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Determination of New Psychoactive Substances in Whole Blood Using Microwave Fast Derivatization and Gas Chromatography/Mass Spectrometry.
J Anal Toxicol. 2020 Jan 07; 44(1):92-102.JA

Abstract

The production and consumption of new psychoactive substances (NPSs) has been raising a major concern worldwide. Due to easy access and available information, many NPSs continue to be synthesized with an alarming increase of those available to purchase, despite all the control efforts created. A new analytical method was developed and validated to determine a group of phenethylamines and synthetic cathinones: cathinone, flephedrone, buphedrone, 4-MTA, α-PVP, methylone, 2C-P, ethylone, pentylone, MDPV and bromo-dragonFLY in whole blood. A mixed-mode solid phase extraction was applied to 250 μL of sample, and the extracts were derivatized with fast microwave technique before being analyzed by gas chromatography-mass spectrometry (GC-MS). The validation procedure followed the Scientific Working Group for Forensic Toxicology (SWGTOX) guidelines with parameters that included selectivity, linearity, limits of detection and quantification, intra- and inter-day precision and accuracy, recoveries and stability. The method presented linearity between 5 and 500 ng/mL for cathinone, buphedrone, 4-MTA, methylone, 2C-P and bromo-dragonFLY, 10-500 ng/mL for flephedrone, ethylone, pentylone and MDPV, and 40-500 ng/mL for α-PVP, with determination coefficients above 0.99 for all analytes. Recoveries ranged between 70.3% and 116.6%, and regarding intra- and inter-day precision, the relative mean errors were typically lower than 8.6%. The method was successfully applied to over 100 authentic samples from 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 - Delegação do Centro, Serviço de Química e Toxicologia Forenses, Largo da Sé Nova, 3000-213, Coimbra Portugal.Instituto Nacional de Medicina Legal e Ciências Forenses - Delegação do Centro, Serviço de Química e Toxicologia Forenses, Largo da Sé Nova, 3000-213, Coimbra Portugal. Centro de Investigação em Ciências da Saúde, Faculdade de Ciências da Saúde da Universidade da Beira Interior (CICS-UBI), Avenida Infante D. Henrique, 6201-506, Covilhã, Portugal.Centro de Investigação em Ciências da Saúde, Faculdade de Ciências da Saúde da Universidade da Beira Interior (CICS-UBI), Avenida Infante D. Henrique, 6201-506, Covilhã, Portugal. Laboratório de Fármaco-Toxicologia-UBIMedical, Universidade da Beira Interior, EM506, 6200-284, Covilhã, Portugal.Instituto Nacional de Medicina Legal e Ciências Forenses - Delegação do Centro, Serviço de Química e Toxicologia Forenses, Largo da Sé Nova, 3000-213, Coimbra Portugal.Centro de Investigação em Ciências da Saúde, Faculdade de Ciências da Saúde da Universidade da Beira Interior (CICS-UBI), Avenida Infante D. Henrique, 6201-506, Covilhã, Portugal. Laboratório de Fármaco-Toxicologia-UBIMedical, Universidade da Beira Interior, EM506, 6200-284, Covilhã, Portugal.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

31436798

Citation

Cláudia, Margalho, et al. "Determination of New Psychoactive Substances in Whole Blood Using Microwave Fast Derivatization and Gas Chromatography/Mass Spectrometry." Journal of Analytical Toxicology, vol. 44, no. 1, 2020, pp. 92-102.
Cláudia M, Pedro A, Tiago R, et al. Determination of New Psychoactive Substances in Whole Blood Using Microwave Fast Derivatization and Gas Chromatography/Mass Spectrometry. J Anal Toxicol. 2020;44(1):92-102.
Cláudia, M., Pedro, A., Tiago, R., Francisco, C. R., & Eugenia, G. (2020). Determination of New Psychoactive Substances in Whole Blood Using Microwave Fast Derivatization and Gas Chromatography/Mass Spectrometry. Journal of Analytical Toxicology, 44(1), 92-102. https://doi.org/10.1093/jat/bkz053
Cláudia M, et al. Determination of New Psychoactive Substances in Whole Blood Using Microwave Fast Derivatization and Gas Chromatography/Mass Spectrometry. J Anal Toxicol. 2020 Jan 7;44(1):92-102. PubMed PMID: 31436798.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of New Psychoactive Substances in Whole Blood Using Microwave Fast Derivatization and Gas Chromatography/Mass Spectrometry. AU - Cláudia,Margalho, AU - Pedro,Almeida, AU - Tiago,Rosado, AU - Francisco,Corte Real, AU - Eugenia,Gallardo, PY - 2018/11/30/received PY - 2019/04/15/revised PY - 2019/06/04/accepted PY - 2019/8/23/pubmed PY - 2020/4/22/medline PY - 2019/8/23/entrez SP - 92 EP - 102 JF - Journal of analytical toxicology JO - J Anal Toxicol VL - 44 IS - 1 N2 - The production and consumption of new psychoactive substances (NPSs) has been raising a major concern worldwide. Due to easy access and available information, many NPSs continue to be synthesized with an alarming increase of those available to purchase, despite all the control efforts created. A new analytical method was developed and validated to determine a group of phenethylamines and synthetic cathinones: cathinone, flephedrone, buphedrone, 4-MTA, α-PVP, methylone, 2C-P, ethylone, pentylone, MDPV and bromo-dragonFLY in whole blood. A mixed-mode solid phase extraction was applied to 250 μL of sample, and the extracts were derivatized with fast microwave technique before being analyzed by gas chromatography-mass spectrometry (GC-MS). The validation procedure followed the Scientific Working Group for Forensic Toxicology (SWGTOX) guidelines with parameters that included selectivity, linearity, limits of detection and quantification, intra- and inter-day precision and accuracy, recoveries and stability. The method presented linearity between 5 and 500 ng/mL for cathinone, buphedrone, 4-MTA, methylone, 2C-P and bromo-dragonFLY, 10-500 ng/mL for flephedrone, ethylone, pentylone and MDPV, and 40-500 ng/mL for α-PVP, with determination coefficients above 0.99 for all analytes. Recoveries ranged between 70.3% and 116.6%, and regarding intra- and inter-day precision, the relative mean errors were typically lower than 8.6%. The method was successfully applied to over 100 authentic samples from the Laboratory of Chemistry and Forensic Toxicology, Centre Branch, of the National Institute of Legal Medicine and Forensic Sciences, Portugal. SN - 1945-2403 UR - https://www.unboundmedicine.com/medline/citation/31436798/Determination_of_New_Psychoactive_Substances_in_Whole_Blood_Using_Microwave_Fast_Derivatization_and_Gas_Chromatography/Mass_Spectrometry_ L2 - https://academic.oup.com/jat/article-lookup/doi/10.1093/jat/bkz053 DB - PRIME DP - Unbound Medicine ER -