LC-MSMS快速测定生物检材中乌头碱的含量.PDF

LC-MS/MS 快速测定生物检材中乌头碱的含量 高瞰，邢俊家( 中国医科大学附属第一医院药剂科，沈阳 110001) 摘要： 目的 建立快速测定生物检材中乌头碱的 LC-MS/MS 方法。方法 生物检材经乙醚-二氯甲烷(3 ∶2)提取后，用 Venusil Mp-C18 柱进行分离，采用 ESI 多反应监测(MRM)扫描方式。结果 测定的线性范围为 3~5 000 ng·mL1 ，RSD1.8% ， 日间和日内精密度分别为 2.5%和 4.6% ，提取回收率为 85.61%~89.04%。结论 该方法简便、快捷，适用于生物检材中乌 头碱的快速测定。 关键词：乌头碱；LC-MS/MS ；生物检材 中图分类号：R917.103 文献标志码：B 文章编号：1007-7693(2010)08-0729-03 A Rapid Method for Determination of Aconitine in Biology Samples by LC-MS/MS GAO Kan, XING Junjia(The First Affiliated Hospital of China Medical University, Shenyang 110001, China) ABSTRACT: OBJECTIVE To develop a rapid method for determination of aconitine in biology samples by LC-MS/MS. METHODS Aconitine and the internal standard tramadol were extracted from biology samples using diethyl ether -dichloromethane (3 ∶2), and separated on a Venusil Mp-C18 column. Detection was carried out by multiple reaction monitoring (MRM) on a Q-trapTM LC-MS/MS system with an ESI interface in the positive ion mode. RESULTS The linear arrang was 35 000 ng·mL1. The accuracy was 1.8% and the intra- and inter-day precision were 2.5% and 4.6%, respectively. The recovery was between 85.61% and 89.04%. CONCLUSION This method is simple and rapid, which can be used for the determination of aconitine in biology samples by LC-MS/MS. KEY WORDS: aconitine; LC-MS/MS; biology samples 川乌、草乌、附子等为毛茛科乌头属植物， 液沉淀血浆中的蛋白，大大增加了基质效应，增 具有抗炎、镇痛、局部麻醉等作用。但该属中药 加了内源性物质的干扰，也容易使精密的仪器和 所含乌头碱(aconitine) 既是有效成分又是剧毒成 色谱柱受到污染。 分，其治疗量与致毒、致死量接近，加之对药物 本试验报道了生物检材(血、尿、肝、肾、胃 耐受性的个体差异及药物炮制等原因，常引起乌 内容) 中测定乌头碱浓度的 LC-MS/MS 分析方法。 头碱中毒[1] 。 仅取 50 L 或 0.5 g 的生物样品，采用乙醚-二氯甲 目前已经报道的乌头碱在生物检材中的检测 烷(3 ∶2)提取，提取回收率高，且大大降低了基质 方 法 有 H