Determination of Iprobenfos Residue in Rice by GC-FTD using Two-dim Ensional Purification  

二维净化火焰热离子测定水稻样品中异稻瘟净残留（英文）

作　　者：万宇[1,2] 张晓波[2] 王军[1] 蒋闳[1] 

机构地区：[1]安徽省化工研究院,安徽合肥230041 [2]合肥工业大学,安徽合肥230009

出　　处：《Agricultural Science & Technology》2015年第7期1325-1328,1331,共5页农业科学与技术（英文版）

基　　金：Supported by Pesticide Registration Residual Test of Institute for the Control of Agrochemicals,Ministry of Agriculture(2013F216)~~

摘　　要：[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.[目的]建立水稻植株和糙米样品中异稻瘟净的残留分析方法。[方法]植株和糙米用丙酮和乙酸乙酯混合溶剂提取,采用SPE C18柱和SPE NH2柱二维净化,气相色谱火焰热离子检测器（FTD）测定。[结果]在0.005~5.0 mg/kg的浓度范围内,异稻瘟净的浓度与峰面积成良好线性关系（r=0.999 8）。在添加浓度分别为0.01、0.1、1.0 mg/kg时,水稻植株中的添加回收率为72.6%~99.7%,相对标准偏差为5.65%~8.48%;糙米中的添加回收率为81.6%~97.6%,相对标准偏差为3.74%~7.63%。异稻瘟净的最低检出量为5×10-12g;水稻植株和糙米最小检出浓度分别为2和0.5μg/kg。[结论]该方法检测限低,灵敏度高、重现性好、可操作性强,满足农业部农药残留试验准则要求（NY788-2004）。

关 键 词：Iprobenfos RICE Solid phase extraction Two-dimensional purification FTD 

分 类 号：S481.8[农业科学—农药学]