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顶空固相微萃取和氮磷检测气相色谱法测定人发中的苯丙胺和甲基苯丙胺

Determination of amphetamine and methamphetamine in human hair by headspace solid-phase microextraction and gas chromatography with nitrogen-phosphorus detection.

作者信息

Koide I, Noguchi O, Okada K, Yokoyama A, Oda H, Yamamoto S, Kataoka H

机构信息

Criminal Investigation Laboratory, Okayama Prefectural Police Headquarters, Japan.

出版信息

J Chromatogr B Biomed Sci Appl. 1998 Apr 10;707(1-2):99-104. doi: 10.1016/s0378-4347(97)00582-3.

Abstract

A simple and rapid method for the determination of amphetamine (AP) and methamphetamine (MA) in human hair was developed by headspace solid-phase microextraction (SPME) and gas chromatography with nitrogen-phosphorus detection (GC-NPD). The hair (1 mg) was dissolved in 0.2 ml of a 5 M sodium hydroxide solution in a tightly sealed vial by shaking at 75 degrees C for about 5 min. In order to adsorb AP and MA on the SPME fiber, 100 microm of polydimethylsiloxane fiber was exposed to the headspace of the vial, and the vial was heated at 55 degrees C for 20 min. Then the fiber was removed from the vial and inserted into the injection port of the GC-NPD system using a CBJ-17 capillary column. The compounds adsorbed on the fiber were analyzed by exposing the fiber at 220 degrees C for 30 s in the GC injection port. By using this method, AP and MA in human hair could be analyzed simply and rapidly without any interference from coexisting substances. The percentages of AP and MA extracted from human hair by the SPME method were 48 and 62%, respectively, and relative standard deviations were below 10% (n=5). The calibration curves for AP and MA were linear in the ranges of 0.4-15 and 4-160 ng/mg hair, respectively. The detection limits of AP and MA at a signal-to-noise ratio of three were 0.1 and 0.4 ng/mg hair, respectively. This method could be applied to the analysis of an abuser's hair sample.

摘要

建立了一种采用顶空固相微萃取(SPME)和氮磷检测气相色谱法(GC-NPD)测定人发中苯丙胺(AP)和甲基苯丙胺(MA)的简单快速方法。将1mg头发置于密封小瓶中,加入0.2ml 5M氢氧化钠溶液,在75℃下振荡约5分钟使其溶解。为了使AP和MA吸附在SPME纤维上,将100μm的聚二甲基硅氧烷纤维暴露于小瓶顶空,小瓶在55℃下加热20分钟。然后将纤维从小瓶中取出,使用CBJ-17毛细管柱插入GC-NPD系统的进样口。通过在GC进样口中于220℃下将纤维暴露30秒来分析吸附在纤维上的化合物。采用该方法,可简单快速地分析人发中的AP和MA,不受共存物质的干扰。通过SPME方法从人发中提取的AP和MA的百分比分别为48%和62%,相对标准偏差低于10%(n = 5)。AP和MA的校准曲线分别在0.4 - 15和4 - 160 ng/mg头发范围内呈线性。在信噪比为3时,AP和MA的检测限分别为0.1和0.4 ng/mg头发。该方法可应用于滥用者头发样本的分析。

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