Simultaneous determination of psychotropic phenylalkylamine derivatives in human hair by gas chromatography/mass spectrometry

A gas chromatography/mass spectrometric (GC/MS) method was developed and validated for the determination of thirteen psychotropic phenylalkylamine derivatives (amphetamine; AP, phentermine; PT, methamphamine; MA, cathinone; Khat, methcathinone; MCAT, fenfluramine; FFA, desmethylselegiline; DSEL, 3,4‐methylenedioxyamphetamine; MDA, 3,4‐methylenedioxymethamphetamine; MDMA, 3,4‐methylenedioxyethylamphetamine; MDEA, norketamine; NKT, mescaline; MES, 4‐bromo‐2,5‐dimethoxyphenethylamine; 2CB) in human hair. Hair samples (20 mg) were washed with distilled water and acetone, cut into small fragments (<1 mm), and incubated in 0.25 M methanolic HCl under ultrasonication at 50°C for 1 h. The resulting solutions were evaporated to dryness, derivatized using trifluoroacetic anhydride (TFAA) at 70°C for 30 min, and analyzed by GC/MS. The linear ranges were 0.02–25.0 ng/mg for AP, PT, Khat, FFA, DSEL, MDMA, and 2CB; 0.05–25.0 ng/mg for MA, MCAT, and MES; 0.05–12.5 ng/mg for MDA; and 0.1–25.0 ng/mg for MDEA and NKT, with good correlation coefficients (r 2  > 0.9985). The intra‐day, inter‐day, and inter‐person precisions were within 12.7%, 14.8%, and 16.8%, respectively. The intra‐day, inter‐day, and inter‐person accuracies were between −10.7 and 13.4%, −12.7 and 11.6%, and −15.3 and 11.9%, respectively. The limits of quantifications (LOQs) for each compound were lower than 0.08 ng/mg. The recoveries were in the range of 76.7–95.6%. The method proved to be suitable for the simultaneous qualification and quantification of phenylalkylamine derivatives in hair specimens. Copyright © 2007 John Wiley & Sons, Ltd.