气相色谱-质谱法同时测定土壤中的4种丙烯酸酯类农药

建立快速溶剂萃取-气相色谱质谱联用法同时测定土壤中的4种丙烯酸酯类(嘧菌酯,嘧菌胺,苯氧菌胺,醚菌酯)残留量的分析方法。将随机采集到的土壤样品自然风干,粉碎过筛。称取过筛后的样品5 g,置于萃取池中,以丙酮-乙酸乙酯(体积比为1∶1)作为萃取溶剂,于加速溶剂萃取仪中进行提取,收集提取液,氮吹至近干,用丙酮定容至1 mL,以0.45μm滤膜过滤后,上GC-MS/MS仪分析,色谱峰面积外标法定量检测。4种丙烯酸酯类的质量浓度在0.05~5.0μg/mL范围内与其色谱峰面积呈良好的线性关系,检出限为0.006~0.010 mg/kg,加标回收率为91.4%~94.6%,测定结果的相对标准偏差为2.48%~4.29%(n=6)。该方法前处理简单,定性及定量结果准确,适用于土壤中丙烯酸酯类残留的监测。

Simultaneous determination of four acrylate pesticides in soil by GC-MS

A rapid solvent extraction–gas chromatography–mass spectrometry method was established for the simultaneous determination of 4 acrylate residues in soil. The randomly collected soil samples were dried naturally,crushed and sifted. 5 g sifted samle was transferred to extract pond and extracted on Accelerate solvent extractor. Acetone–ethyl acetate(volume ratio was 1∶1) was selected as the extraction solvent. The extracted solution was collected and flowed to near dry by nitrogen,and volumned to 1 mL by acetone. After filtration with 0.45 μm filter membrane,samples were analyzed by GC–MS/MS,the external standard was selected for quantitative analysis. There was a good linear relationship between the concentration of 4 kinds of acrylates in the range of 0.05–5.0 μg/mL,the detection limits were 0.006–0.010 mg/kg,the recovery of standard addition was 91.4%–94.6%,and the relative standard deviation of determination results was 2.48%–4.29%(n=6). The method is simple in pretreatment with accurate qualitative and quantitative results,which is suitable for the monitoring of acrylate residues in soil.