QuEChERS—高效液相色谱法检测柑桔中毒死蜱、吡虫啉和残杀威农残

Detected chlorpyrifos,imidacloprid,and propoxur residues in citrus by QuEChERS-high performance liquid chromatography method

将改进的QuEChERS方法与GB/T 24691—2009中农药提取方法进行比较,通过高效液相色谱法检测2种方法对柑桔农残的分离效果。结果显示:改进的QuEChERS方法检测毒死蜱、吡虫啉和残杀威时出峰时间分别约为5.1,3.8,11.5min;当空白加标水平分别为0.8~80.0,0.5~40.0,0.8~80.0μg/mL时,检出限分别为0.89,0.55,0.39μg/mL;当空白加标水平分别为1~20,1~20,5~30μg/mL时,回收率分别为68%~109%,94%~108%,109%~125%,相对标准偏差分别为2.48%~5.03%,7.79%~10.92%,2.32%~6.77%。采用GB/T 24691—2009提取毒死蜱、吡虫啉和残杀威时,出峰时间与改进的QuEChERS方法基本相同;当与改进的QuEChERS方法采用相同的空白加标水平,检出限分别为0.80,0.78,0.54μg/mL,回收率分别为107%~195%,25%~87%,53%~93%,相对标准偏差分别为5.61%~7.73%,6.89%~9.42%,5.44%~10.45%。因此,QuEChERS—高效液相色谱法检测毒死蜱、吡虫啉和残杀威农残时优于GB/T 24691—2009方法。

QuEChERS is a simple and efficient extraction method,widely used in the pesticide of residue detection.The purpose of this paper was to compare the extraction methods of pesticides between the improved QuEChERS method and the GB/T 24691—2009（fruit and vegetable detergent）.The extraction of pesticide residue from citrus samples were detected by HPLC.The results showed that when the chlorpyrifos,imidacloprid and propoxur were detected by the improved QuEChERS method,the peak time was about 5.1,3.8,11.5min,respectively.When the spiked blank levels were 0.8～80,0.5～40,0.8～80μg/mL,the detection limits were 0.89,0.55,and 0.39μg/mL.While the spiked blank levels respectively were in1～20,1～20,5～30μg/mL,the recovery rate was 68%～109%,94%～108%,109%～125% and the relative standard deviation was2.48%～5.03%,7.79% ～10.92%,2.32% ～6.77% respectively.When the fruit and vegetable detergent extracted from GB/T24691—2009,the peak time of chlorpyrifos,imidacloprid and propoxur was basically the same as the modified QuEChERS method.Moreover,when the same spiked blank level was applied to the improved QuEChERS method,the detection limits were 0.80,0.78,and 0.54μg/mL,respectively,The recoveries were 107%～195%,25% ～87% and 53% ～93%,and the relative standard deviations were 5.61%～7.73%,6.89%～9.42%and 5.44%～10.45%,respectively.Thus,it indicated that the improved QuEChERS-HPLC was better than GB/T 24691—2009（fruit and vegetable detergent）.