多重乳液法聚羟基丁酸酯基印迹微球的制备、结构与特性
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摘要
本文采用水/油/水多重乳液法制备了平均粒径为101～102μm的聚羟基丁酸酯(PHB)基微球,采用光学显微技术研究了乳液形成过程及其固化成球过程,在此基础上采用包埋法制备了牛血清白蛋白(BSA)印迹的PHB微球、PHB/聚乙二醇(PEG)微球,并对微球的制备、结构和特性进行了较为详细地探讨。
研究表明,多重乳液的结构和稳定性,特别是初乳液滴和复乳液滴的形态和直径是影响微球结构的重要因素,由此最终可得到坍陷、空心或类似蜂巢等不同结构的微球。制备过程中添加PEG组分具有改善乳化效果、提高亲水性和模板致孔等多种作用,对微球结构也有重要影响。微球的最终结构还与成球过程中PHB的结晶行为密切相关。
系统研究了二次乳化搅拌速度、W_1/O比例、(W_1/O)/W_2比例等乳液形成条件,PHB、PEG、PVA、BSA等用量以及PHB/PEG的质量比对微球粒径大小、表面形貌、孔疏密程度的影响规律,探讨了微球结构、包埋率与溶出特性之间的关系,确定了较优化的制备工艺。
吸附行为研究表明,BSA印迹的PHB基微球具有较高的吸附选择性和再生性。适中的模板加入量、较低的PHB分子量以及添加PEG组分等均可使PHB印迹微球显示出更大的平衡吸附量。讨论了PHB作为新型分子印迹基材的原理。
In this dissertation water in oil in water (w1/o/w2) multiple emulsion method was selected to prepare bovine serum albumin (BSA) imprinted Poly(3-hydroxybutyrate) (PHB) microspheres with average diameter from 101μm to 102μm. Optical microscope was used for observation the course of solvent evaporation and solidification of multiple emulsion microdroplets. On the basis of the study BSA molecular imprinted PHB microspheres and PHB/Poly(ethylene glycol) (PEG) microspheres were prepared with embedding technique. The preparation, structure, characteristic and properties of the microspheres were detailedly discussed too.
The result of research showed that structure of the multiple emulsion, especially the microdroplets’diameter and morphology of initial emulsion and multiple emulsion was a crucial factor to influence the structure of microspheres, which would form different structures such as deflated, closed, hollow or honeycomb at last. Participation of Poly(ethylene glycol) (PEG) strengthened the emulsification effect, improved the hydrophilic properties, played a role of pores-maker as templates and had an important influence on the structure of microspheres, The structure of microspheres had close relatively with the crystallizing behavior of PHB during the course of forming microspheres.
The factors that worked on the diameter, surface morphology and porosity of the microspheres were systematically studied, including stirring speed of the second emulsion, volume ratio of W1/O and (W1/O)/W2, concentration of PHB, PEG, polyvinyl alcohol (PVA), BSA and mass ratio of PHB/PEG. Also the relationship between the structure of microspheres and entrapment rate and the property of dissolving out was discussed. The optimized processes parameters were fixed after that.
The research of adsorption behavior showed that molecular imprinted PHB based microspheres had good specific adsorption, recognition and regeneration of the template. Greater absorption capacity could be achieved at equilibrium for the template at the preparation conditions of moderate template adding, lower molecular weight of PHB and the addition of PEG. The principle of PHB as a new molecularly imprinted material was discussed.
研究表明,多重乳液的结构和稳定性,特别是初乳液滴和复乳液滴的形态和直径是影响微球结构的重要因素,由此最终可得到坍陷、空心或类似蜂巢等不同结构的微球。制备过程中添加PEG组分具有改善乳化效果、提高亲水性和模板致孔等多种作用,对微球结构也有重要影响。微球的最终结构还与成球过程中PHB的结晶行为密切相关。
系统研究了二次乳化搅拌速度、W_1/O比例、(W_1/O)/W_2比例等乳液形成条件,PHB、PEG、PVA、BSA等用量以及PHB/PEG的质量比对微球粒径大小、表面形貌、孔疏密程度的影响规律,探讨了微球结构、包埋率与溶出特性之间的关系,确定了较优化的制备工艺。
吸附行为研究表明,BSA印迹的PHB基微球具有较高的吸附选择性和再生性。适中的模板加入量、较低的PHB分子量以及添加PEG组分等均可使PHB印迹微球显示出更大的平衡吸附量。讨论了PHB作为新型分子印迹基材的原理。
In this dissertation water in oil in water (w1/o/w2) multiple emulsion method was selected to prepare bovine serum albumin (BSA) imprinted Poly(3-hydroxybutyrate) (PHB) microspheres with average diameter from 101μm to 102μm. Optical microscope was used for observation the course of solvent evaporation and solidification of multiple emulsion microdroplets. On the basis of the study BSA molecular imprinted PHB microspheres and PHB/Poly(ethylene glycol) (PEG) microspheres were prepared with embedding technique. The preparation, structure, characteristic and properties of the microspheres were detailedly discussed too.
The result of research showed that structure of the multiple emulsion, especially the microdroplets’diameter and morphology of initial emulsion and multiple emulsion was a crucial factor to influence the structure of microspheres, which would form different structures such as deflated, closed, hollow or honeycomb at last. Participation of Poly(ethylene glycol) (PEG) strengthened the emulsification effect, improved the hydrophilic properties, played a role of pores-maker as templates and had an important influence on the structure of microspheres, The structure of microspheres had close relatively with the crystallizing behavior of PHB during the course of forming microspheres.
The factors that worked on the diameter, surface morphology and porosity of the microspheres were systematically studied, including stirring speed of the second emulsion, volume ratio of W1/O and (W1/O)/W2, concentration of PHB, PEG, polyvinyl alcohol (PVA), BSA and mass ratio of PHB/PEG. Also the relationship between the structure of microspheres and entrapment rate and the property of dissolving out was discussed. The optimized processes parameters were fixed after that.
The research of adsorption behavior showed that molecular imprinted PHB based microspheres had good specific adsorption, recognition and regeneration of the template. Greater absorption capacity could be achieved at equilibrium for the template at the preparation conditions of moderate template adding, lower molecular weight of PHB and the addition of PEG. The principle of PHB as a new molecularly imprinted material was discussed.
引文
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