吸附脱水浸提-气相色谱法同时测定植物性食品中甲胺磷和乙酰甲胺磷的残留量
目的 建立吸附脱水浸提-气相色谱法同时测定植物性食品中甲胺磷和乙酰甲胺磷残留量。方法 样品使用组合无机盐(无水硫酸钠和无水硫酸镁)吸附脱水后, 经由乙腈溶液超声提取, 在浓缩、定容后采用火焰光度检测器(flame photometric detector, FPD+)进行气相色谱分析测定, 采用基质标准系列结合循环校正曲线-外标法定量。 结果 甲胺磷和乙酰甲胺磷在20~1000 μg /L范围内线性关系良好, 相关系数(r)均大于0.999。甲胺磷和乙酰甲胺磷的方法检出限分别为5.8 μg/kg和2.9 μg /kg, 定量限分别为20 μg/kg和10 μg/kg。在50、100和500 μg/kg 3个空白加标水平下, 甲胺磷和乙酰甲胺磷回收率分别为81.0%~105.4%和83.5%~101.2%, 相对标准偏差均小于5.0%(n=6)。结论 本方法快速简便且准确稳定, 适用于批量测定植物性食品中甲胺磷和乙酰甲胺磷农药的残留量。
Objective To establish a method for the simultaneous determination of methamidophos and acephate in plant food by adsorption dehydration digestion-gas chromatography. Methods The samples were dehydrated by mixed inorganic salts (anhydrous sodium sulfate and anhydrous magnesium sulfate), and extracted with acetonitrile by ultrasonic extraction. Then the extract was concentrated and redissolved, determined by flame photometric detector (FPD), and quantitative determined by the combined cycle matrix standard series-external standard calibration curve method. Results Methamidophos and acephate had good linearities in the range of 20~1000 μg/L and the relative coefficients were larger than 0.999. The limits of detection (LODs) of methamidophos and acephate were 5.8 μg/kg and 2.9 μg/kg, and the limits of quantification (LOQs) were 20 μg/kg and 10 μg/kg respectively. The average recoveries of methamidophos and acephate spiked at 3 levels of 50, 100 and 500 μg/kg were in range of 81.0%~105.4% and 83.5%~101.2%, and the relative standard deviations (RSDs) were less than 5.0% (n=6). Conclusion This proposed method is quick, convenient, accurate and stable, which is suitable for the batch determination of methamidophos and acephate residues in plant food.
标题：吸附脱水浸提-气相色谱法同时测定植物性食品中甲胺磷和乙酰甲胺磷的残留量
英文标题：Simultaneous determination of methamidophos and acephate pesticide residues in plant food by adsorption dehydration digestion-gas chromatography
作者：
陈惠琴 广州市食品检验所
刘佳 广州市食品检验所
黄松 广州市食品检验所
戚平 广州市食品检验所
中文关键词:甲胺磷,乙酰甲胺磷,无机盐,吸附脱水,气相色谱法,植物性食品,
英文关键词:methamidophos,acephate,inorganic salt,adsorption dehydration,gas chromatography,plant food,
发表日期：2016-12-20
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