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生物样品中p,p'-滴滴伊的固相微萃取和气相色谱-质谱分析

Solid-phase microextraction and gas chromatography-mass spectrometry analysis of p,p' -DDE in biological samples.

作者信息

Kusakabe T, Saito T, Takeichi S

机构信息

Department of Forensic Medicine, Tokai University School of Medicine, Isehara, Kanagawa, Japan.

出版信息

J Chromatogr B Biomed Sci Appl. 2001 Sep 15;761(1):93-8. doi: 10.1016/s0378-4347(01)00308-5.

DOI:10.1016/s0378-4347(01)00308-5
PMID:11585136
Abstract

A simple and rapid extraction method for the analysis of p,p'-DDE from rat whole blood and tissues was developed using headspace solid-phase microextraction (SPME). A vial containing a sample of p,p'-DDE, sodium hydroxide, and benzophenone as internal standard was heated at 120 degrees C. A polydimethylsiloxane-coated SPME fiber was exposed for 15 min in the headspace of the vial. The fiber needle was then injected and desorbed by exposing the fiber in the injection port of a capillary gas chromatography-mass spectrometry system. The calibration curve demonstrated good linearity throughout the concentration range from 0.02 to 50 microg/g for rat whole blood and liver samples. The limit of detection for p,p'-DDE was 0.020 microg/g using 0.5 g rat whole blood and liver samples. Coefficients of variation ranged from 7.0 to 7.9%. This method was used to analyze a rat whole blood sample after administration of p,p'-DDE.

摘要

采用顶空固相微萃取(SPME)技术,开发了一种简单快速的从大鼠全血和组织中分析p,p'-滴滴涕(p,p'-DDE)的提取方法。将含有p,p'-DDE样品、氢氧化钠和作为内标的二苯甲酮的小瓶在120℃下加热。将涂有聚二甲基硅氧烷的SPME纤维在小瓶顶空中暴露15分钟。然后将纤维针注入毛细管气相色谱-质谱系统的进样口中,通过将纤维暴露在进样口中进行解吸。校准曲线在大鼠全血和肝脏样品0.02至50微克/克的整个浓度范围内显示出良好的线性。使用0.5克大鼠全血和肝脏样品时,p,p'-DDE的检测限为0.020微克/克。变异系数范围为7.0%至7.9%。该方法用于分析给予p,p'-DDE后的大鼠全血样品。

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