荧光智能温度响应聚合物水凝胶微球的制备与性质研究
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摘要
敏感性高分子水凝胶表现出的智能特性,使其在药物释放、生物标记、荧光探针、传感器和仿生人工肌肉等方面具有非常广阔的应用前景。本论文设计制备具有多种功能协同响应性质的聚合物水凝胶纳米材料,以获得高灵敏度、高选择性纳米传感器件。制备了以聚苯乙烯PS为核,聚N-异丙基丙烯酰胺PNIPAM为壳的温敏性核壳水凝胶纳米微球体系。利用配位键作用力将稀土配合物复合进核壳纳米微粒中,制备了具有荧光强度和体积温敏性的智能响应聚合物水凝胶微球。随着环境温度的变化,水凝胶微球的荧光强度在较大温度范围内(10℃-50℃)产生线性响应的规律,且具有可逆回复的光学响应性质。另外,利用库仑将具有聚集诱导荧光发射性能(AIE)有机荧光分子与带电荷的微球壳层进行有效的组装,获得了同时具有AIE性质、荧光功能和体积温敏性的多重协同响应性质的聚合物水凝胶微球。组装后该体系荧光强度增强百倍以上。不需要引入其它外界刺激,仅调节环境温度,即可实现在很大温度范围内(2℃-8℃)对微球荧光强度的线性响应和可逆回复控制。进一步考察了该荧光功能微球与不同离子和生物分子的相互作用而产生的荧光性能响应,结果表明水凝胶微球对阴离子CrO42-具有特异性荧光检测性能,以及对生物大分子的识别功能。另一方面,利用核壳水凝胶纳米微球表面亲疏水性质的温度敏感特性,控制环境温度,在具有亲疏水图案的基片上获得具有荧光发射性质的二维有序图案化组装,开拓多重响应性智能材料体系。
Polymeric materials with responses to external stimuli are of great interest in a number of applications include drug delivery、biolable、bioprobe、thermo-sensor、color-tunable crystals and catalysis. PNIPAM, with a coil-to-globule transition in water at LCST of 32℃, is one of the candidates and has been widely studied most. The coil-to-globule transition of PNIPAM-based responsive system could be a total reversible process.
Sensitive and fast monitoring of temperature change is of great importance to the development of bioprobes、chemical valves、drug delivery systems、chemsensors and switches. Usually, various PL organic molecules, nanocrystals and quantum dots were used to engineer the fluorescent PNIPAM hydrogels. The thermo-responsive fluorescence of the reported PNIPAM-based hydrogels was only active in a very narrow temperature window, which was around the LCST. The sudden change of the emission around the LCST, which was documented as an on-off feature, enables the application limitation of these fluorescent PNIPAM hydrogels. There are outstanding needs for fluorescent PNIPAM hydrogels to response effectively and continuously in a broad temperature window without such an on-off element. Therefore, we prepared hybrid thermo-responsive hydroel nanoparticles with their PL intensity reversible, linear, and sensitive to a broad temperature range. We investigated and characterized the PL thermo-response of the hydrogel nanoparticles and discussed their applications in environmental protection, bioprobe and building of functional patterns.
In Chapter 2, we designed the hard core to be PS-co-PNIPAM and the soft shell PNIPAM, PS-co-PNIPAM/PNIPAM hydrogel core/shell nanoparticles which were prepared by two steps of emulsion-free copolymerization. Water-soluble Europium organic complex was designed to coordinate in the shell of core/shell hydrogel nanoparticles.. Our bright Eu-doped PS-co-PNIPAM/PNIPAM hydrogel nanoparticles were detected to be linear, reversible and sensitive, regarding the emission intensity but with little change in the emission peak position. Their temperature-stimuli PL response in a broad temperature range is considerably different from that of the previously reported PNIPAM hydrogels and should bring insights into a universal approach to function nal hydrogels with reversible and linear responses to external stimuli, such as micro-thermometers、bioprobes、drug delivery、thermosensors and building of functional patterns with light emission.
