无分散剂微波辅助离子液体分散液液微萃取/胶束电动色谱检测食用油中丙烯酰胺和5-羟甲基糠醛残留  

Determination of Acrylamide and 5-Hydroxymethylfurfural Residues in Edible Oils by Micellar Electrokinetic Chromatography with Dispersive Solvent-free Microwave-assisted Ionic Liquid Dispersive Liquid-Liquid Microextraction

作　　者：徐蕊 高仕谦[1,2] 吴友谊 毛宇成[1] XU Rui;GAO Shi-qian;WU You-yi;MAO Yu-cheng(School of Environmental Science and Engineering,Suzhou University of Science and Technology,Suzhou 215009,China;Key Laboratory of Environmental Science and Engineering of Jiangsu Province,Suzhou 215009,China)

机构地区：[1]苏州科技大学环境科学与工程学院,江苏苏州215009 [2]江苏省环境科学与工程重点实验室,江苏苏州215009

出　　处：《分析测试学报》2020年第6期722-728,共7页Journal of Instrumental Analysis

基　　金：江苏省环境科学与工程重点实验室项目(Zd1805);国家“十三五”水专项课题(2017ZX07205-02)。

摘　　要：丙烯酰胺(AA)和5-羟甲基糠醛(5-HMF)主要通过美拉德反应形成,因其在食品中广泛存在且毒理效应显著而倍受关注。该文开发了一种无需分散剂的微波辅助离子液体分散液液微萃取结合胶束电动色谱分析食用油中AA和5-HMF的方法。通过实验优化了影响萃取回收率的因素,包括离子液体种类和体积、微波辅助萃取条件、样品体积以及胶束电动色谱的分离条件等。在最佳实验条件下,方法的线性范围为0.5~50μg/mL(r2≥0.997 1),AA和5-HMF检出限(S/N=3)分别为0.11、0.70μg/mL,加标回收率分别为82.5%~96.2%和77.9%~95.9%,相对标准偏差分别为1.3%~5.2%和1.7%~4.9%。利用该方法在3种商品芝麻香油和1种餐馆自制花椒油中检出5-HMF,含量在1.1~3.3μg/mL之间。该方法简单、高效且经济环保,可应用于食用油中AA和5-HMF的分析测定。Acrylamide(AA) and 5-hydroxymethylfurfural(5-HMF) are mainly formed by Maillard reaction,which have attracted much attention due to their widespread existence in foods and their significant toxicological effects.In this paper,a new method was developed for the determination of AA and 5-HMF in edible oils by micellar electrokinetic chromatography with microwave-assisted ionic liquid dispersive liquid-liquid microextraction without dispersant.Factors affecting the recovery were optimized in the experiments,including type and volume of ionic liquid,microwave-assisted extraction conditions,sample volume and separation conditions of micellar electrokinetic chromatography.Under the optimized conditions,the method exhibited a good linearity in the range of 0.5-50 μg/mL with correlation coefficients(r2) not less than 0.997 1.The limits of detections(S/N=3) for AA and 5-HMF were 0.11 μg/mL and 0.70 μg/mL,respectively.The spiked recoveries were in the range of 77.9%-96.2% with relative standard deviations(RSDs) of 1.3%-5.2%.5-HMF was found in three kinds of sesame oils and a pepper oil with concentrations of 1.1-3.3 μg/mL.The proposed method was simple,efficient,inexpensive and ecofriendly,and it was applicable for the analysis of AA and 5-HMF in edible oils.

关 键 词：离子液体 液液微萃取 食用油 胶束电动色谱 丙烯酰胺 5-羟甲基糠醛 

分 类 号：O657.7[理学—分析化学]