UPLC-MS/MS法同时测定鲜黄精中12种杀菌剂残留

Simultaneous determination of 12 fungicide residues in fresh Polygonatum sibiricum by UPLC-MS/MS

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测鲜黄精中12种杀菌剂残留的分析方法。样品采用优化的QuEChERS法进行前处理,乙腈提取,NaCl盐析后经C18净化。12种杀菌剂经Thermo Hypersil GOLD色谱柱分离,使用UPLC-MS/MS电喷雾离子化、正/负源切换,多反应监测模式检测,基质匹配标准溶液外标法定量。结果表明,在5.0×10^(-4)~1.0 mg/L范围内12种杀菌剂线性关系良好,线性相关系数(R^(2))>0.99。在0.001,0.01,0.1,1.0 mg/kg 4个添加水平下,12种杀菌剂的平均添加回收率为72.3%~109.0%,相对标准偏差(RSD)为0.6%~13%。12种杀菌剂在鲜黄精中的定量限均为0.001 mg/kg。该方法符合农药残留分析要求,适用于鲜黄精中12种杀菌剂的批量快速定性定量分析。

An efficient ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was established for the simultaneous determination of 12 fungicide residues in fresh Polygonatum sibiricum.The sample was pretreated by the optimized QuEChERS method,extracted with acetonitrile and salted out by adding NaCl,and cleaned up with C_(18)adsorbent.12 fungicides were separated by Thermo Hypersil GOLD column,detected by UPLC-MS/MS with electrospray ionization,positive/negative source switching multireaction monitoring(MRM)mode,and quantified by matrix matching standard solution external standard method.The results showed that the linear relationships of 12 fungicides were good,and the correlation coefficients(R^(2))were higher than 0.99 in the concentration range of 5.0×10^(-4)-1.0 mg/L.The average recoveries of 12 fungicides were 72.3%-109.0%at spiked concentrations of 0.001,0.01,0.1 and 1.0 mg/kg,with the relative standard deviations(RSDs)ranging from 0.6%to 13%.The limits of quantitation of 12 fungicides in fresh Polygonatum sibiricum were 0.001 mg/kg.This method can meet the requirements of pesticides residues analysis and is suitable for the qualitative and quantitative analysis of 12 fungicides in fresh Polygonatum sibiricum.