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Sensitive determination of THC and main metabolites in human plasma by means of microextraction in packed sorbent and gas chromatography-tandem mass spectrometry.

Abstract

Cannabis is one of the most available and consumed illicit drug in the world and its identification and quantification in biological specimens can be a challenge given its low concentrations in body fluids. The present work describes a fast and fully validated procedure for the simultaneous detection and quantification of ▵9-tetrahydrocannabinol (▵9_THC) and its two main metabolites 11-hydroxy ▵9_tetrahydrocannabinol (11-OH-THC) and 11-nor-9-carboxy-▵9- tetrahydrocannbinol (THC-COOH) in plasma samples using microextraction by packed sorbent (MEPS) and gas chromatography-tandem mass spectrometry (GC-MS/MS). A small plasma volume (0.25mL) pre-diluted (1:20), was extracted with MEPS M1 sorbent as follows: conditioning (4 cycles of 250μL methanol and 4 cycles of 250μL 0.1% formic acid in water); sample load (26 cycles of 250μL); wash (100μL of 3% acetic acid in water followed by 100μL 5% methanol in water); and elution (6 cycles of 100μL of 10% ammonium hydroxide in methanol). The procedure allowed the quantification of all analytes in the range of 0.1-30ng/mL. Recoveries ranged from 53 to 78% (THC), 57 to 66% (11-OH-THC) and 62 to 65% (THC-COOH), allowing the limits of detection and quantification to be set at 0.1ng/mL for all compounds. Intra-day precision and accuracy revealed coefficients of variation (CVs) lower than 10% at the studied concentrations, with a mean relative error within±9%, while inter-day precision and accuracy showed CVs lower than 15% for all analytes at the tested concentrations, with an inaccuracy within±8%.

Authors+Show Affiliations

Centro de Investigação em Ciências da Saúde, Faculdade de Ciências da Saúde da Universidade da Beira Interior (CICS-UBI), Covilhã, Portugal; Laboratório de Fármaco-Toxicologia-UBIMedical, Universidade da Beira Interior, Covilhã, Portugal.Centro de Investigação em Ciências da Saúde, Faculdade de Ciências da Saúde da Universidade da Beira Interior (CICS-UBI), Covilhã, Portugal.Serviço de Química e Toxicologia Forenses, Instituto de Medicina Legal e Ciências Forenses-Delegação do Sul, Rua Manuel Bento de Sousa, Lisboa, Portugal.Centro de Investigação em Ciências da Saúde, Faculdade de Ciências da Saúde da Universidade da Beira Interior (CICS-UBI), Covilhã, Portugal; Laboratório de Fármaco-Toxicologia-UBIMedical, Universidade da Beira Interior, Covilhã, Portugal. Electronic address: egallardo@fcsaude.ubi.pt.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

27617793

Citation

Rosado, T, et al. "Sensitive Determination of THC and Main Metabolites in Human Plasma By Means of Microextraction in Packed Sorbent and Gas Chromatography-tandem Mass Spectrometry." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 1043, 2017, pp. 63-73.
Rosado T, Fernandes L, Barroso M, et al. Sensitive determination of THC and main metabolites in human plasma by means of microextraction in packed sorbent and gas chromatography-tandem mass spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci. 2017;1043:63-73.
Rosado, T., Fernandes, L., Barroso, M., & Gallardo, E. (2017). Sensitive determination of THC and main metabolites in human plasma by means of microextraction in packed sorbent and gas chromatography-tandem mass spectrometry. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 1043, 63-73. https://doi.org/10.1016/j.jchromb.2016.09.007
Rosado T, et al. Sensitive Determination of THC and Main Metabolites in Human Plasma By Means of Microextraction in Packed Sorbent and Gas Chromatography-tandem Mass Spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Feb 1;1043:63-73. PubMed PMID: 27617793.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Sensitive determination of THC and main metabolites in human plasma by means of microextraction in packed sorbent and gas chromatography-tandem mass spectrometry. AU - Rosado,T, AU - Fernandes,L, AU - Barroso,M, AU - Gallardo,E, Y1 - 2016/09/06/ PY - 2016/05/31/received PY - 2016/09/01/revised PY - 2016/09/05/accepted PY - 2016/9/13/pubmed PY - 2017/3/9/medline PY - 2016/9/13/entrez KW - Cannabis KW - Gas chromatography–tandem mass spectrometry KW - Microextraction by packed sorbent KW - Plasma SP - 63 EP - 73 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 1043 N2 - Cannabis is one of the most available and consumed illicit drug in the world and its identification and quantification in biological specimens can be a challenge given its low concentrations in body fluids. The present work describes a fast and fully validated procedure for the simultaneous detection and quantification of ▵9-tetrahydrocannabinol (▵9_THC) and its two main metabolites 11-hydroxy ▵9_tetrahydrocannabinol (11-OH-THC) and 11-nor-9-carboxy-▵9- tetrahydrocannbinol (THC-COOH) in plasma samples using microextraction by packed sorbent (MEPS) and gas chromatography-tandem mass spectrometry (GC-MS/MS). A small plasma volume (0.25mL) pre-diluted (1:20), was extracted with MEPS M1 sorbent as follows: conditioning (4 cycles of 250μL methanol and 4 cycles of 250μL 0.1% formic acid in water); sample load (26 cycles of 250μL); wash (100μL of 3% acetic acid in water followed by 100μL 5% methanol in water); and elution (6 cycles of 100μL of 10% ammonium hydroxide in methanol). The procedure allowed the quantification of all analytes in the range of 0.1-30ng/mL. Recoveries ranged from 53 to 78% (THC), 57 to 66% (11-OH-THC) and 62 to 65% (THC-COOH), allowing the limits of detection and quantification to be set at 0.1ng/mL for all compounds. Intra-day precision and accuracy revealed coefficients of variation (CVs) lower than 10% at the studied concentrations, with a mean relative error within±9%, while inter-day precision and accuracy showed CVs lower than 15% for all analytes at the tested concentrations, with an inaccuracy within±8%. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/27617793/Sensitive_determination_of_THC_and_main_metabolites_in_human_plasma_by_means_of_microextraction_in_packed_sorbent_and_gas_chromatography_tandem_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(16)30791-7 DB - PRIME DP - Unbound Medicine ER -