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快速液相色谱-串联质谱法测定尿液中的苯丙胺、甲基苯丙胺、3,4-亚甲基二氧基苯丙胺、3,4-亚甲基二氧基甲基苯丙胺、3,4-亚甲基二氧基乙基苯丙胺、N-甲基-1-(3,4-亚甲基二氧基苯基)-2-丁胺和苯甲酰甲基芽子碱

Fast LC-MS/MS method for the determination of amphetamine, methamphetamine, MDA, MDMA, MDEA, MBDB and PMA in urine.

作者信息

Concheiro Marta, Simões Susana Maria dos Santos Sadler, Quintela Oscar, de Castro Ana, Dias Mário João Rodrigues, Cruz Angelines, López-Rivadulla Manuel

机构信息

Forensic Toxicology Service, Institute of Legal Medicine, University of Santiago de Compostela, C/San Francisco s/n, 15782 Santiago de Compostela, Spain.

出版信息

Forensic Sci Int. 2007 Aug 24;171(1):44-51. doi: 10.1016/j.forsciint.2006.10.004. Epub 2006 Nov 9.

Abstract

A fast method was designed for the simultaneous determination of amphetamine (A), methamphetamine (MA), PMA, MDA, MDMA, MDEA and MBDB in urine. The drugs were analysed by LC (ESI)-MS/MS, after a simple liquid-liquid extraction in the presence of the deuterated analogues. Reverse phase separation on an Atlantis dC18 Intelligent Speed column was achieved in less than 4 min under gradient conditions, and the total run time was 8 min. The method was fully validated, including linearity (1-1000 ng/mL for A, MDMA, MDEA and MBDB; 2-1000 ng/mL for MDA and PMA; 1-200 ng/mL for MA; r2>0.99 for all compounds), recovery (>80%), within-day and between-day precision and accuracy (CV and MRE<12.7% for intermediate level and ULOQ, and <17.2% for LLOQ), limit of detection (0.2 ng/mL for MDMA, MDEA and MBDB; 0.5 ng/mL for A, MA and PMA; 1 ng/mL for MDA) and quantitation (1 ng/mL for A, MA, MDMA, MDEA and MBDB; 2 ng/mL for MDA and PMA) and relative ion intensities. No matrix effect was observed. The procedure proved to be sensitive, specific and rapid, and was applied to real forensic cases.

摘要

设计了一种快速方法,用于同时测定尿液中的苯丙胺(A)、甲基苯丙胺(MA)、PMA、MDA、MDMA、MDEA和MBDB。在氘代类似物存在的情况下进行简单液液萃取后,通过LC(ESI)-MS/MS对这些药物进行分析。在梯度条件下,使用Atlantis dC18智能速度柱在不到4分钟内实现反相分离,总运行时间为8分钟。该方法经过全面验证,包括线性(A、MDMA、MDEA和MBDB为1-1000 ng/mL;MDA和PMA为2-1000 ng/mL;MA为1-200 ng/mL;所有化合物的r2>0.99)、回收率(>80%)、日内和日间精密度与准确度(中间水平和ULOQ的CV和MRE<12.7%,LLOQ的CV和MRE<17.2%)、检测限(MDMA、MDEA和MBDB为0.2 ng/mL;A、MA和PMA为0.5 ng/mL;MDA为1 ng/mL)和定量限(A、MA、MDMA、MDEA和MBDB为1 ng/mL;MDA和PMA为2 ng/mL)以及相对离子强度。未观察到基质效应。该方法被证明灵敏、特异且快速,并应用于实际法医案件。

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