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
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2~100 μg/L范围内呈良好的线性关系(r2>0.99), 定量限为5 μg/kg。在5.0、10.0、20.0 μg/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 2~100 μg/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 residues in honey.
标题：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
英文标题：Simultaneous determination of 3 kinds of pesticide residues in honey by automatic solid extraction-high performance liquid chromatography-tandem mass spectrometry
作者：
柳菡 江苏出入境检验检疫局
张晓燕 江苏出入境检验检疫局
吕辰 赛默飞世尔科技色谱质谱部
丁涛 江苏出入境检验检疫局
余可垚 江苏出入境检验检疫局
沈伟健 江苏出入境检验检疫局
赵增运 江苏出入境检验检疫局
吴斌 江苏出入境检验检疫局
张睿 江苏出入境检验检疫局
沈崇钰 江苏出入境检验检疫局
邓晓军 上海出入境检验检疫局
伊雄海 上海出入境检验检疫局
郭德华 上海出入境检验检疫局
中文关键词:全自动固相萃取,高效液相色谱-串联质谱法,蜂蜜,农药残留,
英文关键词:automatic solid extraction,high performance liquid chromatography-tandem mass spectrometry,honey,pesticide residues,
发表日期：2016-08-29
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