Concheiro Marta, Simões Susana Maria dos Santos Sadler, Quintela Oscar, de Castro Ana, Dias Mário João Rodrigues, Cruz Angelines, López-Rivadulla Manuel
Forensic Toxicology Service, Institute of Legal Medicine, University of Santiago de Compostela, C/San Francisco s/n, 15782 Santiago de Compostela, Spain.
Forensic Sci Int. 2007 Aug 24;171(1):44-51. doi: 10.1016/j.forsciint.2006.10.004. Epub 2006 Nov 9.
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.
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。
