高性能肌酐吸附材料的制备及吸附特性研究
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摘要
目前，由各种肾脏病所导致的肾脏主要功能渐进性不可逆性减退，即慢性肾衰竭，已成为世界范围内继心脑血管疾病、肿瘤和糖尿病后严重威胁人类健康的一大公害，当肾脏功能完全丧失后，慢性肾衰竭便最终导致尿毒症。肾脏在人体新陈代谢中具有十分重要的作用，肾病患者因肾功能低下或衰竭，在血液中会积累大量包括肌酐（Creatinine）在内的毒性成分，这些毒素严重威胁患者生命。过量的肌酐不仅引起患者的一系列中毒症状，而且还可能进一步加速肾衰竭进程，所以有效地去除病患者体内的过量肌酐，对于人体的健康起着十分重要的作用。因此，研究制备性能良好的肌酐吸附材料，采用血液灌流等血液净化技术，有效清除病患者机体内积累的肌酐，在医学研究领域有着重大的科学意义。
本课题通过精心的分子设计，以具有生物相容性的交联聚乙烯醇（CPVA）微球为出发物质，使交联聚乙烯醇微球表面的羟基与溶液中的铈盐构成氧化还原引发体系，采用表面引发接枝聚合方法，在CPVA微球表面分别接枝聚合甲基丙烯酸（MAA）和对苯乙烯磺酸钠（SSS），制备了两种对肌酐具有强吸附性能的接枝微球CPVA-g-PMAA和CPVA-g-PSSS；还以对苯乙烯磺酸钠为功能单体，采用新的分子表面印迹技术，制备了对肌酐具有特异识别选择性与优良的结合亲和性的肌酐分子表面印迹材料MIP-PSSS/CPVA，较深入地考察研究了上述三种医用高分子材料对肌酐分子的吸附特性及吸附机理，取得了十分满意的研究结果，有望在血液净化治疗技术中发挥积极的作用。
首先，通过以戊二醛为交联剂，在悬浮体系中使用直接交联成球的方法，制备交联聚乙烯醇微球CPVA。在此基础上，利用微球表面的大量羟基，与铈盐构成氧化还原型引发体系，成功地实现了甲基丙烯酸（MAA）在微球表面的接枝聚合，制得了接枝微球CPVA-g-PMAA；采用红外光谱仪（FTIR）、扫描电子显微镜（SEM）、化学分析等多种手段，对接枝微球CPVA-g-PMAA的化学结构、形貌特征和表面电性能进行了表征；考察研究了各种主要因素对接枝聚合反应的影响，深入探讨了接枝聚合反应的机理，优化了反应条件。研究结果表明，接枝微球CPVA-g-PMAA的形成符合铈盐引发的接枝聚合反应的特点，适宜的反应条件为：温度为45℃，时间6h，铈盐浓度4.9×10-3mol·L~(-1)、硫酸浓度0.17mol·L~(-1)、单体浓度0.54mol·L~(-1)。在此条件下可以制得接枝度为30g/100g的接枝微球CPVA-g-PMAA。
接着，本研究以接枝微球CPVA-g-PMAA作为吸附材料，详细考察了其对肌酐的吸附性能，深入研究了接枝微球CPVA-g-PMAA对肌酐的吸附机理与吸附热力学。研究结果表明，凭接枝微球CPVA-g-PMAA表面的羧基与肌酐分子之间的强静电相互作用（辅助以氢键相互作用），导致其对肌酐分子表现出很强的吸附能力，当pH=8.0时，吸附容量具有最大值，可达40mg·g~(-1)；接枝微球CPVA-g-PMAA对肌酐的吸附为放热过程，且是焓驱动的过程；体系中电解质的存在影响吸附性能，随着体系中离子浓度的增加，吸附量减小。
本文也以对苯乙烯磺酸钠作为功能单体，研究制备了接枝微球CPVA-g-PSSS；采用红外光谱仪（FTIR）、扫描电子显微镜（SEM）、化学分析等多种手段表征了接枝微球CPVA-g-PSSS的化学结构、形貌特征和表面电性能；也以接枝微球CPVA-g-PSSS作为吸附材料，详细考察了其对肌酐的吸附性能，深入研究了吸附机理与吸附热力学。研究结果表明，在适宜的反应条件下，可制得接枝度为16g/100g的接枝微球CPVA-g-PSSS。凭接接枝微球CPVA-g-PSSS表面的磺酸根与肌酐分子之间的强静电相互作用，接枝微球CPVA-g-PSSS对肌酐分子表现出很强的吸附能力，介质的pH值越小，吸附容量越高，当pH=1.0时，吸附容量可达15.65mg·g~(-1)。接枝微球CPVA-g-PSSS对肌酐的吸附亦为放热过程，且是焓驱动的过程；并且随着体系中离子浓度的增加，吸附量减小。
最后，本研究基于“表面引发接枝聚合”，在水溶液体系中，以肌酐为模板分子，利用铈盐与羟基构成的氧化-还原引发体系，以SSS为功能单体，N,N′-亚甲基双丙烯酰胺（MBA）为交联剂，通过表面引发接枝聚合方式，实施了肌酐分子的表面印迹，制备了肌酐分子表面印迹微球材料MIP-PSSS/CPVA。以N-羟基琥珀酰亚胺（N-Hy）和肌酸（Cr）为对比物质，详细考察研究了表面印迹材料MIP-PSSS/CPVA对肌酐分子识别特性与结合性能。相对于N-Hy和Cr分子，印迹微球MIP-PSSS/CPVA对CR分子的选择性系数分别为5.51、6.30，显示出很高的识别选择性。
After cardiovascular disease, tumor and diabete, at present, the renal main functionprogressive irreversible decline caused by various kidney diseases, namely chronic renalfailure, has become a great nuisance that has serious threat to human health in the world, andit will transform into uremia as the liver loses its ability completely. The kidney plays animportant rule in the body's metabolism. The toxic sunstances including creatinine will beaccumulated extensively in human blood of kidney disease patients owing to kidney functiondecrease and kidney failure, and it seriously threaten patient's life. The excess creatinine notonly will cause a range of symptoms of poisoning, but also it will accelerate the process ofkidney failure. Therefore, it is very significant to effectively remove the excess creatinine inhuman blood of kidney disease patients. Consequently, it has important science significancein medical research area to research and prepare creatinine-adsobting materials with highperformance and to remove the creatinine accumulated in the body of kidney disease patientsby using blood purification techniquessuch as perfusion technique.
