Department of Forensic Medicine, Faculty of Health Sciences, University of Copenhagen, Copenhagen, Denmark.
Forensic Sci Int. 2010 Mar 20;196(1-3):85-92. doi: 10.1016/j.forsciint.2009.12.027. Epub 2010 Jan 12.
An UPLC-TOF-MS method for simultaneous screening and quantification of 52 drugs in hair was developed and validated. The selected drugs represent the most common classes of pharmaceuticals and drugs of abuse such as amphetamines, analgesics, antidepressants, antipsychotics, benzodiazepines, cocaine, ketamine and opioids. Hair samples were extracted with methanol:acetonitrile:ammonium formate (2 mM, 8% acetonitrile, pH 5.3) overnight at 37 degrees C. The target drugs were separated and quantified using a Waters ACQUITY UPLC coupled to a Waters Micromass LCT Premier XE Time-of-Flight mass spectrometer. Total chromatographic run time was 17min. The data were treated with the MassLynx software ChromaLynx XS and QuanLynx for automated identification and quantification, respectively. The limits of detection ranged from 0.01 to 0.10 ng/mg using a 10-mg hair sample and the limit of quantification was 0.05 ng/mg for 87% of the analytes. A good linear behaviour was achieved for most of the analytes in the range from LOQ to 10 or 25 ng/mg except for the amphetamines. The method showed an acceptable precision and trueness, since the obtained CV and BIAS values were <or=25% for 81% of the analytes. The extraction recoveries for 92% of the analytes ranged between 84 and 106% and the extraction recoveries for all analytes were better than 60%. The method was applied to 15 autopsy hair samples from forensic investigations showing a wide abuse pattern of many pharmaceuticals and drugs of abuse within a period of less than three months. The present study demonstrated that the combination of accurate mass and retention time can provide good selectivity, which demonstrates that the TOF instrument is adequate for both screening and quantification purposes. Furthermore, it was shown that screening with the ChromaLynx XS software is less sensitive and selective for some analytes than the QuanLynx software, especially in low concentrations.
建立并验证了一种超高效液相色谱-飞行时间质谱法（UPLC-TOF-MS），用于同时筛查和定量头发中的 52 种药物。所选药物代表了最常见的药物类别和滥用药物，如苯丙胺类、阿片类药物、麻醉性镇痛药、抗抑郁药、抗精神病药、苯二氮䓬类、可卡因、氯胺酮和类阿片类物质。头发样本在 37°C 下用甲醇：乙腈：甲酸铵（2mM，8%乙腈，pH5.3）整夜提取。采用沃特世 ACQUITY UPLC 与沃特世 Micromass LCT Premier XE 飞行时间质谱联用，对目标药物进行分离和定量。总色谱运行时间为 17 分钟。使用 MassLynx 软件 ChromaLynx XS 和 QuanLynx 分别对数据进行处理，以实现自动识别和定量。使用 10mg 头发样本，检测限（LOD）范围为 0.01-0.10ng/mg，87%的分析物的定量限（LOQ）为 0.05ng/mg。大多数分析物在 LOQ 至 10 或 25ng/mg 的范围内表现出良好的线性行为，除了苯丙胺类物质。该方法的精密度和准确度令人满意，因为 81%的分析物获得的 CV 和 BIAS 值均<或=25%。92%的分析物的提取回收率在 84%至 106%之间，所有分析物的提取回收率均优于 60%。该方法应用于 15 例法医调查的尸检头发样本，结果显示在不到三个月的时间内，许多药物和滥用药物的滥用情况非常广泛。本研究表明，准确质量和保留时间的组合可以提供良好的选择性，这表明飞行时间仪器足以用于筛查和定量目的。此外，结果表明，与 QuanLynx 软件相比，ChromaLynx XS 软件在某些分析物（尤其是低浓度下）的灵敏度和选择性较低。
