Shah Iltaf, Petroczi Andrea, Uvacsek Martina, Ránky Márta, Naughton Declan P
School of Life Sciences, Kingston University, Kingston-upon-Thames, Surrey, UK.
Faculty of Physical Education and Sports Sciences, Semmelweis University, Budapest, Hungary.
Chem Cent J. 2014 Dec 13;8(1):73. doi: 10.1186/s13065-014-0073-0. eCollection 2014.
Considerable efforts are being extended to develop more effective methods to detect drugs in forensic science for applications such as preventing doping in sport. The aim of this study was to develop a sensitive and accurate method for analytes of forensic and toxicological nature in human hair at sub-pg levels.
The hair test covers a range of different classes of drugs and metabolites of forensic and toxicological nature including selected anabolic steroids, cocaine, amphetamines, cannabinoids, opiates, bronchodilators, phencyclidine and ketamine. For extraction purposes, the hair samples were decontaminated using dichloromethane, ground and treated with 1 M sodium hydroxide and neutralised with hydrochloric acid and phosphate buffer and the homogenate was later extracted with hexane using liquid-liquid extraction (LLE). Following extraction from hair samples, drug-screening employed liquid chromatography coupled to tandem mass spectrometric (LC-MS/MS) analysis using dynamic multiple reaction monitoring (DYN-MRM) method using proprietary software. The screening method (for > 200 drugs/metabolites) was calibrated with a tailored drug mixture and was validated for 20 selected drugs for this study. Using standard additions to hair sample extracts, validation was in line with FDA guidance. A Zorbax Eclipse plus C18 (2.1 mm internal diameter × 100 mm length × 1.8 μm particle size) column was used for analysis. Total instrument run time was 8 minutes with no noted matrix interferences. The LOD of compounds ranged between 0.05-0.5 pg/mg of hair. 233 human hair samples were screened using this new method and samples were confirmed positive for 20 different drugs, mainly steroids and drugs of abuse.
This is the first report of the application of this proprietary system to investigate the presence of drugs in human hair samples. The method is selective, sensitive and robust for the screening and confirmation of multiple drugs in a single analysis and has potential as a very useful tool for the analysis of large array of controlled substances and drugs of abuse.
为了开发更有效的方法用于法医学中检测药物，例如防止体育赛事中的兴奋剂使用，人们付出了巨大努力。本研究的目的是开发一种灵敏且准确的方法，用于检测人发中亚皮克水平的具有法医学和毒理学性质的分析物。
毛发检测涵盖了一系列具有法医学和毒理学性质的不同类别药物及其代谢物，包括选定的合成代谢类固醇、可卡因、苯丙胺、大麻素、阿片类药物、支气管扩张剂、苯环己哌啶和氯胺酮。为了提取，毛发样本先用二氯甲烷进行去污处理，研磨后用1 M氢氧化钠处理，再用盐酸和磷酸盐缓冲液中和，然后用液液萃取（LLE）法用己烷对匀浆进行萃取。从毛发样本中萃取后，药物筛选采用液相色谱-串联质谱（LC-MS/MS）分析，使用动态多反应监测（DYN-MRM）方法并借助专用软件。该筛选方法（针对>200种药物/代谢物）用定制的药物混合物进行校准，并针对本研究选定的20种药物进行了验证。通过向毛发样本提取物中添加标准品，验证符合美国食品药品监督管理局（FDA）的指导原则。使用Zorbax Eclipse plus C18（内径2.1 mm×长度100 mm×粒径1.8 μm）色谱柱进行分析。仪器总运行时间为8分钟，未发现基质干扰。化合物的检测限在0.05 - 0.5 pg/mg毛发之间。使用这种新方法对233份人发样本进行了筛选，样本中20种不同药物呈阳性，主要是类固醇和滥用药物。
这是首次报道应用该专有系统研究人发样本中药物的存在情况。该方法在单次分析中对多种药物的筛选和确证具有选择性、灵敏性和稳健性，有潜力成为分析大量受控物质和滥用药物的非常有用的工具。
