Sustained-release butorphanol microparticles

Various butorphanol-loaded microparticles have been prepared with a biodegradable copolymer P(FAD-SA) of erucic acid dimer (FAD) and sebacic acid (SA) and a copolymer P(CPP-SA) of carboxyphenoxypropane (CPP) and SA using a melt compounding and milling method. Drug release was measured in vitro following incubation of drug-loaded microparticles in water for injection at 37°C. It was found that butorphanol was released in a sustained manner, yielding a cumulative drug release of about 100% over a period of 48 hr. Also, drug release was affected by drug loading and the size of the microparticles; however, it was not significantly influenced by the copolymer composition. Scanning electron microscopic (SEM) results showed that most of the particles were irregular in shape with uneven surfaces. The molecular weights of the copolymers were not changed after this fabrication process. In addition, 20% butorphanol-encapsulated microspheres were prepared with copolymer P(FAD-SA) by spray-drying. The SEM micrograph shows that the particle sizes of the microspheres ranged from 2 to 10 μm, and the external surfaces appear smooth. Moreover, rapid drug release was observed for these microspheres, with more than 92% of the encapsulated drug released within the first 2 hr.     

Preparation and evaluation of insulin-loaded polylactide microspheres using factorial design

The aim of this work was to study the influence of the concentration and molecular weight of poly(DL-lactide) (PLA) on the characteristics and in vivo biological activity of protein-loaded microspheres. At the same time, an attempt was made to achieve further optimization of the formulation. In the study, insulin was chosen as a model of protein drugs. Nine formulations of injectable insulin-loaded PLA microspheres were prepared using an emulsification and solvent evaporation process according to a factorial design. The trapping efficiency, drug loading, and the drop percentages of blood glucose levels at 24 hr and 72 hr in mice were used to evaluate the formulations. The results showed that PLA molecular weight and, especially, PLA concentration exerted influences on the characteristics and in vivo biological activity of insulin-loaded microspheres. The drug-trapping efficiency increased with the increase of the polymer concentration. The drug loading decreased with the increase of the polymer concentration and was not obviously affected by PLA molecular weight. The drop percentage of blood glucose level at 24 hr increased with the increase of polymer concentration and molecular weight. At 72 hr, the drop percentages of blood glucose levels were slightly increased with the increase of PLA concentration and then significantly decreased after the PLA concentration was above 150 mg/ml. An optimized formulation was prepared with PLA-10k at a concentration of 200 mg/ml. The experimental values of the response variables were close to the predicted values. The results suggest that the in vivo release behavior should be taken into consideration in the design of protein-loaded PLA microspheres.     

Preparation of cross-linked sodium alginate microparticles using glutaraldehyde in methanol

Polymeric sodium alginate microparticles were prepared by precipitating sodium alginate in methanol, followed by cross-linking with glutaraldehyde. The extent of cross-linking was controlled by the time of exposure to glutaraldehyde. The topology of microparticles was characterized by scanning electron microscopy (SEM), which indicated smooth surfaces. The equilibrium swelling experiments were carried out in water to observe the effect of cross-linking and drug loading for better utility of microparticles. It was found that swelling decreased, but drug loading increased, with an increase in cross-linking of the matrix.     

Preparation and characterization of APTES films on modification titanium by SAMs

In this study, the titanium plates, which were modified by NaOH alkali solution, were associated with 3-Aminopropyltriethoxysilane (APTES) films using self-assembled monolayers (SAMs). The surfaces of titanium before and after modification were characterized by scanning electronic microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and attenuated total refraction-Fourier transform infrared spectroscopy (ATR-FTIR). After bonding the APTES films on the modification titanium, the new peaks located around 1095 cm⁻¹ attributes to siloxane groups indicating that silane agent had been grafted onto the surface of the modification titanium substrate by SAMs. Following the deposition of APTES films on titanium, significant change were seen in the amounts of oxygen, silicon and carbon present on the titanium surface, which were consistent with the anticipated reaction steps.     

