论文部分内容阅读
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 a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of multiple components of Shegan Mixture in animal serum. Methods: Serum samples were treated with internal standard (thioridazine) and precipitated directly with methanol. The mobile phase was eluted with a gradient of Capcell C 18 MGⅢ (2.0 mm × 100 mm, 5 μm) and a mobile phase of water (95: 5) , The flow rate was 0.3 ml · min ~ (-1) and the scanning mode was positive ion multi-ion reaction monitoring (MRM), baicalin, baicalein, wogonin, cantharidin, The ion-selective channels for the standard thioridazine were 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 respectively. Results: The linear range of baicalin, baicalein, wogonin, cantharidin, suberecticitrin, ephedrine hydrochloride was 0.01 ~ 500.00μg · L -1, the lower limit of quantification was 0.01μg · L ~ (- 1), the extraction recovery rate is greater than 90%, intra-batch, inter-batch RSD were less than 10%. Conclusion: The method is simple, specific, sensitive, less blood, in line with the analysis of biological samples, and can be used for pharmacokinetic studies of multiple indicators in Shegan Mixture in animals.