In Chapter 3, we fabricated the hard core to be PS-co-PNIPAM and the soft shell PNIPAM-AA, PS-co-PNIPAM/PNIPAM hydrogel core/shell nanoparticles.The AA provided the shell of nanoparticles carboxyl group to automatically connected with the AIE-type lumophore, TPE derivative, quaternary ammonium salt 1 by coulomb force. Then the PNIPAM-AA chains could hold the 1 tightly to hamper the freely rotation of the phenyl peripheries. As a result, the amphiphilic 1 at the nanoparticles immediately showed a drastic increase in the PL intensity, more hundreds fold intense than those from 1 solution. Meanwhile, it is remarkable that the PL response of the 1-doped PS-co-PNIPAM/PNIPAM-AA hydrogel nanoparticles is reversible and sensitive to temperature-stimuli which are considerably different from that of the previously reported fluorescent AIE molecules、crystals or films.
Furthermore, the nanoparticles with special structures endowed the AIE molecule 1 with bright and controllable PL uniformly dispersed in either polar solution or nonpolar solution. The hydrogel nanoparticles served as a suitable carrier may greatly expand practicality and applicability of the AIE molecules at nanoscale. These novel PL nanoparticles doped with 1 with linear reversible and temperature-sensitivity in a broad temperature range (2℃-80℃) is of great importance to the development of micro-thermometer、explosive detection、biological probing、biological imaging、FL sensors and drug delivery.
In Chapter 4, we systematically investigated the PL responses of 1-doped PS-co-PNIPAM/PNIPAM-AA hydrogel nanoparticles to CrO42- selectively at different temperature.The detection of CrO2- is important as the ion can be carried into humban beings cells and cause oxidative damage to DNA. The ion may also be introduced into drinking water through environmental pollution. The analysis showed that the PL intensity of hydrogel core/shell nanoparticles is sensitively weakened by the addition of a small amount of CrO42- in aqueous media. The PL intensity is decreased progressively with an increase in the amount of added CrO42- with highly selective, reached the discharge standard of national wastewater discharge requirements GB8978-1996 of the highest total chromium (1.5 mg/1 level). The PL intensity of the mixed solution decreased with the increase of temperature. The PL thermo-responsive plots showed that the sensitivity of PL intensity to CrO42- at low temperature was higer than at high temperature. It will be very useful in fast sensitively environmental detection, industrial wastewater discharge and water protection.
Meanwhile, we investigated the behavior of 1-doped PS-co-PNIPAM/PNIPAM-AA hydrogel nanoparticles as a bioprobe and to find bioprobing systems with higher sensitivities. In BSA、DNA and RNA solutions of the same concentration, all the PL intensity of the solutions decreased. But the PL intensity of RNA mixed solution decreased more than the other two sample above, revealing that the hybrid hydrogel nanoparticles showed higher sensitivity to RNA. Although the PL intensity of the mixed biomolecular solution decreased with the increase of temperature, the PL thermo-response could only be achieved at lower temperature ( On the other hand, we introduce a new approach to prepare a large-area array of specifically periodical regions through assemble of Eu-doped PS-co-PNIPAM/PNIPAM hydrogel nanoparticles, only by controlling environment temperature. Surface property of the particles shells undergoes a hydrophilic to hydrophobic transition below and above LCST. Several drops of latex containing particles spread on a HDT and MHA modified substrate which had a periodical alternative hydrophilic and hydrophobic strips pattern. Large-area two-dimensional assemble with red light emission were obtained simply after drying of water.
Polymeric materials with responses to external stimuli are of great interest in a number of applications include drug delivery、biolable、bioprobe、thermo-sensor、color-tunable crystals and catalysis. PNIPAM, with a coil-to-globule transition in water at LCST of 32℃, is one of the candidates and has been widely studied most. The coil-to-globule transition of PNIPAM-based responsive system could be a total reversible process.
Sensitive and fast monitoring of temperature change is of great importance to the development of bioprobes、chemical valves、drug delivery systems、chemsensors and switches. Usually, various PL organic molecules, nanocrystals and quantum dots were used to engineer the fluorescent PNIPAM hydrogels. The thermo-responsive fluorescence of the reported PNIPAM-based hydrogels was only active in a very narrow temperature window, which was around the LCST. The sudden change of the emission around the LCST, which was documented as an on-off feature, enables the application limitation of these fluorescent PNIPAM hydrogels. There are outstanding needs for fluorescent PNIPAM hydrogels to response effectively and continuously in a broad temperature window without such an on-off element. Therefore, we prepared hybrid thermo-responsive hydroel nanoparticles with their PL intensity reversible, linear, and sensitive to a broad temperature range. We investigated and characterized the PL thermo-response of the hydrogel nanoparticles and discussed their applications in environmental protection, bioprobe and building of functional patterns.
