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Determination of "new psychoactive substances" in postmortem matrices using microwave derivatization and gas chromatography-mass spectrometry.

Abstract

Despite worldwide efforts aiming to ban the marketing and subsequent abuse of psychoactive substances such as synthetic cathinones and phenethylamines, there has been an alarming growth of both in recent years. Different compounds similar to those already existing are continuously appearing in the market in order to circumvent the legislation. An analytical methodology has been validated for qualitative and quantitative determinations of D-cathine (D-norpseudoehedrine), ephedrine, methcathinone, 1-(4-methoxyphenyl)-propan-2-amine (PMA), mephedrone, methedrone, 2,5-dimethoxy-4-methylamphetamine (DOM), 4-bromo-2,5-dimethoxyamphetamine (DOB), 2,5-dimethoxyphenethylamine (2C-H), 4-bromo-2,5-dimethoxyphenethylamine (2C-B), 4-iodo-2,5-dimethoxyphenethylamine (2C-I), 2-[2,5-dimethoxy-4-(ethylthio)phenyl]ethanamine (2C-T-2), 2,5-dimethoxy-4-isopropylthiophenethylamine (2C-T-4) and 2-[2,5-dimethoxy-4-(propylthio)phenyl]ethanamine (2C-T-7), in low volumes of vitreous humor (100 μL), pericardial fluid (250 μL) and whole blood (250 μL), using deutered amphetamine, ephedrine and mephedrone as internal standards. The validation parameters included selectivity, linearity and limits of detection and quantification, intra- and interday precision and trueness, recovery and stability. The method included mixed-mode solid phase extraction, followed by microwave fast derivatization and analysis by gas chromatography-mass spectrometry operated in selected ion monitoring mode. The procedure was linear between 5 and 600 ng/mL, with determination coefficients higher than 0.99 for all analytes. Intra- and interday precision ranged from 0.1 to 13.6%, while accuracy variability was within 80-120% interval from the nominal concentration at all studied levels. The extraction efficiencies ranged from 76.6 to 112.8%. Stability was considered acceptable for all compounds in the studied matrices. The developed assay was applied to authentic samples of the Laboratory of Chemistry and Forensic Toxicology, Centre Branch, of the National Institute of Legal Medicine and Forensic Sciences, Portugal.

Authors+Show Affiliations

Instituto Nacional de Medicina Legal e Ciências Forenses, I.P. (INMLCF, I.P.)-Delegação do Centro, Coimbra, Portugal. Electronic address: claudia.i.margalho@inmlcf.mj.pt.Instituto Nacional de Medicina Legal e Ciências Forenses, I.P. (INMLCF, I.P.)-Delegação do Centro, Coimbra, Portugal.Instituto Nacional de Medicina Legal e Ciências Forenses, I.P. (INMLCF, I.P.)-Delegação do Centro, Coimbra, Portugal; Faculdade de Medicina da Universidade de Coimbra, Portugal.CICS-UBI-Centro de Investigação em Ciências da Saúde, Universidade da Beira Interior, Portugal.Servicio de Toxicología Forense, Instituto Universitario de Ciencias Forenses Universidad de Santiago de Compostela, Spain.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

26994330

Citation

Margalho, Cláudia, et al. "Determination of "new Psychoactive Substances" in Postmortem Matrices Using Microwave Derivatization and Gas Chromatography-mass Spectrometry." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 1020, 2016, pp. 14-23.
Margalho C, Castanheira A, Real FC, et al. Determination of "new psychoactive substances" in postmortem matrices using microwave derivatization and gas chromatography-mass spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci. 2016;1020:14-23.
Margalho, C., Castanheira, A., Real, F. C., Gallardo, E., & López-Rivadulla, M. (2016). Determination of "new psychoactive substances" in postmortem matrices using microwave derivatization and gas chromatography-mass spectrometry. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 1020, 14-23. https://doi.org/10.1016/j.jchromb.2016.03.001
Margalho C, et al. Determination of "new Psychoactive Substances" in Postmortem Matrices Using Microwave Derivatization and Gas Chromatography-mass Spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci. 2016 May 1;1020:14-23. PubMed PMID: 26994330.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of "new psychoactive substances" in postmortem matrices using microwave derivatization and gas chromatography-mass spectrometry. AU - Margalho,Cláudia, AU - Castanheira,Alice, AU - Real,Francisco Corte, AU - Gallardo,Eugenia, AU - López-Rivadulla,Manuel, Y1 - 2016/03/10/ PY - 2015/12/07/received PY - 2016/03/01/revised PY - 2016/03/02/accepted PY - 2016/3/20/entrez PY - 2016/3/20/pubmed PY - 2016/12/15/medline KW - Alternative biological matrices KW - Cathinones KW - Gas chromatography–mass spectrometry KW - Microwave fast derivatization KW - Phenethylamines SP - 14 EP - 23 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. VL - 1020 N2 - Despite worldwide efforts aiming to ban the marketing and subsequent abuse of psychoactive substances such as synthetic cathinones and phenethylamines, there has been an alarming growth of both in recent years. Different compounds similar to those already existing are continuously appearing in the market in order to circumvent the legislation. An analytical methodology has been validated for qualitative and quantitative determinations of D-cathine (D-norpseudoehedrine), ephedrine, methcathinone, 1-(4-methoxyphenyl)-propan-2-amine (PMA), mephedrone, methedrone, 2,5-dimethoxy-4-methylamphetamine (DOM), 4-bromo-2,5-dimethoxyamphetamine (DOB), 2,5-dimethoxyphenethylamine (2C-H), 4-bromo-2,5-dimethoxyphenethylamine (2C-B), 4-iodo-2,5-dimethoxyphenethylamine (2C-I), 2-[2,5-dimethoxy-4-(ethylthio)phenyl]ethanamine (2C-T-2), 2,5-dimethoxy-4-isopropylthiophenethylamine (2C-T-4) and 2-[2,5-dimethoxy-4-(propylthio)phenyl]ethanamine (2C-T-7), in low volumes of vitreous humor (100 μL), pericardial fluid (250 μL) and whole blood (250 μL), using deutered amphetamine, ephedrine and mephedrone as internal standards. The validation parameters included selectivity, linearity and limits of detection and quantification, intra- and interday precision and trueness, recovery and stability. The method included mixed-mode solid phase extraction, followed by microwave fast derivatization and analysis by gas chromatography-mass spectrometry operated in selected ion monitoring mode. The procedure was linear between 5 and 600 ng/mL, with determination coefficients higher than 0.99 for all analytes. Intra- and interday precision ranged from 0.1 to 13.6%, while accuracy variability was within 80-120% interval from the nominal concentration at all studied levels. The extraction efficiencies ranged from 76.6 to 112.8%. Stability was considered acceptable for all compounds in the studied matrices. The developed assay was applied to authentic samples of the Laboratory of Chemistry and Forensic Toxicology, Centre Branch, of the National Institute of Legal Medicine and Forensic Sciences, Portugal. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/26994330/Determination_of_"new_psychoactive_substances"_in_postmortem_matrices_using_microwave_derivatization_and_gas_chromatography_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(16)30132-5 DB - PRIME DP - Unbound Medicine ER -