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[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。
[Objective] The aim of the study was to establish a tandem rapid liquid chromatography method for the determination of spinosad residues in cauliflower, and to evaluate the digestion tendency and residual level of spinosad on cauliflower. [Method] After the acetonitrile was homogenized, the pH value was adjusted to 10 with sodium carbonate and extracted with ultrasonic. The mixture was suction filtered, concentrated with saturated sodium chloride and extracted with dichloromethane. The organic phase was concentrated to near dryness, 0.22μm membrane, using liquid chromatography - mass spectrometry for detection. [Result] The recoveries of spinosad in Cauliflower were 85.6% ~ 90.3% and the relative standard deviations were 2.2% ~ 4.1%. The recoveries of spinosad in cauliflower were 85.1% ~ 101.7% The relative standard deviations were 2.5% -4.3%, the lowest detected mass fraction was 0.02 mg / kg. [Conclusion] The method is simple, rapid, accurate and precise.