大鼠血浆中积雪草酸氨丁三醇盐的LC-MSMS法测定.pdfVIP

中国医药工业杂志 Chinese Joumal of Pharmaceuticals 2014, 45 (1) • 63 • 大鼠血浆中积雪草酸氨丁三醇盐的 LC-MS瓜IS 法测定 顾玲玲l ，陈志祥l ，陆伟根1 ，刘全海2 ，刘 英2 (1.中国医药工业研究总院药物制剂国家工程研究中心，上海 200437; 2. 中国医药工业研究总院上海医药工业研究院，上海 200437) 摘要:建立了高效液相色谱，串联质谱法测定大鼠血浆中的积雪草酸氨丁三醇盐。采用 Kromasil C8 柱，以乙睛: 0.1% 甲酸为流动相，梯度洗脱，以醋酸泼尼松龙为内标， ESI 源负离子模式、多反应监测扫描，药物与内标的监测离子对为 mlz 533.00 → 487.25 和 m々 447.00 → 40 1.1 50 结果表明，药物在 10 ~ 1000 nglml 浓度范围内线性关系良好，批内和批间 RSD 均小于 10% 。低、中、高浓度标准血样的提取回收率分别为 77.3% 、 8 1.0%和 73.9% ， RSD 分别 12.3% 、 5.3%和 3.1% 。 关键词:积雪草酸氨丁三醇盐:高效液相色谱-串联质谱:测定 中图分类号: 0657.7+2 文献标志码:A 文章编号: 1001-8255 (2014) 01-0063-03 Determination ofAsiatic Acid Tromethamine in Rat Plasma by LC-MS岛fS 2 2 GU Lingling , CHEN Zhixiang , LU Weigen , LlU Quanhai , LlU Ying (1. National Pharmaceutical Engineering Research Center. China State Institute 01Pharmaceutical Indust.η\ Shanghai 200437; 2. Shanghai lnstitute 01Pharmaceutical lndustη China State lnstitute 01Pharmaceutical Industη Shanghai 200437) ABSTRACT: A LC-MS岛1S method was established for the determination of asiatic acid tromethamine (AAS) in rat plasma. A Kromasi1 C8 column was used with the mobile phase of acetonitrile : 0.1 % formic acid by gradient elution. Prednisolone acetate was used as the intemal standard. Samples were detected by electrospray negative ionization mass spectrometry and multiple-reaction monitoring mode. The transitions ofAAS and intemal standard were m/z 533.00• 487.25 and m/z 447.00• 40 1.15, respectively. The calibration cu凹e was linear in the concentration range of 10 - 1 000 ng/m 1. The inter- and intra-assay RSDs were less than 10%. The extraction recoveries of the standard blood samples oflow, mediu