吡蚜酮与噻虫胺在柑橘和土壤中的残留分析

Residue Analysis of Pymetrozine and Clothianidin in Citrus and Soil

[目的]建立了柑橘和土壤中吡蚜酮、噻虫胺的高效液相色谱-串联质谱(HPLC-MS/MS)同时检测分析方法。[方法]采用外标法进行定量,柑橘和土壤中的吡蚜酮和噻虫胺先经0.1%氨水乙腈溶液振荡提取,然后采用中性氧化铝、无水硫酸钠净化,最后经HPLC-MS/MS检测。[结果]在0.01、0.05、0.1、0.5、1.0 mg/kg标准工作溶液浓度下,吡蚜酮相关系数0.999,噻虫胺相关系数0.9999;在0.05、0.5、1 mg/kg添加水平下,吡蚜酮在土壤、果肉以及全果中的平均回收率为89%~108%,其相对标准偏差(RSD)在5%~20%范围内;噻虫胺的平均回收率达到92%~109%,其相对标准偏差为3%~16%。吡蚜酮与噻虫胺在试验中的检出限(LOD)均为0.01 mg/kg,其定量限(LOQ)均为0.05 mg/kg。[结论]该方法精准快捷,重复性、灵敏度均符合农药残留分析要求,可以用于实际生产中同时检测柑橘、土壤基质上吡蚜酮和噻虫胺的残留量。

[Aims]A practical and effective method was established and verified for determination of pymetrozine and clothianidin in citrus and soil through high performance liquid chromatography equipped mass spectrometry(HPLC-MS/MS).[Methods]The external standard method was used for quantification.Pymetrozine and clothianidin in citrus and soil were extracted with 0.1%ammonia acetonitrile solution,then purified by neutral alumina and anhydrous sodium sulfate,and finally detected by HPLC-MS/MS.[Results]At 0.01-1.00 mg/L,the correlation coefficient of pymetrozine was R^2=0.999,the correlation coefficient of clothianidin was R^2=0.9999.At 0.05-1 mg/L,the average recoveries of pymetrozine and clothianidin in citrus and soil range from 89 to 108%with relative standard deviation(RSD)of 5-20%,and 92 to 109%with relative standard deviation(RSD)of 3-16%,respectively.The LOD of pymetrozine and clothianidin was 0.1 mg/kg,and the LOQ in citrus and soil was both 0.05 mg/kg.[Conclusions]The method is accurate and reliable,and the repeatability and sensitivity meet the requirements of pesticide residue analysis.It can be used for the simultaneous determination of pymetrozine and clothianidin in citrus and soil.