法医学杂志

法医学杂志 ›› 2008, Vol. 0 ›› Issue (4): 268-272.

• 论文 • 上一篇    下一篇

LC-MS/MS测定尿液中可卡因及其代谢物苯甲酰爱康宁

孙其然;向平;严慧;沈敏;   

  1. 复旦大学上海医学院法医系;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:2008-08-25 出版日期:2008-08-28

Simultaneous Analyses of Cocaine and its Metabolite Benzoylecgonine in Urine by LC-MS/MS

SUN QI-RAN1,2,XIANG PING2,YAN HUI1,2,SHEN MIN2(1.DEPARTMENT OF FORENSIC SCIENCE,SHANGHAI MEDICAL COLLEGE,FUDAN UNIVERSITY,SHANGHAI 200032,CHINA;2.SHANGHAI KEY LABORATORY OF FORENSIC MEDICINE,INSTITUTE OF FORENSIC SCIENCE,MINISTRY OF JUSTICE,P.R.CHINA,SHAN   

  • Online:2008-08-25 Published:2008-08-28

摘要： 目的建立尿液中可卡因(cocaine,COC)及其代谢物苯甲酰爱康宁(benzoylecgonine,BZE)的液相色谱-串联质谱分析方法。方法尿液经固相萃取后,用AllurePFP丙基柱分离,以V(甲醇):V(20mmol/L乙酸胺和0.1%甲酸的缓冲溶液)=80∶20为流动相,采用二级质谱多反应监测模式检测COC和BZE。按10mg/kg的剂量对豚鼠腹腔注射可卡因,给药后收集7d尿液。结果尿液中COC和BZE在2.0～100ng/mL质量浓度范围内线性关系良好(r=0.9995),最低检测限(LOD)为0.5ng/mL;回收率大于90%;日内和日间精密度均小于6%;豚鼠尿液中主要检测目标物是BZE,且BZE检测时限也较COC长。结论所建方法灵敏度高,选择性好,适用于尿液中可卡因和苯甲酰爱康宁的检测。

关键词: 法医毒理学, 色谱法, 高压液相, 串联质谱法, 固相萃取, 尿液, 可卡因, 苯甲酰爱康宁

Abstract: Objective To establish a liquid chromatography-tandem mass spectrometry(LC-MS/MS) method for the simultaneous analysis of cocaine(COC) and its metabolite benzoylecgonine(BZE) in urine samples.Methods A single dose of COC(10 mg/kg) was injected intraperitoneally into guinea pigs and urine samples were collected for 7 days.The urine samples were extracted by auto solid phase extraction(SPE),separated by the Allure PFP propyl column with a mobile phase consisting of methanol and 20 mmol/L ammonium acetate buffer 0.1% formic acid(80:20,V/V),and then analyzed by LC-MS/MS.Multiple reaction monitoring(MRM) mode was used to analyze COC(m/z 304.2→182.3,m/z 304.2→150.1) and BZE(m/z 290.2→168.3,m/z 290.2→105.0).Results COC and BZE showed a fairly good linearity over the range of 2.0～100 ng/mL(r=0.999 5).The detection limit was 0.5 ng/mL.The recovery rate was greater than 90% and the deviation of intra-and inter-day precision was less than 6%.BZE was the major target detected in urine samples,and its detection window was longer than COC.Conclusion This newly developed method shows high sensitivity and selectivity,and is suitable for the simultaneous analysis of cocaine and benzoylecgonine in urine samples.

Key words: forensic toxicology, chromatography, high pressure liquid, tandem mass spectrometry, solid phase extraction, urine, cocaine, benzoylecgonine