大体积进样技术在气相色谱-质谱法测定二噁英类化合物中的应用  

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

作　　者：王亚韡[1] 张庆华[1] 江桂斌[1] 贺卿[2] 

机构地区：[1]中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室,北京100085 [2]Focus科技有限公司ATAS中国技术服务中心,北京100012

出　　处：《色谱》2007年第1期21-24,共4页Chinese Journal of Chromatography

基　　金：国家科学技术部"973"基金资助项目(2003CB415001)

摘　　要：利用大体积进样技术(large vo lum e in jec tion,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100μL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。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 100μL. 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 1 - 2 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.

关 键 词：气相色谱-质谱法 大体积进样 二噁英 环境样品 

分 类 号：O658[理学—分析化学]