气相色谱质谱法同时测定土壤中4种常见除螨剂残留

Simultaneous determination of four common acaricide residues in soil by GC-MS

本文建立了一种以体积比为1∶1的正已烷/丙酮混合试剂提取土壤样品,以石墨化碳黑柱进行富集净化土壤提取液,气相色谱质谱法测定土壤中三氯杀螨醇、噻螨酮、噻嗪酮、哒螨灵残留量的方法。4种除螨剂农药在10.0~200μg·L^(-1)范围内线性相关系数均大于0.995,方法检出限为0.005~0.009mg·kg^(-1),3种浓度的加标回收率为87.3%~104.2%,方法标准偏差小于5%。本方法操作快速、简便,净化富集效果好,定性定量结果准确,检出限低,精密度和加标回收率良好,适用于土壤中三氯杀螨醇、噻螨酮、噻嗪酮、哒螨灵等除螨类农药残留的分析。

In this paper,a method was established to extract soil samples with a volume ratio of 1∶1 n-hexane/acetone mixed reagent,enrich and purify the soil extract with a graphitized carbon black column,and determine the residues of dicofol,thiothiazone,thiazidone and pyridaben in soil by gas chromatography-mass spectrometry.The linear correlation coefficients of the four acaricide pesticides were greater than 0.995 in the range of 10.0~200μg·L^(-1),the detection limit of the method was 0.005~0.009mg·kg^(-1),the add standard recoveries of the three concentrations were 87.3%~104.2%,and the standard deviation of the method was less than 5%.The method has the advantages of fast and simple operation,good purification and enrichment effect,accurate qualitative and quantitative results,low detection limit,good precision and add standard recovery.It is suitable for the analysis of acaricide residues in soil,such as dicofol,thiothiazone,thiazidone,pyridaben and so on.