SPE-HPLC/MS/MS法检测人唾液中地西泮及其代谢物  

The simultaneous determination of diazepam and its metabolites in oral fluids by SPE-HPLC/MS/MS

作　　者：王乐乐[1] 任昕昕[2] 崔冠峰[2] 尉志文[1] 何毅[2] 丛斌[1,3] 刘耀[1,2] 贠克明[1] 

机构地区：[1]山西医科大学法医学院,山西太原030001 [2]公安部物证鉴定中心,北京100038 [3]河北医科大学法医学系,河北石家庄050017

出　　处：《中国法医学杂志》2016年第2期130-133,共4页Chinese Journal of Forensic Medicine

基　　金：十二五国家科技支撑计划项目(2012BAK02B02);国家自然科学基金(81172906);山西省科技攻关项目(20130313020-2)

摘　　要：目的采用固相萃取-高效液相色谱-串联质谱法(SPE-HPLC/MS/MS)检测人唾液中地西泮及其代谢物。方法采用固相萃取法(SPE)处理唾液,HPLC/MS/MS法检测,MRM记录方式,保留时间和定性离子对定性,内标法和标准曲线法定量。结果地西泮及其代谢物去甲地西泮、去甲羟基西泮、去甲羟基地西泮葡萄糖醛酸苷(OG)、羟基地西泮葡萄糖醛酸苷(TG)的检测限在0.01ng/m L^0.5ng/m L之间,线性范围0.1ng/m L或0.5ng/m L^100ng/m L,回收率为84.9%~106%。口服5mg地西泮后15d内唾液中可检出地西泮及去甲西泮,但检出时间有个体差异,但去甲羟基西泮、TG和OG则不能检出。结论 SPE-HPLC/MS/MS检测法可应用于人唾液中地西泮及其代谢物的检测。人口服常量地西泮后唾液中可检出地西泮和去甲西泮,且检测窗口期较宽,但存在个体差异。Objective To establish the analytical method of diazepam and its metabolites in oral fluids by SPE-HPLC / MS / MS. Methods Diazepam,nordiazepam,oxazepam,oxazepam glucuronide,temazepam glucuronide in oral fluids were extracted with a solid phase extraction（ SPE） and determined by HPLC / MS /MS. The qualitative analysis was based on retention time and MRM ions. The quantitative analysis was based on an internal standard method and calibration curve,in which estazolam was used as internal standard. Results For all analytes,LODs were 0. 01 ng / mL - 0. 5ng / mL,linear curve covered the range0. 1ng / mL or 0. 01 ng / mL - 0. 5ng / mL,recoveries were 84. 9% - 106%. Only diazepam and nordazepam could be detected in human saliva after a oral dose of 5mg diazepam in fifteen days. Conclusion It had showed that a simultaneous analysis of diazepam and its metabolites in oral fluids by SPE-HPLC / MS / MS was established with a reasonable LOQ,linear range and recovery,which can be used for determination of diazepam and its metabolites in saliva.

关 键 词：法医毒物分析 高效液相色谱-串联质谱 唾液 地西泮 代谢物 

分 类 号：D919[医药卫生—法医学]