二氧化硅納米棒的制備、熒光功能化及其在免疫檢測(cè)中的應(yīng)用
發(fā)布時(shí)間：2018-08-21 13:08
【摘要】：一維二氧化硅納米材料由于具有各向異性的結(jié)構(gòu)、大的長(zhǎng)徑比和表面易功能化等優(yōu)點(diǎn),使其在生物檢測(cè)、藥物運(yùn)輸和疾病治療等生物醫(yī)學(xué)領(lǐng)域展現(xiàn)了廣闊的應(yīng)用前景。截止目前,相比于球形納米材料,一維二氧化硅納米材料的發(fā)展依舊十分緩慢,制備形貌、尺寸和化學(xué)組成精確可控的一維二氧化硅納米材料還存在一定的技術(shù)壁壘,限制了一維二氧化硅納米材料的開(kāi)發(fā)與應(yīng)用。為此,本論文設(shè)計(jì)并采用了一種簡(jiǎn)單、高效的一鍋合成法,利用聚乙烯吡咯烷酮、檸檬酸鈉、戊醇和水構(gòu)建反相微乳液體系,以硅酸乙酯(TEOS)作為硅源,在氨水催化下制備了長(zhǎng)徑比和紅外吸收指紋信號(hào)精確可調(diào)的一維二氧化硅納米棒,系統(tǒng)研究了其形成機(jī)理,實(shí)現(xiàn)了基于二氧化硅納米棒形狀信息和紅外吸收指紋信號(hào)的雙模超靈敏免疫檢測(cè);并將該方法拓展至熒光二氧化硅納米棒的制備,實(shí)現(xiàn)了超靈敏熒光免疫檢測(cè)。主要研究?jī)?nèi)容如下:(1)針對(duì)現(xiàn)有合成方法難以精確、便捷調(diào)控二氧化硅納米棒長(zhǎng)徑比及其相關(guān)特性的問(wèn)題,我們?cè)O(shè)計(jì)并采用了簡(jiǎn)單的一鍋反相微乳液合成法,在4小時(shí)、靜置條件下成功制備了二氧化硅納米棒。通過(guò)控制反應(yīng)體系中氨水的濃度,實(shí)現(xiàn)了二氧化硅納米棒長(zhǎng)徑比1.0到11.6的精確調(diào)控。TEOS的消耗速率、反應(yīng)溶液電導(dǎo)率及紅外吸收光譜分析表明,二氧化硅納米棒的形貌、尺寸、橫光學(xué)波(TO)和縱光學(xué)波(LO)紅外光譜指紋信號(hào)是由TEOS的水解和縮合反應(yīng)速率共同決定的。我們構(gòu)建了三明治型免疫檢測(cè)器件,開(kāi)發(fā)了基于二氧化硅納米棒的雙模免疫檢測(cè):利用二氧化硅納米棒獨(dú)特的、在光學(xué)顯微鏡下易識(shí)別的形狀信息,實(shí)現(xiàn)了目標(biāo)蛋白的快速篩查及半定量檢測(cè);利用其TO、LO紅外光譜指紋信號(hào),實(shí)現(xiàn)了目標(biāo)蛋白的準(zhǔn)確、超靈敏定量檢測(cè),檢測(cè)下限可以達(dá)到0.5 pM,線性檢測(cè)區(qū)間為1 pM到10 nM。該研究為推進(jìn)一維二氧化硅納米材料的工業(yè)化生產(chǎn),加快其實(shí)用化進(jìn)程開(kāi)辟了新道路。(2)為了驗(yàn)證一鍋反相微乳液合成法的普適性,實(shí)現(xiàn)二氧化硅納米棒的熒光功能化拓展,我們選用了光化學(xué)性質(zhì)相對(duì)穩(wěn)定的傒四羧酸二酐與氨基硅烷反應(yīng),制得了傒硅烷衍生物,以其和TEOS為硅源,利用一鍋反相微乳液合成法,成功制備了熒光二氧化硅納米棒。由于傒染料是以共價(jià)鍵的形式連接到二氧化硅納米棒的結(jié)構(gòu)中,因此有效解決了染料的泄露問(wèn)題,提高了染料的光穩(wěn)定性。通過(guò)控制反應(yīng)過(guò)程中氨水的濃度、反應(yīng)時(shí)間和反應(yīng)溫度,實(shí)現(xiàn)了熒光二氧化硅納米棒長(zhǎng)徑比由1.0到13.4的精確調(diào)控。我們構(gòu)建了三明治免疫檢測(cè)器件,利用熒光二氧化硅納米棒的熒光信號(hào)作為檢測(cè)信號(hào),實(shí)現(xiàn)了目標(biāo)蛋白高靈敏度、高穩(wěn)定性和高特異性的檢測(cè),檢測(cè)下限為0.3 pM,線性區(qū)間為1 pM到20 nM。這種一鍋反相微乳液合成法有望推廣用于二氧化硅納米棒其它相關(guān)材料體系的制備。
[Abstract]:Due to its anisotropic structure, large aspect ratio and easy surface functionalization, one-dimensional silica nanomaterials have been widely used in biomedical fields such as biological detection, drug transportation and disease treatment. Up to now, compared with spherical nanomaterials, the development of one-dimensional silica nanomaterials is still very slow, and there are still some technical barriers to the preparation of one-dimensional silica nanomaterials with precise and controllable morphology, size and chemical composition. The development and application of one-dimensional silica nanomaterials are limited. In this paper, a simple and efficient one-pot synthesis method was designed and used to construct reverse microemulsion system using polyvinylpyrrolidone, sodium citrate, pentanol and water. Ethyl silicate (TEOS) was used as silicon source. One-dimensional silica nanorods with precise aspect ratio and infrared absorption fingerprint signal were prepared under the catalysis of ammonia. The formation mechanism of the nanorods was systematically studied. The double mode hypersensitive