纳米氧化锆的制备新工艺研究

以ZroCl2·8H2O和H2O2为原料,采用中和沉淀法制备纳米氧化锆,在制备工艺过程中2次(前驱体制备过程和研磨过程)加入分散剂(表面活性剂)来抑制粉体的团聚.探讨了有关因素对制备氧化锆产品的影响,例如前驱体氢氧化锆的煅烧温度对氧化锆晶型的影响,表面活性剂对产品粒径的影响,煅烧时间对ZrO2平均粒径的影响,研磨助剂对ZrO2平均粒径的影响等,研究得到了最佳工艺条件,并在优化实验条件下制备出平均粒径为50nm、粒径分布均匀的球形纳米氧化锆粉末.     

铬绿颜料细化工艺优化

探索湿法卧式砂磨机制备微、纳尺度粉体制备方法及最优制备工艺;结合粉碎理论确定需要优化的工艺参数及参数范围,利用正交试验法得到各影响参数对颜料粒径的影响权重。结果显示,转速(6.26)研磨时间(3.68)研磨介质填充率(1.232)研磨介质粒径(0.96),在优化参数转速为3 000 r/min、研磨时间为240 min、研磨介质填充率为85%、研磨介质粒径为0.7 mm下,制备出D90为336 nm且分布窄的铬绿颜料;在优化参数下,分别研究转速、研磨时间、研磨介质填充率和研磨介质粒径对颜料粒径的影响,其中可控制备所需粒径颜料的工艺是,转速为3 000 r/min,研磨介质填充率为85%,研磨介质粒径为0.7 mm,通过控制研磨时间制备所需粒径颜料。     

CMP专用大粒径硅溶胶研磨料生长及控制机理

为满足甚大规模集成电路(ULSI)互连结构高质量、高效率化学机械抛光(CMP)的要求,以LaMer模型为理论指导,对恒液面聚合生长法制备大粒径、低分散度硅溶胶研磨料的粒径增长阶段进行了机理分析,并讨论了加料速率对平均粒径及分散度的影响;优化加料速率为3.6 mL/min,以此控制体系中硅酸浓度的变化趋势,避免产生两种类型的新晶核,实现了单纯的粒径增长.以胶粒平均粒径28nm、分散度1.13的母液制备出粒径57nm、分散度1.07的硅溶胶.通过工艺调整并按照分级生长模式,进一步制得符合高质量、高效率CMP专用的大粒径(平均粒径为112nm)、低分散度(接近于1.00)硅溶胶研磨料.     

柠檬酸盐凝胶法制备纳米氧化镍的研究

优化了柠檬酸盐凝胶法制备纳米氧化镍粉体的工艺条件.采用傅立叶红外光谱(FTIR)、热分析(TG/DTA)、X射线衍射(XRD)、扫描电镜(SEM)和BET法对柠檬酸镍络合物的形成,凝胶热分解过程,产物的形貌、粒径和比表面积大小以及同材料配比、热处理温度、热处理时间之间的关系进行了研究,确定了制备纳米氧化镍的最佳工艺条件(柠檬酸与镍离子摩尔比1.2:1.0,400℃热处理1h),并在此条件下成功制备了粒径达30nm,比表面积达181.29m²/g的NiO粉体.通过热力学计算,解释了在凝胶热分解过程中金属镍相出现的可能原因.     

超临界反溶剂法制备吸入式给药微粉

利用自制的超临界反溶剂装置,以枸橼酸喷托维林为研究对象,制备粒径小、粒径分布较窄的枸橼酸喷托维林微粉,研究压力、温度、进样速率和溶剂等工艺参数对微粉形貌、粒径及粒径分布的影响。结果表明:制备的微粉微观形貌均为片状;各工艺参数对微粉粒径及粒径分布影响不同,通过优化工艺参数可制备出几何粒径为0. 5～12μm、空气动力学粒径为1. 2μm的微粉,符合吸入式给药对微粉粒径的要求。     

一种制备单分散超小粒径氧化硅颗粒的新方法

在氨水催化水解正硅酸乙酯(TEOS)过程中,采用一种新方法制备了单分散的超小粒径氧化硅。加入聚乙烯吡咯烷酮(PVP)能够有效的减小氧化硅颗粒的粒径大小,氧化硅粒径随着PVP的增加而减小。通过优化工艺参数,制备得到了单分散的、粒径只有11nm的氧化硅颗粒。而且,在相同的反应体系中,所制备的氧化硅颗粒能够作为晶种再次生长,通过滴加不同浓度的TEOS能够得到粒径大小可控的氧化硅颗粒。     

5-氟尿嘧啶载药微球的制备工艺及性能研究

以PLA为载体材料,以5-Fu为模型药物,制备5-Fu/PLA载药微球,通过正交设计优化微球制备工艺.另外,检测了载药微球的回收率、稳定性、缓释性能等物理性质.用紫外分光光度计测定药物含量,激光粒度仪分析粒径. 结果表明,载药微球的平均粒径为(133.2±32.5)nm,平均包封率为(11.3±5.0)%,缓释时间延长至80～100h,具有良好的缓释功能.     

