Development and Validation of a High-Performance Liquid Chromatography - Mass Spectrometry Assay for Determination of Amphetamine, Methamphetamine, and Methylenedioxy Derivatives in Meconium

Simona Pichini, Roberta Pacifici, Manuela Pellegrini, Emilia Marchei, Jaime Lozano, Janeth Murillo, Oriol Vall, Óscar García-Algar

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Abstract

A procedure based on liquid chromatography-mass spectrometry (LC-MS) is described for determination of amphetamine, methamphetamine, and methylendioxy derivatives in meconium, using 3,4-methylendioxypropylamphetamine as internal standard. The analytes were initially extracted from the matrix by 17 mM methanolic HCl. Subsequently, a solid-phase extraction with Bondelut Certify columns was applied. Chromatography was performed on a C18 reversed-phase column using a linear gradient of 10 mM ammonium bicarbonate, pH 9.0-methanol as a mobile phase. Analytes were determined in LC-MS single ion monitoring mode with an atmospheric pressure ionization-electrospray interface. The method was validated in the range 0.005-1.00 μg/g using 1 g of meconium per assay. Mean recoveries ranged between 61.1 and 87.2% for different analytes. The quantification limits were 0.005 μg/g meconium for amphetamine, methamphetamine, and 4-hydroxy-3-methoxymethamphetamine and 0.004 μg/g meconium for 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyethylamphetamine, and N-methyl-1-(3,4-methylenedioxyphenyl)-2-butanamine. The method was applied to analysis of meconium in newborns to assess eventual fetal exposure to amphetamine derivatives.
Original languageEnglish
Pages (from-to)2124-2132
JournalAnalytical Chemistry
Volume76
Issue number7
DOIs
Publication statusPublished - 1 Apr 2004

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