Johansen Sys Stybe, Jornil Jakob
Section of Forensic Chemistry, Department of Forensic Medicine, Faculty of Health Sciences, University of Copenhagen, Denmark.
Scand J Clin Lab Invest. 2009;69(1):113-20. doi: 10.1080/00365510802439072.
The aim of this study was to develop a quantitative gas chromatography mass spectrometry (GC-MS) method to determine the classical amphetamines and their methylenedioxylated derivatives in human hair. The procedure involved liquid-liquid extraction of hydrolysed hair spiked with deuterated internal standards and direct derivatization with perfluorooctanoyl chloride. After evaporation of the organic phase and dissolution in butylacetate, the derivatized compounds were injected into a GC-MS. Method validation results showed a linear range from 0.25 to 25 ng/mg for the target compounds: amphetamine (AM), methamphetamine (MA), methylenedioxyamphetamine (MDA) and methylenedioxymethamphetamine (MDMA or ecstasy). An intra-day precision of 3-6% RSD and an inter-day precision of 3-17% RSD were observed. Trueness was between 96 % and 106% for the target compounds. The limit of detection ranged from 0.07 to 0.14 ng/mg and of quantification from 0.24 to 0.46 ng/mg, depending on compound. The method was applied on 40 authentic hair samples (segmented or pooled hair), of which 15 cases involved amphetamine and/or ecstasy. The hair concentrations ranged from LOD to 3.2 ng/mg of AM in 7 cases, to 0.4 ng/mg of MDA in 3 cases and to 5.9 ng/mg of MDMA in 13 cases. MA was only detected once at trace level. The method, including the derivatization procedure, is simple and robust with a sensitivity that is satisfactory for measurement of amphetamines and ecstasy in hair from abusers.
本研究的目的是开发一种定量气相色谱 - 质谱（GC-MS）方法，用于测定人发中的经典苯丙胺及其亚甲基二氧基化衍生物。该程序包括用氘代内标对水解头发进行液 - 液萃取，并用全氟辛酰氯直接衍生化。有机相蒸发并溶解于乙酸丁酯后，将衍生化的化合物注入GC-MS。方法验证结果表明，目标化合物：苯丙胺（AM）、甲基苯丙胺（MA）、亚甲基二氧基苯丙胺（MDA）和亚甲基二氧基甲基苯丙胺（MDMA或摇头丸）的线性范围为0.25至25 ng/mg。日内精密度为3 - 6%RSD，日间精密度为3 - 17%RSD。目标化合物的准确度在96%至106%之间。检测限范围为0.07至0.14 ng/mg，定量限范围为0.24至0.46 ng/mg，具体取决于化合物。该方法应用于40份真实头发样本（分段或混合头发），其中15例涉及苯丙胺和/或摇头丸。头发浓度范围为：7例中AM从检测限到3.2 ng/mg，3例中MDA到0.4 ng/mg，13例中MDMA到5.9 ng/mg。MA仅在痕量水平被检测到一次。该方法，包括衍生化程序，简单且稳健，灵敏度对于测量滥用者头发中的苯丙胺和摇头丸而言令人满意。
