气相色谱-质谱法测定含乳饮料中5种农药残留

Simultaneous Determination of Five Pesticide Residues in Milk Beverages by Gas Chromatography-Mass Spectrometry

建立了一种含乳饮料中多种农药残留的气相色谱-质谱测定方法。样品用乙腈提取,提取液经Prime-HLB柱富集净化后,气相色谱-质谱法测定,采用选择离子扫描(SIM)模式检测。结果表明,5种目标农药在5~120μg/L浓度范围内线性良好,相关系数(R^2)大于0.995,方法检出限0.5~1.0μg/kg。在5.0、15.0、75.0μg/kg^3个加标水平下的平均回收率为85.3%~96.7%,相对标准偏差为1.8%~4.7%。本实验所建立的方法,可以满足含乳饮料中5种目标农药残留的分析要求。

A robust analytical method was established for the determination of five pesticide residues in milk beverages using gas chromatography-mass spectrometry(GC-MS).Samples were extracted by acetonitrile and the extracted solutions were pretreated using Prime-HLB solid phase extraction(SPE)column.Determination of the analytes were conducted by GC-MS using selected ion monitoring(SIM)mode.The results showed that calibration curves of five pesticide residues were linear in the range of 5-120μg/L with correlation coefficients larger than 0.995.The limits of detection ranged from 0.5 to 1.0μg/kg.The recoveries at three concentration levels of 5.0,15.0 and 75.0μg/kg were 85.3%-96.7%with relative standard deviations ranged from 1.8%to 3.0%.The proposed method meets the current requirements for the pesticide residues analysis,and provides experimental basis for the analysis of multi-pesticide residues in milk beverages.