食品与机械2023,Vol.39Issue(12):48-54,87,8.DOI:10.13652/j.spjx.1003.5788.2022.81068
分散固相萃取—超高效液相色谱—串联质谱法测定液态奶中11种农药残留量
Determination of 11 kinds of pesticide residues in liquid milk by dispersive solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
Objective:This study aimed to evaluate the safety of pesticide residues in liquid milk.Methods:A method for simultaneous determination of 11 kinds of pesticide residues by ultra-high-performance liquid chromatography-tandem mass spectrometry was established.The samples were extracted by acetonitrile,purified by C18 and PSA solid phase extractants,separated on a column Xbridge BEH C18(100 mm × 2.1 mm.1.7 μm),determined in multi-reaction monitoring mode,and optimized for pre-treatment parameters using response surface method.Results:The optimal conditions for pretreatment were 10 mL acetonitrile,50 mg C18 and 30 mg PSA.The linear relationships of 11 kinds of pesticides were good in the concentration range of 1.0~100.0 μg/L,and the correlation coefficients(R2)were all>0.999.With addition of 10,20,100 μg/kg,the average recoveries were 82.7%~102.0%,the relative standard deviations were 2.89%to 8.87%,and the limits of detection(LOD)and limits of quantitation(LOQ)were 2.0~3.0 μg/kg and 5.0~10.0 μg/kg,respectively.Conclusion:The method is simple,convenient,rapid,high recovery rate and high reproducibility,which could accurately determine 11 kinds of pesticide residues in liquid milk.关键词
分散固相萃取/超高效液相色谱—串联质谱/液态乳/农药残留Key words
dispersive solid phase extraction/UPLC-MS/MS/liquid milk/pesticide residue引用本文复制引用
黄曼谷,罗永浩,严婉盈,许丽珠..分散固相萃取—超高效液相色谱—串联质谱法测定液态奶中11种农药残留量[J].食品与机械,2023,39(12):48-54,87,8.基金项目
广州市市场监督管理局科技项目(编号:2022kj49) (编号:2022kj49)