SPE-LC-MS/MS测定生物检材中4-甲氧基甲基安非他明  

Determination of 4-methoxymethamphetamine in biological specimens by SPE-LC-MS / MS

作　　者：朱焕慧[1] 梁敏思[2] 

机构地区：[1]广州市刑事科学技术研究所,广东广州510030 [2]中山大学测试中心,广东广州510275

出　　处：《中国法医学杂志》2015年第5期471-474,共4页Chinese Journal of Forensic Medicine

摘　　要：目的建立全血和尿液中4-甲氧基甲基安非他明（PMMA）的液相色谱-质谱（LC-MS/MS）联用检测方法。方法血液、尿液添加样本经MCX柱固相萃取（SPE）后,采用电喷雾正离子模式离子化、多反应监测模式检测PMMA,外标法定量,并对PMMA和甲基安非他明（MA）进行比较,对方法学指标进行考察。结果采用SPE-LC-MS/MS法,血液和尿液中PMMA含量在0.1-100μg/L范围内呈良好的线性关系,相关系数R2为0.998 8（血液,n=6）和0.999 5（尿液,n=6）;标准回收率分别为71%-80%（血液）和76%-89%（尿液）,日内与日间精密度均小于6%。PMMA的方法检测限（LOD）0.03μg/L,定量下限（LOQ）为0.1μg/L。结论采用本文SPE-LC-MS/MS方法,可对血液和尿液中PMMA准确定性,且检出限低,回收率高,选择性强,可适用于相关毒品检验。Objective This research was aimed to establish a method of liquid chromatography-tandem mass spectrometry for determination of 4-methoxymethamphetamine in whole blood and urine. Methods Both blood and urine spiked samples were extracted using MCX solid phase extraction. Following solid phase extraction,the analytes were confirmed and quantified by MS / MS with external standard in the multiple reaction monitoring（ MRM） mode via positive electrospray ionization mode. In addition,a comparison of the method between PMMA and MA was assessed. A LC-MS / MS method for the determination of PMMA was developed and validated. Results Using SPE-LC-MS / MS,an excellent linearity was observed in the range of 0. 1 ~ 100μg / L for both whole blood and urine,with the coefficient of correlation（ R2） of 0. 998 8and 0. 999 5,respectively（ n = 6）. Recoveries were in the range of 71% to 80% for blood and 76% to89% for urine with intra and interassay precisions of less than 6%. The limits of detection（ LOD） was0. 03μg / L and limits of quantitation（ LOQ） was 0. 1μg / L. Conclusion A proper assay with high recovery and selectivity was found for the quantization of PMMA in whole blood and urine sample. The present method was proved to be reliable for drug screening in forensic toxicological analysis.

关 键 词：法医毒物分析 4-甲氧基甲基安非他明 固相萃取 液相色谱-质谱 生物检材 

分 类 号：D919[医药卫生—法医学]