Determination of amphetamine-type stimulants, ketamine and metabolites in fingernails by gas chromatography–mass spectrometry

Abstract 

A gas chromatography–mass spectrometry (GC–MS) method was developed and validated for the simultaneous qualification and quantification of methamphetamine (MA), amphetamine (AP), 3,4-methylenedioxy-N-methylamphetamine (MDMA), 3,4-methylenedioxy-N-amphetamine (MDA), ketamine (KET) and norketamine (NKT) in fingernails. Fingernail samples (20mg) were washed with distilled water and methanol, digested with 1.0M sodium hydroxide at 95°C for 30min, and then extracted with ethyl acetate. Extract solutions were evaporated to dryness, derivatized using heptafluorobutyric anhydride (HFBA) at 60°C for 30min, and analyzed by GC–MS. The linear ranges were 0.1–20.0ng/mg for AP, MDMA and NKT, 0.2–20.0ng/mg for MA and MDA, and 0.4–20.0ng/mg for KET, with the coefficients of determination (r²≥0.9989). The intra- and inter-day precisions were within 7.1% and 10.6%, respectively. The intra- and inter-day accuracies were −10.9% to 0.8% and −4.3% to 4.5%, respectively. The limits of detections (LODs) and the limits of quantifications (LOQs) for each analyte were lower than 0.094ng/mg and 0.314ng/mg, respectively. The recoveries were in the range of 72.3–94.9%. The average fingernail growth rates of two subjects for three years and six subjects for two months were 3.12mm/month and 3.16mm/month, respectively. The method proved to be suitable also for the simultaneous detection and quantification of MA, MDMA, KET and their metabolites in fingernails.

Keywords: Amphetamine-type stimulants, Ketamine, GC–MS, Nail analysis