Division of Clinical Pharmacology & Toxicology, Hospital for Sick Children, Department of Pharmacology & Toxicology, University of Toronto, Toronto, Ontario, Canada.
Forensic Sci Int. 2010 Mar 20;196(1-3):64-9. doi: 10.1016/j.forsciint.2009.12.046. Epub 2010 Jan 18.
Opiate hair analysis continues to prove difficult due to the scarcity of hair sample and low drug concentrations. For this reason, we developed a sensitive method utilizing headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) for the detection of three principle opiates; codeine, morphine, and 6-acetylmorphine.
Experimental conditions for HS-SPME and GC-MS were systematically optimized to produce the sensitive analytical method reported. Briefly, opiates were extracted from adult hair with methanol under agitation. The methanolic extract was then decanted into SPME autosampler vials, where deuterated standards of each of the 3 opiates were added at a concentration of 2 ng/mg. Samples were dried under N(2), derivatized, and subjected to HS-SPME coupled with GC/MS for analysis.
Preliminary datum for this study indicates detection limits for these 3 opiates are superior to that reported in the literature; an LOQ of 0.01 ng/mg for morphine and 6-acetylmorphine and 0.005 ng/mg for codeine. Linearity was evident between 0.01 ng/mg and 5 ng/mg for each opiate, with R(2) above 0.992. The robustness of the method was demonstrated to be acceptable as inter-day and intra-day precision fell below 15% for each opiate analyzed.
Compared with conventional methods, this method of detection for opiates is fast, simple, and accurate, with the sensitivity and specificity required in forensic and clinical toxicology.
由于毛发样本量少且药物浓度低，阿片类物质的毛发分析仍然具有挑战性。为此，我们开发了一种利用顶空固相微萃取（HS-SPME）与气相色谱-质谱联用（GC-MS）检测三种主要阿片类物质（可待因、吗啡和 6-乙酰吗啡）的灵敏方法。
对 HS-SPME 和 GC-MS 的实验条件进行了系统优化，以产生所报道的灵敏分析方法。简要地说，阿片类物质在搅拌下用甲醇从成人毛发中提取。然后将甲醇提取物倾入 SPME 自动进样瓶中，在每个 3 种阿片类物质的浓度为 2ng/mg 的情况下加入氘代标准品。样品在 N(2)下干燥，衍生化，然后进行 HS-SPME 与 GC/MS 分析。
本研究的初步数据表明，这些 3 种阿片类物质的检测限优于文献报道的检测限；吗啡和 6-乙酰吗啡的定量限为 0.01ng/mg，可待因的定量限为 0.005ng/mg。每种阿片类物质在 0.01ng/mg 至 5ng/mg 之间具有明显的线性关系，R(2)值均大于 0.992。该方法的稳健性可接受，因为每种分析的阿片类物质的日内和日间精密度均低于 15%。
与传统方法相比，这种阿片类物质的检测方法快速、简单、准确，具有法医毒理学和临床毒理学所需的灵敏度和特异性。
