2D-HPLC柱切换法测定蔬菜中的阿维菌素

Determination of Avermectin in Vegetables by 2D-HPLC Column Switching Method

目的:建立2D-HPLC柱切换法检测蔬菜中阿维菌素的方法。方法:采用高效液相色谱法,参数如下:第一维色谱柱为ACQUITY UPLC BEH C_(18)(2.1 mm×100 mm,1.7μm),流动相为甲醇:水=90:10,流速0.2 mL/min;第二维色谱柱为ECOSILC_(18)-eco100A C_(18)(4.6 mm×250 mm,5μm),流动相为甲醇:水=90:10,流速1.0 mL/min,检测波长245 nm,进样体积20μL,柱温35℃。捕集柱为ZORBAX Eclipse Plus C_(18)(4.6 mm×100 mm,5μm);阀切换时间:0~2.8 min,位置1~2;2.81~3.9min,位置1~6;3.91~16 min,位置1~2。结果:阿维菌素在0.05~1.0 mg/L线性关系良好,相关系数R^(2)=0.99972,方法的定量限为0.012 mg/kg。三浓度加标水平的回收率为82.5%~105.3%,重复性好,相对标准偏差(RSD)为1.8%~2.7%。结论:该方法灵敏度高、重复性好、稳定性好、回收率满足复杂基质样品前处理的要求,适用于蔬菜中阿维菌素的快速检测。

Objective:To establish a 2D-HPLC column switching method for the determination of avermectin in vegetables.Methods:The first dimensional column was ACQUITY UPLC BEH C_(18)(2.1 mm×100 mm,1.7μm),the mobile phase was methanol:water=90:10,the flow rate was 0.2 mL/min,the second column was ECOSIL C_(18)-eco100A C_(18)(4.6 mm×250 mm,5μm),the mobile phase was methanol:water=90:10,the flow rate was 1.0 mL/min,the detection wavelength was 245 nm;injection volume:20μL,column temperature:35℃.Trapping column:ZORBAX Eclipse Plus C_(18)(4.6 mm×100 mm,5μm);valve switching time:0~2.8 min:position 1~2;2.81~3.9 min:position 1~6;3.91~16 min:position 1~2.Results:Avermectin had a good linear relationship in the range of 0.05~1.0 mg/L,the correlation coefficient was 0.99972,and the quantitative limit of the method was 0.012 mg/kg.The recovery rate of the three concentration addition level is 82.5%~105.3%,the repeatability is good,and the relative standard deviation(RSD)is between 1.8%~2.7%.Conclusion:The method has high sensitivity,good reproducibility and good stability,and the recovery rate meets the requirements of pretreatment of complex matrix samples,and is suitable for the rapid detection of avermectin in vegetables.