immunoassay based on the shape information of silica nanorods and infrared fingerprint signal was realized, and the method was extended to the preparation of fluorescent silica nanorods, and the hypersensitive fluorescence immunoassay was realized. The main research contents are as follows: (1) in order to control the aspect ratio of silicon dioxide nanorods and its related characteristics, we designed and adopted a simple one-pot reverse microemulsion synthesis method in 4 hours. Silica nanorods were successfully prepared under static conditions. By controlling the concentration of ammonia in the reaction system, the consumption rate of TEOS was accurately regulated by the aspect ratio between 1.0 and 11.6 of silica nanorods. The conductivity of the reaction solution and the infrared absorption spectrum analysis showed that the morphology and size of SiO2 nanorods were obtained. The infrared fingerprint signals of transverse optical wave (TO) and longitudinal optical wave (LO) are determined by the rate of hydrolysis and condensation of TEOS. We built a sandwich immune detector and developed a dual-mode immunoassay based on silica nanorods: shape information that is unique to silica nanorods and easily recognized under optical microscopy. The fast screening and semi-quantitative detection of target protein were realized, and the accurate and hypersensitive quantitative detection of target protein was realized by using its TOLO IR fingerprint signal. The detection limit could reach 0.5 pm, and the linear detection range was from 1 pm to 10 nm. This research has opened up a new way to promote the industrial production of one-dimensional silica nanomaterials and speed up its practical process. (2) in order to verify the universality of one-pot reverse microemulsion synthesis method, the fluorescent functionalization of silica nanorods can be expanded. The siloxane derivatives were prepared by the reaction of tetracarboxylic anhydride with aminosilane, which has relatively stable photochemical properties. The fluorescent silica nanorods were successfully prepared by one-pot reverse microemulsion synthesis with TEOS as the silicon source. Because the dyes are connected to the structure of silica nanorods in the form of covalent bonds, the problem of dye leakage is effectively solved and the photostability of the dyes is improved. By controlling the concentration of ammonia water, reaction time and reaction temperature, the ratio of length to diameter of fluorescent silica nanorods from 1.0 to 13.4 was achieved. A sandwich immunodetector was constructed, and the fluorescence signal of fluorescent silica nanorods was used as the detection signal. The target protein was detected with high sensitivity, high stability and high specificity. The detection limit is 0.3 pm and the linear range is from 1 pm to 20 nm. The one-pot reverse microemulsion synthesis method is expected to be used in the preparation of silica nanorods.
