固相微萃取-气相色谱/三重四级质谱法 测定土壤中氯代苯胺类残留  

Determination of Chlorinated Anilines Residues in Soil by Gas Chromatography-Triple Quadrupole Mass Spectrometry Coupled with Solid Phase Microextraction

作　　者：陈烨[1] 许秀艳[1] 王超[1] 吕怡兵[1] 

机构地区：[1]中国环境监测总站,北京100012

出　　处：《分析化学》2015年第7期1009-1015,共7页Chinese Journal of Analytical Chemistry

基　　金：国家高技术研究发展计划基金资助项目(No.2013AA06A308)~~

摘　　要：建立了固相微萃取-气相色谱/三重四级质谱法（ SPME-GC/QQQ）同时测定土壤中多种氯代苯胺的方法。优化了多反应监测（ MRM）的仪器条件,研究了土壤取样量、加水量、萃取温度、萃取时间对SPME富集效果的影响,确定最佳实验条件为：取8 g土壤样品加入4 mL纯净水中,80℃下萃取40 min。方法的检出限为1-10 pg/g,线性范围为5-1000 pg/g。200 pg/g加标土壤的回收率在96.8%-144.2%,相对标准偏差在13.4%-27.8%（n=5）。方法综合了SPME简便快捷和MRM高选择性的优点,尤其适合于土壤中痕量氯代苯胺类污染物的大量快速筛查分析。A gas chromatography-triple quadrupole mass spectrometry coupled with solid phase microextraction method （ SPME-GC/QQQ） was developed for the determination of chlorinated anilines （ CAs） residues in soil. The multi-reaction monitoring （ MRM ） parameters were optimized. The SPME conditions such as amount of soil sample, volume of added water, extraction temperature and absorption time were investigated. Optimum SPME conditions including 8 g of soil sample, 4 mL of water, 80℃ of extraction temperature and 40 min of absorption time were employed in the experiment. Method detection limits were within the range of 1-10 pg/g, while linearities were within the range of 5-1000 pg/g. Under the optimized conditions, the soil samples spiked with 200 pg/g targets were determined with recoveries of 96. 8%-144. 2%and relative standard deviations of 13 . 4%-27 . 8% （ n=5 ） . The proposed method combines simplicity and rapidity of SPME and high selectivity of MRM. It is especially suitable for the quick screening and determination of trace amounts of chlorinated anilines residues in soil.

关 键 词：固相微萃取 气相色谱/三重四级质谱联用 土壤 氯代苯胺类 

分 类 号：O657.63[理学—分析化学] X833[理学—化学]