基于分子印迹与荧光探针的三聚氰胺高灵敏检测

发布时间：2018-03-31 05:15

  本文选题：分子印迹　切入点：荧光探针　出处：《天津科技大学》2016年硕士论文

【摘要】：食品安全一直与人们的生活息息相关,直接影响着人类生命的健康和社会经济稳定的发展。在2008年,发生在国内婴幼儿奶粉非法添加三聚氰胺导致婴儿肾结石事件,使得三聚氰胺的检测成为关注的热点。因此,开发出高效、快速的定量检测牛奶中非法添加剂三聚氰胺残留技术成为当前有效解决安全问题的关键。分子印迹技术(Molecular imprinting technique,MIT)是一种能够制备出对目标分子具有特异性结合能力的聚合物的技术,这种聚合物稳定性好,对目标物具有高度的选择性,可以对复杂样品前处理,已广泛应用于食品安全分析。荧光化学传感器(Fluorescent chemosensor)因其具有高特异性、高灵敏性、可实现实时快速分析等优点,逐渐成为检测各种金属阳离子、小分子、生物活性物质以及一些阴离子的理想检测手段。本实验研究制备了具有特异性识别性能以及高结合容量的三聚氰胺分子印迹聚合物,达到良好的富集效果,并利用罗丹明B有机合成罗丹明乙二醛酰腙制备了荧光化学传感器用于三聚氰胺的定量检测。结合这两种方法的优势,建立了一种高灵敏性定量检测牛奶样品中三聚氰胺残留方法。研究成果如下:(一):利用沉淀聚合法,通过优化模板分子与功能单体之间的摩尔比以及复合溶剂之间的体积比,制备了对三聚氰胺具有特异性识别能力和高容量结合性能的分子印迹聚合物,印迹因子为3.072。其最优制备条件为:0.3 mmol(37.8g)三聚氰胺作为模板分子,2mg纳米CaC03作为致孔剂,60mL乙腈与甲醇的混合溶液(10/50,V/V)作为溶剂,3.6 mmol(0.3 mL)甲基丙烯酸作为功能单体,26.5 mmol(5 mL)乙二醇二甲基丙烯酸酯作为交联剂,以及30 mg偶氮二异丁腈作为引发剂,混合后进行超声脱气10 min,通N2除去氧气15 min,密封,在恒温60 ℃C水浴锅中反应24 h。(二):利用罗丹明B两步合成制备的荧光化学传感器RB1定量检测三聚氰胺。选择在530 nm处激发,在590 nm处出现荧光发射峰。随着三聚氰胺溶液浓度的增大,荧光强度也随之增强,同时表现出良好的线性关系。对三聚氰胺的检测线为1.55 × 10-4 mmol/L,线性范围为6.25 × 10-4-8 × 10-2 mmol/L,相对标准偏差从3.18到4.91%。本实验建立了一种有效的牛奶中检测三聚氰胺方法,采用分子印迹聚合物富集三聚氰胺,并利用荧光化学传感器检测三聚氰胺。
[Abstract]:Food safety has always been closely related to people's lives, directly affecting the health of human life and the development of social and economic stability. In 2008, the illegal addition of melamine to infant milk powder in China caused kidney stones in infants. The detection of melamine has become the focus of attention. Therefore, the development of high efficiency, Rapid and quantitative detection of melamine residues as an illegal additive in milk has become the key to solve the safety problems. Molecular imprinting technique (mitt) is a kind of molecular imprinting technology, which can produce specific binding ability to target molecules. Of the polymer technology, This kind of polymer has good stability, high selectivity to the target, and can be used for the pretreatment of complex samples. It has been widely used in food safety analysis. Fluorochemical sensor Fluorescent chemosensorhas high specificity and high sensitivity. With the advantages of real-time and rapid analysis, it has gradually become the detection of various metal cations and small molecules. In this study, melamine molecularly imprinted polymers with specific recognition and high binding capacity were prepared. A fluorescent chemical sensor was prepared by using rhodamine B organic synthesis of Rhodamine Glyoxal acyl Hydrazone for quantitative detection of melamine. A highly sensitive and quantitative method for the determination of melamine residues in milk samples was established. The results were as follows: (1) by means of precipitation polymerization, the molar ratio of template molecules to functional monomers and the volume ratio of complex solvents were optimized. Molecularly imprinted polymers with specific recognition and high capacity binding to melamine were prepared. The imprinting factor was 3.072.The optimum preparation conditions were as follows: 0.3 mmol / mL 37.8 g) melamine was used as template molecule and 2 mg / CaC03 was used as pore-inducing agent 60 mL mixed solution of acetonitrile and methanol (10 / 50 V / V / V) as solvent 3.6 mmol(0.3 mL) methacrylic acid as functional monomer (26.5 mmol(5 mL) ethylene diethylene. Alcohol dimethacrylate as crosslinking agent, And 30 mg azo diisobutyronitrile was used as initiator. After mixing, ultrasonic degassing was carried out for 10 mins, oxygen was removed by N2 for 15 mins, and sealed. In a constant temperature 60 鈩，

本文编号：1689300