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采用填充吸附剂微萃取与气相色谱-质谱联用技术测定尿样中的大麻素。

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

机构信息

Centro de Investigação em Ciências da Saúde, Universidade da Beira Interior (CICS-UBI), Av. Infante D. Henrique, 6201-506 Covilhã, Portugal.

Laboratório de Fármaco-Toxicologia, Ubimedical, Universidade da Beira Interior, Estrada Municipal 506, 6200-284 Covilhã, Portugal.

出版信息

Molecules. 2022 Aug 27;27(17):5503. doi: 10.3390/molecules27175503.

Abstract

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-tetrahydrocannabinol (THC), 11-hydroxy-Δ-tetrahydrocannabinol (11-OH-THC), 11-nor-9-carboxy-Δ-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.

摘要

大麻是全球范围内使用最广泛的非法药物,其法律地位是一个令人关注的问题。本研究提出了一种快速程序,用于同时定量检测尿液样品中的Δ-四氢大麻酚(THC)、11-羟基-Δ-四氢大麻酚(11-OH-THC)、11-去甲-9-羧酸-Δ-四氢大麻酚(THC-COOH)、大麻二酚(CBD)和大麻酚(CBN)。微萃取填充固相(MEPS)用于预浓缩分析物,然后通过气相色谱-质谱法进行检测。该程序已预先优化,最终条件为:用 50 µL 甲醇和 50 µL 水进行预处理,用两个抽吸-推出循环进行样品加载,用 310 µL 含 5%异丙醇的 0.1%甲酸水溶液进行洗涤;用 35 µL 甲醇中的 0.1%氨水中洗脱。这种快速提取程序允许在 THC 和 CBD 的 1-400 ng/mL、CBN 和 11-OH-THC 的 5-400 ng/mL 以及 THC-COOH 的 10-400 ng/mL 范围内进行定量分析,相关系数均高于 0.99。使用 0.25 mL 样品,定量限和检测限在 1 至 10 ng/mL 之间。提取效率在 26%至 85%之间变化。该分析方法是第一个使用 MEPS 测定尿液中大麻素的方法,是一种快速、简单且成本低廉的替代传统技术的方法。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/2fe4/9457599/a1d6913c7316/molecules-27-05503-g001.jpg

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