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。
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 （10mg/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 2.0-100ng/mL （r=0.9995）. 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.
出处
《法医学杂志》
CAS
CSCD
2008年第4期268-272,共5页
Journal of Forensic Medicine
基金
科研院所社会公益研究专项资助项目(GY0601)
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
forensic toxicology, chromatography, high pressure liquid
tandem mass spectrometry
solid phase extraction
urine
cocaine
benzoylecgonine
