液相色谱-串联质谱法检验全血中的斑蝥素  

Determination of cantharidin in blood by liquid chromatography-tandem mass spectrometry

作　　者：张蕾萍[1] 舒翠霞[2] 黄霜 崔冠峰[1] 于忠山[1] 何毅[1] 

机构地区：[1]公安部物证鉴定中心北京市现场物证检验工程技术研究中心,北京100038 [2]苏州市公安局,江苏苏州215000 [3]泰州公安局,江苏泰州225300

出　　处：《中国法医学杂志》2015年第2期125-127,共3页Chinese Journal of Forensic Medicine

基　　金："十二五"国家科技支撑计划课题(2012BAK02B02)

摘　　要：目的建立固相萃取-液相色谱/串联质谱法,用于分离检测全血中的斑蝥素。方法血液经HLB小柱固相萃取后,用电喷雾正离子模式离子化、多反应监测-信息依赖性采集-增强子离子扫描（MRM-IDA-EPI）模式检测斑蝥素,谱库检索分析,外标法定量。结果采用本文方法可有效分离血样中的斑蝥素,血中斑蝥素在5~200ng/m L范围内线性关系良好,相关系数为0.9972,最低检出限为2ng/m L,回收率为80%以上,日内与日间精密度均小于6%。结论本文所建方法简便、快速、分离度好,适用于生物样品中的检测。Objective To establish a method of solid phase extraction-liquid chromatography /tandem mass spectrometry for determination of cantharidin in blood. Methods Blood sample was extracted by using HLB solid phase extraction. The sample was confirmed and quantified by MS-MS in the multiple reaction monitoring（ MRM） mode via positive electrospray ionization mode and an enhanced product ion（ EPI） scan in an information dependent achanced（ IDA） experiment. Results Cantharidin in blood were separated well. Calibration curves were linear within the range of 5 - 200 ng / m L（ R^2= 0. 997 2）,and the limits of detection were 2ng / m L. The recoveries were more than 80%,the inter-day and intra-day precision were less than 6%. Conclusion This method is fast and good separated,and suitable for determination of cantharidin in blood.

关 键 词：法医毒物分析 斑蝥素 固相萃取 液相色谱-质谱 

分 类 号：D919[医药卫生—法医学]