Nishida Manami, Yashiki Mikio, Namera Akira, Kimura Kojiro
Department of Legal Medicine, Graduate School of Biomedical Sciences, Hiroshima University, 1-2-3 Kasumi, Hiroshima 734-8551, Japan.
J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Oct 2;842(2):106-10. doi: 10.1016/j.jchromb.2006.07.039. Epub 2006 Sep 12.
A sensitive method for detection of methamphetamine (MA) and amphetamine (AP) in human hair was developed using solid phase microextraction (SPME) and one-pot derivatization. MA and AP were directly derivatized to N-propoxycarbonyl derivatives in an aqueous solution by propylchloroformate in a one-pot reaction before extraction by SPME. The derivatives were extracted to a coating of SPME from a headspace of the vial. The adsorbed derivatives were thermally desorbed in the injection port of a gas chromatograph. Pentadeuterated MA was used as an internal standard. The absolute recoveries of MA and AP from the spiked hair were 2.80-17.5%, respectively. The calibration curves showed linearity in the range of 0.05-20 ng/0.08 mg/vial for MA and 0.1-20 ng/0.08 mg/vial for AP in hair. Detection limits (S/N = 3) of MA and AP were 0.02 and 0.05 ng/0.08 mg/vial. The coefficients of variation of intraday were 1.04-26.4%. Additionally, this proposed method was applied to segmental analysis in clinical and medico-legal cases of MA intoxication.
采用固相微萃取(SPME)和一锅法衍生化技术,建立了一种检测人发中甲基苯丙胺(MA)和苯丙胺(AP)的灵敏方法。在通过SPME萃取之前,MA和AP在水溶液中通过氯甲酸丙酯在一锅反应中直接衍生化为N - 丙氧基羰基衍生物。衍生物从小瓶的顶空萃取到SPME涂层上。吸附的衍生物在气相色谱仪的进样口中进行热解吸。五氘代甲基苯丙胺用作内标。加标毛发中MA和AP的绝对回收率分别为2.80 - 17.5%。校准曲线表明,毛发中MA在0.05 - 20 ng/0.08 mg/小瓶范围内、AP在0.1 - 20 ng/0.08 mg/小瓶范围内呈线性。MA和AP的检测限(S/N = 3)分别为0.02和0.05 ng/0.08 mg/小瓶。日内变异系数为1.04 - 26.4%。此外,该方法还应用于MA中毒临床和法医案件的分段分析。