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《化学分析计量》 2020年第03期
DOI:10.3969/j.issn.1008-6145.2020.03.010
气相色谱-质谱法同时测定土壤中的4种丙烯酸酯类农药
章彦琳,沈荷美
浙江杭康检测技术有限公司,杭州 310011 
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. 
关键词:加速溶剂萃取;气相色谱串联质谱;土壤;嘧菌酯;嘧菌胺;苯氧菌胺;醚菌酯 
Keywords:rapid solvent extraction; GC-MS; soil; azoxystrobin; mepanipyrim; metominostrobin; ethofenprox 
本文引用格式:
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. 

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