家兔血清、尿中甲基苯丙胺及其代谢产物苯丙胺的气相色谱/质谱分析  

Determination of methamphetamine and its main active metabolite amphetamine in serum and urine by GC/MS

作　　者：王玉瑾[1] 张昀[1] 贾娟[1] 王英元[1] 

机构地区：[1]山西医科大学法医学院,山西太原030001

出　　处：《中国医院药学杂志》2007年第3期296-299,共4页Chinese Journal of Hospital Pharmacy

基　　金：山西省自然科学基金资助项目(20011066);山西高校科技研究开发项目(20041319)

摘　　要：目的：建立血清、尿中甲基苯丙胺（MA）及其主要活性代谢产物苯丙胺（AP）的气相色谱／质谱（GC／MS）定性定量分析方法，探讨样品稳定性和家兔血、尿中AP和MA的比值关系。方法：样品中加入内标物丙基解痉素（SKR525A）后碱化，乙醚萃取，三氟醋酸酐衍生化，GC／MS法分析甲基苯丙胺和苯丙胺。结果：血清和尿中甲基苯丙胺与苯丙胺的线性范围分别为0．01～5．0mg·L^-1和0．1～50．0mg·L^-1；最低检出限为0．005mg·L^-1（S／N≥3）；提取回收率均大于74．3％；方法回收率为95．50％～103．16％；日内及日间RSD均小于10％。18h内苯丙胺与甲基苯丙胺在血、尿中比值分别为0．16～1．5和0．021～0．079。血清样品在室温和冷冻条件下存放24h甲基苯丙胺、苯丙胺的相对误差为5．3％～6．1％。结论：甲基苯丙胺中毒血清样品在室温和冷冻条件下稳定，建立的GC／MS分析方法同时测定血清和尿液中甲基苯丙胺及其主要代谢产物苯丙胺，方法简便、灵敏、重复性好，适用于甲基苯丙胺中毒与滥用案例的快速鉴定。OBJECTIVE To develop a qualitative and quantitative method for the simultaneous determination of methamphetamine（MA） and its main active metabolite amphetamine（AP） in serum and urine by GC/MS. To study the stability of specimens and the ratio of MA and AP in serum and urine. METHODS After adding SKF525A （internal standard, IS）, serum and urine samples were alkalized and extracted with diethyl ether, derivatized with trifluoroacetic anhydride （TFA）. The methamphetamine and amphetamine in serum and urine were analyzed by GC/MS. RESULTS The linear range for methamphetamine and amphetamine in serum and urine by GC/MS was 0. 01-5.0 mg·L^-1 and 0. 1-50. 0mg·L^-1 respectively. The limit of detection was 0. 005 mg·L^-1. The overall extraction recovery of the analytes in serum and urine were more than 74. 3 %. The analytical recovery were 95.50%-103. 16%;The inter-day and intra-day relative standard deviation were less than 10. 0%. The Ratio of AP and MA in serum and urine was 0. 16 - 1.50 and 0. 021 - 0. （179 in 18 h. The relative error of specimens reserved under 20 ℃ and - 20 ℃ was between - 5.3 % and 6. 1 %. CONCLUSION The specimens were stable under 20 ℃and - 20 ℃. The GC/MS method for the simultaneous determination of methamphetamine and its main metabolite amphetamine in biological materialis proved to be simple, sensitive and reproducible and could be applied to analyse intoxication and abuse cases of methamphetamine rapidly.

关 键 词：甲基苯丙胺 苯丙胺 气相色谱/质谱法 

分 类 号：R927[医药卫生—药学]