In this work, via elaborate molecular designing, crosslinking polyvinyl alcohol (CPVA)microspheres that have biocompatibility were used as the starting substance, and two graftedmicrospheres that have strong adsorption ability for creatinine were successfully prepared. Aredox initiating system was consisted of the hydroxyl groups on CPVA microspheres and theceric salt in the solution, and the two functional monomers, methacrylic acid (MAA) andsodium styrene sulfonate (SSS), were graft-polymerized onto CPVA microspheres throughsurface-initiated graft-polymerization method, respectively, resulting in two graftedmicrospheres, CPVA-g-PMAA and CPVA-g-PSSS. Besides, a creatinine molecule-imprintedmaterial MIP-PSSS/CPVA, which has special molecular recognition selectivity and excellentbinding affinity for creatinine, was also prepared with SSS as the functional monomer and creatinine as template and by using a novel molecular surface-impriting technique. Theadsorption characters and mechanisms of the above three medical macromolecular materialtowards creatinine were investigated in depth, and the satisfactory study results were achived.These materials are promising in the blood purification application.
Crosslinked polyvinyl alcohol (CPVA) microspheres were first prepared by usingdirectly crosslinking-balling method in a suspension system and with glutaraldehyde ascrosslinking agent. On that basis, a redox initiation system was constructed with a great dealof hydroxyl group on CPVA microspheres and cerium ammonium sulfate, and thesurface-initiated graft polymerization of methacrylic acid (MAA) was performed in anaqueous solution, resulting in the grafted microspheres CPVA-g-PMAA. The chemicalstructure and physicochemistry characters were adequately characterized with infraredspectrum (FTIR), scanning electron microscope (SEM) and zeta potential determination.Theeffects of the main factors on the graft polymerization were examined, and the mechanism ofthe graft-polymerization was explored, and the conditions of the graft-polymerization wereoptimized. The experimental results show that hydroxyl group-cerium salt redox initiationsystem can effectively initiates the graft polymerization of MAA on CPVA microspheresunder the suitable conditions such as at45℃, at a cerium salt concentration of4.9×10-3mol·L~(-1), at a sulfuric acid concentration of0.17mol·L~(-1)and at a MAA concentration of0.55mol·L~(-1), and the grafted microspheres CPVA-g-PMAA with a PMAA grafting degree of30g/100g can be prepared.
