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

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 degrees C for 1 h. The resulting solutions were evaporated to dryness, derivatized using trifluoroacetic anhydride (TFAA) at 70 degrees 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.

Development of a simultaneous analytical method for selected anorectics, methamphetamine, MDMA, and their metabolites in hair using LC-MS/MS to prove anorectics abuse

“…The abuse of phentermine has previously been reported using human hair [1,7], but that of phendimetrazine was first proved by hair analysis in the current study. Most phendimetrazine abusers were multidrug abusers of phendimetrazine, phentermine, and/or methamphetamine (13 of 14 subjects).…”

“…For example, hair analysis demonstrated that opioid analgesics and benzodiazepines were illegally abused especially by medical professionals, who can easily obtain those drugs [5,6]. Chronic use of some anorectic agents was also proved by hair analysis [1,3,7].…”

Simultaneous determination of amphetamine-type stimulants and cannabinoids in fingernails by gas chromatography-mass spectrometry

“…The application of the described methodology allows the simultaneous detection and quantification of the mentioned compounds in nail samples. The simultaneous detection and quantification of several kinds of abused drugs is advantageous to toxicologists who are frequently confronted with limited sample size and detection of multiple drug use (Kim et al, 2007).…”

Chemical Reagents and Derivatization Procedures in Drug Analysis

“…Acylation of the NH or NH 2 functional group present in all these compounds with either PFAA or HFAA lowers the basicity of the amine, which allows other fragmentation pathways to occur, resulting in clear distinguishing MS spectra. Comparable approaches using TFAA for derivatization of phenylalkylamines such as methamphetamine (31) and others including phenteramine, cathinone, and mescaline (32) or ketamines (33) and subsequent GC/MS have been reported. Human metabolism of ephedrines including ephedrine and phenylpropanolamine was generally found to be low based on TFAA derivatization and GC/MS results.…”