液相色谱-串联三重四极杆质谱仪快速测定鱼腥草中152种农药残留

Rapid determination of 152 pesticide residues in Houttuynia cordata by liquid chromatography tandem triple quadrupole mass spectrometer

建立QuEChERS结合液相色谱-串联三重四极杆质谱仪快速测定鱼腥草中152种农药残留的方法。样品用10 mL乙腈提取,经过分散固相萃取净化,以含体积分数0.01%甲酸的5 mmol/L乙酸铵溶液(A)与甲醇(B)作为流动相进行梯度洗脱,采用多反应监测模式(MRM)进行定性定量分析。结果表明:152种农药在质量浓度0.001~0.100 mg/kg范围内具有良好的线性关系,相关系数均大于0.995,检出限为3.2×10^(-3)~0.843μg/kg,定量限为1.97×10^(-3)~2.81μg/kg,回收率为63.7%~109.2%,相对标准偏差(RSD,n=6)为0.42%~12.60%。

A method for rapid determination of 152 pesticide residues in Houtuynia cordata using QuEChERS combined with liquid chromatography tandem triple quadrupole mass spectrometry was estab-lished.The sample was extracted with 10 mL of acetonitrile and purified by dispersed solid-phase extrac-tion.A gradient elution was performed using 5 mmol/L ammonium acetate solution containing volume frac-tion 0.01%formic acid(A)and methanol(B)as the mobile phase,and qualitative and quantitative analy-sis was performed using multiple reaction monitoring mode(MRM).The results showed that 152 pesticides had a good linear relationship within the mass concentration range of 0.001-0.100 mg/kg,with correla-tion coefficients greater than 0.995.The limit of detection was 3.2×10^(-3)-0.843μg/kg,and the limit of quantitotion was 1.97×10^(-3)-2.81μg/kg.The recovery rate was 63.7%-109.2%,and the relative standard deviation(RSD,n=6)was 0.42%-12.60%.