Preparation and characterization of heparin-loaded polymeric microparticles

Microparticles containing heparin were prepared by a water-in-oil-in-water emulsification and evaporation process with pure or blends of biodegradable (poly-epsilon-caprolactone and poly(D,L-lactic-co-glycolic acid)) and of positively-charged non-biodegradable (Eudragit RS and RL) polymers. The influence of polymers and some excipients (gelatin A and B, NaCl) on the particle size, the morphology, the heparin encapsulation rate as well as the in vitro drug release was investigated. The diameter of the microparticles prepared with the various polymers ranged from 80 to 130 microns and was found to increase significantly with the addition of gelatin A into the internal aqueous phase. Microparticles prepared with Eudragit RS and RL exhibited higher drug entrapment efficiency (49 and 80% respectively) but lower drug release within 24 h (17 and 3.5% respectively) than those prepared with PCL and PLAGA. The use of blends of two polymers in the organic phase was found to modify the drug entrapment as well as the heparin release kinetics compared with microparticles prepared with a single polymer. In addition, microparticles prepared with gelatin A showed higher entrapment efficiency, but a significant initial burst effect was observed during the heparin release. The in vitro biological activity of heparin released from the formulations affording a suitable drug release has been tested by measuring the anti-Xa activity by a colorimetric assay with a chromogenic substrate. The results confirmed that heparin remained unaltered after the entrapment process.     

A novel technology to manufacture biodegradable polylactide bead foam products

Bead foaming technology with double crystal melting peak structure has been recognized as a promising method to produce high-performance low-density foams with complex geometries. Polylactide (PLA) bead foaming has been of the great interest of researchers due to its origin from renewal resources and biodegradability. However, due to the PLA’s low melt strength and slow crystallization kinetics, the attempts have been limited to the manufacturing methods used for expanded polystyrene (EPS). In this study, we developed microcellular PLA bead foams with double crystal melting peak structure in a large content using a lab-scale autoclave system followed by molding of the beads. PLA bead foams were produced with expansion ratios and average cell sizes ranging from 6 to 31-fold and 6 to 50 μm, respectively. The high-melting point crystals generated during gas-saturation significantly affected the expansion ratio and cell density of the PLA bead foams by enhancing the PLA’s melt strength and promoting cell nucleation around the crystals. The tensile properties of the molded EPLA bead foams showed that EPLA bead foams with double crystal melting peak can be a promising substitute not only for EPS but also for expanded polypropylene (EPP) bead foams.     

聚乳酸/蒙脱石纳米复合材料的制备与表征

对纳基蒙脱石(MMT)有机改性后,采用溶液插层薄膜塑造工艺制备蒙脱石/聚乳酸(PLA)纳米复合物,采用X-Ray粉晶衍射(XRD)、综合热分析(TGA&DSC)、红外吸收光谱(IR)等方法对复合材料进行表征,讨论了蒙脱石对插层结果的影响.结果表明,PLA能够插入MMT层间;MMT的层间距由1.40nm增大到2.16nm;复合材料的热稳定性能得到改善.     

Preparation and characterization of enteric microparticles by coacervation

The aim of this study was to produce cinnarizine loaded Eudragit^® L100-55 microparticles by coacervation technique in order to achieve pH responsive drug release using hydroxypropyl methycellulose (HPMC) as stabilizer. The effect of enteric polymer: HPMC ratio on properties of microparticles was investigated with regard to particle size distribution, morphology, yield, encapsulation efficiency, in vitro drug release profiles and interaction between cinnarizine and Eudragit^® L100-55. High drug encapsulation efficiency was seen in all microparticles. Particle diameter increased when the enteric polymer content was higher relative to HPMC. In vitro dissolution studies demonstrated that the drug release from the microparticles was dependent upon enteric polymer: HPMC ratio and particle size distribution. At the ratio of at least 3.75:1 of enteric polymer: HPMC, drug release was suppressed most significantly in low pH (hydrochloric acid as medium) while rapid drug release was observed in pH 7.4.     

聚苯胺水基乳胶微粒的制备与性能研究

采用水溶性高聚物聚乙烯吡咯烷酮(PVP)作为空间稳定剂,利用分散聚合的原理成功地制备出了稳定的聚苯胺水基胶体分散液,聚苯胺复合乳胶粒子尺寸为几十至几百纳米,其粒径大小受PVP浓度、苯胺含量和反应温度等因素的影响.空间稳定剂可以提供胶体成核点.当PVP浓度较低时,聚合反应速率较小,当PVP浓度达到2%(质量分数)以后,聚合反应开始加速.红外光谱结果表明PAn-PVP复合物形成了分子内氢键.随着苯胺浓度的增加,聚苯胺电导率先增大后减少,最大值达到8.74×10-3S/cm,具有较好的应用前景.     

