固相萃取-气质联用法测定苹果中甲胺磷、地虫磷、甲基对硫磷和对硫磷的残留量

Determination of methamidophos, fonofos, parathion methyl and parathion in apple by solid-phase extraction and gas chromatography-mass spectrometry

中文关键词:  气相色谱-质谱法  固相萃取  有机磷农药  苹果

英文关键词:gas chromatography-mass spectrometry  solid-phase extraction  organophosphorus pesticides  apple

中文摘要:

      目的 建立一种经固相萃取, 以气相色谱-质谱法(gas chromatography-mass spectrometer, GC-MS)测定苹果中甲胺磷、地虫磷、甲基对硫磷和对硫磷残留量的方法。方法 采用乙腈提取, 石墨化碳/氨基复合固相萃取柱对苹果中的甲胺磷、地虫磷、甲基对硫磷和对硫磷进行净化, 氮吹浓缩后利用气质联用仪测定其农药残留量。结果 4种有机磷农残在20~200 μg/L线性范围内关系良好, 相关系数(r2)均大于0.995, 检出限和定量限分别为1.4~3.5 μg/kg和5.1~9.8 μg/kg, 当添加浓度为10~50 μg/kg, 回收率为81.2%~112.5%, 测量结果RSD(n=5)在5.3%~13.7%之间。结论 本法干扰低、快速高效, 适合苹果中的甲胺磷、地虫磷、甲基对硫磷和对硫磷的残留量的测定。

英文摘要:

      Objective To establish a method for determination of methamidophos, fonofos, parathion methyl and parathion in apple by solid-phase extraction and gas chromatography-mass spectrometry (GC-MS). Methods Methamidophos, fonofos, parathion methyl and parathion were extracted with acetonitrile, purified by solid-phase extraction with Carb/NH2 and determined by GC-MS. Results The results showed that the 4 organophosphorus pesticides had good linearity in the range of 20~200 μg/L, with the correlation coefficients higher than 0.995. The limits of detection (LODs) and limits of quantitation (LOQs) were 1.4~3.5 μg/kg and 5.1~9.8 μg/kg, respectively. For the samples, the spiked recoveries were 81.2%~112.5%, with RSDs of 5.3%~13.7%. Conclusion The proposed method is rapid and accurate with less interference, which is suitable for determination of methamidophos, fonofos, parathion methyl and parathion in apple.