色谱

色谱

• 研究论文 • 上一篇    下一篇

大体积进样技术在气相色谱-质谱法测定
二英类化合物中的应用

王亚韡1,张庆华1,江桂斌1，贺卿2

  

  1. 1.State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-
    Environmental Sciences, the Chinese Academy of Sciences, Beijing 100085, China;
    2.Service Center of ATAS in China, Focus Technology Co., Ltd, Beijing 100012, China
  • 收稿日期:2006-05-11 修回日期:2006-07-19 出版日期:2007-01-30 发布日期:1986-03-25
  • 通讯作者: 江桂斌

Determination of Dioxins by Gas Chromatography-Mass
Spectrometry Coupled with Large Volume Injection

WANG Yawei1, ZHANG Qinghua1, JIANG Guibin1, HE Qing2   

  1. 1.State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-
    Environmental Sciences, the Chinese Academy of Sciences, Beijing 100085, China;
    2.Service Center of ATAS in China, Focus Technology Co., Ltd, Beijing 100012, China
  • Received:2006-05-11 Revised:2006-07-19 Online:2007-01-30 Published:1986-03-25

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摘要：

利用大体积进样技术(large volume injection,LVI),结合气相色谱-质谱方法对二英的测定效果进行了研究。同时与传统分流/不分流进样技术进行了对比。对进样体积为1,5,10,25,50和100 μL的色谱图进行了分析。研究表明使用大体积进样方式,在不影响色谱分离度的同时,大幅度提高了分析灵敏度。通过对土壤样品的检测,证明该方法可以用于环境样品的实际测定。

关键词: 大体积进样, 二英, 环境样品 , 气相色谱-质谱法

Abstract:

The common analytical instrument for dioxin analysis/determination is gas chromatograph (GC) coupled with an electron capture detector (ECD), a flame ionization detector (FID), and a mass spectrometer (MS), etc. Generally, since the concentration levels in environmental samples are pg/g or pg/L, it requires a very high resolution and sensitivity for the analytical system. To solve the problem one way is to increase the amount of a sample, however, which can significantly increase the pretreatment work load. The other way is to increase the injection volume. In this paper, a method for dioxin determination was developed using GC-MS coupled with the large volume injection （LVI）. Under the condition of maintaining the same amount of solute, the comparison was studied for the changes of peak areas and peak widths by the injection of different volumes from 1 to 100 μL. The results showed that the peak area and peak width did not have obvious changes, and the separation performance was not affected compared with the traditional split/splitless injection. The detection limits obtained are improved by 12 orders of magnitude over those using split/splitless injections. Once the operation conditions are optimized, LVI is more flexible in handling samples of wide concentration ranges than the traditional split/splitless inlet approach.

Key words: dioxins, environmental sample , large volume injection, gas chromatography-mass spectrometry (GC-MS)