液相色谱串联质谱法测定油料作物中3种双酰胺类杀虫剂残留量

Determination of 3 kinds of diamide insecticides in oil crops by liquid chromatography-tandem mass spectrometry

中文关键词:  液相色谱-串联质谱法  氯虫苯甲酰胺  氟苯虫酰胺  溴氰虫酰胺  油料作物

英文关键词:liquid chromatography-tandem mass spectrometry  chlorantraniliprole  flubendiamide  cyantraniliprole  oil crops

中文摘要:

      目的 建立液相色谱-串联质谱法测定油料作物中3种双酰胺类药物残留量的分析方法。方法 油料作物样品经乙腈振荡超声提取, Oasis PRiMEHLB固相萃取柱净化, 液相色谱串联质谱测定, 外标法定量。 结果 氯虫苯甲酰胺、氟苯虫酰胺、溴氰虫酰胺检出限分别为: 0.050、0.010、0.010 μg/kg, 定量限分别为0.20、0.030、0.030 μg/kg。在不同基质中, 氯虫苯甲酰胺在0.20、0.40、2.0 μg/kg添加水平下的平均回收率为78.4%~88.5%, 相对标准偏差在1.7%~5.7%之间; 氟苯虫酰胺、溴氰虫酰胺在0.030、0.060、0.30 μg/kg添加水平下的平均回收率为79.9%~100.5%, 相对标准偏差为1.1%~5.6%。结论 该方法快速简便、灵敏度高、准确性强等特点, 适用于油料作物中氯虫苯甲酰胺、氟苯虫酰胺、溴氰虫酰胺残留量的检测。

英文摘要:

      Objective To establish an analytical method for the determination of 3 bisamide residues in oil crops by liquid chromatography-tandem mass spectrometry. Methods Oil crop samples were extracted by acetonitrile oscillating ultrasonic, purified by Oasis Prim EHLB solid phase extraction column, determined by liquid chromatography-tandem mass spectrometry, and quantified by external standard method. Results The detection limits of chloranthionamide, fluorobenzamide and bromofenamide were 0.050, 0.010 and 0.010 μg/kg respectively, and the quantitative limits were 0.20, 0.030 and 0.030 μg/kg respectively. The average recoveries were 78.4%–88.5% and the relative standard deviations were 1.7%–5.7% at 0.20, 0.40 and 2.0 μg/kg in different substrates for chlorantraniliprole; The average recoveries were 79.9%–100.5% and the relative standard deviations were 1.1%–5.6% at 0.030, 0.060 and 0.30 μg/kg in different substrates for flubendiamide,cyantraniliprole. Conclusion This method is highly sensitive, simple, accurate and suitable for the confirmation and quantification of chlorantraniliprole, flubendiamide and cyantraniliprole in oil crops.