Centro Regionale Antidoping e di Tossicologia "A. Bertinaria", Turin, Italy.
Dipartimento di Chimica, Università degli Studi di Torino, Turin, Italy.
J Sep Sci. 2019 Apr;42(8):1577-1584. doi: 10.1002/jssc.201801249. Epub 2019 Feb 27.
Most routine practices for drugs-of-abuse testing do not include screening procedures for new psychoactive substances, despite their increasing diffusion, preventing clear knowledge of the real consumption of these drugs in the populations. To make up for this shortcoming, a gas chromatography with mass spectrometry method was developed for the simultaneous determination of 18 synthetic cathinones and one amphetamine-like compound in human urine. The sample preparation was based on liquid-liquid extraction under alkaline condition followed by derivatization with trifluoroacetic anhydride. The separation of the 19 analytes was achieved in less than 10 min. The whole methodology was validated according to national and international guidelines. Selectivity, linearity range, limit of detection and limit of quantitation, precision and accuracy were evaluated. For all the analytes, the calibration curve was linear in the 100-1000 ng/mL concentration range. The limits of detection ranged from 10 to 30 ng/mL and limits of quantitation from 30 to 100 ng/mL. Precisions were in the ranges 0.1-10.4%, and 1.0-12.1% for low (100 ng/mL) and high (1000 ng/mL) concentration, respectively. The accuracy, expressed as bias% was within ±20% for all the analytes. The present method was successfully applied to urine samples originating from autopsies, drug abuse/withdrawal controls, clinical investigations, roadside controls, driving re-licensing, and workplace testing.
大多数药物滥用检测的常规做法都不包括新精神活性物质的筛选程序,尽管它们的传播越来越广泛,但却无法清楚地了解这些药物在人群中的实际使用情况。为了弥补这一不足,开发了一种气相色谱-质谱联用方法,用于同时测定人尿中 18 种合成苯丙胺类兴奋剂和一种苯丙胺类化合物。样品制备基于在碱性条件下进行液-液萃取,然后用三氟乙酸酐衍生化。19 种分析物在不到 10 分钟的时间内得到分离。整个方法学均根据国家和国际指南进行了验证。评估了选择性、线性范围、检测限和定量限、精密度和准确度。对于所有分析物,校准曲线在 100-1000ng/mL 浓度范围内呈线性。检测限范围为 10-30ng/mL,定量限范围为 30-100ng/mL。精密度分别在 0.1-10.4%和 1.0-12.1%之间,分别用于低浓度(100ng/mL)和高浓度(1000ng/mL)。所有分析物的准确度,以偏倚%表示,均在±20%范围内。该方法成功应用于尸检、药物滥用/戒断对照、临床研究、路边控制、驾驶重新许可和工作场所测试的尿样。