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

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• 作者：Marta Concheiro ; Susana Maria dos Santos Sadler Simõ ; es ; Ó ; scar Quintela ; Ana de Castro ; Má ; rio Joã ; o Rodrigues Dias ; Angelines Cruz ; Manuel Ló ; pez-Rivadulla
• 关键词：Amphetamine ; MDMA ; PMA ; LC– ; MS/MS ; Urine
• 刊名：Forensic Science International
• 出版年：2007
• 期刊代码：104_03790738
• 类别：med
• 出版时间：24 August 2007
• 卷：171
• 期：1
• 页码：44-51
• 文件大小：602 K

摘要

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.