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| Determination of Pyraflufen-ethyl and Its Metabolite in Cotton Field by QuEChERS/High Performance Liquid Chromatography |
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| DOI：10.3969/j.issn.1004-4957.年份.月份 |
| KeyWord:QuEChERS high performance liquid chromatography（HPLC） cotton pyraflufen-ethyl and its metabolite residue |
| Author | Institution |
| QIN Xu,XU Ying-ming*,SUN Yang,ZHAO Li-jie,WANG Lin,SUN Yue-bing,LIANG Xue-feng |
农业部环境保护科研监测所农业部产地环境质量重点实验室/天津市农业环境与农产品安全重点实验室 |
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| Abstract: |
| A method was developed for the determination of pyraflufen-ethyl and its metabolite E-1 residues in cotton plant,cotton seeds and soil by using QuEChERS/high performance liquid chromatography coupled with variable wavelength detector（HPLC/VWD）.The residues in the samples were extracted with acetonitrile-water,cleaned up by the developed QuEChERS method,and separated on a Welch Ultimate XB-C18 column（250 mm×4.6 mm,5 μm）,then analyzed by HPLC/VWD at a detection wavelength of 246 nm.The pyraflufen-ethyl and E-1 residues were quantified by the external standard method using the matched standard solution to compensate for matrix effect.Under the optimal conditions,the calibration curves showed good linearities in the range of 0.01-1.0 mg/L for pyraflufen-ethyl and E-1,with correlation coefficients（r2 ） more than 0.999.The average recoveries of pyraflufen ethyl and E-1 at three spiked levels were in the ranges of 83.5%-106.3% and 74.9%-102.3%,respectively,with relative standard deviations（RSDs,n=5） of 0.5%-5.2% and 1.6%-19.2%,respectively.The limits of detection（LOD,S/N>3） of two analytes were both 0.1 ng,the limits of quantitation（LOQ） were 0.04 mg/kg for cotton plant,0.04 mg/kg for cotton seeds and 0.02 mg/kg for soil.The method is rapid,simple,inexpensive,and could be applicable to confirm the residues of pyraflufen-ethyl and its metabolite E-1 in cotton plant,cotton seeds and soil in routine laboratories. |
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