Rapid and Simple GC–MS Method for Determination of Psychotropic Phenylalkylamine Derivatives in Nails Using Micro‐Pulverized Extraction*

Abstract

A rapid and simple gas chromatography-mass spectrometry (GC-MS) method was developed and validated for the simultaneous detection and quantification of five psychotropic phenylalkylamines (amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, and norketamine) in toenails. After external decontamination, nail clippings were mechanically pulverized with a bead mill and then incubated in methanol under ultrasonication at 50°C for 1 h. The resulting solutions were evaporated to dryness, derivatized, and analyzed by GC-MS. The intra- and inter-day precisions were within 10.7% and 13.9%, respectively. The intra- and inter-day accuracies were -4.2% to 5.0% and -2.4% to 8.4%, respectively. Limits of detection and quantification for each analyte were lower than 0.024 and 0.08 ng/mg, respectively. The recoveries were in the range of 80.6-87.5%. The results indicated that the proposed method is a simple, rapid, accurate, and precise for quantification of five phenylalkylamines in nails. The method was successfully applied to the simultaneous detection and quantification of phenylalkylamines in nail samples of possible drug abusers.

Nail analysis for the detection of drugs of abuse and pharmaceuticals: a review

“…Fingernails of seven drug abusers were analyzed for mAMP (six positive cases; 0.23-2.09 ng/mg), AMP (four positive cases; \0.063 ng/mg), MDA (one positive case; \0.143 ng/mg), and MDMA (one positive case; 0.46 ng/mg) [24]. In toenails of four drug abusers, mAMP and AMP were both detected in one case (concentrations not provided) [25]. A larger study in 97 female AMP and/or opiate drug users, who were currently under treatment, reported the duration of detectability and deposition characteristics of mAMP and AMP in fingernails [16]; 62 subjects were found positive for mAMP and/or AMP, with concentrations ranging from 0.46 to 61.5 ng/mg and from\0.2 to 5.42 ng/mg, respectively.…”

“…Washing has usually been followed by alkaline extraction and further clean-up with liquid-liquid extraction (LLE) [8,16,[22][23][24]. In recent years, a rapid and easy sample preparation procedure was proposed in which decontamination was immediately followed by mechanical pulverization of the nail, methanol extraction, and purification by high speed centrifugation [25]. Thereby, alkaline extraction, which can result in the loss of amphetamines by evaporation, was avoided.…”

“…Thereby, alkaline extraction, which can result in the loss of amphetamines by evaporation, was avoided. Moreover, compared to the extracts achieved by alkaline hydrolysis and subsequent LLE, the procedure resulted in cleaner extracts and enhanced detection sensitivity of amphetamines, with low limits of quantification (LOQs) (e.g., 0.05 ng/mg for MDMA) [25].…”

“…Pre-analytical and analytical techniques Gas chromatography coupled to mass spectrometry (GC-MS) operated in electron ionization (EI) mode has been the preferred technique for the detection of methamphetamine (mAMP), amphetamine (AMP), 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyamphetamine (MDA) in nails [16,[21][22][23][24][25]. Decontamination consisting of water and methanol washes was found to be efficient as no substances were detected in a methanol wash performed after the normal decontamination procedure [23].…”

Quantitative mass spectrometry of unconventional human biological matrices

“…However, following such digestion, some components of interest may be decomposed. Thus, alternative methods of extraction are occasionally implemented; for example, ultrasound-assisted extraction with methanol (after micropulverization of the specimen) [50,51]. To remove matrix interferences (especially after digestion), subsequent clean-up by solid-phase extraction (SPE) is necessary [48].…”