【摘要】：近年來,由于經(jīng)濟利益的驅(qū)使、科學(xué)知識的匱乏以及監(jiān)督體制的漏洞,出現(xiàn)了許許多多的食品質(zhì)量安全問題,隨著這些重大食品安全問題的曝光,人們也越來越關(guān)注食品質(zhì)量安全與膳食營養(yǎng)等問題�，F(xiàn)如今的許多化學(xué)分析方法均已被許多研究者深入研究,很多方法已經(jīng)趨于成熟,但是仍有許多問題不能夠突破,如果想要得到更簡便、快捷、靈敏的分析方法,就要開發(fā)新的方式。上轉(zhuǎn)換熒光分析是一種比較先進(jìn)的化學(xué)分析方法,上轉(zhuǎn)換納米發(fā)光材料的最大特點是:化學(xué)性質(zhì)穩(wěn)定、無毒、無光閃爍和光漂泊以及近紅外激發(fā)�，F(xiàn)如今,應(yīng)用上轉(zhuǎn)換熒光分析的方法檢測食品中的有益有害物質(zhì)并不多見,本文致力于建立一種食品檢測方法,將上轉(zhuǎn)換熒光分析的方法與之融合,開發(fā)一種全新的、簡便的、靈敏的食品檢測方法。(1)基于苯胺單體在上轉(zhuǎn)換納米粒子表面原位聚合的檢測方法的建立:本文合成了一種上轉(zhuǎn)換發(fā)光納米材料(Na YF4:Yb~(3+)/Er~(3+)納米粒子)并在表面以聚丙烯酸(PAA MW=1800)包裹。本文建立了基于聚苯胺使上轉(zhuǎn)換納米粒子熒光淬滅的檢測方法。膽堿在37℃下通過膽堿氧化酶催化而分解成過氧化氫(H2O2)和甜菜堿。在p H 3.0的環(huán)境下苯胺單體的正電荷與上轉(zhuǎn)換納米粒子表面上的負(fù)電荷發(fā)生靜電相互作用,并且在HRP和H2O2的存在下,使得苯胺單體在上轉(zhuǎn)換納米粒子的表面上原位聚合形成聚苯胺后,上轉(zhuǎn)換納米粒子熒光淬滅。根據(jù)熒光光譜圖,可以分析樣品中H2O2和膽堿的含量。膽堿的檢測濃度范圍為1-200μM,檢出限為50 n M。在嬰兒配方奶粉以及雞蛋中進(jìn)行了實際應(yīng)用,對膽堿檢測的回收率在97.7%-102.7%之間。這種上轉(zhuǎn)換發(fā)光檢測方法不僅可以避免其他熒光物質(zhì)的干擾,還具有選擇性高、靈敏、快捷、操作簡單的特點。(2)基于三價鐵離子淬滅上轉(zhuǎn)換納米熒光材料的檢測方法的建立:本文合成了一種上轉(zhuǎn)換納米熒光材料(Na YF4:Yb~(3+)/Tm~(3+)納米粒子)并在表面以聚丙烯酸(PAA MW=1800)包裹。試驗中發(fā)現(xiàn)三價鐵離子對上轉(zhuǎn)換發(fā)光納米材料具有明顯的淬滅效應(yīng),而其他常見離子對其熒光不產(chǎn)生明顯影響。另外,過氧化氫(H2O2)可以將二價鐵離子(Fe2+)氧化成三價鐵離子(Fe~(3+)),這從而能使上轉(zhuǎn)換納米材料熒光淬滅。基于此,我們開發(fā)了一種新的過氧化氫檢測方法。因為膽堿在37℃下通過膽堿氧化酶的催化分解成H2O2和甜菜堿,然后H2O2可以將二價鐵離子氧化為三價鐵離子,三價鐵離子進(jìn)一步使上轉(zhuǎn)換納米材料熒光淬滅。因此,我們開發(fā)了膽堿的檢測方法。根據(jù)熒光光譜圖,可以分析樣品中H2O2和膽堿的含量。H2O2的檢測濃度范圍為0.25-5μM,檢出限為0.1μM。膽堿的檢測濃度范圍為1-60μM,檢出限為0.5μM。在嬰兒配方奶粉進(jìn)行了實際應(yīng)用,對膽堿檢測的回收率在95.0%-100.07%之間。這種使用近紅外光進(jìn)行測試的方法在生物分析中具有重要意義,它也可用于測試其他有機物質(zhì)和反應(yīng),在生物體中產(chǎn)生過氧化氫。這種檢測方法具有選擇性高、靈敏、快捷、操作簡單的特點。
[Abstract]:In recent years, driven by economic interests, lack of scientific knowledge and loopholes in the supervision system, there have been many food quality and safety problems. With the exposure of these major food safety issues, people are increasingly concerned about food quality and safety and dietary nutrition. Now many chemical analysis methods have been approved. Up-conversion fluorescence analysis is a relatively advanced chemical analysis method. The most important characteristics of up-conversion nanoluminescent materials are chemical properties. Nowadays, it is rare to use up-conversion fluorescence analysis to detect the beneficial and harmful substances in food. This paper is devoted to establish a food detection method, which combines up-conversion fluorescence analysis with it to develop a new, simple and sensitive food. Detection methods. (1) Based on the in-situ polymerization of aniline monomers on the surface of