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Optimization of HS-SPME/GC-MS analysis and its use in the profiling of illicit ecstasy tablets (Part 1).
Forensic Sci Int. 2009 May 30; 187(1-3):73-80.FS

Abstract

A headspace solid-phase microextraction procedure (HS-SPME) was developed for the profiling of traces present in 3,4-methylenedioxymethylampethamine (MDMA). Traces were first extracted using HS-SPME and then analyzed by gas chromatography-mass spectroscopy (GC-MS). The HS-SPME conditions were optimized using varying conditions. Optimal results were obtained when 40 mg of crushed MDMA sample was heated at 80 degrees C for 15 min, followed by extraction at 80 degrees C for 15 min with a polydimethylsiloxane/divinylbenzene coated fibre. A total of 31 compounds were identified as traces related to MDMA synthesis, namely precursors, intermediates or by-products. In addition some fatty acids used as tabletting materials and caffeine used as adulterant, were also detected. The use of a restricted set of 10 target compounds was also proposed for developing a screening tool for clustering samples having close profile. 114 seizures were analyzed using an SPME auto-sampler (MultiPurpose Samples MPS2), purchased from Gerstel GMBH & Co. (Germany), and coupled to GC-MS. The data was handled using various pre-treatment methods, followed by the study of similarities between sample pairs based on the Pearson correlation. The results show that HS-SPME, coupled with the suitable statistical method is a powerful tool for distinguishing specimens coming from the same seizure and specimens coming from different seizures. This information can be used by law enforcement personnel to visualize the ecstasy distribution network as well as the clandestine tablet manufacturing.

Authors+Show Affiliations

Ecole des Sciences Criminelles, Institut de Police Scientifique, University of Lausanne, Batochime, CH-1015, Lausanne-Dorigny, Switzerland.No affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

19356870

Citation

Bonadio, Federica, et al. "Optimization of HS-SPME/GC-MS Analysis and Its Use in the Profiling of Illicit Ecstasy Tablets (Part 1)." Forensic Science International, vol. 187, no. 1-3, 2009, pp. 73-80.
Bonadio F, Margot P, Delémont O, et al. Optimization of HS-SPME/GC-MS analysis and its use in the profiling of illicit ecstasy tablets (Part 1). Forensic Sci Int. 2009;187(1-3):73-80.
Bonadio, F., Margot, P., Delémont, O., & Esseiva, P. (2009). Optimization of HS-SPME/GC-MS analysis and its use in the profiling of illicit ecstasy tablets (Part 1). Forensic Science International, 187(1-3), 73-80. https://doi.org/10.1016/j.forsciint.2009.03.004
Bonadio F, et al. Optimization of HS-SPME/GC-MS Analysis and Its Use in the Profiling of Illicit Ecstasy Tablets (Part 1). Forensic Sci Int. 2009 May 30;187(1-3):73-80. PubMed PMID: 19356870.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Optimization of HS-SPME/GC-MS analysis and its use in the profiling of illicit ecstasy tablets (Part 1). AU - Bonadio,Federica, AU - Margot,Pierre, AU - Delémont,Olivier, AU - Esseiva,Pierre, Y1 - 2009/04/07/ PY - 2008/09/14/received PY - 2009/01/09/revised PY - 2009/03/02/accepted PY - 2009/4/10/entrez PY - 2009/4/10/pubmed PY - 2009/7/25/medline SP - 73 EP - 80 JF - Forensic science international JO - Forensic Sci. Int. VL - 187 IS - 1-3 N2 - A headspace solid-phase microextraction procedure (HS-SPME) was developed for the profiling of traces present in 3,4-methylenedioxymethylampethamine (MDMA). Traces were first extracted using HS-SPME and then analyzed by gas chromatography-mass spectroscopy (GC-MS). The HS-SPME conditions were optimized using varying conditions. Optimal results were obtained when 40 mg of crushed MDMA sample was heated at 80 degrees C for 15 min, followed by extraction at 80 degrees C for 15 min with a polydimethylsiloxane/divinylbenzene coated fibre. A total of 31 compounds were identified as traces related to MDMA synthesis, namely precursors, intermediates or by-products. In addition some fatty acids used as tabletting materials and caffeine used as adulterant, were also detected. The use of a restricted set of 10 target compounds was also proposed for developing a screening tool for clustering samples having close profile. 114 seizures were analyzed using an SPME auto-sampler (MultiPurpose Samples MPS2), purchased from Gerstel GMBH & Co. (Germany), and coupled to GC-MS. The data was handled using various pre-treatment methods, followed by the study of similarities between sample pairs based on the Pearson correlation. The results show that HS-SPME, coupled with the suitable statistical method is a powerful tool for distinguishing specimens coming from the same seizure and specimens coming from different seizures. This information can be used by law enforcement personnel to visualize the ecstasy distribution network as well as the clandestine tablet manufacturing. SN - 1872-6283 UR - https://www.unboundmedicine.com/medline/citation/19356870/Optimization_of_HS_SPME/GC_MS_analysis_and_its_use_in_the_profiling_of_illicit_ecstasy_tablets__Part_1__ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0379-0738(09)00095-4 DB - PRIME DP - Unbound Medicine ER -