Simultaneous determination of four acrylate pesticides in soil by GC-MS
ZHANG Yanlin, SHEN Hemei
Zhejiang Hangkang Testing Technology Co., Ltd., Hanzhou 310011, China
摘要：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0.45 μm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0.05～5.0 μg/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。
Abstract：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.
Keywords：rapid solvent extraction; GC-MS; soil; azoxystrobin; mepanipyrim; metominostrobin; ethofenprox
章彦琳，沈荷美.气相色谱-质谱法同时测定土壤中的4种丙烯酸酯类农药[J].化学分析计量，2020，29(3)：43-46. ZHANG Y L，SHEN H M. Simultaneous determination of four acrylate pesticides in soil by GC-MS[J]. Chemical analysis and meterage，2020，29(3)：43-46.