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建立了微波辅助萃取-固相微萃取-气相色谱/三重四极质谱法(MAE-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,研究了微波萃取温度、保持时间、溶剂体积对萃取效果的影响,确定最佳实验条件为4 g土壤样品加入30 m L水,在100℃下微波萃取5 min.各目标物的线性范围为0.005—20μg·L-1,方法检出限为0.003—0.4 ng·g-1.测定0.5 ng·g-1和5 ng·g-1加标土壤样品,回收率为38.6%—116.4%和24.8%—82.0%,相对标准偏差为3.2%—27.7%和12.5%—22.7%(n=7).方法综合了MAE快速高效、SPME富集浓缩以及GC/QQQ抗干扰强的优势,适合于非高有机质含量土壤中氯代苯胺类残留的快速痕量分析.
A method for simultaneous determination of various chloroanilines in soil by microwave-assisted extraction-solid phase microextraction-gas chromatography / triple quadrupole mass spectrometry (MAE-SPME-GC / QQQ) Conditions, microwave extraction temperature, holding time, solvent volume on the extraction effect of the study to determine the best experimental conditions for the 4 g soil samples by adding 30 m L of water at 100 ℃ microwave extraction 5 min linear range of each target The detection limits were 0.003-0.4 ng · g-1. The soil samples were spiked at 0.5 ng · g-1 and 5 ng · g-1 with the recoveries of 38.6% -116.4% And 24.8% -82.0% with relative standard deviations of 3.2% -27.7% and 12.5% -22.7% (n = 7), respectively.The method combines the advantage of rapid and efficient MAE, enrichment and concentration of SPME and good GC / QQQ anti-interference Fast Trace Analysis of Chloroanilines Residues in Non - organic Matter Soils.