QuECHERS结合GC-MS/MS测定水果中12种有机磷农药残留

Determination of 12 Organophosphorus Pesticide Residues in Fruits by Using QuEChERS Combined with GC-MS/MS

该试验旨在建立水果中12种有机磷农药残留的QuEChERS结合GC-MS/MS检测方法,分析12种有机磷农药在不同水果中的基质效应。结果表明,12种有机磷农药在10~500 ng/mL质量浓度范围内相关系数r^(2)>0.99,方法检出限(S_(LOD))和定量限(S_(LOQ))分别为0.001 7~0.003 7 mg/kg和0.005 9~0.012 0 mg/kg,在0.03,0.08和0.15 mg/kg这3个添加水平下,加标回收率为80.9%~119.8%,精密度为0.76%~5.00%(n=6)。该方法下有机磷农药浓度与不同水果基质效应没有明显相关性,在相同浓度不同农药条件下,氧乐果、杀扑磷、丙溴磷在5种水果基质中均呈基质增强效应,而甲胺磷、敌敌畏、速灭磷在除橙子以外的4种水果基质中均呈基质减弱效应,说明不同水果基质对农药残留的准确定量影响较大,在检测水果中农药残留时应采用基质标液校准。

The QuEChERS combined with GC-MS/MS detection method for 12 organophosphorus pesticide residues in fruits was established,and the matrix effect of 12 organophosphorus pesticides in different fruits was analyzed.The results showed that the correlation coefficient r^(2) was more than 0.99 for 12 organophosphorus pesticides in the mass concentration range of10-500 ng/mL,and the detection limit (S_(LOD)) and limit of quantification (S_(LOQ)) of the method were 0.001 7-0.003 7 mg/kg and 0.005 9-0.012 0 mg/kg,respectively.At the three addition levels of 0.03,0.08,and 0.15 mg/kg,the recovery of standard addition was 80.9%-119.8%,and the precision was 0.76%-5.00%(n=6).By this method,there was no obvious correlation between the concentration of organophosphorus pesticides and the effects of different fruit substrates.Under the condition of the same concentration of different pesticides,omethoate,fenfos and profenofos all exhibited a matrix enhancement effect in the five fruit substrates,and methamidophos,dichlorvos and sulfaphos showed a matrix weakening effect in the four fruit matrices except oranges,indicated that different fruit matrices had a greater impact on the accurate quantification of pesticide residues.Matrix standard solution should be used for calibration when detecting pesticide residues in fruits.