The Determination of Cannabinoids in Urine Samples Using Microextraction by Packed Sorbent and Gas Chromatography-Mass Spectrometry

Cannabis is the most consumed illicit drug worldwide, and its legal status is a source of concern. This study proposes a rapid procedure for the simultaneous quantification of Δ<sup>9</sup>-tetrahydrocannabinol (THC), 11-hydroxy-Δ<sup>9</sup>-tetrahydrocannabinol (11-OH-THC),...

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Main Authors: Luana M. Rosendo, Tiago Rosado, Patrik Oliveira, Ana Y. Simão, Cláudia Margalho, Suzel Costa, Luís A. Passarinha, Mário Barroso, Eugenia Gallardo
Format: Article
Language:English
Published: MDPI AG 2022-08-01
Series:Molecules
Subjects:
Online Access:https://www.mdpi.com/1420-3049/27/17/5503
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author Luana M. Rosendo
Tiago Rosado
Patrik Oliveira
Ana Y. Simão
Cláudia Margalho
Suzel Costa
Luís A. Passarinha
Mário Barroso
Eugenia Gallardo
author_facet Luana M. Rosendo
Tiago Rosado
Patrik Oliveira
Ana Y. Simão
Cláudia Margalho
Suzel Costa
Luís A. Passarinha
Mário Barroso
Eugenia Gallardo
author_sort Luana M. Rosendo
collection DOAJ
description Cannabis is the most consumed illicit drug worldwide, and its legal status is a source of concern. This study proposes a rapid procedure for the simultaneous quantification of Δ<sup>9</sup>-tetrahydrocannabinol (THC), 11-hydroxy-Δ<sup>9</sup>-tetrahydrocannabinol (11-OH-THC), 11-nor-9-carboxy-Δ<sup>9</sup>-tetrahydrocannabinol (THC-COOH), cannabidiol (CBD), and cannabinol (CBN) in urine samples. Microextraction by packed sorbent (MEPS) was used to pre-concentrate the analytes, which were detected by gas chromatography–mass spectrometry. The procedure was previously optimized, and the final conditions were: conditioning with 50 µL methanol and 50 µL of water, sample load with two draw–eject cycles, and washing with 310 µL of 0.1% formic acid in water with 5% isopropanol; the elution was made with 35 µL of 0.1% ammonium hydroxide in methanol. This fast extraction procedure allowed quantification in the ranges of 1–400 ng/mL for THC and CBD, 5–400 ng/mL for CBN and 11-OH-THC, and 10–400 ng/mL for THC-COOH with coefficients of determination higher than 0.99. The limits of quantification and detection were between 1 and 10 ng/mL using 0.25 mL of sample. The extraction efficiencies varied between 26 and 85%. This analytical method is the first allowing the for determination of cannabinoids in urine samples using MEPS, a fast, simple, and low-cost alternative to conventional techniques.
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spelling doaj.art-b105b3d3801d415cbbeef02117c5fd042023-11-23T13:43:08ZengMDPI AGMolecules1420-30492022-08-012717550310.3390/molecules27175503The Determination of Cannabinoids in Urine Samples Using Microextraction by Packed Sorbent and Gas Chromatography-Mass SpectrometryLuana M. Rosendo0Tiago Rosado1Patrik Oliveira2Ana Y. Simão3Cláudia Margalho4Suzel Costa5Luís A. Passarinha6Mário Barroso7Eugenia Gallardo8Centro de Investigação em Ciências da Saúde, Universidade da Beira Interior (CICS-UBI), Av. Infante D. Henrique, 6201-506 Covilhã, PortugalCentro de Investigação em Ciências da Saúde, Universidade da Beira Interior (CICS-UBI), Av. Infante D. Henrique, 6201-506 Covilhã, PortugalCentro de Investigação em Ciências da Saúde, Universidade da Beira Interior (CICS-UBI), Av. Infante D. Henrique, 6201-506 Covilhã, PortugalCentro de Investigação em Ciências da Saúde, Universidade da Beira Interior (CICS-UBI), Av. Infante D. Henrique, 6201-506 Covilhã, PortugalServiço de Química e Toxicologia Forenses, Instituto de Medicina Legal e Ciências