QuEChERS-HPLC-MS/MS法测定九华黄精中26种农药残留

Simultaneous Determination of Residues of 26 pesticide in Jiuhua Polygonatum cyrtonema by QuEChERS-HPLC-MS/MS

建立了固相萃取高效液相色谱串联质谱法测定九华黄精中26种农药残留的方法。试样采用乙腈提取,所得提取液经分散固相萃取净化后,用超高效液相色谱串联质谱检测,以外标法定量。26种农药的标准曲线在0.002~0.200μg·mL^(-1)线性良好,相关系数均在0.996以上,方法检出限在0.01~0.05 mg·kg^(-1),定量限在0.03~0.15 mg·kg^(-1)。不同加标水平的平均回收率在62.8%~108.6%,回收率相对标准偏差范围在0.5%~9.1%(n=6)。经优化后的前处理方法,操作简便,重现性较好,回收率能够满足要求,可提高检测效率,降低检测成本。

A method was developed for the determination of 26 pesticide residues in Polygonatum cyrtonema by ultra-high performance liquid chromatography-tandem mass spectrometry.The samples were extracted by acetonitrile,and the extracted liquid was purified by dispersed solid phase extraction,detected by HPLC-MS/MS,and quantitative analysed by external standard method.The standard curves of 26 pesticides had good linearity in the concentration range of 0.002~0.200μg·mL^(-1),and the correlation coefficients were all above 0.996.The detection limit of the method is 0.01~0.05 mg·kg^(-1),and the quantitative limit is 0.03~0.15 mg·kg^(-1).The average recovery was 62.8%~108.6%,and the relative standard deviation of recovery was 0.5%~9.1%(n=6).The optimized pretreatment method has the advantages of simpler operation,better reproducibility,better recovery rate,higher detection efficiency and lower detection cost.