全自动固相萃取-高效液相色谱-串联质谱法测定蜂蜜中3种农药残留

Simultaneous determination of 3 kinds of pesticide residues in honey by automatic solid extraction-high performance liquid chromatography-tandem mass spectrometry

目的建立蜂蜜中多菌灵、甲基托布津和乙基托布津3种农药的全自动固相萃取-高效液相色谱-串联质谱检测方法。方法蜂蜜样品经磷酸盐缓冲液(pH=7.8)溶解,稀释,全自动固相萃取净化后,采用高效液相色谱-串联质谱测定,内标法定量。结果 3种农药在2~100μg/L范围内呈良好的线性关系(r^2>0.99),定量限为5μg/kg。在5.0、10.0、20.0μg/kg 3个加标水平下,3种农药的回收率为75.6%~97.1%,相对标准偏差小于13.2%。结论该方法简单、快速,准确度和精密度良好,可用于蜂蜜中多菌灵、甲基托布津和乙基托布津的同时测定。

Objective To establish a method for the determination of carbendazim, thiophanate-methyl and thiophanate-ethyl in honey by automatic solid extraction-high performance liquid chromatography-tandem mass spectrometric （LC-MS/MS）. Methods The samples were dissolved and diluted by phosphate buffer （pH=7.8）, then cleaned up by automatic solid phase extraction. The extract was analyzed by LC-MS/MS and quantified by internal standard method. Results The carbendazim, thiophanate-methyl and thiophanate-ethyl had good linearity in the range of 2~100μg/L with r2 higher than 0.99. The limit of quantification was 5 μg/kg. The recoveries of carbendazim, thiophanate-methyl, and thiophanate-ethyl were from 75.6% to 97.1% at 3 spiked levels （5.0, 10.0 and 20.0 μg/kg） with relative standard deviations （RSDs） less than 13.2%. Conclusion This method is simple, quick, accurate, and precise and suitable for the simultaneous determination of carbendazim, thiophanate-methyl, and thiophanate-ethyl＆nbsp;residues in honey.