Development of a validated method for the simultaneous determination of amphetamine, methamphetamine and methylenedioxyamphetamines (MDA, MDMA, MDEA) in serum by GC-MS after derivatisation with perfluorooctanoyl chloride

Abstract

A rapid and simple method for the simultaneous detection and quantitation of amphetamine, methamphetamine, methylenedioxyamphetamine (MDA), methylenedioxymethamphetamine (MDMA) and methylenedioxyethylamphetamine (MDEA) in human serum was developed and fully validated. Serum samples were extracted with cyclohexane, derivatised with perfluorooctanoyl chloride without prior evaporation of the solvent and analysed with gas chromatography-mass spectrometry (GC-MS) in the selected ion monitoring mode (SIM). For quantitation, deuterated analogues were used as the internal standards. The limit of detection (LOD) and lower limit of quantitation (LLOQ), bias and within-day and between-day precision were determined. LODs calculated as the average of the six calibration curves were below 5 ng/mL for all of the measured compounds; LLOQs obtained in the same manner were below 20 ng/mL, with the exception of MDA (24.1 ng/mL). The coefficients of variation were below 7% within series, 10% or less between series and the bias was below 8% for all compounds. The calibration curves were linear between the lower limits of quantitation and 800 ng/mL.