Development and Validation of a High-Performance Liquid Chromatography-Mass Spectrometry Assay for Determination of Amphetamine, Methamphetamine, and Methylenedioxy Derivatives in Meconium
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- 作者：Simona Pichini ; Roberta Pacifici ; Manuela Pellegrini ; Emilia Marchei ; Jaime Lozano ; Janeth Murillo ; Oriol Vall ; and Ó ; scar Garcí ; a-Algar
- 刊名：Analytical Chemistry
- 出版年：2004
- 出版时间：April 1, 2004
- 年：2004
- 卷：76
- 期：7
- 页码：2124 - 2132
- 全文大小：248K
- 年卷期：v.76,no.7(April 1, 2004)
- ISSN：1520-6882
文摘
A procedure based on liquid chromatography-massspectrometry (LC-MS) is described for determination ofamphetamine, methamphetamine, and methylendioxyderivatives in meconium, using 3,4-methylendioxypropylamphetamine as internal standard. The analytes wereinitially extracted from the matrix by 17 mM methanolicHCl. Subsequently, a solid-phase extraction with BondelutCertify columns was applied. Chromatography was performed on a C18 reversed-phase column using a lineargradient of 10 mM ammonium bicarbonate, pH 9.0-methanol as a mobile phase. Analytes were determinedin LC-MS single ion monitoring mode with an atmospheric pressure ionization-electrospray interface. Themethod was validated in the range 0.005-1.00 
g/gusing 1 g of meconium per assay. Mean recoveries rangedbetween 61.1 and 87.2% for different analytes. Thequantification limits were 0.005 g/g meconium foramphetamine, methamphetamine, and 4-hydroxy-3-methoxymethamphetamine and 0.004 g/g meconium for 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyethylamphetamine, andN-methyl-1-(3,4-methylenedioxyphenyl)-2-butanamine. Themethod was applied to analysis of meconium in newbornsto assess eventual fetal exposure to amphetamine derivatives.
g/gusing 1 g of meconium per assay. Mean recoveries rangedbetween 61.1 and 87.2% for different analytes. Thequantification limits were 0.005 g/g meconium foramphetamine, methamphetamine, and 4-hydroxy-3-methoxymethamphetamine and 0.004 g/g meconium for 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyethylamphetamine, andN-methyl-1-(3,4-methylenedioxyphenyl)-2-butanamine. Themethod was applied to analysis of meconium in newbornsto assess eventual fetal exposure to amphetamine derivatives.