LC-MS/MS测定血液中利眠宁成分  

Determination of Chlordiazepoxide in Blood Sample by LC-MS/MS

作　　者：孙会会 仲建军 翟晚枫[2] 

机构地区：[1]德州市公安局物证鉴定研究中心,山东德州253000 [2]公安部物证鉴定中心,北京100038

出　　处：《刑事技术》2016年第5期376-379,共4页Forensic Science and Technology

摘　　要：目的建立一种液相色谱一串联质谱（LC—MS／MS）方法对血液中利眠宁成分进行定性定量分析。方法采用LC—MS／MS的多反应监测模式，通过利眠宁的保留时间和两对母离子／子离子对进行分析。前处理利用乙腈作为沉淀剂，沉淀血液中的蛋白，振荡离心后，过有机微孔滤膜，上清液通过LC—MS／MS进行检测。结果通过该方法测定，血液中利眠宁成分在0．5～200ng／mL浓度范围内具有良好线性，相关系数达0．9987。该方法最低检出限0．1ng／mL，日内精密度在3％以下，日间精密度在4％以下，重现性好，回收率高。结论采用该方法检测血液中的利眠宁成分，快速、简便、准确、可靠，能够满足公安机关侦破利用利眠宁杀人、抢劫、强奸等案件的检验要求。Objective To develop and validate a sensitive, specific and rapid method for determining the chlordiazepoxide in blood sample by liquid chromatography-quadrupole ion trap mass spectrometry （LC-MS/MS）. Methods Chlordiazepoxide was qualitatively analyzed by its retention time and two ion pairs of precursor/product in multiple reaction monitoring （MRM） mode. The blood sample was precipitated with acetonitrile, and then oscillated and centrifugalized. After filtration with organic membrane, the supernatant was analyzed by LC-MS/MS. Results With the optimized method, the correlation coefficient of chlordiazepoxide was 0.9987 within the linear range of 0.5-200ng/mL. The limit of detection （LOD） for chlordiazepoxide in blood was 0.1ng/mL. The intra- and inter-day relative standard deviations （RSDs） were below 3% and 4%, respectively. The results of recovery met the acceptance criteria. Conclusion This method was simple, rapid, reliable and highly accurate for analysis of chlordiazepoxide in blood, suitable for chlordiazepoxide-invloved cases of murder, robbery and rape.

关 键 词：液相色谱-串联质谱 血液 利眠宁 

分 类 号：DF795.1[医药卫生—法医学]