Solid-phase microextraction/capillary gas chromatography for the profiling of confiscated ecstacy and amphetamine

Abstract

SummaryImpurity profiling ofecstacy and amphetamine seizures was accomplished by solid-phase microextraction (SPME) combined with capillary gas chromatography (GC). Samples were dissolved in 0.1 M aqueous acetate buffer (pH 5.0) as the only manual operation and subsequently subjected to SPME-GC. Ecstacy tablets were analyzed by head-space SPME to avoid contamination of SPME fibers with insoluble tablet components, while illicit amphetamine powders were exposed to immersed SPME. A SPME fiber of polydimethylsiloxane-divinylbenzene was found to provide excellent extraction of both polar and non-polar impurities. For both illicit ecstacy and amphetamine, complex impurity profiles were obtained by SPME providing a high information content. For ecstacy, profiles (relative peak areas) were repeatable within 2.2 to 12.6% RSD (n = 6), while similar data on amphetamine varied between 2.0 and 10.9 % RSD (n = 6). No carry-over was observed although each fiber was used for 50 to 100 extractions.

Development of a harmonised method for the profiling of amphetamines

“…Based on the work of Alm et al [1], Kärkkäinen et al [5] developed a new method to analyse target compounds in street amphetamine, which entailed the use of a 50 m HP Ultra 2 column (5% diphenyl, 95% dimethyl silicone) for separation and a FID for detection; the analysis was performed in 57 min, with hydrogen as carrier gas. Kongshauh et al [6] separated amphetamine target compounds on an SPB 1 column (100% dimethyl silicone) in 26.5 min, and used a NPD for detection. Methods other than gas chromatography have also been used to analyse target compounds.…”

“…Normally, such profiling analysis is performed by gas chromatography (GC) with a flame ionisation detector (FID) [1][2][3][4][5][6], although GC in combination with a electron capture detector (ECD) [2], nitrogen phosphorous detector (NPD) [6], and mass spectrometry (MS) [3] have also been used for this purpose. As early as 1973, Strömberg [2] used a packed OV-17 column (3% www.elsevier.com/locate/forsciint Forensic Science International 169 (2007) 50-63 diphenyl, 97% dimethyl silicone) to separate target compounds in Leuckart amphetamine in 26 min, and detection was accomplished simultaneously with a FID and a ECD.…”

Determination of synthesis route of 1-(3,4-methylenedioxyphenyl)-2-propanone (MDP-2-P) based on impurity profiles of MDMA

“…Numerous papers have been devoted to the route specific impurities in these drugs and the procedures of impurity profiling [1][2][3][4][5][6]. Other synthetic drugs, such as 3,4-methylenedioxyamphetamine (MDA) or 3,4-methylenedioxymethamphetamine (MDMA, ecstasy) have not been sufficiently investigated so far [7][8][9][10][11][12][13].…”

Development of a harmonised method for the profiling of amphetamines

“…Lambrechts and Rasmussen [7] studied the suitability of SPE, using octadecyl, octyl and ethyl sorbents to isolate target compounds from a solution of amphetamine synthesised by the Leuckart route (i.e., Leuckart amphetamine dissolved in 0.063 M phosphate buffer, pH 7.0) and subsequently employing a number of different solvents to elute the analytes from the sorbent. Kongshaug et al [10] demonstrated the usefulness of SPME by using two different fibres (polydimethylsiloxane and polydimethylsiloxane-divinylbenzene) to extract target compounds from Leuckart amphetamine dissolved in acetate buffer (pH 5.0). To our knowledge, no other studies have focused on developing a sample preparation technique for amphetamine profiling.…”

“…Caffeine is often used as a cutting agent, and it is therefore commonly found in large amounts in street amphetamine. Besides liquid-liquid extraction (LLE), some authors have tested solid-phase extraction (SPE) [7,8] and solid-phase micro extraction (SPME) [10] to prepare samples for amphetamine profiling. Lambrechts and Rasmussen [7] studied the suitability of SPE, using octadecyl, octyl and ethyl sorbents to isolate target compounds from a solution of amphetamine synthesised by the Leuckart route (i.e., Leuckart amphetamine dissolved in 0.063 M phosphate buffer, pH 7.0) and subsequently employing a number of different solvents to elute the analytes from the sorbent.…”