In Chapter 2, we designed the hard core to be PS-co-PNIPAM and the soft shell PNIPAM, PS-co-PNIPAM/PNIPAM hydrogel core/shell nanoparticles which were prepared by two steps of emulsion-free copolymerization. Water-soluble Europium organic complex was designed to coordinate in the shell of core/shell hydrogel nanoparticles.. Our bright Eu-doped PS-co-PNIPAM/PNIPAM hydrogel nanoparticles were detected to be linear, reversible and sensitive, regarding the emission intensity but with little change in the emission peak position. Their temperature-stimuli PL response in a broad temperature range is considerably different from that of the previously reported PNIPAM hydrogels and should bring insights into a universal approach to function nal hydrogels with reversible and linear responses to external stimuli, such as micro-thermometers、bioprobes、drug delivery、thermosensors and building of functional patterns with light emission.
In Chapter 3, we fabricated the hard core to be PS-co-PNIPAM and the soft shell PNIPAM-AA, PS-co-PNIPAM/PNIPAM hydrogel core/shell nanoparticles.The AA provided the shell of nanoparticles carboxyl group to automatically connected with the AIE-type lumophore, TPE derivative, quaternary ammonium salt 1 by coulomb force. Then the PNIPAM-AA chains could hold the 1 tightly to hamper the freely rotation of the phenyl peripheries. As a result, the amphiphilic 1 at the nanoparticles immediately showed a drastic increase in the PL intensity, more hundreds fold intense than those from 1 solution. Meanwhile, it is remarkable that the PL response of the 1-doped PS-co-PNIPAM/PNIPAM-AA hydrogel nanoparticles is reversible and sensitive to temperature-stimuli which are considerably different from that of the previously reported fluorescent AIE molecules、crystals or films.
Furthermore, the nanoparticles with special structures endowed the AIE molecule 1 with bright and controllable PL uniformly dispersed in either polar solution or nonpolar solution. The hydrogel nanoparticles served as a suitable carrier may greatly expand practicality and applicability of the AIE molecules at nanoscale. These novel PL nanoparticles doped with 1 with linear reversible and temperature-sensitivity in a broad temperature range (2℃-80℃) is of great importance to the development of micro-thermometer、explosive detection、biological probing、biological imaging、FL sensors and drug delivery.
In Chapter 4, we systematically investigated the PL responses of 1-doped PS-co-PNIPAM/PNIPAM-AA hydrogel nanoparticles to CrO42- selectively at different temperature.The detection of CrO2- is important as the ion can be carried into humban beings cells and cause oxidative damage to DNA. The ion may also be introduced into drinking water through environmental pollution. The analysis showed that the PL intensity of hydrogel core/shell nanoparticles is sensitively weakened by the addition of a small amount of CrO42- in aqueous media. The PL intensity is decreased progressively with an increase in the amount of added CrO42- with highly selective, reached the discharge standard of national wastewater discharge requirements GB8978-1996 of the highest total chromium (1.5 mg/1 level). The PL intensity of the mixed solution decreased with the increase of temperature. The PL thermo-responsive plots showed that the sensitivity of PL intensity to CrO42- at low temperature was higer than at high temperature. It will be very useful in fast sensitively environmental detection, industrial wastewater discharge and water protection.
Meanwhile, we investigated the behavior of 1-doped PS-co-PNIPAM/PNIPAM-AA hydrogel nanoparticles as a bioprobe and to find bioprobing systems with higher sensitivities. In BSA、DNA and RNA solutions of the same concentration, all the PL intensity of the solutions decreased. But the PL intensity of RNA mixed solution decreased more than the other two sample above, revealing that the hybrid hydrogel nanoparticles showed higher sensitivity to RNA. Although the PL intensity of the mixed biomolecular solution decreased with the increase of temperature, the PL thermo-response could only be achieved at lower temperature (
引文
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