本文選題：雙酚A + 分子印跡聚合物　； 參考：《江蘇大學(xué)》2017年碩士論文

【摘要】：雙酚A是一種低毒性化學(xué)物質(zhì),對人體皮膚、消化道、呼吸道、角膜等有中等強(qiáng)度刺激性,并且雙酚A具有模擬雌激素的效果,能破壞荷爾蒙。因此,研究一種既簡便有效的方法去檢測環(huán)境樣品中痕量雙酚A,非常有意義。實(shí)驗(yàn)采用表面分子印跡技術(shù),以雙酚A為目標(biāo)分子,制備了雙酚A分子印跡聚合物,以分子印跡材料、石墨烯、四氧化三鐵、納米金為電極修飾材料,制備了三種修飾電極,考察了修飾電極的電化學(xué)性能,研究了pH值、印跡材料用量、掃描速率、吸附時間對電化學(xué)性能的影響,優(yōu)化了電化學(xué)工作站的分析檢測條件,在最優(yōu)條件下考察了方法的檢出限,線性范圍。并且將三種電極都用于環(huán)境樣品中雙酚A的分析檢測。主要研究內(nèi)容包括以下三個方面:(I)以雙酚A為模板分子,4-乙烯基吡啶為功能單體,沉淀聚合法制備了雙酚A分子印跡聚合物,采用Hummers法制備氧化石墨烯,并將其還原得到石墨烯。利用自制的石墨烯和分子印跡材料對碳糊電極進(jìn)行修飾,對石墨烯和分子印跡材料的進(jìn)行了表征,研究了自制電極的電化學(xué)性能,考察了MIPs濃度、時間、掃描速率對電化學(xué)傳感器分析檢測的影響,優(yōu)化了最佳分析檢測條件,在最優(yōu)條件下,方法的檢出限為9.63×10-11 g/L。并將其用于環(huán)四種實(shí)際環(huán)境樣品中雙酚A的分析檢測,相對標(biāo)準(zhǔn)偏差為1.7-3.5%(N=5),加標(biāo)回收率在95%-103%之間,實(shí)驗(yàn)還將此法與傳統(tǒng)高效液相色譜法對比,研究結(jié)果表明,液相色譜和實(shí)驗(yàn)所用方法具有顯著相關(guān)性。(II)用石墨烯、四氧化三鐵、分子印跡聚合物修飾乙炔黑糊電極得到新型碳糊電極,研究了自制電極的電化學(xué)性能,考察了分子印跡材料濃度、吸附時間、掃描速率、pH等對電極分析檢測性能的影響,在最優(yōu)條件下,考察了自制電極對雙酚A的分析檢測性能,方法的檢出限為6.34×10-10 g/L(3σ),最后將此電極用于環(huán)境樣品中雙酚A的分析檢測,相對標(biāo)準(zhǔn)偏差為2.8%—3.6%(N=5),加標(biāo)回收率在90%-102%之間。(III)為了減輕石墨烯的氧化團(tuán)聚,實(shí)驗(yàn)選擇加入納米金,制備得到納米金-還原石墨烯復(fù)合材料,將雙酚A分子印跡材料和納米金-還原石墨烯復(fù)合材料修飾到碳糊電極表面得到納米金-石墨烯-分子印跡聚合物修飾碳糊電極,研究了自制電極的電化學(xué)性能,考察了pH值、分子印跡材料濃度、吸附時間、掃描速率等條件對電化學(xué)工作站分析檢測性能的影響,優(yōu)化了分析檢測條件,考察了方法的檢出限,此法的檢出限為1.27×10-11 g/L,并將此方法用于環(huán)境樣品中四種實(shí)際樣品的分析檢測,相對標(biāo)準(zhǔn)偏差為2.1%-3.6%(N=5),加標(biāo)回收率在95%-100%之間。
[Abstract]:Bisphenol A (BPA) is a low toxic chemical substance which has moderate irritation to human skin, digestive tract, respiratory tract, cornea and so on. Bisphenol A has the effect of mimicking estrogen and can destroy hormones. Therefore, it is of great significance to study a simple and effective method for the determination of trace bisphenol A in environmental samples. Using surface molecular imprinting technique and bisphenol A as target molecule, three kinds of modified electrodes were prepared by using molecularly imprinted materials, graphene, ferric oxide and gold nanoparticles as electrode modification materials. The effects of pH value, amount of imprinted materials, scanning rate and adsorption time on the electrochemical performance of the modified electrode were investigated. The analytical conditions of the electrochemical workstation were optimized. The detection limit and linear range of the method are investigated under the optimal conditions. The three kinds of electrodes were used for the analysis and detection of bisphenol A in environmental samples. The main research contents include the following three aspects: (I) bisphenol A molecularly imprinted polymer was prepared by precipitation polymerization and graphene oxide was prepared by Hummers method using bisphenol A as template molecule and vinyl pyridine as functional monomer. It was reduced to graphene. The carbon paste electrode was modified with graphene and molecularly imprinted materials. The electrochemical properties of the electrode were studied. The concentration and time of MIPs were investigated. The effect of scanning rate on the analysis and detection of electrochemical sensors was studied. The optimum analytical and detection conditions were optimized. The detection limit of the method was 9.63 脳 10 ~ (-11) g / L under the optimal conditions. The method was applied to the determination of bisphenol A in four real environmental samples. The relative standard deviation was 1.7-3.5% (N5), and the recovery rate was between 95% and 103%. The method was also compared with the traditional high performance liquid chromatography (HPLC). There is a significant correlation between liquid chromatography and experimental methods. (II) A new type of carbon paste electrode was prepared by modifying acetylene black paste electrode with graphene, iron trioxide and molecularly imprinted polymer. The electrochemical properties of the self-made electrode were studied. The effects of the concentration of molecularly imprinted materials, adsorption time, scanning rate and pH on the performance of the electrode were investigated. Under the optimum conditions, the analytical performance of the self-made electrode for bisphenol A was investigated. The detection limit of the method was 6.34 脳 10 ~ (-10) g / L (3 蟽). Finally, the electrode was used for the determination of bisphenol A in environmental samples. The relative standard deviation was 2.8% -3.6% (N5), and the recovery rate was between 90% and 102%. (III) in order to reduce the oxidation agglomeration of graphene, nano-gold was added. The nano-gold-reduced graphene composite was prepared. The nano-gold graphene-molecularly imprinted polymer modified carbon paste electrode was prepared by modifying bisphenol A molecularly imprinted material and nano-gold-reduced graphene composite onto the surface of the carbon paste electrode. The electrochemical performance of self-made electrode was studied. The effects of pH value, concentration of molecularly imprinted materials, adsorption time and scanning rate on the performance of electrochemical workstation were investigated. The detection limit of this method was 1.27 脳 10 ~ (-11) g / L, and the method was applied to the analysis of four kinds of environmental samples. The relative standard deviation was 2.1 ~ 3.6% (N5) and the recovery rate was between 95% and 100%.
【學(xué)位授予單位】：江蘇大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O657.1;TB383.1

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