大鼠胆汁中参松养心胶囊三种活性成分的UPLC-MSMS法测定.pdfVIP

中国医药工业杂志 Chinese Journal of Pharmaceuticals 2013 , 44 (1 0) • 1025 • 大鼠胆汁中参松养心胶囊三种活性成分的 UPLC-MS/MS 法测定 刘敏彦1 ，2 ，赵韶华2 ，李松2 ，王宏涛2 ，屠鹏飞1* (1 北京大学药学院天然药物及仿生药物国家重点实验室，北京 100191; 2. 石家庄以岭药业股份有限公司，河北石家庄 050035) 摘要:建立了超高效液相色谱串联质谱法测定大鼠灌胃给予参松养心胶囊后胆汁中的苟药营、斯皮诺素和五昧子甲 素。采用 Waters UPLC C8 色谱柱，乙腊-0.1% 甲酸为流动相，梯度洗脱，正离子多反应监测 (MRM) 。苟药营、斯皮 诺素和五味子甲素分别在24.6 ~ 1 720、 28.6 ~ 1430 和 2.8 ~ 700 ng/ml 范围内线性关系良好，提取回收率为 88.7%~ 100.9% ，基质效应为 91.28%~ 102.70% ，日内和日间 RSD 均小于 6.22% ，相对误差为一6.58 ~ 7.51 %。 关键词:参松养心胶囊:苟药背:斯皮诺素:五味子甲素:胆汁:超高效液相色谱串联质谱:测定 中图分类号: 0657.7+2; R969 文献标志码:A 文章编号: 1001-8255 (2013) 10-1025-04 Determination of Three Active Compounds of Shensong Yangxin Capsules in Rat Bile by UPLC-MS/M S 12 2 2 1 LIU Minyan . , ZHAO Shaohua , LI Song , WANG Hongta02 , TU Pengfei * (1. State Key Lab. ofNatural and Biomimetic Drngs, School ofPharmaceutical Science, Peking University. Beijing 100191; 2. Shijiazhuang Yìling Pharmaceutical Co., Ltd., Shijiazhuang 050035) ABSTRACT: An UPLC-MS/MS method was established for the determination of paeoniflorin , spinosin and deoxyschizandrin in rat bile after intragastric administration of Shensong Yangxin capsules. A Waters UPLC C18 column was used with the mobile phase of acetonitrile-O.l % formic acid by gradient elution. Electrospray ionization (ESI) source was employed and the three analytes were detected by multiple reaction monitoring (MRM) scanning under the positive ionization mode. The calibration curves for paeoniflorin , spinosin and deoxyschizandrin were linear in the concentration ranges of 24.6 - 1 720, 28.6 - 1 430 and 2.8 - 700 nglml , respectively. Their extraction recoveries were 88.7% - 100.9% and the matrix