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建立了糙米和土壤中氟啶虫酰胺、氯虫苯甲酰胺、甲氧虫酰肼、氟虫双酰胺、虫螨腈和虱螨脲6种杀虫剂残留的高效液相色谱检测方法。样品用乙腈浸泡过夜后振荡提取,其中糙米过氨基小柱净化,土壤无需净化;采用高效液相色谱仪,以甲醇-乙腈-水为流动相,利用C18柱和二极管阵列检测器(检测波长:265、254、230 nm)对待测组分进行分离和测定。结果表明,在0.05~5 mg/L范围内,标准品质量浓度与峰面积之间呈良好的线性关系(R2=0.999 4~1)。在0.1、0.5和1 mg/kg 3个添加水平下,糙米和土壤中氟啶虫酰胺、氯虫苯甲酰胺、甲氧虫酰肼、氟虫双酰胺、虫螨腈和虱螨脲的平均回收率在84.5%~113.2%之间,相对标准偏差(RSD)≤9.3%;供试6种农药在样品中的检出限(LOD)为0.010~0.016 mg/kg,定量限(LOQ)为0.03~0.05 mg/kg。所建立的方法具有准确、快速、简便、重复性好等特点,其准确度和精密度均能满足农药残留分析的要求。
A high performance liquid chromatography (HPLC) method was established for the determination of six insecticides in brown rice and soil, including flonicamid, chlorantraniliprole, methoxyfenozide, flubendiamide, chlorfenapyr and lufenuron. The sample was soaked in acetonitrile overnight and then extracted by shaking. The brown rice was purified with a small column of amino and the soil did not need to be purified. The mobile phase consisted of C18 column and diode array detector with high performance liquid chromatography (HPLC) 265, 254, 230 nm) The components to be tested were separated and assayed. The results showed that there was a good linear relationship between standard concentration and peak area in the range of 0.05-5 mg / L (R2 = 0.999 4-1). Mean values of flonicamid, chlorantran, methoxyfenozide, flubendiamide, chlorfenapyr and lufenuron in brown rice and soil at the three addition levels of 0.1, 0.5 and 1 mg / kg The recoveries ranged from 84.5% to 113.2% with relative standard deviations (RSDs) ≤9.3%. The detection limits (LODs) of the six pesticides in the samples ranged from 0.010 to 0.016 mg / kg and the limits of quantitation (LOQ) 0.03 ~ 0.05 mg / kg. The established method is accurate, rapid, simple and reproducible, and its accuracy and precision can meet the requirements of pesticide residue analysis.