Then the adsorption property of the grafted microspheres CPVA-g-PMAA for creatininewas examined in more detail, and the adsorption mechanism and thermodynamics werestudied. The experimental results show that there exist strong interactions, electrostaticinteraction (main action force) and hydrogen bonding (a supporting role) between the graftedmicrospheres CPVA-g-PMAA and creatinine molecule, and it lead to that the graftedmicrospheres display very strong adsorption ability towards creatinine. As pH=8.0, theadsorption capacity has a maximum value,40mg·g~(-1). The adsorption process is exothermic,and it is driven by enthalpy. The presence of electrolyte in the solution affects negatively the adsorption property of the grafted microspheres CPVA-g-PMAA, and the adsorption capacitydecreases with the increase of the ion concentration.
In this work, another kinds of grafted microspheres, CPVA-g-PSSS, were also preparedwith the surface-initiated graft-polymerization method and with SSS monomer. The chemicalstructure, morphology character and the surface electrical property of the graftedmicrospheres CPVA-g-PSSS were characterized by using several means such as FTIR, SEMand zeta potential determination. The adsorption ability, mechanism and adsorption of thegrafted microspheres CPVA-g-PSSS for creatinine were also examined and reseached indepth. The study results show that under the suitable conditions the grafted microspheresCPVA-g-PSSS with a grafting degree of16g/100g can be smoothfully prepared. By right ofthe strong electrostatic interaction between the sulfonate groups of the grafted microspheresCPVA-g-PSSS and creatinine molecule, the microspheres CPVA-g-PSSS can produce verystrong adsorption ability. The adsorption capacity is pH-dependent, and the greater theadsorption capacity, the lower the pH value. At pH=1, the adsorption capacity can reach15.65mg·g~(-1). The adsorption of the microspheres CPVA-g-PSSS for creatinine is also anexothermic process, and this process is also drived by enthalpy.
Finally, based on “surface-initiated graft-polymerization”, in an aqueous solution system,creatinine molecule-surface imprinting was conducted with SSS as monomer and N,N'-methylene-bis-acrylamide (MBA) as crosslingking agent by using hydroxyl-ceric saltredox ionitiating system and SSS, and the imprinted microspheres MIP-PSSS/CPVA wereobtained. With N-hydroxysuccinimide (N-Hy) and creatine (Cr) as two contrast substances,the recognition character and binding property of the creatinine molecule-surface imprintedmaterial MIP-PSSS/CPVA for creatinine were researched detailedly. The selectivitycoefficients of MIP-PSSS/CPVA for creatinine relative to the contrast substances, N-Hy andCr, are5.51and6.60, respectively, displaying high recognition selectivity.
本课题通过精心的分子设计，以具有生物相容性的交联聚乙烯醇（CPVA）微球为出发物质，使交联聚乙烯醇微球表面的羟基与溶液中的铈盐构成氧化还原引发体系，采用表面引发接枝聚合方法，在CPVA微球表面分别接枝聚合甲基丙烯酸（MAA）和对苯乙烯磺酸钠（SSS），制备了两种对肌酐具有强吸附性能的接枝微球CPVA-g-PMAA和CPVA-g-PSSS；还以对苯乙烯磺酸钠为功能单体，采用新的分子表面印迹技术，制备了对肌酐具有特异识别选择性与优良的结合亲和性的肌酐分子表面印迹材料MIP-PSSS/CPVA，较深入地考察研究了上述三种医用高分子材料对肌酐分子的吸附特性及吸附机理，取得了十分满意的研究结果，有望在血液净化治疗技术中发挥积极的作用。
首先，通过以戊二醛为交联剂，在悬浮体系中使用直接交联成球的方法，制备交联聚乙烯醇微球CPVA。在此基础上，利用微球表面的大量羟基，与铈盐构成氧化还原型引发体系，成功地实现了甲基丙烯酸（MAA）在微球表面的接枝聚合，制得了接枝微球CPVA-g-PMAA；采用红外光谱仪（FTIR）、扫描电子显微镜（SEM）、化学分析等多种手段，对接枝微球CPVA-g-PMAA的化学结构、形貌特征和表面电性能进行了表征；考察研究了各种主要因素对接枝聚合反应的影响，深入探讨了接枝聚合反应的机理，优化了反应条件。研究结果表明，接枝微球CPVA-g-PMAA的形成符合铈盐引发的接枝聚合反应的特点，适宜的反应条件为：温度为45℃，时间6h，铈盐浓度4.9×10-3mol·L~(-1)、硫酸浓度0.17mol·L~(-1)、单体浓度0.54mol·L~(-1)。在此条件下可以制得接枝度为30g/100g的接枝微球CPVA-g-PMAA。
