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通过固相微萃取结合基质衍生化对甲基苯丙胺和苯丙胺进行单根毛发分析。

Single hair analysis of methamphetamine and amphetamine by solid phase microextraction coupled with in matrix derivatization.

作者信息

Nishida Manami, Yashiki Mikio, Namera Akira, Kimura Kojiro

机构信息

Department of Legal Medicine, Graduate School of Biomedical Sciences, Hiroshima University, 1-2-3 Kasumi, Hiroshima 734-8551, Japan.

出版信息

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.

Abstract

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.

摘要

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。

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