载药淀粉微球的合成研究

以可溶性淀粉为原料,环氧氯丙烷为交联剂,Span60为乳化剂,甲苯和蓖麻油的混合物为油相,采用逆相悬浮交联聚合法合成淀粉微球。实验运用正交优化设计,选择淀粉浓度、油水相之比、乳化剂用量和交联剂用量四个因素为考察对象,对淀粉微球的制备条件进行了优化。利用红外（IR）、扫描电镜（SEM）、激光粒度分析仪（LPA）等对产物进行了表征。     

悬浮聚合法制备聚甲基丙烯酸甲酯微球的研究

以明胶为稳定剂采用悬浮聚合法合成了微米级聚甲基丙烯酸甲酯微球。通过研究搅拌速度、聚合温度及稳定剂用量,确定了较理想的合成工艺条件。     

悬浮聚合法制备PGMA-MMA-EGDMA共聚物交联微球

以甲基丙烯酸缩水甘油酯(GMA)为主单体、甲基丙烯酸甲酯(MMA)为共单体、乙二醇二甲基丙烯酸酯(EGDMA)为交联剂、聚乙烯醇(PVA)为分散剂,采用悬浮聚合法制备了三元共聚交联微球GMA-MMA-EGDMA,采用FT-IR和SEM对其化学结构和微球进行了表征,考察了分散剂用量、搅拌速度、油/水相比、交联剂用量、NaCl用量对交联微球的成球性能及粒度的影响规律. 结果表明,分散剂用量、搅拌速度与油/水相比是影响交联微球制备的主要因素,当分散剂用量<1%、搅拌速度<250 r/min、油/水相比>1:4(j)时,共聚合体系中均不能成球. 在水相中加入电解质NaCl有助于成球,交联微球的粒径随NaCl用量增大而减小. 控制悬浮聚合的反应条件可以制备出球形度好、粒径在100~400 mm范围内可控的交联微球GMA-MMA-EGDMA.     

替米考星交联淀粉载药微球的制备研究

以可溶性淀粉为原料,采用反相悬浮聚合法,合成了替米考星淀粉交联共聚载药微球。探讨了投药量、反应时间、交联剂、乳化剂对替米考星淀粉微球载药量、包封率和微球形貌的影响,运用红外、热重、电镜、粒度分析仪对产物进行了表征。结果表明,最佳制备条件为:替米考星0.02 g,淀粉4 g,乳化剂0.75 g,交联剂0.95 g,反应1.5 h,合成的替米考星淀粉微球载药量2.43%,包封率88.6%。微球粒径分布均匀,外观圆整,表面粗糙,具有较好的热稳定性。     

悬浮聚合制备微米级聚苯乙烯微球

以羟乙基纤维素和白明胶为稳定剂、甲苯和庚烷为致孔剂,经悬浮聚合制备了单分散交联聚苯乙烯微球。考察了单体用量、引发剂和交联剂含量、搅拌速度对微球粒径的影响。结果表明,最佳的悬浮聚合条件为：单体苯乙烯的用量为水相的质量分数20%、交联剂二乙烯基苯为单体的质量分数4%、引发剂过氧化苯甲酰为单体的质量分数1%、聚合温度为60 ℃、搅拌速度为500 r/min、反应时间为24 h。在此条件下制备的交联聚苯乙烯微球平均直径为40 μm左右,扫描电镜观察结果显示,合成的交联聚苯乙烯微球的形态良好且表面有微孔,分散性好。     

悬浮聚合法制备磁性微球的粒度分布特性

本文研究了含有微细铁黑颗粒的混合单体悬浮聚合产物的粒度分布特性。分析了分散剂、超声预分散和无机铁黑颗粒对形成粒度多峰分布的影响。结果表明,分散剂是体系中形成小颗粒的主要因素;超声波的预分散作用使悬浮体系的液滴破裂以“腐蚀破碎（erosive breakage)”为主;无机铁黑颗粒由于其表面亲水性,倾向于分布在油性单体液表面,不仅有利于悬浮液滴的“磨蚀破碎”,同时也对分散液滴具有良好的稳定作用。上述因素的共同作用使得聚合产物的粒度呈三峰分布。     

种子溶胀悬浮聚合法制备分子印迹聚合物微球的研究进展

分子印迹聚合物微球是一种具有特异性识别性能的新型高分子材料.种子溶胀悬浮聚合法所制备的印迹聚合物微球可应用于极性环境中,能够满足诸如酶模拟等实际应用环境的要求.本文综述了几种不同的制备分子印迹聚合物微球的种子溶胀悬浮聚合法,并对其研究方向做了展望.     

