摘要
为实现烘焙食品中晚期糖基化终末产物(Advanced Glycation End Products,AGEs)的准确、高灵敏测定,建立基于磁性共价有机骨架(Covalent Organic Frameworks,COFs)材料的磁固相萃取(Magnetic Solid Phase Extraction,MSPE)技术,实现烘焙食品中两种主要AGEs,即羧甲基赖氨酸(N^(ε)-(carboxymethyl)lysine),(CML)和羧乙基赖氨酸(N^(ε)-(carboxyethyl)lysine,CEL)的选择性、高效富集,并结合高效液相色谱-串联质谱法对其进行定量分析。结果表明:所合成的磁性COFs材料具有较大的比表面积和较高的磁化强度,适合应用于MSPE技术。MSPE的适宜条件为吸附剂用量20 mg,涡旋萃取时间20 min,洗脱溶剂选用5%氨水/甲醇溶液,洗脱溶剂体积4 mL,洗脱时间15 min。CML和CEL的检出限分别为2.05 ng/mL和2.31 ng/mL,定量限分别为6.83 ng/mL和7.71 ng/mL;日内及日间精密度良好(RSD_(日内)≤4.74%,RSD_(日间)≤5.38%);在饼干、坚果2种典型样品基质中,CML和CEL的加标回收率分别为90.70%~108.74%、85.50%~113.00%。将本文所建立的分析方法应用于市售的26种烘焙食品中CML和CEL的含量测定发现,饼干、糕点类烘焙食品中二者含量分别为(9.60±0.16)~(78.10±1.12)mg/kg、(4.37±0.23)~(26.70±1.27)mg/kg;坚果类烘焙食品中二者含量分别为(6.49±0.13)~(82.00±0.98)mg/kg、(6.65±0.30)~(55.90±0.67)mg/kg,该方法能有效净化样品,显著降低基质效应,定量分析准确性较高,且所合成的磁性COFs材料可再生使用5次,适合烘焙食品中CML和CEL的检测。
To achieve accurate and highly sensitive determination of advanced glycation end products(AGEs)in baked food,a magnetic solid phase extraction(MSPE)technique based on magnetic covalent organic frameworks(COFs)material was established to achieve the selective and efficient enrichment of two major AGEs(i.e.N^(ε)-(carboxymethyl)lysine(CML)and N^(ε)-(carboxyethyl)lysine(CEL))in baked foods.The quantitative analysis of CML and CEL was conducted with high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)method.Results showed that the synthesized magnetic COFs material showed big specific surface area and strong magnetism,which was suitable for MSPE.The optimum conditions of MSPE were as follows:the amount of adsorbent was 20 mg,the time of vortex extraction was 20 min,the elution solvent was 5%ammonia/methanol solution,the volume of elution solvent was 4 mL,the elution time was 15 min.The limits of detection of CML and CEL for the established method were 2.05 ng/mL and 2.31 ng/mL,respectively,while the limits of quantification were 6.83 ng/mL and 7.71 ng/mL,respectively.And intra-day and inter-day precisions were good(RSD_(intra-day)≤4.74%,RSD_(inter-day)≤5.38%).The recoveries of CML and CEL in typical food matrixes(i.e.biscuits and nuts)were in the range of 90.70%~108.74%and 85.50%~113.00%,respectively.Applying the analytical method established in this article to the determination of CML and CEL contents in 26 commercially available baked goods,it was found that the contents of CML and CEL in biscuits and pastries were in the range of(9.60±0.16)~(78.10±1.12)mg/kg,and(4.37±0.23)~(26.70±1.27)mg/kg,respectively;while the contents of CML and CEL in nuts were in the range of(6.49±0.13)~(82.00±0.98)mg/kg,and(6.65±0.30)~(55.90±0.67)mg/kg,respectively.The established method could effectively purify samples and significantly reduce matrix effect,and thus showed high accuracy for quantitative analysis.Furthermore,the synthesized magnetic COFs material could be recycled for 5 times,which was su
作者
余晶晶
史莉莉
刘雨欣
陈满堂
刘瑞红
刘伟
YU Jingjing;SHI Lili;LIU Yuxin;CHEN Mantang;LIU Ruihong;LIU Wei(Zhengzhou Tobacco Research Institute of CNTC,Zhengzhou 450001,China;School of Food Science and Technology,Henan University of Technology,Zhengzhou 450001,China)
出处
《轻工学报》
CAS
北大核心
2023年第6期52-61,共10页
Journal of Light Industry
基金
国家自然科学基金青年科学基金项目(31901768)。
关键词
晚期糖基化终末产物
共价有机骨架
磁固相萃取
高效液相色谱-串联质谱
烘焙食品
advanced glycation end products
covalent organic frameworks
magnetic solid phase extraction
high performance liquid chromatography-tandem mass spectrometry
baked food
