基于X射线衍射的香兰素快速检测技术研究  

Investigation of Novel Method for Detecting Vanillin Based on X-Ray Diffraction Technology

作　　者：石志锋[1,2] 刘佳[2] 肖娟[2] 郑志雯[1] SHI Zhi-feng;LIU Jia;XIAO Juan;ZHENG Zhi-wen(National Engineering Research Center for Tissue Restoration and Reconstruction and Key Laboratory of Biomedical Engineering of Guangdong Province,South China University of Technology,Guangzhou 510006,China;Medical Devices Research and Testing Center,South China University of Technology,Guangzhou 510006,China)

机构地区：[1]华南理工大学,国家人体组织功能重建工程技术研究中心,广东广州510006 [2]华南理工大学,医疗器械研究检验中心,广东广州510006

出　　处：《光谱学与光谱分析》2023年第5期1563-1568,共6页Spectroscopy and Spectral Analysis

基　　金：国家重点研发计划项目(2021YFC2400700);广州市应用基础研究计划项目(202102080430,202102080437)资助。

摘　　要：婴幼儿非母乳喂养时奶粉是摄取营养的主要制品,“三聚氰胺”、“香兰素”等添加剂安全事件的频频发生,引起全社会的高度关注。如何快速检测并高效识别奶粉中的不良物质,是国内外乳制品安全领域的研究热点,对保障婴幼儿成长健康具有十分重要的现实意义。由于淀粉和香兰素的红外和拉曼光谱均存在大量的吸收峰,基质与添加物的光谱信号重合区域广信噪比低,谱峰重叠干扰严重,仪器越灵敏检测筛选的难度越大。研究基于X射线衍射(XRD)建立了适用于食品添加剂香兰素的无损快速、高灵敏度检测方法,食品乳制品中的淀粉、蛋白质等基质材料在XRD下均不具有复杂的衍射花样,基于XRD的香兰素快速检测方法消除了食品乳制品中各类基质的背景干扰,结合XRD图谱的指纹特性对香兰素的掺杂进行快速鉴别和定性识别检测。结果表明,掺杂香兰素后衍射图谱13.03°出现明显尖锐的衍射峰,峰形好,响应值高,该衍射峰是快速检测香兰素是否存在的特征指纹峰。XRD法快速检测香兰素采用直接进样、精细扫描,在去除基质影响的同时,相对于气相色谱法、电泳法,该方法更加方便、快速,定性确认更准确,结果可靠,适用性强。香兰素晶体衍射峰明显,结构稳定,同时制样简单,极大地缩短了检测时间。本研究中香兰素最低掺杂量为202μg·g^(-1),可用于市售加香食品中香兰素的含量的快速检测,灵敏度可满足建议限量和超量掺加的检测需求。Milk powder is the main nutritional product for infants when they are not breast-fed.The frequent occurrence of melamine,vanillin and other additives has aroused great concern for society.How to more quickly detect and efficiently identify the adverse substances in milk powder is a research hotspot in the field of dairy product safety at home and abroad,which has very important practical significance to ensure the growth and health of infants.Due to a large number of absorption peaks in IR and Raman spectra of starch and vanillin,the overlap region of spectral signals between substrate and additive was wide,and the signal-to-noise ratio was low,which led to serious speak overlap.The more sensitive the instrument is,the more difficult it is to detect and screen.In this study,a non-destructive,rapid and highly sensitive method for determining vanillin as a food additive was established based on X-ray diffraction(XRD).The matrix materials,such as starch and protein of food dairy products,did not have complex diffraction patterns under XRD.Therefore,the detection method of vanillin based on XRD eliminated the background interference of various substrates in food and dairy products.The doping of vanillin could be quickly identified and qualitatively identified by combining the fingerprint characteristics of XRD patterns.The results showed a sharp diffraction peak at 13.03°with good peak shape and high response value in the diffraction pattern after doping vanillin,which would be a characteristic fingerprint peak for rapid detection of vanillin.Compared with gas chromatography and electrophoresis,this method could be more convenient,rapid,accurate in qualitative confirmation to obtain more reliable results and strong applicability while removing matrix influence by direct injection and fine scanning.In this study,the minimum doping amount of vanillin was 202μg·g^(-1).The method can be used to rapidly detect vanillin in commercial flavoring foods,and the sensitivity can meet the requirements of recommended limit and

关 键 词：X射线衍射 香兰素 食品安全 快速检测 补充检验 

分 类 号：TK6[动力工程及工程热物理—生物能]