悬浮聚合法制备微球状压敏胶的研究

以丙烯酸-2-乙基己酯(2-EHA)、丙烯酸甲酯(MA)和丙烯酸(AA)为共聚单体,聚乙烯醇(PVA)为分散剂,过氧化苯甲酰(BPO)为引发剂,采用悬浮聚合法制备了可重复粘贴的微球状PSA(压敏胶).研究了水油比(即水与主单体质量比)、软硬单体质量比、分散剂种类和搅拌速率等对聚合物粒径及PSA性能的影响.结果表明:当水...     

用作活性物载体聚苯乙烯-二乙烯苯多孔交联微球的悬浮聚合制备及表征

Functional porous microspheres used for the slow release carrier of actives in cosmetics or pharmaceuticals were prepared by modified suspension polymerization of styrene （ST） with divinylbenzene （DVB） in the presence of toluene, cyclohexanol and heptane as porogenic diluents. The use of ultrasonic dispersion decreases the beads＇ size and improves the uniformity. The effects of the porogen mixture, DVB content and solvent extraction on the surface performance of the synthesized beads were studied. The microspheres were characterized by scanning electron microscopy （SEM） and BET surface area determination. It was found that a great proportion of the non-solvating porogen increases the pore diameter and the specific surface area. High DVB concentration also results in the great specific surface area and porosity. When the ratio of toluene/cyclohexanol is 1：2, DVB content is at the range of 40%-60% and methylene chloride was used as extractant, the beads with good spherical shape and pore size were obtained. The prepared porous microspheres were applied as active carriers and showed satisfactory slow release effect. Over 10h constantly sustained release was observed in vitro releasing test for hydroquinone-loaded microspheres. Great surface area promoted high concentration of released hydroquinone.     

木薯淀粉微球合成条件的研究

以木薯淀粉为材料,大豆色拉油为油相,淀粉水溶液为水相,环氧氯丙烷为交联剂,山梨醇脂肪酸酯(Span-60)为乳化剂,采用逆相悬浮交联聚合法制备淀粉微球,实验运用正交优化设计,选择淀粉浓度、油水相之比、乳化剂用量和交联剂用量4个因素为考察对象,对淀粉微球的制备条件进行了优化。对所得的淀粉微球用扫描电镜、红外光谱进行了表征。     

淀粉接枝共聚物微球的合成研究

用V(环己烷)∶V(淀粉溶液)=4∶1构成反相悬浮体系,m(Span60)∶m(Tween60)=2∶1复配为分散剂,在60℃下以K2S2O8-NaHSO3引发N,N’-亚甲基双丙烯酰胺(MBAA)与淀粉的接枝共聚,制备了淀粉接枝共聚物微球。正交实验表明,合成共聚微球的较优工艺条件为:淀粉液浓度20%,引发剂用量0.2 g,MBAA用量0.4 g,油水比为3∶1,乳化剂用量1.0 g。用SEM和粒度分析仪对微球形貌和粒度分布进行了研究,用FT-IR对其结构进行了表征,用XRD,TGA对其物性进行了分析。结果显示,共聚物微球形态圆整,平均粒径50.2μm,微球中存在酰氨基结构,与淀粉颗粒相比,结晶度降低,热稳定性提高。     

复合玉米淀粉微球的合成与其性能研究

以复合淀粉(玉米淀粉和β-环糊精)为原料,N,N’-亚甲基双丙烯酰胺和环氧氯丙烷为交联剂,采用反相乳液聚合法,合成复合玉米淀粉微球。利用红外光谱、扫描电镜、差热分析等方法对微球进行了表征,并用溶胀度法测定微球交联程度,通过微球对无机金属粒子和有机色素吸附量测定微球的吸附性能。结果表明,制备的复合玉米淀粉微球外型规则,粒度均匀,分散性好。复合玉米淀粉微球的溶胀度比玉米淀粉降低,对无机物Ca2+、有机物胭脂红的吸附作用比玉米淀粉更强,可以作为良好的吸附剂。     

反相悬浮法合成大颗粒珠状高吸水性聚合物及其性能研究

采用反相悬浮法一步合成了大颗粒珠状聚丙烯酸钠高吸水性树脂(SAP),研究了交联剂、搅拌速率、油水比、分散剂、引发剂用量及比例等因素对该SAP粒径及吸水倍率的影响。研究结果表明,该SAP的最大粒径超过2mm、吸水率超过100倍,并且其合成工艺简单、产品后处理操作方便。     

免疫淀粉微球的制备及其结合特性

研究反相微乳法合成淀粉微球,采用环氧氯丙烷活化淀粉微球,考察了活化过程中的影响因素,确定了活化的最佳优化条件;再将制备的肝特异性脂蛋白(liver specific lipoprotein,LSP)抗体与淀粉微球交联,得到免疫淀粉微球;阐述了免疫淀粉微球对抗原肝特异性脂蛋白(LSP)的结合特性。经测定单位淀粉微球交联LSP抗体的量为7.7 mg/g,单位免疫淀粉微球结合LSP的量为0.5 mg/g,表明被交联的抗体保持了较高的生物活性。     

