LC-MS/MS法测定动物血清中射干合剂多指标成分的浓度  

Determination of Multiple Index Components in Shegan Mixtures in Animal Serum by LC-MS/MS

作　　者：唐跃年[1] 陈婷[1] 魏昕[1] 陆晓彤[1] 金樑[1] 孙朝荣[1] 胡松浩[1] 杨传敏[1] 张健[1] 

机构地区：[1]上海交通大学医学院附属新华医院药剂科,上海200092

出　　处：《中国药师》2013年第2期190-193,共4页China Pharmacist

基　　金：上海市科委基金(编号:11D21972500);上海交通大学医学院科技基金((编号:JYY0905);上海市卫生局中医药科研基金(编号:2012G003A)

摘　　要：目的:建立测定动物血清中射干合剂多指标成分的液相色谱-串联质谱(LC-MS/MS)方法。方法:血清样品中加入内标(硫利达嗪),甲醇直接沉淀;用Capcell C_(18)MGⅢ(2.0 mm×100 mm,5μm);流动相为水:乙腈(95:5)梯度洗脱,流量为0.3 ml·min^(-1),扫描方式为正离子多离子反应监测(MRM),黄芩苷、黄芩素、汉黄芩素、射干苷、次野鸢尾黄素、盐酸麻黄碱和内标硫利达嗪的离子选择通道分别为m/z 447.2→271.2、271.2→123.2、285.2→270.2、463.2→301.2、387.1→357.1、166.2→148.2、371.2→126.2。结果:黄芩苷、黄芩素、汉黄芩素、射干苷、次野鸢尾黄素、盐酸麻黄碱的线性范围为0.01～500.00μg·L^(-1),定量下限为0.01μg·L^(-1),提取回收率均大于90%,批内、批间RSD均小于10%。结论:本法操作简便,特异性强,灵敏度高,取血量少,符合生物样品的分析要求,可用于射干合剂中多指标成分在动物体内的药动学研究。Objective： To establish an LC-MS/MS method for the determination of the components in Shegan mixtures in animal serum. Method： The samples were analyzed using thioridazine as the internal standard. After extracted from serum by methyl alcohol, the samples were separated on a Capcell C18 MGIII（2.0 mm × 100 mm, 5 μm） column with water-acetonitrile （95：5 ） as the mobile phase with gradient elution at a flow rate of 0.3 ml min- 1. The detection was carried out by multiple reaction monitoring in the posi- tive ion mode. The ion channel of baicalin, baicalein, wogonin, belamcandin, risflorentin, ephedrine hydrochloride and thioridazine was m/z 447.2→271.2,271.2→123.2, 285.2→270.2, 463.2→301.2,387.1→357.1, 166.2→148.2 and 371.2-→126.2, re- spectively. Result： The linear range of baicalin, baicalein, wogonin, belamcandin, irisflorentin and ephedrine hydrochloride was 0.01- 500.00 μg L - 1 with the limit of quantification of 0.01 μg L - 1. The method recovery was above 90%, and RSD was less than 10%. Conclusion： The method is simple, accurate and sensitive in the determination of Shegan mixtures. It is suitable for the pharmacoki- netic study of the preparation.

关 键 词：液相色谱-串联质谱法 黄酮类化合物 麻黄碱 射干合剂 

分 类 号：R969.1[医药卫生—药理学]