生物样品中去痛片4种成分及其8种代谢物的GC-MS/MS法检测  

Simultaneous determination of somedon and its metabolites by GC–MS/MS

作　　者：申亚男 贾娟[1] 郑锋[1] 范爱爱 尉志文[1] 刘耀[1,2] 傅善林 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]澳大利亚悉尼科技大学法庭科学研究中心

出　　处：《中国法医学杂志》2017年第6期573-577,587,共6页Chinese Journal of Forensic Medicine

基　　金：国家科技支撑计划项目(2007BAK26B05);科技基础性工作专项(2015FY111400);山西省回国留学人员科研资助项目(2014-032)

摘　　要：目的建立固相支撑液液萃取(supported liquid-liquid extraction,SLE),GC-MS/MS法同时测定生物样品中去痛片4种成分及其8种代谢物的方法,为去痛片相关案件的法医学鉴定提供依据。方法采用SLE萃取,GC-MS/MS检测,MRM记录方式,利用保留时间和离子对比例定性,内标法和工作曲线法定量,建立血液和组织中去痛片及其代谢物的GC-MS/MS检测方法。结果经SLE萃取,GC-MS/MS法同时检测大鼠血和组织中去痛片及其代谢物,萃取率为37.57%~95.87%,检测线性范围为0.12μg/m L^16.00μg/m L,相关系数(r)为0.989 6~0.999 7,LOD为0.23ng/m L^14.48ng/m L,检测准确度为79.63%~122.90%,日内和日间精密度分别为0.99%~7.43%和2.19%~10.6%。结论 SLE萃取、GC-MS/MS法可检测生物样品中去痛片成分及其代谢物,具有快速、简便、准确度和精密度高的特点,可应用于去痛片相关案件的法医学鉴定。Objective To develop a method of support liquid-liquid extraction（SLE） and simultaneous determination of 4 components in somedon and its 8 metabolites by GC–MS/MS.Methods Somedon and its metabolites were extracted by SLE and determined by GC-MS/MS in MRM mode.The qualitative analysis was based on retention time and ratio of ions.The quantitative analysis was based on internal standard method and calibration curve.Results After SLE and determination of 4 components in somedon and its 8 metabolites,the extraction rate were 37.57%~95.87%,the linear range were 0.12μg/m L^16.00μg/m L,the correlation coefficient（r）were 0.989 6~0.999 7,LOD were 0.08 ng/m L^14.48 ng/m L,the accuracy were 79.63%~122.90%,the interday and intraday precision were 0.99%~7.43% and 2.19%~10.60% respectively.Conclusion Simultaneous determination of somedon and its metabolites by GC–MS/MS in biological samples,which was rapid,simple,accurate and was high precision and recovery,can be used for qualitative and quantitative analysis in forensic cases.

关 键 词：法医毒物分析 去痛片 固相支撑液液萃取 GC-MS/MS 

分 类 号：D919[医药卫生—法医学]