Liu Hsiu-Chuan, Liu Ray H, Lin Dong-Liang
Department of Forensic Toxicology, Institute of Forensic Medicine, Ministry of Justice, Taipei, Taiwan.
Department of Justice Sciences, University of Alabama at Birmingham, Birmingham, AL, USA.
J Anal Toxicol. 2015 Apr;39(3):183-91. doi: 10.1093/jat/bku174. Epub 2015 Jan 6.
In this study, an incubation, solid-phase extraction (SPE) and LC-MS-MS procedure was developed, validated and used for simultaneous analysis of amphetamine (AP), methamphetamine (MA), morphine (MOR), codeine (COD), 6-acetylmorphine (6-AM) and 6-acetylcodeine (6-AC) in hair. Hair samples were initially cut into sections, washed with dichloromethane, then sonicated in a methanol-trifluoroacetic acid mixture. The resulting solutions were processed with a SPE procedure before undergoing LC-MS-MS analysis. Mass spectrometric analysis was performed in positive-ion, multiple reactions monitoring (MRM) mode, using appropriate collision energy for each selected precursor ion. The overall protocol, when applied to the analysis of hair (50 mg) samples fortified with 100-10,000 pg/mg of the analytes, was found to achieve 55.5-74.6% recovery of the six analytes with the following analytical parameters: (i) intra- and interday precision/accuracy data for the six analytes in the 1.6-7.6%/-6.0-12.8% and 1.3-6.6%/-6.9-9.3% ranges, respectively; (ii) r(2) > 0.998 for all six analytes and (iii) LOD 2 pg/mg for AP and MA, and 8 pg/mg for MOR, COD, 6-AM and 6-AC; LOQ 10 pg/mg for all six analytes. This method was then utilized to (i) analyze hair samples collected from 86 self-reported drug users and (ii) evaluate the deposition pattern of drugs in head hairs from four female MA and heroin users in a rehabilitation facility. This relatively simple protocol was found superior over the GC-MS methods we have previously developed and utilized in our laboratory for the analysis of these six analytes.
在本研究中,开发、验证了一种孵育、固相萃取(SPE)和液相色谱-串联质谱(LC-MS-MS)方法,并用于同时分析毛发中的苯丙胺(AP)、甲基苯丙胺(MA)、吗啡(MOR)、可待因(COD)、6-乙酰吗啡(6-AM)和6-乙酰可待因(6-AC)。毛发样品首先被切成小段,用二氯甲烷洗涤,然后在甲醇-三氟乙酸混合物中超声处理。所得溶液在进行LC-MS-MS分析之前先采用SPE方法处理。质谱分析在正离子、多反应监测(MRM)模式下进行,对每个选定的前体离子使用适当的碰撞能量。当将该总体方案应用于分析添加了100 - 10,000 pg/mg分析物的毛发(50 mg)样品时,发现六种分析物的回收率为55.5 - 74.6%,具有以下分析参数:(i)六种分析物的日内和日间精密度/准确度数据分别在1.6 - 7.6% / -6.0 - 12.8%和1.3 - 6.6% / -6.9 - 9.3%范围内;(ii)所有六种分析物的r(2) > 0.998;(iii)AP和MA的检测限为2 pg/mg,MOR、COD、6-AM和6-AC的检测限为8 pg/mg;所有六种分析物的定量限为10 pg/mg。然后利用该方法(i)分析从86名自我报告的吸毒者收集的毛发样品,以及(ii)评估一家康复机构中四名女性甲基苯丙胺和海洛因使用者头发生长过程中药物的沉积模式。发现这个相对简单的方案优于我们实验室之前开发并用于分析这六种分析物的气相色谱-质谱(GC-MS)方法。