基于分子印跡與熒光探針的三聚氰胺高靈敏檢測(cè)
發(fā)布時(shí)間:2018-03-31 05:15
本文選題:分子印跡 切入點(diǎn):熒光探針 出處:《天津科技大學(xué)》2016年碩士論文
【摘要】:食品安全一直與人們的生活息息相關(guān),直接影響著人類生命的健康和社會(huì)經(jīng)濟(jì)穩(wěn)定的發(fā)展。在2008年,發(fā)生在國(guó)內(nèi)嬰幼兒奶粉非法添加三聚氰胺導(dǎo)致嬰兒腎結(jié)石事件,使得三聚氰胺的檢測(cè)成為關(guān)注的熱點(diǎn)。因此,開發(fā)出高效、快速的定量檢測(cè)牛奶中非法添加劑三聚氰胺殘留技術(shù)成為當(dāng)前有效解決安全問題的關(guān)鍵。分子印跡技術(shù)(Molecular imprinting technique,MIT)是一種能夠制備出對(duì)目標(biāo)分子具有特異性結(jié)合能力的聚合物的技術(shù),這種聚合物穩(wěn)定性好,對(duì)目標(biāo)物具有高度的選擇性,可以對(duì)復(fù)雜樣品前處理,已廣泛應(yīng)用于食品安全分析。熒光化學(xué)傳感器(Fluorescent chemosensor)因其具有高特異性、高靈敏性、可實(shí)現(xiàn)實(shí)時(shí)快速分析等優(yōu)點(diǎn),逐漸成為檢測(cè)各種金屬陽離子、小分子、生物活性物質(zhì)以及一些陰離子的理想檢測(cè)手段。本實(shí)驗(yàn)研究制備了具有特異性識(shí)別性能以及高結(jié)合容量的三聚氰胺分子印跡聚合物,達(dá)到良好的富集效果,并利用羅丹明B有機(jī)合成羅丹明乙二醛酰腙制備了熒光化學(xué)傳感器用于三聚氰胺的定量檢測(cè)。結(jié)合這兩種方法的優(yōu)勢(shì),建立了一種高靈敏性定量檢測(cè)牛奶樣品中三聚氰胺殘留方法。研究成果如下:(一):利用沉淀聚合法,通過優(yōu)化模板分子與功能單體之間的摩爾比以及復(fù)合溶劑之間的體積比,制備了對(duì)三聚氰胺具有特異性識(shí)別能力和高容量結(jié)合性能的分子印跡聚合物,印跡因子為3.072。其最優(yōu)制備條件為:0.3 mmol(37.8g)三聚氰胺作為模板分子,2mg納米CaC03作為致孔劑,60mL乙腈與甲醇的混合溶液(10/50,V/V)作為溶劑,3.6 mmol(0.3 mL)甲基丙烯酸作為功能單體,26.5 mmol(5 mL)乙二醇二甲基丙烯酸酯作為交聯(lián)劑,以及30 mg偶氮二異丁腈作為引發(fā)劑,混合后進(jìn)行超聲脫氣10 min,通N2除去氧氣15 min,密封,在恒溫60 ℃C水浴鍋中反應(yīng)24 h。(二):利用羅丹明B兩步合成制備的熒光化學(xué)傳感器RB1定量檢測(cè)三聚氰胺。選擇在530 nm處激發(fā),在590 nm處出現(xiàn)熒光發(fā)射峰。隨著三聚氰胺溶液濃度的增大,熒光強(qiáng)度也隨之增強(qiáng),同時(shí)表現(xiàn)出良好的線性關(guān)系。對(duì)三聚氰胺的檢測(cè)線為1.55 × 10-4 mmol/L,線性范圍為6.25 × 10-4-8 × 10-2 mmol/L,相對(duì)標(biāo)準(zhǔn)偏差從3.18到4.91%。本實(shí)驗(yàn)建立了一種有效的牛奶中檢測(cè)三聚氰胺方法,采用分子印跡聚合物富集三聚氰胺,并利用熒光化學(xué)傳感器檢測(cè)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,
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