【學(xué)位授予單位】：東北師范大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：TB383.1;O657.3
[Abstract]:Due to its anisotropic structure, large aspect ratio and easy surface functionalization, one-dimensional silica nanomaterials have been widely used in biomedical fields such as biological detection, drug transportation and disease treatment. Up to now, compared with spherical nanomaterials, the development of one-dimensional silica nanomaterials is still very slow, and there are still some technical barriers to the preparation of one-dimensional silica nanomaterials with precise and controllable morphology, size and chemical composition. The development and application of one-dimensional silica nanomaterials are limited. In this paper, a simple and efficient one-pot synthesis method was designed and used to construct reverse microemulsion system using polyvinylpyrrolidone, sodium citrate, pentanol and water. Ethyl silicate (TEOS) was used as silicon source. One-dimensional silica nanorods with precise aspect ratio and infrared absorption fingerprint signal were prepared under the catalysis of ammonia. The formation mechanism of the nanorods was systematically studied. The double mode hypersensitive immunoassay based on the shape information of silica nanorods and infrared fingerprint signal was realized, and the method was extended to the preparation of fluorescent silica nanorods, and the hypersensitive fluorescence immunoassay was realized. The main research contents are as follows: (1) in order to control the aspect ratio of silicon dioxide nanorods and its related characteristics, we designed and adopted a simple one-pot reverse microemulsion synthesis method in 4 hours. Silica nanorods were successfully prepared under static conditions. By controlling the concentration of ammonia in the reaction system, the consumption rate of TEOS was accurately regulated by the aspect ratio between 1.0 and 11.6 of silica nanorods. The conductivity of the reaction solution and the infrared absorption spectrum analysis showed that the morphology and size of SiO2 nanorods were obtained. The infrared fingerprint signals of transverse optical wave (TO) and longitudinal optical wave (LO) are determined by the rate of hydrolysis and condensation of TEOS. We built a sandwich immune detector and developed a dual-mode immunoassay based on silica nanorods: shape information that is unique to silica nanorods and easily recognized under optical microscopy. The fast screening and semi-quantitative detection of target protein were realized, and the accurate and hypersensitive quantitative detection of target protein was realized by using its TOLO IR fingerprint signal. The detection limit could reach 0.5 pm, and the linear detection range was from 1 pm to 10 nm. This research has opened up a new way to promote the industrial production of one-dimensional silica nanomaterials and speed up its practical process. (2) in order to verify the universality of one-pot reverse microemulsion synthesis method, the fluorescent functionalization of silica nanorods can be expanded. The siloxane derivatives were prepared by the reaction of tetracarboxylic anhydride with aminosilane, which has relatively stable photochemical properties. The fluorescent silica nanorods were successfully prepared by one-pot reverse microemulsion synthesis with TEOS as the silicon source. Because the dyes are connected to the structure of silica nanorods in the form of covalent bonds, the problem of dye leakage is effectively solved and the photostability of the dyes is improved. By controlling the concentration of ammonia water, reaction time and reaction temperature, the ratio of length to diameter of fluorescent silica nanorods from 1.0 to 13.4 was achieved. A sandwich immunodetector was constructed, and the fluorescence signal of fluorescent silica nanorods was used as the detection signal. The target protein was detected with high sensitivity, high stability and high specificity. The detection limit is 0.3 pm and the linear range is from 1 pm to 20 nm. The one-pot reverse microemulsion synthesis method is expected to be used in the preparation of silica nanorods.
【學(xué)位授予單位】：東北師范大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：TB383.1;O657.3
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