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Determination of opiates in whole blood using microextraction by packed sorbent and gas chromatography-tandem mass spectrometry.
J Chromatogr A. 2019 Sep 27; 1602:1-10.JC

Abstract

In Portugal, and worldwide, the abuse of psychoactive substances is increasing, with a significant incidence of deaths related to their consumption. Opiates are one of the most prevalent group of substances in that context, and they are responsible for a significant impact of the mentioned harms. Therefore, it becomes necessary to equip labs with faster and effective methods to identify and quantify these substances. This work describes the development and validation of a novel analytical method for the simultaneous determination of morphine, codeine and 6-monoacetylmorphine in blood samples by gas chromatography-tandem mass spectrometry (GC-MS/MS), using microextraction by packed sorbent (MEPS) for sample preparation. Before the MEPS procedure, a precipitation step with acetonitrile was performed. The MEPS parameters were optimized using the fractional factorial planning (2k-1) and surface response methodology. The final optimized conditions were: number of strokes (20), amount of formic acid in the washing solution (3.36%), number of washes of the sorbent (1), amount of ammonium hydroxide in the elution solution (2.36%) and number of elution cycles (11). After the extraction procedure, the analytes were derivatized with MSTFA with 5% TMS. Using a sample volume of 250 μL, the method was validated according to internationally accepted standards. The method proved to be linear in the range of 5-1000 ng/mL with coefficients of determination greater than 0.99 for all analytes. Intra-and inter-day precision and accuracy were in accordance with the above-mentioned criteria, presenting coefficients of variation ≤15% and relative errors within a range of ± 15% of the theoretical concentration. The absolute recoveries ranged from 6 to 23%. The validated method was applied to the analysis of real samples, being an advantageous tool for the detection of those substances in blood. This is the first time that GCMS/MS with MEPS was used for the determination of these compounds in biological fluids.

Authors+Show Affiliations

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.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.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; Nal von Minden, GmbH, Friedenstraβe 32, 93053, Regensburg, Germany.Instituto Politécnico da Guarda (IPG), Escola Superior de Saúde, Avenida Rainha D. Amélia, S/N, 6300-749, Guarda, Portugal; Unidade de Investigação para o Desenvolvimento do Interior do Instituto Politécnico da Guarda (UDI/IPG), Avenida Rainha D. Amélia S/N, 6300-749, Guarda, Portugal; Laboratório de Química Aplicada (LAQV, Requimte), Departamento de Ciências Químicas, Faculdade de Farmácia, Universidade do Porto, Rua de Jorge Viterbo de Ferreira 228, 4050 - 313, Porto, Portugal.Serviço de Química e Toxicologia Forenses, Instituto Nacional de Medicina Legal e Ciências Forenses - Delegação do Sul, Rua Manuel Bento de Sousa 3, 1169-201, Lisboa, Portugal.Serviço de Química e Toxicologia Forenses, Instituto Nacional de Medicina Legal e Ciências Forenses - Delegação do Sul, Rua Manuel Bento de Sousa 3, 1169-201, Lisboa, 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. Electronic address: egallardo@fcsaude.ubi.pt.

Pub Type(s)

Journal Article
Validation Study

Language

eng

PubMed ID

31178159

Citation

Prata, Margarida, et al. "Determination of Opiates in Whole Blood Using Microextraction By Packed Sorbent and Gas Chromatography-tandem Mass Spectrometry." Journal of Chromatography. A, vol. 1602, 2019, pp. 1-10.
Prata M, Ribeiro A, Figueirinha D, et al. Determination of opiates in whole blood using microextraction by packed sorbent and gas chromatography-tandem mass spectrometry. J Chromatogr A. 2019;1602:1-10.
Prata, M., Ribeiro, A., Figueirinha, D., Rosado, T., Oppolzer, D., Restolho, J., Araújo, A. R. T. S., Costa, S., Barroso, M., & Gallardo, E. (2019). Determination of opiates in whole blood using microextraction by packed sorbent and gas chromatography-tandem mass spectrometry. Journal of Chromatography. A, 1602, 1-10. https://doi.org/10.1016/j.chroma.2019.05.021
Prata M, et al. Determination of Opiates in Whole Blood Using Microextraction By Packed Sorbent and Gas Chromatography-tandem Mass Spectrometry. J Chromatogr A. 2019 Sep 27;1602:1-10. PubMed PMID: 31178159.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of opiates in whole blood using microextraction by packed sorbent and gas chromatography-tandem mass spectrometry. AU - Prata,Margarida, AU - Ribeiro,Andreia, AU - Figueirinha,David, AU - Rosado,Tiago, AU - Oppolzer,David, AU - Restolho,José, AU - Araújo,André R T S, AU - Costa,Suzel, AU - Barroso,Mário, AU - Gallardo,Eugenia, Y1 - 2019/05/15/ PY - 2018/12/10/received PY - 2019/05/07/revised PY - 2019/05/12/accepted PY - 2019/6/11/pubmed PY - 2019/10/12/medline PY - 2019/6/11/entrez KW - Blood KW - GC–MS/MS KW - Microextraction by packed sorbent KW - Opiates SP - 1 EP - 10 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1602 N2 - In Portugal, and worldwide, the abuse of psychoactive substances is increasing, with a significant incidence of deaths related to their consumption. Opiates are one of the most prevalent group of substances in that context, and they are responsible for a significant impact of the mentioned harms. Therefore, it becomes necessary to equip labs with faster and effective methods to identify and quantify these substances. This work describes the development and validation of a novel analytical method for the simultaneous determination of morphine, codeine and 6-monoacetylmorphine in blood samples by gas chromatography-tandem mass spectrometry (GC-MS/MS), using microextraction by packed sorbent (MEPS) for sample preparation. Before the MEPS procedure, a precipitation step with acetonitrile was performed. The MEPS parameters were optimized using the fractional factorial planning (2k-1) and surface response methodology. The final optimized conditions were: number of strokes (20), amount of formic acid in the washing solution (3.36%), number of washes of the sorbent (1), amount of ammonium hydroxide in the elution solution (2.36%) and number of elution cycles (11). After the extraction procedure, the analytes were derivatized with MSTFA with 5% TMS. Using a sample volume of 250 μL, the method was validated according to internationally accepted standards. The method proved to be linear in the range of 5-1000 ng/mL with coefficients of determination greater than 0.99 for all analytes. Intra-and inter-day precision and accuracy were in accordance with the above-mentioned criteria, presenting coefficients of variation ≤15% and relative errors within a range of ± 15% of the theoretical concentration. The absolute recoveries ranged from 6 to 23%. The validated method was applied to the analysis of real samples, being an advantageous tool for the detection of those substances in blood. This is the first time that GCMS/MS with MEPS was used for the determination of these compounds in biological fluids. SN - 1873-3778 UR - https://www.unboundmedicine.com/medline/citation/31178159/Determination_of_opiates_in_whole_blood_using_microextraction_by_packed_sorbent_and_gas_chromatography_tandem_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(19)30526-6 DB - PRIME DP - Unbound Medicine ER -