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Target analysis of psychoactive drugs in oral fluid by QuEChERS extraction and LC-MS/MS
Journal of Pharmaceutical and Biomedical Analysis ( IF 3.4 ) Pub Date : 2024-04-08 , DOI: 10.1016/j.jpba.2024.116139
Ettore Ferrari Júnior , Victor Souza Bitencourt , Ágatha Beatriz Mariano de Souza , Eloisa Dutra Caldas

This study aimed to validate a modified QuEChERS method, followed by liquid chromatography-tandem mass spectrometry, for the determination of 51 psychoactive substances and screening of 22 ones in oral fluid from electronic dance music party (EDM) attendees. Unstimulated oral fluid was collected in a polypropylene tube and stored in a glass vial at −20 ºC. The sample was extracted with acetonitrile:water and MgSO/NaOAc, followed by cleanup with primary secondary amine and MgSO. The effectiveness of the sample storage conditions was shown to be comparable to when the Quantisal™ buffer was used, with no substantial concentration loss (< 15%) for all the substances after up to 72 hours at −20º C. The method was satisfactorily validated, with limits of detection (LOD) and quantification (LOQ) ranging from 0.04 to 0.5 ng/mL and 0.1–1.5 ng/mL, respectively, and was applied to the analysis of 62 real samples. The main substances detected were 3,4-methylenedioxymethamphetamine (MDMA) (<0.5–829 ng/mL) and/or methylenedioxyamphetamine (MDA) (10.1 – 460.6 ng/mL), found in 27 samples, and cocaine (13.0–407.3 ng/mL) and its metabolites (benzoylecgonine 0.17–214.1 ng/mL; ecgonine methyl ester 1.8–150.1 ng/mL) in eight samples. Methamphetamine (11–439 ng/mL) was detected in eight samples, along with MDMA and MDA; eutylone was detected in two cases (4.7 and 24.1 ng/mL) reported as "ecstasy" ingestion. A comparison between self-reported drug use and results of oral fluid analysis indicated that the use of illicit substances is often underreported among EDM attendees, who are often unaware of the substances they consume.

中文翻译:

QuEChERS 萃取和 LC-MS/MS 对口腔液中精神活性药物的目标分析

本研究旨在验证改进的 QuEChERS 方法,然后采用液相色谱-串联质谱法测定电子舞曲派对 (EDM) 参加者口腔液中的 51 种精神活性物质并筛查 22 种精神活性物质。将未刺激的口腔液收集在聚丙烯管中,并在-20 ℃下储存在玻璃瓶中。用乙腈:水和 MgSO4/NaOAc 萃取样品,然后用伯仲胺和 MgSO4 净化。样品储存条件的有效性与使用 Quantisal™ 缓冲液时相当,在 -20°C 下长达 72 小时后,所有物质的浓度均没有显着损失 (< 15%)。该方法得到了令人满意的验证,检测限 (LOD) 和定量限 (LOQ) 分别为 0.04 至 0.5 ng/mL 和 0.1–1.5 ng/mL,并应用于 62 个真实样品的分析。检测到的主要物质是 27 个样品中发现的 3,4-亚甲二氧基甲基苯丙胺 (MDMA)(<0.5–829 ng/mL)和/或亚甲二氧基苯丙胺 (MDA)(10.1 – 460.6 ng/mL)以及可卡因(13.0–407.3 ng/mL) /mL)及其代谢物(苯甲酰爱康宁 0.17–214.1 ng/mL;爱康宁甲酯 1.8–150.1 ng/mL)在八个样品中。在 8 个样品中检测到甲基苯丙胺 (11–439 ng/mL),以及 MDMA 和 MDA;在两例报告为“摇头丸”摄入的病例中检测到了 eutylon(4.7 ng/mL 和 24.1 ng/mL)。自我报告的药物使用情况与口腔液分析结果之间的比较表明,EDM 参加者中非法物质的使用情况往往被低估,他们往往不知道自己消耗了哪些物质。
更新日期:2024-04-08
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