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出 处:《农药》2016年第5期374-376,共3页Agrochemicals
摘 要:[目的]建立花椰菜中多杀霉素残留的液质串联快速分析检测方法,评价多杀霉素在花椰菜上的消解趋势、残留水平。[方法]采用乙腈匀浆后,用碳酸钠调pH值为10,再超声提取,抽滤浓缩后用饱和氯化钠盐析,二氯甲烷萃取、有机相浓缩至近干,甲醇定容后过0.22μm滤膜,采用液相色谱-质谱法进行检测。[结果]该分析方法的多杀霉素在花椰菜植株中的添加回收率为85.6%~90.3%,相对标准偏差为2.2%~4.1%;在花椰菜中的添加回收率为85.1%~101.7%,相对标准偏差为2.5%~4.3%,最低检出质量分数为0.02 mg/kg。[结论]方法简便、快速、准确度高、精密度好。[Aims] The aims were to establish a method for rapid analysis of spinosad by LC-MS/MS, and evaluate the degradation trend and residues of spinosad in cauliflower. [Methods] The samples were extracted with acetonitrile, and the pH value ofhomogenate was adjusted to 10 with sodium carbonate solution, then the homogenate was suction filtration concentrated, salted out with saturated sodium chloride solution extracted by dichloromethane, finally, organic phase was evaporated to near dryness, filtered after constant volume with methanol, detected by LC-MS/MS. [Results] The recovery rate of spinosad in cauliflower plant was 85.6-90.3%, the relative standard deviation was 2.2-4.1%. The recovery rate of spinosad in cauliflower was 85.1-101.7%, the relative standard deviation was 2.5-4.3%, and the limit of detection was 0.02 mg/kg. [Conclusions] The method has the advantage of fast, simple, accurate and good repeatability.
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