UPLC-MS/MS分析尿液中阿片类化合物  

Simultaneous Determination of Opioid Compounds in Human Urine by UPLC-MS/MS

作　　者：展长淑[1,2] 沈保华[2] 卓先义[2] 

机构地区：[1]苏州大学医学部法医学系,江苏苏州215123 [2]司法部司法鉴定科学技术研究所上海市法医学重点实验室,上海200063

出　　处：《法医学杂志》2010年第3期188-191,共4页Journal of Forensic Medicine

基　　金：国家质检公益性行业科研专项(10-137);科研院所社会公益研究专项(GY0807)

摘　　要：目的建立尿液中同时分析可待因(codeine,COD)、6-单乙酰吗啡(6-monoacetylmorphine,6-MAM)、吗啡(morphine,MOR)、吗啡-3-葡萄糖醛酸苷(morphine-3-glucuronide,M3G)和吗啡-6-葡萄糖醛酸苷(morphine-6-glucuronide,M6G)的超高效液相色谱-串联质谱(UPLC-MS/MS)方法。方法以吗啡-d3(MOR-d3)和吗啡-3-葡萄糖醛酸苷-d3(M3G-d3)为内标,尿液用乙腈沉淀蛋白后,过SiroccoTM蛋白沉淀板,UPLC-MS/MS法分离检测。结果尿液中COD和MAM检出限为0.2 ng/mL,定量限为0.5 ng/mL;MOR、M3G和M6G检出限为0.5 ng/mL,定量限为1 ng/mL;线性相关系数r≥0.999 7;日内精密度和日间精密度均在10%以内;回收率70.0%～98.3%,基质效应50.5%～99.0%。结论所建方法简便、快速、准确,可以满足法庭毒物分析的需要。Objective To propose a method for simultaneous determination of codeine（COD）,6-monoacetyl-morphine（6-MAM）,morphine（MOR）,morphine-3-glucuronide（M3G） and morphine-6-glucuronide（M6G） in human urine by ultra performance liquid chromatography with tandem mass spectrometry（UPLC-MS/MS）.Methods After precipitation of protein by acetonitrile,the urine samples,with added the morphine-d3（MOR-d3） and morphine-3-Glucuronide-d3（M3G-d3） as internal standards,were pre-treated by SiroccoTM protein precipitation plate,and then analyzed by UPLC-MS/MS.Results The limit of detection was 0.2 ng/mL for both COD and MAM,the limit of quantitation was 0.5 ng/mL for both COD and MAM.The limit of detection was 0.5 ng/mL for MOR,M3G and M6G,the limit of quantitation was 1 ng/mL for them.The linear correlation coefficients were not less than 0.999 7,both the inter-day and intra-day precisions were less than 10%,the recoveries were in the range of 70.0% to 98.3%,the matrix effects were about 50.5% to 99.0%.Conclusion This proposed method is simple,rapid and accurate,it could be applied in forensic toxicological analysis.

关 键 词：法医毒理学 可待因 海洛因 尿 UPLC-MS/MS 

分 类 号：R446.12[医药卫生—诊断学]