[Objective] This study aimed to establish a determination method for iprobenfos residue in rice straw and husked rice. [Method] The rice straw and husked rice samples were extracted by acetone-ethyl acetate mixed solv...[Objective] This study aimed to establish a determination method for iprobenfos residue in rice straw and husked rice. [Method] The rice straw and husked rice samples were extracted by acetone-ethyl acetate mixed solvent. The extracts were purified using SPE C18 column and SPE NH2 column, and the iprobenfos residues were determined by GC-FTD. [Result] In the concentration range of 0.005-5.0 mg/kg, iprobenfos concentration showed a good linear relationship with peak area （r=0.999 8）. When the iprobenfos concentrations were 0.01, 0.1 and 1.0 mg/kg respectively, the recoveries of added iprobenfos from rice straw ranged from 72.6% to 99.7% with relative standard deviation ranging from 5.65% to 8.48%; the recoveries of added iprobenfos from husked rice ranged from 81.6% to 97.6% with relative standard deviation ranging from 3.74% to 7.63%. The minimum detectable quantity of iprobenfos was 5×10^-12 g, and the minimum detectable concentrations of iprobenfos in rice straw and husked rice samples were 2.0 and 0.5 μg/kg, respec- tively. [Conclusion] The established determination method is characterized by low de- termination limit, high sensitivity, good reproducibility and high operability, which all meet the requirements by Guideline on Pesticide Residue Trials of the Ministry of Agriculture.展开更多
基金Supported by Pesticide Registration Residual Test of Institute for the Control of Agrochemicals,Ministry of Agriculture(2013F216)~~
文摘[Objective] This study aimed to establish a determination method for iprobenfos residue in rice straw and husked rice. [Method] The rice straw and husked rice samples were extracted by acetone-ethyl acetate mixed solvent. The extracts were purified using SPE C18 column and SPE NH2 column, and the iprobenfos residues were determined by GC-FTD. [Result] In the concentration range of 0.005-5.0 mg/kg, iprobenfos concentration showed a good linear relationship with peak area （r=0.999 8）. When the iprobenfos concentrations were 0.01, 0.1 and 1.0 mg/kg respectively, the recoveries of added iprobenfos from rice straw ranged from 72.6% to 99.7% with relative standard deviation ranging from 5.65% to 8.48%; the recoveries of added iprobenfos from husked rice ranged from 81.6% to 97.6% with relative standard deviation ranging from 3.74% to 7.63%. The minimum detectable quantity of iprobenfos was 5×10^-12 g, and the minimum detectable concentrations of iprobenfos in rice straw and husked rice samples were 2.0 and 0.5 μg/kg, respec- tively. [Conclusion] The established determination method is characterized by low de- termination limit, high sensitivity, good reproducibility and high operability, which all meet the requirements by Guideline on Pesticide Residue Trials of the Ministry of Agriculture.
