法医学杂志

法医学杂志 ›› 2010, Vol. 0 ›› Issue (3): 188-191.

• 论文 • 上一篇    下一篇

UPLC-MS/MS分析尿液中阿片类化合物

展长淑;沈保华;卓先义;   

  1. 苏州大学医学部法医学系;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;
  • 发布日期:2010-06-25 出版日期:2010-06-28

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

ZHAN CHANG-SHU1,2,SHEN BAO-HUA2,ZHUO XIAN-YI2(1.DEPARTMENT OF FORENSIC MEDICINE,MEDICAL COLLEGE OF SOOCHOW UNIVERSITY,SUZHOU 215123,CHINA;2.SHANGHAI KEY LABORATORY OF FORENSIC MEDICINE,INSTITUTE OF FORENSIC SCIENCE,MINISTRY OF JUSTICE,P.R.CHINA,SHANGHAI 2   

  • Online:2010-06-25 Published:2010-06-28

被引次数

5

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。

关键词: 法医毒理学, 可待因, 海洛因, 尿, UPLC-MS/MS

Abstract: 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.

Key words: forensic toxicology, codeine, heroin, urine, UPLC-MS/MS