液相色谱-串联质谱法测定人体汗液中的合法和非法药物及代谢物,Analytical Methods

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液相色谱-串联质谱法测定人体汗液中的合法和非法药物及代谢物
Analytical Methods ( IF 2.7 ) Pub Date : 2023-08-02 , DOI: 10.1039/d3ay00678f
Margaret Sotom ₁ , Paul Bowdler ₁ , Kevin C Honeychurch ₁

Affiliation

开发了汗液中的液相色谱-串联质谱筛查方法，用于同时测定三种合法药物（尼古丁、扑热息痛和咖啡因）；四种非法药物（可卡因、氯胺酮、25I-NBOMe 和甲基苯丙胺）和两种代谢物（苯甲酰爱康宁和可替宁）。使用 pH 5 的乙酸钠缓冲液从汗斑中释放出目标药物，并利用 Strata-X-Drug B 柱通过固相萃取 (SPE) 进一步纯化。SPE 有机洗涤和洗脱的最佳溶剂成分分别为去离子水中的 70% v/v 甲醇和甲醇中的 5% v/v 氢氧化铵。使用具有梯度洗脱的表面多孔颗粒 C18 柱实现色谱分离，使用 (A) 0.1% 甲酸水溶液和 (B) 乙腈作为流动相成分。结合保留时间和多反应监测 (MRM) 模式下监测的每个分析物的两个前体-产物离子跃迁的离子比来识别目标药物。该方法对于 1.0–150.0 ng mL ^-1的所有目标药物均呈线性，相应的定量限为 1.0 ng mL ^-1。发现检测限为每个贴片 0.1–0.6 ng。该方法随后被应用于分析 5 名男性和 4 名女性参与者（年龄 20-25 岁）的汗液样本。使用纱布保护层从两个区域（右前臂和左大腿）收集汗水。所有 18 个贴片的至少一种目标分析物检测结果呈阳性。这项研究的结果不仅表明实现了多物质筛查方法，而且汗斑可以用来指示个人的药物使用情况。因此，他们可以为法医应用提供替代的非侵入性技术。

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Determination of licit and illicit drugs and metabolites in human sweat by liquid chromatography-tandem mass spectrometry

A liquid chromatography-tandem mass spectrometry screening method in sweat was developed for the simultaneous determination of three licit drugs (nicotine, paracetamol, and caffeine); four illicit drugs (cocaine, ketamine, 25I-NBOMe and methamphetamine) and two metabolites (benzoylecgonine and cotinine). Target drugs were liberated from sweat patches with pH 5 sodium acetate buffer and further purified by solid phase extraction (SPE) utilising Strata-X-Drug B cartridges. Optimal solvent constituents for SPE organic wash and elution were 70% v/v methanol in deionised water and 5% v/v ammonium hydroxide in methanol respectively. Chromatographic separation was achieved using a superficially porous particle C18 column with gradient elution, using (A) 0.1% formic acid in water and (B) acetonitrile as mobile phase constituents. Target drugs were identified using a combination of retention time, and the ion ratios for two precursor-product ion transitions for each analyte monitored in multiple reaction monitoring (MRM) mode. The method was linear for all target drugs from 1.0–150.0 ng mL⁻¹ with corresponding limits of quantitation of 1.0 ng mL⁻¹. Limits of detection were found to range from 0.1–0.6 ng per patch. The method was subsequently applied to the analysis of sweat samples from five male and four female participants aged 20–25 years. Sweat was collected from two areas (right forearm and left thigh) using protected layers of gauze. All eighteen patches tested positive for at least one target analyte. The results of this study not only show a multi-substance screening method was achieved but also that sweat patches can be used to indicate an individual's drug use. Therefore, they can provide an alternative non-invasive technique for forensic applications.

更新日期：2023-08-07

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