Solid-phase extraction followed by dispersive liquid-liquid microextraction for the sensitive determination of ecstasy compounds and amphetamines in biological samples

H A Mashayekhi,M Rezaee,F Khalilian

doi:10.4314/bcse.v28i3.3

Abstract

A novel approach for the determination of ecstasy and amphetamines (3,4-methylenedioxymethylamphetamine (MDMA, Ecstasy), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxyethylamphetamine (MDEA) and 3,4-methylenedioxypropylamphetamine (MDPA)) in biological samples is presented. The analytes were extracted from the matrix and transferred to a small volume of a high density, water insoluble solvent using solid-phase extraction (SPE) followed by dispersive liquid-liquid microextraction (DLLME). This combination not only resulted in a high enrichment factor, but also it could be used in complex matrices (biological samples). Some important extraction parameters, such as sample solution flow rate, sample pH, type and volume of extraction and disperser solvents as well as the salt addition, were studied and optimized. Under the optimized conditions, the calibration graphs were linear in the range of 0.5-500 µg L-1 and 1.0-500 µg L-1 with detection limits in the range of 0.1-0.3 µg L-1 and 0.2-0.7 µg L-1 in urine and plasma samples, respectively. The results showed that SPE-DLLME is a suitable method for the determination of ecstasy components and amphetamines in biological and water samples. KEY WORDS: Dispersive liquid-liquid microextraction, Solid-phase extraction, Ecstasy compounds, Amphetamines, Gas chromatography, Biological samples Bull. Chem. Soc. Ethiop. 2014, 28(3), 339-348.DOI: http://dx.doi.org/10.4314/bcse.v28i3.3

Highlights

Due to the widespread abuse of amphetamine, methamphetamine and the designer drugs 3,4methylenedioxymethylamphetamine (MDMA, Ecstasy), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxyethylamphetamine (MDEA) and 3,4-methylenedioxypropylamphetamine (MDPA), drug testing for amphetamines is routinely done in forensic toxicology
solid-phase extraction (SPE)-dispersive liquid-liquid microextraction (DLLME)-gas chromatography (GC)-FID was applied to the determination of ecstasy and amphetamine compounds from biological samples
Performance of DLLME is mainly determined by the type and volume of extractant [26,27,28]

Summary

Introduction

Due to the widespread abuse of amphetamine, methamphetamine and the designer drugs 3,4methylenedioxymethylamphetamine (MDMA, Ecstasy), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxyethylamphetamine (MDEA) and 3,4-methylenedioxypropylamphetamine (MDPA), drug testing for amphetamines is routinely done in forensic toxicology. Chronic abuse of amphetamines causes hallucinations and psychosis, in addition to dysphoria and depression upon withdrawal [2]. Abuse of amphetamines remains a serious social problem worldwide. Amphetamines are generally assessed by urine analysis. Many methods have been reported to assess amphetamines compounds in human urine samples using gas chromatography (GC) [3], high-performance liquid chromatography (HPLC) [4, 5], GC/mass spectrometry (MS) [6,7,8,9,10,11,12], HPLC-MS [13, 14], capillary electrophoresis (CE) [15], and CE-MS [16]. GC and GC-MS methods are often preferred for quantitative determination of ecstasy and amphetamines compounds

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