高效液相色谱法测定糙米和土壤中6种杀虫剂的残留
Residues of six novel insecticides in unpolished rice and soil by high-performance liquid chromatography method
-
摘要: 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。Abstract: A high-performance liquid chromatography(HPLC) method was developed for the determination of flonicamid,chlorantraniliprole,methoxyfenozide,flubendiamide,chlorfenapyr and lufenuron in unpolished rice and soil.The residues were extracted with acetonitrile,and cleaned up with NH2 solid-phase extraction for unpolished rice samples (no cleanup for soil).Determination of analytes was completed using HPLC with DAD detection at 265,254 and 230 nm.The results showed that the coefficient of determination (R2) of this method was above 0.999 4 and the calibration curve was linear in the range of 0.05-5 mg/L.The fortified recoveries of these six pesticides in rice and soil samples at three levels(0.1,0.5,1 mg/kg) were in range of 84.5%-113.2%,with relative standard deviations(RSDs) less than 9.3%.The limit of detection(LOD) of the method was estimated to be 0.010-0.016 mg/kg,and the limit of quantification was 0.03-0.05 mg/kg in these samples.
下载: