本文關(guān)鍵詞：硅基熒光表面印跡復(fù)合材料的制備及其靶向檢測(cè)環(huán)境中擬除蟲(chóng)菊酯的研究　出處：《江蘇大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

  更多相關(guān)文章： 熒光印跡復(fù)合材料 分子印跡技術(shù) 擬除蟲(chóng)菊酯 表面印跡技術(shù) 熒光檢測(cè)

【摘要】：在工業(yè)和農(nóng)業(yè)生產(chǎn)生活中,擬除蟲(chóng)菊酯殺蟲(chóng)劑(Pyrethroid pesticides,PPs)的濫用已導(dǎo)致其在水體中殘留含量嚴(yán)重超標(biāo),危害人體健康和生態(tài)平衡。研究表明在使用PPs防治靶向害蟲(chóng)的同時(shí),還會(huì)對(duì)非靶向生物帶來(lái)較大的危害,如魚(yú)、蝦、蟹等水生物,甚至對(duì)蜜蜂也會(huì)帶來(lái)巨大的傷害,部分PPs殘留會(huì)影響到人類神經(jīng)系統(tǒng)和生殖系統(tǒng)。針對(duì)復(fù)雜環(huán)境中識(shí)別痕量PPs殘留問(wèn)題,探索新型、快速有效、靈敏的檢測(cè)方法已經(jīng)成為當(dāng)務(wù)之急。本課題以熒光識(shí)別技術(shù)為基礎(chǔ)結(jié)合分子印跡技術(shù)的特異選擇性,建立了一種新型選擇性識(shí)別特定目標(biāo)物的熒光分析技術(shù)。選擇窄發(fā)射譜、高熒光量子產(chǎn)率的有機(jī)熒光染料作為熒光團(tuán),選用無(wú)機(jī)納米顆粒為載體,在載體表面上包覆上印跡層,構(gòu)建了一類具有穩(wěn)定性好、快速高效、選擇識(shí)別性熒光印跡復(fù)合材料,來(lái)實(shí)現(xiàn)復(fù)雜環(huán)境中三種殘留PPs(三氟氯氰菊酯LC、高效氟氯氰菊酯BC、氟胺氰菊酯FL)的選擇性識(shí)別。本課題主要開(kāi)展的工作如下:(1)設(shè)計(jì)并使用沉淀聚合制備一種熒光印跡復(fù)合材料來(lái)選擇性識(shí)別環(huán)境水樣中痕量的LC。本研究以納米SiO_2顆粒為基體材料,將熒光單體FITC通過(guò)硅烷偶聯(lián)劑APTS接枝到SiO_2顆粒表面,分別加入模板分子(LC)、功能單體(AM)、交聯(lián)劑(DVB)、引發(fā)劑(AIBN),用沉淀聚合法制備了SiO_2@FITC-APTS@MIPs熒光印跡復(fù)合材料。分別用紅外波譜(FT-IR),熱失重儀器(TGA),掃描電子顯微鏡(SEM)和透射電子顯微鏡(TEM)等表征手段來(lái)對(duì)這種熒光復(fù)合材料進(jìn)行測(cè)試。測(cè)試分析顯示這種熒光復(fù)合材料呈現(xiàn)均勻球形形貌,并具有明顯的核-殼結(jié)構(gòu)(殼厚約為100 nm)。通過(guò)Stern-Volmer公式,建立了熒光強(qiáng)度F與LC濃度C之間的線性關(guān)系,并得到了線性回歸方程F0/F-1=0.0162C+0.0272,檢出限LOD為9.17 nM。(2)采用沉淀聚合法,以KH570修飾的SiO_2為載體材料,模板分子(BC)、熒光功能單體(AF)、交聯(lián)劑(TRIM)、引發(fā)劑(AIBN)在加熱的條件下制備出熒光印跡復(fù)合材料用于選擇性識(shí)別農(nóng)產(chǎn)品水樣中的BC。通過(guò)FT-IR、SEM和TEM等手段對(duì)其形貌特征進(jìn)行了表征,結(jié)果發(fā)現(xiàn)此熒光印跡復(fù)合材料擁有較好的單分散性,以及較薄的印跡聚合層(約50 nm),通過(guò)熒光檢測(cè)和選擇性實(shí)驗(yàn)分析該熒光印跡復(fù)合材料具有良好的選擇識(shí)別性能,在10.11-80 n M范圍內(nèi)具有良好的線性關(guān)系,線性回歸方程為F0/F-1=0.0213C+0.0859,相關(guān)系數(shù)R2=0.9919,LOD=10.11 nM。(3)利用沉淀聚合法在SiO_2-KH570納米粒子表面包覆上一層具有選擇識(shí)別性能的表面分子印跡聚合物層,在反應(yīng)體系中分別加入模板分子(FL)、熒光單體(AF)、功能單體(AM)、交聯(lián)劑(TRIM),在AIBN引發(fā)聚合得到SiO_2-KH570@FL-FMIPs復(fù)合材料用于環(huán)境水樣中痕量FL檢測(cè)識(shí)別。運(yùn)用各種表征手段檢測(cè)展示了其較好的單分散性、穩(wěn)定性和熒光特性,該熒光印跡復(fù)合材料展現(xiàn)了優(yōu)異的選擇識(shí)別能力。通過(guò)熒光識(shí)別技術(shù)和選擇性實(shí)驗(yàn)分析了熒光強(qiáng)度F與FL濃度C在濃度為12.145-120 nM內(nèi)具有良好的線性關(guān)系,并建立了線性回歸方程F0/F-1=0.0164C-0.0067,相關(guān)系數(shù)為0.9975,LOD=12.145 nM。
[Abstract]:In the industrial and agricultural production and life, pyrethroid insecticides (Pyrethroid pesticides PPs) has led to the abuse of residues in water content exceed the standard seriously, endanger human health and ecological balance. The study showed that in the use of PPs control target pests at the same time, but also on the non target biology bring harm, such as fish. Shrimp, crab and other aquatic organisms, and even will bring great harm to the bees, part of the PPs residue will affect the human nervous system and reproductive system. According to the PPs identification in the complex environment of trace residues, to explore a new, rapid and effective, sensitive detection method has become a pressing matter of the moment. A specific and selective subject to the fluorescence based recognition technique combination of molecular imprinting technique, a fluorescent target identification new selective analysis technology. Selection of narrow emission spectra, high fluorescence quantum yield of organic fluorescent dyes as The fluorophore, using the inorganic nanoparticles as the carrier, on the imprinted layer coated on the surface of carrier, constructed a kind of good stability, fast and efficient, selective recognition of fluorescent imprinted composite materials, to achieve three kinds of residual PPs in complex environment (three cyfluthrin LC, Cyhalothrin BC, amine fluoride cypermethrin FL) selective recognition. The main work is as follows: (1) the design and use of polymerization to prepare a fluorescent imprinted composite material to selective recognition of trace LC. in environmental water samples in this study, nano SiO_2 particles as the base material of precipitation, fluorescent monomer FITC by silane coupling agent APTS was grafted to SiO_2 the particle surface, were added to the template molecule (LC), functional monomer (AM), crosslinking agent (DVB), initiator (AIBN), SiO_2@FITC-APTS@MIPs fluorescent imprinted materials were prepared by precipitation polymerization. By using infrared spectroscopy (FT-IR), thermogravimetric instrument (T GA), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) characterization methods to test the fluorescent composites. The test analysis showed that the fluorescent composite showed uniform spherical morphology, and has a clear core-shell structure (the shell thickness is about 100 nm). By using the Stern-Volmer formula, a linear the relationship between the fluorescence intensity and the concentration of LC F C, and obtained the F0/F-1=0.0162C+0.0272 linear regression equation, the detection limit is 9.17 nM. (2 LOD) by precipitation polymerization, modified by KH570 SiO_2 as the carrier material, the template molecule (BC), fluorescent functional monomer (AF), crosslinking agent, initiator (TRIM) (AIBN) prepared by fluorescence imprinted materials for selective recognition of agricultural products in water samples by BC. FT-IR under the condition of heating, its morphology is characterized by SEM and TEM methods. Results showed that the fluorescence of imprinted materials has a good single Dispersion, and thin MIP (about 50 nm), by fluorescence detection and selective experiment analysis of the fluorescence imprinted composite material has good recognition ability, has a good linear relationship in the range of M 10.11-80 n, the linear regression equation was F0/F-1=0.0213C+ 0.0859, the correlation coefficient R2=0.9919, LOD=10.11 (3) by nM. polymerization in coated SiO_2-KH570 nanoparticles on the surface layer has the recognition performance of surface imprinted polymer layer deposition, the template molecules were added in the reaction system (FL), fluorescent monomer (AF), functional monomer (AM), crosslinking agent, initiator (TRIM) SiO_2-KH570@FL-FMIPs composites for trace FL sample detection and recognition in AIBN. Using various characterization methods of detection showed its good monodispersity, stability and fluorescence, the fluorescence imprinted materials displayed an excellent selection of knowledge Other abilities. Through fluorescence recognition technology and selective experiment, the fluorescence intensity F and FL concentration C have a good linear relationship in the concentration of 12.145-120 nM, and a linear regression equation F0/F-1=0.0164C-0.0067 is established, the correlation coefficient is 0.9975, LOD=12.145 nM..

【學(xué)位授予單位】：江蘇大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：X830.2;O631.3

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本文編號(hào)：1438057