Cappelle Delphine, De Doncker Mireille, Gys Celine, Krysiak Kamelia, De Keukeleire Steven, Maho Walid, Crunelle Cleo L, Dom Geert, Covaci Adrian, van Nuijs Alexander L N, Neels Hugo
Toxicological Centre, University of Antwerp, Universiteitsplein 1, B2610 Antwerp, Belgium.
Toxicology and TDM Laboratory, ZNA Stuivenberg Hospital, Lange Beeldekenstraat 267, B2060 Antwerp, Belgium.
Anal Chim Acta. 2017 Apr 1;960:101-109. doi: 10.1016/j.aca.2017.01.022. Epub 2017 Jan 25.
Hair and nails allow for a stable accumulation of compounds over time and retrospective investigation of past exposure and/or consumption. Owing to their long window of detection (weeks to months), analysis of these matrices can provide information complementary to blood and urine analysis or can be used in standalone when e.g. elimination from the body has already occurred. Drugs of abuse are often used together and, therefore, multi-analyte methods capable of detecting several substances and their metabolites in a single run are of importance. This paper presents the development and validation of a method based on liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) for the simultaneous detection of nine drugs of abuse and their metabolites in hair and nails. We focused on a simple and straightforward sample preparation to reduce costs, and allow application in routine laboratory practice. Chromatographic and mass spectrometric parameters, such as column type, mobile phase, and multiple reaction monitoring transitions were optimized. The method was validated according to the European Medicine Agency guidelines with an assessment of specificity, limit of quantification (LOQ), linearity, accuracy, precision, carry-over, matrix effects, recovery, and process efficiency. Linearity ranged from 25 to 20 000 pg mg hair and from 50 to 20 000 pg mg nails, and the lowest calibration point achieved the requirements for the LOQ (25 pg mg for hair and 50 pg mg for nails). Although it was not the main focus of the article, the reliability of the method was proven through successful participation in a proficiency test, and by investigation of authentic hair and nail samples from self-reported drug users. In the future, the method should allow comparison between the two matrices to acquire an in-depth knowledge of nail analysis and to define cutoff levels for nail analysis, as they exist for hair.
头发和指甲能够随着时间稳定地积累化合物，从而对过去的接触和/或摄入情况进行回顾性调查。由于它们的检测窗口期较长（数周至数月），对这些基质的分析可以提供与血液和尿液分析互补的信息，或者在例如体内物质已被清除的情况下单独使用。滥用药物常常同时使用，因此，能够在一次运行中检测多种物质及其代谢物的多分析物方法至关重要。本文介绍了一种基于液相色谱-串联质谱联用（LC-MS/MS）的方法的开发与验证，该方法用于同时检测头发和指甲中的九种滥用药物及其代谢物。我们专注于一种简单直接的样品制备方法，以降低成本，并使其适用于常规实验室操作。对色谱和质谱参数，如柱类型、流动相和多反应监测跃迁进行了优化。该方法根据欧洲药品管理局的指南进行了验证，评估了特异性、定量限（LOQ）、线性、准确度、精密度、残留、基质效应、回收率和过程效率。线性范围为头发中25至20000 pg/mg，指甲中50至20000 pg/mg，最低校准点达到了LOQ的要求（头发为25 pg/mg，指甲为50 pg/mg）。尽管这不是本文的主要重点，但通过成功参加能力验证测试以及对自我报告的吸毒者的真实头发和指甲样本进行调查，证明了该方法的可靠性。未来，该方法应能实现两种基质之间的比较，以深入了解指甲分析，并确定指甲分析的临界值，就像头发分析那样。