upconversion nanoparticles, a novel upconversion luminescent nanomaterial (Na YF4: Yb ~ (3 +) / Er ~ (3 +) nanoparticles) was synthesized and coated with polyacrylic acid (PAA MW = 1800). A fluorescence quenching method for upconversion nanoparticles based on polyaniline was established. Detection method. Choline is decomposed into hydrogen peroxide (H2O2) and betaine catalyzed by choline oxidase at 37 C. The positive charge of aniline monomer interacts electrostatically with the negative charge on the surface of upconversion nanoparticles in the presence of HRP and H2O2, enabling the aniline monomer to be on the surface of upconversion nanoparticles. According to the fluorescence spectrum, the content of H2O2 and choline in the sample can be analyzed. The detection concentration range of choline is 1-200 mu M, and the detection limit is 50 N M. It has been applied in infant formula milk powder and eggs. The recovery of choline detection is 97.7% - 102.7%. (2) Based on the determination method of up-conversion Nanofluorescent materials by ferric ion quenching, a novel up-conversion Nanofluorescent material (Na YF4: Yb ~ (3 +) / Tm ~ (3 +) nanometer was synthesized. In addition, hydrogen peroxide (H2O2) can oxidize divalent iron ions (Fe2 +) to trivalent iron ions (Fe 3 +), which leads to an obvious quenching effect. Based on this, we developed a new method for the determination of hydrogen peroxide. Choline is decomposed into H2O2 and betaine by choline oxidase catalysis at 37 C, and then H2O2 oxidizes divalent iron ions to trivalent iron ions. Trivalent iron ions further quench the fluorescence of up-conversion nanomaterials. Therefore, we have developed a method for the determination of choline. According to the fluorescence spectrogram, the content of H2O2 and choline in the sample can be analyzed. The detection concentration range of H2O2 is 0.25-5 mu M, the detection limit is 0.1 mu M. The detection concentration range of choline is 1-60 mu M, the detection limit is 0.5 mu M. In the range of 95.0%-100.07%. This method is of great significance in biological analysis. It can also be used to test other organic substances and reactions and produce hydrogen peroxide in organisms. This method has the characteristics of high selectivity, sensitivity, rapidity and simple operation.
【學(xué)位授予單位】：吉林大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O657.3;TS207.3

【參考文獻(xiàn)】

相關(guān)期刊論文 前1條

1 陳志鋼;宋岳林;田啟威;胡俊青;李富友;;稀土上轉(zhuǎn)換發(fā)光納米材料的研究進(jìn)展[J];現(xiàn)代化工;2010年07期

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本文編號：2215334