Forensic Toxicology Service, Faculty of Medicine, Institute of Legal Medicine, University of Santiago de Compostela, 15782, Santiago de Compostela, Spain.
Department of Analytical Chemistry, Faculty of Chemistry and Health Research Institute of Santiago de Compostela (IDIS), University of Santiago de Compostela, 15782, Santiago de Compostela, Spain.
Anal Bioanal Chem. 2019 Jan;411(1):193-203. doi: 10.1007/s00216-018-1428-5. Epub 2018 Oct 25.
Drugs of abuse and new psychoactive substances (NPS) for recreational purposes are in constant evolution, and their consumption constitutes a significant risk to public health and road safety. The development of an analytical methodology to confirm the intake of illicit drugs in biological fluids is required for an effective control of these substances. An ultra-performance liquid chromatography-tandem mass spectrometry method (UPLC-MS/MS) was developed for simultaneous determination of 10 synthetic cathinones and 10 illicit drugs in oral fluid easily sampled through non-invasive maneuvers. The UPLC-MS/MS method was coupled to an ultrasound-assisted dispersive liquid-liquid microextraction (US-DLLME), which is a miniaturized and inexpensive technique that uses reduced volumes of solvents and samples. The US-DLLME was optimized by using a 234//18 asymmetric screening design and a Doehlert design. Sample volume, dispersion and extraction solvent volumes, pH, US time, and amount of sodium chloride were evaluated. The US-DLLME-UPLC-MS/MS method was validated according to international guidelines. Limits of quantitation (LOQs) ranged from 0.25 to 5 ng mL, and the linear range spanned from LOQ to 500 ng mL with R higher than 0.9907, for most of the target drugs. Precision ranged from 1.7 to 14.8 %RSD. Accuracy, i.e., extraction recovery, ranged from 74 to 129%. The proposed method was successfully applied to the analysis of 15 samples from patients on a drug detoxification program.
滥用药物和新型精神活性物质（NPS）被用于娱乐目的，它们的使用对公共健康和道路安全构成了重大风险。为了有效控制这些物质，需要开发一种分析方法来确认生物液中非法药物的摄入。本文建立了一种超高效液相色谱-串联质谱法（UPLC-MS/MS），用于同时检测唾液中 10 种合成卡西酮和 10 种非法药物。UPLC-MS/MS 法与超声辅助分散液-液微萃取（US-DLLME）联用，后者是一种微型化、廉价的技术，使用较少的溶剂和样品量。采用 234//18 不对称筛选设计和 Doehlert 设计对 US-DLLME 进行了优化。评估了样品体积、分散和萃取溶剂体积、pH 值、超声时间和氯化钠用量。US-DLLME-UPLC-MS/MS 方法按照国际指南进行了验证。大多数目标药物的定量限（LOQ）范围为 0.25 至 5 ng/mL，线性范围从 LOQ 到 500 ng/mL，相关系数（R）均高于 0.9907。精密度范围为 1.7%至 14.8%RSD。准确度，即萃取回收率，范围为 74%至 129%。该方法成功应用于 15 名戒毒患者样本的分析。
