Okajima K, Namera A, Yashiki M, Tsukue I, Kojima T
Department of Legal Medicine, Faculty of Medicine, Hiroshima University, 1-2-3 Kasumi, Minami-ku, Hiroshima 734-8551, Japan.
Forensic Sci Int. 2001 Feb 1;116(1):15-22. doi: 10.1016/s0379-0738(00)00341-8.
A simple and highly sensitive method for analysis of derivatized methamphetamine (MA) and amphetamine (AM) in whole blood was developed using headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry electron impact ionization selected ion monitoring (GC-MS-EI-SIM). A whole blood sample, deuterated-MA (d(5)-MA), as an internal standard (IS), tri-n-propylamine and pentafluorobenzyl bromide were placed in a vial. The vial was heated and stirred at 90 degrees C for 30min. Then the extraction fiber of the SPME was exposed at 90 degrees C for 30min in the headspace of the vial while being stirred. The derivatives adsorbed on the fiber were desorbed by exposing the fiber in the injection port of a GC-MS. The calibration curves showed linearity in the range of 0.5-1000ng/g for both MA and AM. The time for analysis was about 80min per sample. In addition, this proposed method was applied to two autopsy cases where MA ingestion was suspected. In one case, MA and AM concentrations in the mixed left and right heart blood were 165 and 36.9ng/g, respectively. In the other case, MA and AM concentrations were 1.79 and 0.119 microg/g in the left heart blood, and 1.27 and 0.074 microg/g in the right heart blood, respectively.
采用顶空固相微萃取（HS-SPME）和气相色谱-质谱电子轰击电离选择离子监测（GC-MS-EI-SIM）技术，建立了一种简单且高灵敏度的全血中衍生化甲基苯丙胺（MA）和苯丙胺（AM）的分析方法。将全血样品、作为内标（IS）的氘代甲基苯丙胺（d(5)-MA）、三正丙胺和五氟苄基溴置于小瓶中。小瓶在90℃下加热搅拌30分钟。然后，在搅拌的同时，将SPME的萃取纤维在小瓶顶空中于90℃下暴露30分钟。通过将纤维暴露于GC-MS的进样口，使吸附在纤维上的衍生物解吸。校准曲线显示MA和AM在0.5-1000ng/g范围内呈线性。每个样品的分析时间约为80分钟。此外，该方法应用于两例疑似甲基苯丙胺摄入的尸检病例。在一例中，左右混合心脏血液中MA和AM的浓度分别为165和36.9ng/g。在另一例中，左心血液中MA和AM的浓度分别为1.79和0.119μg/g，右心血液中分别为1.27和0.074μg/g。
