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

A gas chromatography/mass spectrometric method was developed and validated to measure thirteen psychotropic phenylalkylamine derivatives in human hair. Hair samples were washed, cut, and incubated in methanolic HCl, then derivatized with trifluoroacetic anhydride and analyzed. The method showed linear ranges from 0.02 to 25.0 ng/mg for most compounds, with good correlation coefficients above 0.9985. Precisions were within 16.8%, accuracies between −15.3 and 13.4%, and recoveries from 76.7 to 95.6%. Limits of quantification were below 0.08 ng/mg. The method is suitable for simultaneous qualification and quantification of these compounds in hair.

Study at a glance

Abstract

Abstract 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.