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吡草醚在棉花及土壤中的残留分析方法研究
朱玉杰,施艳红,操海群,花日茂,李学德,吴祥为,唐俊
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(安徽农业大学植物保护学院,安徽省农产品安全重点实验室,合肥 230036;安徽农业大学资源与环境学院,安徽省农产品安全重点实验室,合肥 230036)
摘要:
研究建立了吡草醚在棉花及土壤中的残留分析方法。棉叶和棉籽样品以乙腈提取,GCB/PSA固相萃取小柱净化,高效液相色谱测定。土壤样品以丙酮提取,C18小柱净化。吡草醚在棉叶、棉籽和土壤中的最低检测浓度均为0.02 mg·kg-1。吡草醚在棉叶、棉籽和土壤中的平均添加回收率(添加浓度为0.02~1 mg·kg-1)分别为93.94%~101.65%、84.88%~98.62% 和85.49%~90.71%,变异系数分别为3.96%~8.06%、7.59%~10.37% 和5.59%~ 8.69%。方法的准确性、精确性和灵敏度均达到农药残留分析的要求。
关键词:  吡草醚  棉花  土壤  残留分析  高效液相色谱
DOI:10.13610/j.cnki.1672-352x.20141029.026
基金项目:农业部农药残留田间试验项目资助。
An analytical method for determination of pyraflufen-ethyl residues in the cotton plant and soil
ZHU Yujie,SHI Yanhong,CAO Haiqun,HUA Rimao,LI Xuede,WU Xiangwei,TANG Jun
(Key Laboratory of Agri-Food Safety of Anhui Province, School of Plant Protection , Anhui Agricultural University, Hefei, 230036;Key Laboratory of Agri-Food Safety of Anhui Province, School of Resources and Environment, Anhui Agricultural University, Hefei, 230036)
Abstract:
High performance liquid chromatography (HPLC) was used to analyze pyraflufen-ethyl residues in the cotton plant and soil. Pyraflufen-ethyl residues were extracted from leaves and cottonseeds with acetonitrile and purified using GCB/PSA SPE microcolumn. The residues were determined using HPLC equipped by PDA. Pyraflufen-ethyl residues in the soil were extracted with acetone and purified using C18 SPE microcolumn. The minimum detectable concentration of pyraflufen-ethyl in the cotton leaf, cottonseed, and the soil was 0.02 mg·kg-1. The average recoveries of pyraflufen-ethyl in the cotton leaf, cottonseed, and the soil were 93.94%-101.65%, 84.88%-98.62%, and 85.49%-90.71%, respectively, and their variation coefficients were 3.96%-8.06%, 7.59%-10.37% and 5.59%-8.69%, respectively. The results showed that this method met all criteria for the pesticide residue analysis.
Key words:  pyraflufen-ethyl  cotton  soil  residue analysis  HPLC

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