern Applied Pharmacy
基金
浙江省中医药科技计划项目(2016ZA170)
杭州市卫生科技计划项目(2016B36)
北京医卫健康公益基金会项目(YWJKJJHKYJJ-B17160)