遗传算法结合响应面法优化番茄红素纳米结构脂质载体的制备

目的 提高脂溶性番茄红素的生物利用率和稳定性。方法 采用熔融-高速剪切法制备番茄红素纳米结构脂质载体。以包封率、平均粒径为主要评价指标，进行单因素实验，并在单因素基础上通过遗传算法结合Box-Behnken响应面法对制备工艺进行优化。结果 遗传算法和Box-Behnken响应面法优化得到的理论包封率分别为86.208 2%、86.169 5%。通过验证实验得到实际包封率为(86.267±0.44)%，平均粒径为(121.8±5.20)nm。结论 结果表明遗传算法结合Box-Behnken响应面法优化番茄红素纳米结构脂质载体模型可靠。     

BSA-PLGA微球的优化制备及特性

目的:优化BSA-PLGA微球制备工艺,并对其包封率、形态、体外释放药物及微球包裹前后BSA的稳定性进行评价。方法:以PLGA为载体,采用复乳溶剂挥发法制备BSA-PLGA微球。Micro BCA法测定微球的包封率和载药量,扫描电子显微镜观察微球的形态,激光粒度仪测定粒度及分布,聚丙烯酰胺凝胶电泳(SDS-PAGE)研究微球包裹前后BSA分子结构的完整性,同时考察体外释药性能。结果:根据优化工艺制备的微球外观圆整,平均粒径(2275.8±256.9)nm,包封率(82.59±2.92)%,载药量(13.76±0.49)×10-2%,包裹前后BSA结构稳定,体外释放28天以上,释放曲线符合Higuchi方程。结论:本研究获得了较优化的BSA-PLGA微球制备工艺,所制备的微球具有较高的包封率和明显的缓释效果。     

基于BP神经网络的超细石英粉体制备工艺参数研究

简要分析了工艺参数对高能球磨法制备超细石英粉体的影响,采用正交试验和均匀实验研究了球磨法制备超细石英粉体的具体工艺试验方法,应用人工神经网络技术建立了粉体参数预测模型,利用遗传算法的全局搜索能力,优化了BP网络权值,从而完善了基于BP网络的石英粉体粒径预测模型.试验结果表明:该模型具有较高的精度,较好地实现了球磨法制备石英粉体的粒径预测,为工艺参数选择提供理论依据.     

Microspheres for the oral delivery of insulin: preparation,evaluation and hypoglycaemic effect in streptozotocin-induced diabetic rats

Insulin-loaded microspheres were prepared by alternating deposition film layers that were composed of insulin and poly(vinyl sulfate) potassium on the surface of poly(lactic acid) (PLA) microspheres. The preparation of the insulin-loaded microspheres was optimized by an orthogonal test design, and the relationship between drug loading (DL) and film layers was studied. The particle size, DL and encapsulation efficiency of the obtained insulin-loaded microspheres with 10 films were 5.25?±?0.15?µm, 111.33?±?1.15?mg/g and 33.7?±?0.19%, respectively. Following this, the physical characteristics of the insulin-loaded microspheres were investigated. The results from scanning electron microscopy and a laser particle size analyzer (LPSA) indicated the spherical morphology, rough surface and increasing particle sizes of the insulin-loaded microspheres, which were compared to those of PLA microspheres. An in vitro release study showed that the insulin-loaded microspheres were stable in HCl solution (pH 1.0) and released insulin slowly in phosphate-buffered solution (pH 6.8). Finally, the drug efficacy of the prepared insulin-loaded microspheres via oral administration was evaluated in rats with diabetes induced by streptozotocin, and an obvious dose-dependent hypoglycemic effect was observed. This preliminary data could illustrate the prospect of using microspheres for the oral delivery of insulin.     

Preparation, Characterization and In-Vitro Release Kinetics of Salbutamol Sulphate Loaded Albumin Microspheres

Salbutamol sulphate loaded Bovine serum albumin microspheres were prepared by heat denaturation method. The effects of such preparation conditions as denaturation temperature, denaturation time, protein concentration and phase volume ratio on the extent of drug loading, size and size distribution and drug release were studied. An increase in protein concentration from 5% w/v to 15% w/v increased the mean particle size from 8.5 μm to 16.6 μm and decreased the drug loading from 46% w/w to 18% w/w. A decrease in the phase volume ratio substantially lowered mean particle size and size distribution. An increase in the severity of denaturaion conditions lowered both the drug incorporated and drug released. The kinetics of drug release from microspheres were compared to the theoretical models of Higuchi diffusional release and first order release. Both the models gave an adequate fit to the data. Scanning electron microscopy revealed that the dummy microspheres are spherical with smooth surfaces. As the drug-protein ratio increased, the microspheres exhibited rough surfaces showing the presence of drug crystals.     