Forenses-Delegação do Centro, 3000-213 Coimbra, PortugalServiço de Química e Toxicologia Forenses, Instituto de Medicina Legal e Ciências Forenses-Delegação do Sul, 1169-201 Lisboa, PortugalCentro de Investigação em Ciências da Saúde, Universidade da Beira Interior (CICS-UBI), Av. Infante D. Henrique, 6201-506 Covilhã, PortugalServiço de Química e Toxicologia Forenses, Instituto de Medicina Legal e Ciências Forenses-Delegação do Sul, 1169-201 Lisboa, PortugalCentro de Investigação em Ciências da Saúde, Universidade da Beira Interior (CICS-UBI), Av. Infante D. Henrique, 6201-506 Covilhã, PortugalCannabis is the most consumed illicit drug worldwide, and its legal status is a source of concern. This study proposes a rapid procedure for the simultaneous quantification of Δ<sup>9</sup>-tetrahydrocannabinol (THC), 11-hydroxy-Δ<sup>9</sup>-tetrahydrocannabinol (11-OH-THC), 11-nor-9-carboxy-Δ<sup>9</sup>-tetrahydrocannabinol (THC-COOH), cannabidiol (CBD), and cannabinol (CBN) in urine samples. Microextraction by packed sorbent (MEPS) was used to pre-concentrate the analytes, which were detected by gas chromatography–mass spectrometry. The procedure was previously optimized, and the final conditions were: conditioning with 50 µL methanol and 50 µL of water, sample load with two draw–eject cycles, and washing with 310 µL of 0.1% formic acid in water with 5% isopropanol; the elution was made with 35 µL of 0.1% ammonium hydroxide in methanol. This fast extraction procedure allowed quantification in the ranges of 1–400 ng/mL for THC and CBD, 5–400 ng/mL for CBN and 11-OH-THC, and 10–400 ng/mL for THC-COOH with coefficients of determination higher than 0.99. The limits of quantification and detection were between 1 and 10 ng/mL using 0.25 mL of sample. The extraction efficiencies varied between 26 and 85%. This analytical method is the first allowing the for determination of cannabinoids in urine samples using MEPS, a fast, simple, and low-cost alternative to conventional techniques.https://www.mdpi.com/1420-3049/27/17/5503cannabinoidsΔ<sup>9</sup>-tetrahydrocannabinolurinemicroextraction by packed sorbentgas chromatography-mass spectrometry
spellingShingle Luana M. Rosendo
Tiago Rosado
Patrik Oliveira
Ana Y. Simão
Cláudia Margalho
Suzel Costa
Luís A. Passarinha
Mário Barroso
Eugenia Gallardo
The Determination of Cannabinoids in Urine Samples Using Microextraction by Packed Sorbent and Gas Chromatography-Mass Spectrometry
Molecules
cannabinoids
Δ<sup>9</sup>-tetrahydrocannabinol
urine
microextraction by packed sorbent
gas chromatography-mass spectrometry
title The Determination of Cannabinoids in Urine Samples Using Microextraction by Packed Sorbent and Gas Chromatography-Mass Spectrometry
title_full The Determination of Cannabinoids in Urine Samples Using Microextraction by Packed Sorbent and Gas Chromatography-Mass Spectrometry
title_fullStr The Determination of Cannabinoids in Urine Samples Using Microextraction by Packed Sorbent and Gas Chromatography-Mass Spectrometry
title_full_unstemmed The Determination of Cannabinoids in Urine Samples Using Microextraction by Packed Sorbent and Gas Chromatography-Mass Spectrometry
title_short The Determination of Cannabinoids in Urine Samples Using Microextraction by Packed Sorbent and Gas Chromatography-Mass Spectrometry
title_sort determination of cannabinoids in urine samples using microextraction by packed sorbent and gas chromatography mass spectrometry
topic cannabinoids
Δ<sup>9</sup>-tetrahydrocannabinol
urine
microextraction by packed sorbent
gas chromatography-mass spectrometry
url https://www.mdpi.com/1420-3049/27/17/5503
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