淀粉微球吸附胭脂红动力学研究

以模型药物胭脂红为吸附质,考察淀粉微球的吸附动力学特性。分别采用5种常用的吸附动力学方程对不同吸附质初始质量浓度的实验数据进行拟合,结果显示淀粉微球对胭脂红的吸附过程较好地符合Lagergren二级吸附动力学模型。然后通过考虑胭脂红初始质量浓度、体系温度和微球平均粒径对吸附的影响,运用多元回归方法建立了平衡吸附量与质量浓度、温度和平均粒径之间的综合吸附动力学模型。该模型确定了影响淀粉微球吸附载药各种因素的主次关系,为研究淀粉微球的吸附载药作用提供了一种研究方法。     

Molecularly imprinted polymer microspheres prepared by precipitation polymerization using a sacrificial covalent bond

Molecularly imprinted polymer microspheres were prepared by precipitation polymerization using a sacrificial covalent bond. In the present model, cholesteryl (4‐vinyl)phenyl carbonate was used as a template monomer. The imprinted microspheres were prepared using ethylene glycol dimethacrylate (EDMA) and divinylbenzene (DVB) as crosslinker. The base‐labile carbonate ester bond was easily hydrolyzed to leave imprinted cavities in the resulting polymers. Radioligand binding analysis, elemental analysis, and scanning electron microscopy were used to characterize the imprinted materials. Imprinted microspheres prepared from DVB crosslinker had larger and more defined spherical shape, and displayed better imprinting effect than did the EDMA‐based microparticles. For comparison, imprinted bulk polymers were also prepared in the same reaction solvent as that used in precipitation polymerization. Elemental analysis results indicated that imprinted microspheres contained more template monomer units than bulk materials. The efficiency of template removal by hydrolysis treatment for microspheres was also higher than that for bulk polymers. For DVB‐based polymers, imprinted microspheres displayed higher specific cholesterol uptake than did the corresponding bulk polymer. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 99: 1390–1398, 2006     

Monodisperse hydrophilic polymer microspheres having carboxylic acid groups prepared by distillation precipitation polymerization

Monodisperse hydrophilic polymer microspheres having carboxyl acid group with spherical shape in the range of 160 nm and 1.52 μm were prepared by distillation copolymerizations of (meth)acrylic acid with either ethyleneglycol dimethacrylate (EGDMA) or divinylbenzene (DVB) as crosslinker. Polymerization was carried out with 2,2′-azobisisobutyronitrile (AIBN) as initiator in neat acetonitrile without stirring. The polymer microspheres were formed and precipitated out from the reaction medium during the distillation of the solvent from the reaction system through an entropic precipitation polymerization manner. The effects of the crosslinker degree on the morphology and the loading capacity of the carboxylic acid group of the resultant polymer microspheres were investigated. The growth procedures of poly(DVB-co-AA) microspheres were traced by SEM characterization. The steric stabilization through the pendent chains and surface gel and the electrostatic repulsion from the carboxyl acid groups contribute to the formation of monodisperse polymer microspheres.     

应用响应曲面优化交联淀粉微球的合成工艺

为了优化采用反相悬浮法合成的交联淀粉微球(CSM)的工艺,采用响应曲面法(RSM)分析了交联剂质量分数、反应温度和引发剂浓度对于CSM品质(溶胀度、平均粒径)的影响,并建立了相应的预测模型。方差分析的结果表明:交联剂质量分数、反应温度和引发剂浓度对于CSM溶胀度和平均粒径这2项指标都有着极为显著的影响。优化所得的较优工艺参数:交联剂质量分数为0.5%,交联温度为48℃,引发剂浓度为3.7 mmol/L。对应的CMS溶胀度及平均粒径的预测值分别为246%和16.5μm。经实验证明:应用响应曲面法所得到的CMS合成工艺参数是可行的。     

淀粉微球对玫瑰香精的吸附及缓释性能研究

以可溶性淀粉为原料,环氧氯丙烷为交联剂,采用反相悬乳法合成淀粉微球(SM),制备具有一定缓释性能的香精缓释制剂。使用倒置荧光显微镜观察其表面粗糙,呈圆球形。在玫瑰香精体积分数40%、吸附时间1.5 h、45℃条件下,其对玫瑰香精的吸附量达到0.85 g/g。紫外分光光度法得出,随着时间的延长,质量相等固体中香精含量缓慢下降,释放速率也逐渐减小。