Preparation,Characterization and In-Vitro Release Kinetics of Salbutamol Sulphate Loaded Albumin Microspheres

Abstract

Salbutamol sulphate loaded Bovine serum albumin microspheres were prepared by heat denaturation method. The effects of such preparation conditions as denaturation temperature, denaturation time, protein concentration and phase volume ratio on the extent of drug loading, size and size distribution and drug release were studied. An increase in protein concentration from 5% w/v to 15% w/v increased the mean particle size from 8.5 μm to 16.6 μm and decreased the drug loading from 46% w/w to 18% w/w. A decrease in the phase volume ratio substantially lowered mean particle size and size distribution. An increase in the severity of denaturaion conditions lowered both the drug incorporated and drug released. The kinetics of drug release from microspheres were compared to the theoretical models of Higuchi diffusional release and first order release. Both the models gave an adequate fit to the data. Scanning electron microscopy revealed that the dummy microspheres are spherical with smooth surfaces. As the drug-protein ratio increased, the microspheres exhibited rough surfaces showing the presence of drug crystals.     

Carnauba Wax Microspheres Loaded with Valproic Acid: Preparation and Evaluation of Drug Release

To minimize unwanted toxic effects of valproic acid (1) by the kinetic control of drug release, gastroresistant carnauba wax microspheres loaded with the antiepileptic agent were prepared. The preparation was based on a technique involving melting and dispersion of drug-containing wax in an aqueous medium. The resulting emulsion after cooling under rapid stirring produced solid, discrete, reproducible free flowing microspheres which converted the liquid drug droplets into solid material. About 94% of the isolated microspheres were of particle size range 200-425 μm. The microspheres were analyzed to determine the drug content in various particle size range and to characterize the in vitro release profile. The average drug content was 26% w/w. The intestinal drug discharge of 1 from the carnauba wax microspheres was studied and compared with the release patterns observed for white beeswax and hexadecanol microspheres previously described. The drug release performance was greatly affected by the material used in the microencapsulation process. In the intestinal environment carnauba wax microspheres exhibited more rapid initial rate of release and about 80% of the entrapped drug was discharged in 120 min while complete release occurred in about 8 h.     

Preparation and In Vitro Evaluation of Chitosan Microspheres Containing Prednisolone: Comparison of Simple and Conjugate Microspheres

The purpose of the present study was to obtain a novel microparticulate formulation of prednisolone, which was adequate for the treatment of inflammatory bowel disease (IBD). The formulations prepared were evaluated in vitro. Two types of chitosan microspheres containing prednisolone, named Ch-Pred and Ch-SP-MS, were prepared by an emulsification-solvent evaporation method using a chitosan-prednisolone mixture and a chitosan-succinyl-prednisolone conjugate (Ch-SP), respectively. Ch-Pred and Ch-SP-MS were obtained in almost spherical shape. Ch-Pred showed a relatively high drug content of 13.2% (w/w), but the particle size was distributed from 10 to 45 µm, and a large initial burst release of approximately 60% was observed. On the other hand, although Ch-SP-MS exhibited a fairly low drug content of 3.5% (w/w), their particle size ranged from several hundred nanometers to 20 µm, with the mean diameter of 5 µm, and a gradual drug release profile was achieved. These characteristics on particle size and in vitro release suggested that Ch-SP-MS should have good potential as a microparticulate system for the treatment of IBD.     

Carnauba Wax Microspheres Loaded with Valproic Acid: Preparation and Evaluation of Drug Release

Abstract

To minimize unwanted toxic effects of valproic acid (1) by the kinetic control of drug release, gastroresistant carnauba wax microspheres loaded with the antiepileptic agent were prepared. The preparation was based on a technique involving melting and dispersion of drug-containing wax in an aqueous medium. The resulting emulsion after cooling under rapid stirring produced solid, discrete, reproducible free flowing microspheres which converted the liquid drug droplets into solid material. About 94% of the isolated microspheres were of particle size range 200-425 μm. The microspheres were analyzed to determine the drug content in various particle size range and to characterize the in vitro release profile. The average drug content was 26% w/w. The intestinal drug discharge of 1 from the carnauba wax microspheres was studied and compared with the release patterns observed for white beeswax and hexadecanol microspheres previously described. The drug release performance was greatly affected by the material used in the microencapsulation process. In the intestinal environment carnauba wax microspheres exhibited more rapid initial rate of release and about 80% of the entrapped drug was discharged in 120 min while complete release occurred in about 8 h.     