Preparation,characterization and mechanical properties of the polylactide/perlite and the polylactide/montmorillonite composites

In this study polylactide (PLA)/perlite and PLA/montmorillonite (MMT) composites were prepared by melt extrusion and solvent dissolution methods. The effects of organic/inorganic ratios and the kind of inorganic compounds on the characterization of the composite materials were investigated. The thermal stability of the organic–inorganic composite materials was evaluated by TGA and DSC, and the morphology of these composites was measured as SEM images. The modulus of elasticity was evaluated by Dynamic mechanical analysis (DMA). The PLA/inorganic composites exhibited remarkable improvement of mechanical and thermal properties when compared with those of the pure PLA.     

Preparation and characterization of safe microparticles based on xylan

This work describes the preparation and evaluation of safe xylan-based microparticles prepared by cross-linking polymerization using sodium trimetaphosphate. The resulting microparticles were evaluated for morphology, particle size, polymer-cross-link agent interaction, and in vitro toxicity. The microparticles showed narrow monodisperse size distributions with their mean sizes being between 3.5 and 12.5?µm in dried state. FT-IR analyzes confirmed the interaction between sodium trimetaphosphate and xylan during the cross-linking process with formation of phosphate ester bonds. Additionally, the X-ray diffraction patterns and FT-IR analyzes suggested that little or no cross-linking agent remained inside the microparticles. Furthermore, the in-vitro studies using Artemia salina and human erythrocytes revealed that the microparticles are not toxic. Therefore, the overall results suggest that these xylan microparticles can be used as a platform for new drug delivery system.     

Preparation,characterization and dissolution behavior of artemisinin microparticles

In the present study, a modified 4-fluid nozzle spray drier was used to prepare microparticles of a poorly water soluble drug, artemisinin with the aim of improving its solubility. We also investigated the effect of process variables on the physical properties and dissolution rate of spray dried artemisinin. A full factorial experimentally designed study was performed to investigate the following spray drying variables: inlet temperature and feed concentration. The artemisinin powder and spray dried artemisinin microparticles were characterized by scanning electron microscopy (SEM), differential scanning calorimetric (DSC), X-ray diffraction (XRD) and dissolution. SEM study suggested that the inlet temperature and feed concentration impacted on the particle size of the spray dried particles. The crystallinity of spray dried particles was slightly decreased with increasing inlet temperature and concentration. The dissolution of spray dried particles was markedly improved as compared to commercial artemisinin. A dissolution surface-response model was used to elucidate the significant and direct relationships between drug feed concentration and inlet temperature on one hand and dissolution on the other hand. The best dissolution was found to be 117.00 ± 5.15 μg/mL at the drug feed concentration of 10 g/L and inlet temperature of 140 °C.     

纳米TiO2/聚乳酸复合材料的制备和表征

采用原位聚合的方法制备了有机化处理过的纳米 TiO 2粒子质量分数分别为 1 wt %、3 wt %、5 wt %和10 wt %的 4种纳米 TiO 2/聚乳酸复合材料。SEM结果表明 , 当纳米 TiO 2粒子质量分数较低时 , 纳米 TiO 2在聚乳酸基体中呈现均匀稳定分散 , 而质量分数较高时则发生团聚。通过力学和热学等性能测试发现复合材料的最大热分解温度、 玻璃化转变温度和力学性能相对于聚乳酸有较大幅度提高 , 其中纳米 TiO 2的质量分数为 3 wt %时改善效果最明显 , 其最大热分解温度、 玻璃化转变温度分别比聚乳酸提高了 25. 3℃和 4. 9℃, 拉伸强度、 断裂伸长率和弹性模量分别提高了 83. 6 %、 6. 73 %和 129. 4 %。     

Oxidative fabrication of spherical polycarbazole-based microparticles

A straightforward oxidative liquid phase polymerization (LPP) method has been successfully developed for the fabrication of spherical functional (polyCOOH) polycarbazole-based microparticles from corresponding carbazole-containing monomers. The influence of the chemical structure of starting carbazole monomers on the LPP-based microparticle formation has been deeply examined using scanning electron microscopy (SEM).     

