本文選題：表面增強(qiáng)拉曼光譜 + 構(gòu)筑　； 參考：《中國(guó)農(nóng)業(yè)科學(xué)院》2017年博士論文

【摘要】：目前,飼料與畜產(chǎn)品質(zhì)量安全快速分析技術(shù)亟需補(bǔ)充和完善�；诩{米結(jié)構(gòu)的表面增強(qiáng)拉曼光譜技術(shù)發(fā)展迅速,其中也面臨眾多技術(shù)難點(diǎn),如基底均一性、增強(qiáng)信號(hào)穩(wěn)定性以及對(duì)目標(biāo)分子靶向富集等問(wèn)題。若將SERS技術(shù)引入到飼料與畜產(chǎn)品快速分析領(lǐng)域,解決其中關(guān)鍵技術(shù)問(wèn)題,將會(huì)是一個(gè)巨大的飛躍。本論文制備了深度氧化石墨烯負(fù)載納米金復(fù)合物、納米銀陣列和納米金溶膠等三種SERS增強(qiáng)基底,研究了它們的光學(xué)性質(zhì)、穩(wěn)定性、均一性及增強(qiáng)活性,探究了關(guān)鍵制備參數(shù)、形貌參數(shù)對(duì)基底增強(qiáng)性能調(diào)控規(guī)律,揭示了影響基底增強(qiáng)信號(hào)穩(wěn)定性的關(guān)鍵因素和控制方法。論文還以納米銀陣列為例,闡明了三聚氰胺關(guān)鍵結(jié)構(gòu)在納米銀陣列表面作用的系統(tǒng)屬性及作用方式,重點(diǎn)研究了納米銀陣列對(duì)三聚氰胺的兩種SERS增強(qiáng)作用機(jī)制:一是基于納米銀棒間“熱點(diǎn)”形成的電磁場(chǎng)局域增強(qiáng),二是基于Ag-Melamine之間電荷轉(zhuǎn)移的化學(xué)增強(qiáng)。論文所得的結(jié)論可為SERS在實(shí)際應(yīng)用中提供科學(xué)參考。論文選取了三聚氰胺、克倫特羅等常見(jiàn)違禁添加物,首次構(gòu)建了飼料中三聚氰胺的兩種SERS快速分析方法。方法一是以均一性良好的AgNR為增強(qiáng)基底,以甲醇為提取凈化溶劑一步法處理,以Δv=682 cm~(-1)處特征拉曼吸收為定性定量峰,檢測(cè)限和定量限分別為0.9,2μg·g~(-1),分析時(shí)間約3 min/樣;二是以AuNPs為增強(qiáng)基底,以pH=3~4 HCl水溶液及混合溶劑(正丁醇:乙酸乙酯,6:1 v/v)為兩相溶劑,兩次液液萃取進(jìn)行樣品前處理,以731 cm~(-1)為歸一化峰,707 cm~(-1)作為定量峰進(jìn)行計(jì)算,檢測(cè)限和定量限分別為0.5,2μg·g~(-1),分析時(shí)間約5 min/樣。論文還建立了動(dòng)物尿液中克倫特羅的SERS快速分析方法,以深度氧化石墨烯負(fù)載納米金為增強(qiáng)體系,利用克倫特羅抗體標(biāo)記磁珠富集凈化尿液中的克倫特羅目標(biāo)物,以Δv=1474 cm~(-1)為定性定量峰,檢測(cè)限和定量限分別為0.5,1 ng·mL~(-1),分析時(shí)間約15 min/樣。建立的三套SERS速測(cè)方法為飼料和畜產(chǎn)品質(zhì)量安全監(jiān)管提供技術(shù)支撐。
[Abstract]:At present, feed and animal products quality and safety analysis technology needs to be supplemented and improved. Surface enhanced Raman spectroscopy based on nanostructures has been developed rapidly, among which many technical difficulties are faced, such as homogeneity of substrate, enhancement of signal stability and targeted enrichment of target molecules. If SERS technology is introduced into the field of fast analysis of feed and livestock products, it will be a great leap forward to solve the key technical problems. In this paper, three kinds of SERS enhanced substrates, such as deep graphene oxide supported nano-gold complex, nano-silver array and nano-gold sol, were prepared. Their optical properties, stability, homogeneity and enhancement activity were studied, and the key preparation parameters were investigated. The regulation of morphology parameters on the performance of substrate enhancement reveals the key factors and control methods that affect the stability of substrate enhancement signal. Taking the nano-silver array as an example, the system properties and action modes of the key structure of melamine on the surface of the nano-silver array are expounded in this paper. Two kinds of SERS enhancement mechanisms of nano-silver arrays on melamine are studied: one is based on the local enhancement of electromagnetic field formed by "hot spot" between silver nanorods, the other is based on the chemical enhancement of charge transfer between Ag-Melamine. The conclusion can provide scientific reference for the application of SERS. In this paper, melamine, clenbuterol and other common prohibited additives were selected, and two rapid SERS analysis methods of melamine in feed were constructed for the first time. The first method was to take the homogeneous AgNR as the enhanced substrate, methanol as the extraction solvent, and the characteristic Raman absorption as the qualitative and quantitative peak. The detection limit and the quantitative limit were 0.9 ~ 2 渭 g / g, respectively, and the analytical time was about 3 min/. The results were as follows: (1) the analytical time was about 3 min/, and the detection limit and the quantitative limit were 0.9 ~ 2 渭 g / g ~ (-1) ~ (-1), respectively, with the characteristic Raman absorption at 螖 V ~ (682) cm ~ (-1). Secondly, the AuNPs was used as the enhancement substrate, the pH ~ (3 +) ~ (4) HCl solution and the mixed solvent (n-butanol: ethyl acetate 6: 1 / v) were used as two-phase solvent, the sample was pretreated by twice liquid-liquid extraction, and the normalized peak of 731 cm ~ (-1) was taken as the peak of 707 cm ~ (-1) as the quantitative peak. The detection limit and the quantitative limit were 0.5 ~ 2 渭 g / g ~ (-1) ~ (-1), respectively, and the analysis time was about 5 min/. A rapid SERS method for the determination of clenbuterol in animal urine was established, in which deep graphene oxide loaded nanocrystalline gold was used as an enhanced system, and clenbuterol antibody was used to label magnetic beads to enrich and purify clenbuterol target in urine. The detection limit and the quantitative limit were 0.5 ~ (1) ng / mL ~ (-1), respectively, and the analytical time was about 15 min/ for the sample with 螖 V ~ (1) 1474 cm ~ (-1) 路m ~ (-1) ~ (-1) as the qualitative and quantitative peak. The established three sets of SERS methods provide technical support for the quality and safety supervision of feed and animal products.
【學(xué)位授予單位】：中國(guó)農(nóng)業(yè)科學(xué)院
【學(xué)位級(jí)別】：博士
【學(xué)位授予年份】：2017
【分類號(hào)】：TB383.1;O657.37

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