接着，本研究以接枝微球CPVA-g-PMAA作为吸附材料，详细考察了其对肌酐的吸附性能，深入研究了接枝微球CPVA-g-PMAA对肌酐的吸附机理与吸附热力学。研究结果表明，凭接枝微球CPVA-g-PMAA表面的羧基与肌酐分子之间的强静电相互作用（辅助以氢键相互作用），导致其对肌酐分子表现出很强的吸附能力，当pH=8.0时，吸附容量具有最大值，可达40mg·g~(-1)；接枝微球CPVA-g-PMAA对肌酐的吸附为放热过程，且是焓驱动的过程；体系中电解质的存在影响吸附性能，随着体系中离子浓度的增加，吸附量减小。
本文也以对苯乙烯磺酸钠作为功能单体，研究制备了接枝微球CPVA-g-PSSS；采用红外光谱仪（FTIR）、扫描电子显微镜（SEM）、化学分析等多种手段表征了接枝微球CPVA-g-PSSS的化学结构、形貌特征和表面电性能；也以接枝微球CPVA-g-PSSS作为吸附材料，详细考察了其对肌酐的吸附性能，深入研究了吸附机理与吸附热力学。研究结果表明，在适宜的反应条件下，可制得接枝度为16g/100g的接枝微球CPVA-g-PSSS。凭接接枝微球CPVA-g-PSSS表面的磺酸根与肌酐分子之间的强静电相互作用，接枝微球CPVA-g-PSSS对肌酐分子表现出很强的吸附能力，介质的pH值越小，吸附容量越高，当pH=1.0时，吸附容量可达15.65mg·g~(-1)。接枝微球CPVA-g-PSSS对肌酐的吸附亦为放热过程，且是焓驱动的过程；并且随着体系中离子浓度的增加，吸附量减小。
最后，本研究基于“表面引发接枝聚合”，在水溶液体系中，以肌酐为模板分子，利用铈盐与羟基构成的氧化-还原引发体系，以SSS为功能单体，N,N′-亚甲基双丙烯酰胺（MBA）为交联剂，通过表面引发接枝聚合方式，实施了肌酐分子的表面印迹，制备了肌酐分子表面印迹微球材料MIP-PSSS/CPVA。以N-羟基琥珀酰亚胺（N-Hy）和肌酸（Cr）为对比物质，详细考察研究了表面印迹材料MIP-PSSS/CPVA对肌酐分子识别特性与结合性能。相对于N-Hy和Cr分子，印迹微球MIP-PSSS/CPVA对CR分子的选择性系数分别为5.51、6.30，显示出很高的识别选择性。
After cardiovascular disease, tumor and diabete, at present, the renal main functionprogressive irreversible decline caused by various kidney diseases, namely chronic renalfailure, has become a great nuisance that has serious threat to human health in the world, andit will transform into uremia as the liver loses its ability completely. The kidney plays animportant rule in the body's metabolism. The toxic sunstances including creatinine will beaccumulated extensively in human blood of kidney disease patients owing to kidney functiondecrease and kidney failure, and it seriously threaten patient's life. The excess creatinine notonly will cause a range of symptoms of poisoning, but also it will accelerate the process ofkidney failure. Therefore, it is very significant to effectively remove the excess creatinine inhuman blood of kidney disease patients. Consequently, it has important science significancein medical research area to research and prepare creatinine-adsobting materials with highperformance and to remove the creatinine accumulated in the body of kidney disease patientsby using blood purification techniquessuch as perfusion technique.
In this work, via elaborate molecular designing, crosslinking polyvinyl alcohol (CPVA)microspheres that have biocompatibility were used as the starting substance, and two graftedmicrospheres that have strong adsorption ability for creatinine were successfully prepared. Aredox initiating system was consisted of the hydroxyl groups on CPVA microspheres and theceric salt in the solution, and the two functional monomers, methacrylic acid (MAA) andsodium styrene sulfonate (SSS), were graft-polymerized onto CPVA microspheres throughsurface-initiated graft-polymerization method, respectively, resulting in two graftedmicrospheres, CPVA-g-PMAA and CPVA-g-PSSS. Besides, a creatinine molecule-imprintedmaterial MIP-PSSS/CPVA, which has special molecular recognition selectivity and excellentbinding affinity for creatinine, was also prepared with SSS as the functional monomer and creatinine as template and by using a novel molecular surface-impriting technique. Theadsorption characters and mechanisms of the above three medical macromolecular materialtowards creatinine were investigated in depth, and the satisfactory study results were achived.These materials are promising in the blood purification application.
