title: Development and validation of a high-performance liquid chromatography-mass spectrometry assay for determination of amphetamine, methamphetamine, and methylenedioxy derivatives in meconium.
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 C(18) 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 microg/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 microg/g meconium for amphetamine, methamphetamine, and 4-hydroxy-3-methoxymethamphetamine and 0.004 microg/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.
authors.affiliation: Drug Research and Control Department, Istituto Superiore di Sanità, Viale Regina Elena 299, 00161 Rome, Italy. pichini@iss.it
authors.forename: Simona
authors.initials: S
authors.lastname: Pichini
authors.forename: Roberta
authors.initials: R
authors.lastname: Pacifici
authors.forename: Manuela
authors.initials: M
authors.lastname: Pellegrini
authors.forename: Emilia
authors.initials: E
authors.lastname: Marchei
authors.forename: Jaime
authors.initials: J
authors.lastname: Lozano
authors.forename: Janeth
authors.initials: J
authors.lastname: Murillo
authors.forename: Oriol
authors.initials: O
authors.lastname: Vall
authors.forename: Oscar
authors.initials: O
authors.lastname: García-Algar