原位聚合法制备纳米凹凸棒土/聚乳酸复合材料

将凹凸棒土（AT）进行提纯和有机改性后, 采用原位聚合法制备了OAT质量分数为1%、 3%、 5%的纳米凹凸棒土/聚乳酸复合材料（OAT/PLA-x）。采用红外、 扫描电镜、 X射线衍射等对复合材料进行了表征, SEM结果表明, 凹凸棒土粒子在复合材料中实现了均匀稳定分散。复合材料的力学性能和综合热性能测试表明: OAT/PLA-3复合材料的拉伸强度、 弹性模量分别比纯PLA增加98.6%和130.0%; 复合材料的热稳定性明显提高。同时, 复合材料的溶液降解速率也明显加快。      

Preparation and characterization of spironolactone-loaded gelucire microparticles using spray-drying technique

The basic objectives of this study were to prepare and characterize solid dispersions of poorly soluble drug spironolactone (SP) using gelucire carriers by spray-drying technique. The properties of the microparticles produced were studied by differential scanning calorimetry (DSC), scanning electron microscopy, saturation solubility, encapsulation efficiency, and dissolution studies. The absence of SP peaks in DSC profiles of microparticles suggests the transformation of crystalline SP into an amorphous form. The in vitro dissolution test showed a significant increase in the dissolution rate of microparticles as compared with pure SP and physical mixtures (PMs) of drug with gelucire carriers. Therefore, the dissolution rate of poorly water-soluble drug SP can be significantly enhanced by the preparation of solid dispersion using spray-drying technique.     

利用静电纺丝技术制备纳米黏土/聚乳酸复合纳米纤维与其表征

利用静电纺丝技术制备了纳米黏土/聚乳酸(PLA)复合纳米纤维,并将该复合纳米纤维收集成无纺布薄膜,采用SEM和TEM观察了复合纳米纤维的微观形貌和结构,分别利用XRD和TGA测试了复合纳米纤维的结晶行为及热学行为,并分析了复合纳米纤维薄膜的拉伸力学性能随纳米黏土含量的变化关系。结果表明:当PLA含量为10wt%、纳米黏土含量为1wt%、CHCl3与DMF体积比为3∶1溶剂条件下,所制备的纳米黏土/PLA复合纳米纤维的细度和均匀性均得到改善;XRD测试结果表明,纳米黏土成功附着在PLA中。TGA和力学测试结果表明,纳米黏土/PLA复合纳米纤维的热稳定性和力学性能相对于纯PLA纤维有较大幅度提高,当纳米黏土含量为1wt%时,其初始分解温度提高了60℃,拉伸强度、断裂伸长率和弹性模量分别提高了111.3%、74.9%和20.0%。     

SiO2包覆纳米SiC的制备及表征

采用正硅酸乙酯水解法在SiC表面包覆SiO2,并通过实验探讨了TEOS用量、总体系CTEOS等因素对包覆效果影响。实验确定了制备包覆粒子的优化工艺条件：SiC／TEOS的最佳物质量比值为5：1,最佳总体系CTEOS为0．2mol／L。采用ZETA、IR、XRD等测试手段对SiO2改性的碳化硅粉体进行了表征。沉降实验表明：碳化硅表面改性后,在硅溶胶中浆料的稳定悬浮性提高。     

基于激光捕捉微粒子实现微细加工的新概念研究

利用高倍显微物镜所聚合的激光在粒子表面所产生的辐射压可捕捉几个微米大小的高强度粒子,这些被捕捉的粒子在激光驱动下,能移动、转动及振动,可成为微加工工具,在被加工表面上形成微米乃至纳米级的表面微细切削。基于几何光学模型对捕捉进行数字仿真,所设计形状粒子的加工力最大可达到mW/N101.210-。     

Preparation and characterization of copolymerized methylsilsesquioxane-benzylsilsesquioxane microparticles for electrophoretic sol-gel deposition

Copolymerized methylsilsesquioxane-benzylsilsesquioxane, (100 – x)MeSiO_3/2·xBnSiO_3/2 (mol%), microparticles of 0.3–0.4 m in average diameter have been prepared by the sol-gel method and applied to the formation of thick films on indium tin oxide (ITO)-coated glass substrates by the electrophoretic deposition. The microparticles obtained were considered to be hybrid containing both methyl and benzyl groups from thermal analyses and structural investigations. The microparticles became fusible at x 80 by a heat treatment. Thick film, ca. 5 m thick, consisting of electrophoretically deposited pure BnO_3/2 microparticles became transparent upon thermal sintering of the particles during heat treatment at temperatures higher than 100°C. On the other hand, the increase in optical transmittance during the heat treatment of the films consisting of 20MeSiO_3/2·80BnSiO_3/2 microparticles was as small as about 20% in visible range even after the heat treatment. The smaller increase in transmittance is probably due to the relatively high viscosity of the 20MeSiO_3/2·80BnSiO_3/2 upon sintering in comparison with pure BnO_3/2 for elimination of the voids in the films.