Crosslinked polyvinyl alcohol (CPVA) microspheres were first prepared by usingdirectly crosslinking-balling method in a suspension system and with glutaraldehyde ascrosslinking agent. On that basis, a redox initiation system was constructed with a great dealof hydroxyl group on CPVA microspheres and cerium ammonium sulfate, and thesurface-initiated graft polymerization of methacrylic acid (MAA) was performed in anaqueous solution, resulting in the grafted microspheres CPVA-g-PMAA. The chemicalstructure and physicochemistry characters were adequately characterized with infraredspectrum (FTIR), scanning electron microscope (SEM) and zeta potential determination.Theeffects of the main factors on the graft polymerization were examined, and the mechanism ofthe graft-polymerization was explored, and the conditions of the graft-polymerization wereoptimized. The experimental results show that hydroxyl group-cerium salt redox initiationsystem can effectively initiates the graft polymerization of MAA on CPVA microspheresunder the suitable conditions such as at45℃, at a cerium salt concentration of4.9×10-3mol·L~(-1), at a sulfuric acid concentration of0.17mol·L~(-1)and at a MAA concentration of0.55mol·L~(-1), and the grafted microspheres CPVA-g-PMAA with a PMAA grafting degree of30g/100g can be prepared.
Then the adsorption property of the grafted microspheres CPVA-g-PMAA for creatininewas examined in more detail, and the adsorption mechanism and thermodynamics werestudied. The experimental results show that there exist strong interactions, electrostaticinteraction (main action force) and hydrogen bonding (a supporting role) between the graftedmicrospheres CPVA-g-PMAA and creatinine molecule, and it lead to that the graftedmicrospheres display very strong adsorption ability towards creatinine. As pH=8.0, theadsorption capacity has a maximum value,40mg·g~(-1). The adsorption process is exothermic,and it is driven by enthalpy. The presence of electrolyte in the solution affects negatively the adsorption property of the grafted microspheres CPVA-g-PMAA, and the adsorption capacitydecreases with the increase of the ion concentration.
In this work, another kinds of grafted microspheres, CPVA-g-PSSS, were also preparedwith the surface-initiated graft-polymerization method and with SSS monomer. The chemicalstructure, morphology character and the surface electrical property of the graftedmicrospheres CPVA-g-PSSS were characterized by using several means such as FTIR, SEMand zeta potential determination. The adsorption ability, mechanism and adsorption of thegrafted microspheres CPVA-g-PSSS for creatinine were also examined and reseached indepth. The study results show that under the suitable conditions the grafted microspheresCPVA-g-PSSS with a grafting degree of16g/100g can be smoothfully prepared. By right ofthe strong electrostatic interaction between the sulfonate groups of the grafted microspheresCPVA-g-PSSS and creatinine molecule, the microspheres CPVA-g-PSSS can produce verystrong adsorption ability. The adsorption capacity is pH-dependent, and the greater theadsorption capacity, the lower the pH value. At pH=1, the adsorption capacity can reach15.65mg·g~(-1). The adsorption of the microspheres CPVA-g-PSSS for creatinine is also anexothermic process, and this process is also drived by enthalpy.
Finally, based on “surface-initiated graft-polymerization”, in an aqueous solution system,creatinine molecule-surface imprinting was conducted with SSS as monomer and N,N'-methylene-bis-acrylamide (MBA) as crosslingking agent by using hydroxyl-ceric saltredox ionitiating system and SSS, and the imprinted microspheres MIP-PSSS/CPVA wereobtained. With N-hydroxysuccinimide (N-Hy) and creatine (Cr) as two contrast substances,the recognition character and binding property of the creatinine molecule-surface imprintedmaterial MIP-PSSS/CPVA for creatinine were researched detailedly. The selectivitycoefficients of MIP-PSSS/CPVA for creatinine relative to the contrast substances, N-Hy andCr, are5.51and6.60, respectively, displaying high recognition selectivity.
引文
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