Preparation and in vitro evaluation of chitosan microspheres containing prednisolone: comparison of simple and conjugate microspheres

The purpose of the present study was to obtain a novel microparticulate formulation of prednisolone, which was adequate for the treatment of inflammatory bowel disease (IBD). The formulations prepared were evaluated in vitro. Two types of chitosan microspheres containing prednisolone, named Ch-Pred and Ch-SP-MS, were prepared by an emulsification-solvent evaporation method using a chitosan-prednisolone mixture and a chitosan-succinyl-prednisolone conjugate (Ch-SP), respectively. Ch-Pred and Ch-SP-MS were obtained in almost spherical shape. Ch-Pred showed a relatively high drug content of 13.2% (w/w), but the particle size was distributed from 10 to 45 µm, and a large initial burst release of approximately 60% was observed. On the other hand, although Ch-SP-MS exhibited a fairly low drug content of 3.5% (w/w), their particle size ranged from several hundred nanometers to 20 µm, with the mean diameter of 5 µm, and a gradual drug release profile was achieved. These characteristics on particle size and in vitro release suggested that Ch-SP-MS should have good potential as a microparticulate system for the treatment of IBD.     

Encapsulation of superparamagnetic iron oxide nanoparticles in poly-(lactide-co-glycolic acid) microspheres for biomedical applications

Magnetic microspheres were prepared using a single step coaxial electrohydrodynamic atomization technique at ambient temperature and pressure, with poly(lactic-co-glycolic acid) as the coating and iron oxide (Fe₃O₄) nanoparticles dispersed in polyethylene glycol as the encapsulated material. The morphology and particle size distributions of the prepared magnetic microspheres were investigated by scanning electron microscopy. The particles were spherical with mean diameters ranging from ~ 2 μm to 18 μm, depending on the combination of processing parameters (flow rate and applied voltage). Analysis by infrared spectroscopy and focused ion-beam sectioning confirmed incorporation of iron oxide nanoparticles into the microspheres and the prepared samples were shown to be responsive to an applied magnetic field. This study demonstrates a convenient method for the preparation of nanoparticle loaded microspheres, which could be used potentially as transverse relaxation contrast agents in magnetic resonance imaging, as well as for magnetically guided drug delivery.     

Chitosan-Drug Conjugate Microspheres: Preparation and Drug Release Properties of Microspheres Composed of the Conjugate of 2'- or 3'-(4-Carboxy-butyryl)-5- Fluorouridine with Chitosan

The conjugate microspheres (Chi-glu-FUR-m) were prepared by the dry-in-oil method using chitosan-5-fuorouridine conjugate. Chi-glu-FUR-m were characterized by drug content, particle shape and size, swelling property, and drug release. Their characteristics were compared with those of the simple microspheres (Chi/ FUR-m), which were prepared under similar conditions using a mixture of chitosan and 5-fluorouridine. Both microspheres prepared showed a high retention of the drug after preparation and similar particle size and shape. Swelling ratios after incubation in aqueous buflers of pH 7.4 for 6 hr were similar for both microspheres. Chi-glu-FUR-m swelled quickly in aqueous buffers of pH 7.4 and the disintegration was observed to occur gradually from 24 hr afrer the incubation. Chi-glu-FUR-m showed a gradual drug release (50% release time = 61 hr), while Chi/FUR-m released the drug very rapidly, Such characteristics of Chi-glu-FURm as swelling, slow disintegration, and gradual drug release propose its usefulness for localization or chemoembolization therapy.     

Lyoprotected nanosphere formulations for paclitaxel controlled delivery

The preparation and technological characterization of nanosphere formulations (NS) containing the anticancer drug paclitaxel (PTX) are reported. Poly(lactide) (PLA) and poly(lactide-co-glycolide) (PLGA) nanospheres (NS) were prepared by a solvent displacement method. They showed a mean particle size in the range 150-300 nm, with a high homogeneity (polydispersity index < 0.3). For long term stability, NS require additional procedures, such as freeze-drying. In this study, the effect on NS particle size and surface charge of different lyoprotectants (mono- and disaccharides, polyalcohols, and hydroxypropyl-beta-cyclodextrin) at various concentrations was tested by means of light scattering size analysis. The formulations freeze-dried with the addition of 10% glucose (w/v) showed interesting characteristics after freeze-drying. They were chosen for specific studies on drug encapsulation efficiency, in vitro drug release and biological activity on the human anaplastic thyroid carcinoma cell line 8305C. The PLGA NS, in particular, showed a cell growth inhibitory activity comparable to the free drug.