人血浆中螺内酯及其代谢物坎利酮的LC-MS测定.pdfVIP

• 842 • 中国民药工业杂志 Chinese Joumal of Phannaceuticals 2008 , 39 (11) 人血浆中螺内酣及其代谢物坎利酬的LC-MS测定 刘 萍，正本杰，魏春敏，在桂艳，郭瑞臣* (山东大学齐鲁医院l 临床药理研究所，山东济南25ω12) 摘要: ~章也了LC-MSr.去测定人血浆中的螺内酷(1) 及其代谢物坎利酬。)。以劳拉西伴(3) 为内标，乙酸L酶二氧阳炕 (4: 1) 为提取溶剂，采用C 桩，流动相为甲醇·水(65: 35). 采用大气压化学离子化源，选挥性监测质衔比(m!z) 为 18 34 1.2(1和2) 和32 1.0(3) 的离子峰。碎片电Æ分别为130V(1和2) 和140V(3) 。结巢~示1和2均在2-30Onglml浓度范闹内线 性关系良好，定量限为2.0nglml，日内、日间RSD均小子10% 。 关键词:蝶内酶:坎利酣1 劳拉回泞.;液相色谱帽质i普:测定 中朋分类号: TQ460.7+2; 0657.7+2 文献标识码:A 文章编号: 1001-8255 (2008) 11-0842-04 Detennination of Spironolactone and Its Metabolite Canrenone in Human Plasma by LC唰MS LIU Ping, WANG Ben-jie , WEI Chun咄in， YUAN Gui-yan, GUO Rui-chen* (Jnstitute 01Clínical Pharmacology, Qilu Hospital 01Shandong Universi.纱~ Jinan 250012) ABSTRACT: A LC-MS method was established for the determination of spironolactone (1) and its metabolite canrenone (2) in human plasma with lorazepam (3) as the intemal standard. 1 and 2 in plasma were ex:衍acted with ethyl acetate-dichlormethane (4: 1). A C18 column was used with mobile ph削e of methanol帽water (65: 35). The compounds were ionized in the atmospheric pressure chemical ionization (APC I) and detected in the selected ion monitoring (SIM) mode (m/z 34 1.2 for 1and 2, m/z 321.0 for 3) , and the fragment voltage of 130V for 1and 2, 140V for 3. The calibration curve was linear for 1 and 2 in the concentration range of 2 - 300nglml with the LLOQ of 2.仇19lml.白le intra.帽 and inter-day RSDs were less than 10%. Key Words: spironolactone; canrenone; lorazepam; LC-MS; determination 螺内酣(spironolactone， 1) 又称安体舒迎，是 1化学结构修饰和复合制剂研究较多，但1 原药 人工合成的简体化合物，结构与酵固酣相似(圈