多壁碳纳米管改进QuEChERS-液相色谱-串联质谱法测定豆类中12种酰胺类杀菌剂残留量

Determination of 12 amide fungicides in legumes by multi-walled carbon nanotubes QuEChERS-liquid chromatography-tandem mass spectrometry

建立基于多壁碳纳米管改进分散固相萃取净化技术(QuEChERS),结合液相色谱-串联质谱法(LC-MS/MS),测定豆类中12种酰胺类杀菌剂残留量。结果表明:改进的QuEChERS最佳条件为无水MgSO4添加量800 mg、PSA添加量200 mg、HC-C18添加量100 mg、MWCNTs添加量25 mg;在此条件下测得的12种酰胺类杀菌剂在0.1~2.5μg/L范围内均具有良好的线性关系,相关系数均大于0.99;方法检出限为0.05~2.00μg/kg,定量限为0.2~5.0μg/kg;加标实验平均回收率为70.7%~115.0%,相对标准偏差为0.4%~7.4%。该方法操作快捷,净化效果好,灵敏度高,适用于豆类中酰胺类杀菌剂残留量的分析。

An improved dispersive solid-phase extraction purification technology(QuEChERS)based on multi-walled carbon nanotubes was established to determine the residues of 12 amide fungicides in legumes by LC-MS/MS.The results showed that the optimal conditions for the improved QuEChERS were anhydrous MgSO_(4) addition 800 mg,PSA addition 200 mg,HC-C_(18) addition 100 mg and MWCNTs addition 25 mg.Under these conditions,the 12 amide pesticides showed good linearity in the mass concentration range of 0.1-2.5μg/L,and correlation coefficients were above 0.99.The limits of detection and quantification were 0.05-2.00μg/kg and 0.2-5.0μg/kg,respectively.The average recoveries were 70.7%-115.0% and the relative standard deviations were 0.4%-7.4%.This method had the advantages of fast operation,good purification efficiency and was sensitive,suitable for the determination of amide fungicide residues in legumes.