高压微波催化合成肉桂酸甲酯

采用微波辐射技术，以一水硫酸氢钠为催化剂，由肉桂酸和甲醇直接酯化合成肉桂酸甲酯，用正交试验研究了各反应因素对产品收率的影响。确定其最佳反应条件为：酸醇摩尔比为1：5，催化剂用量为0.6g。微波功率为729W，辐射时间为5min，产品收率为98.8%。催化剂可重复使用。     

一水合硫酸氢钠催化β-萘甲醚的合成

利用一水合硫酸氢钠催化合成 β 萘甲醚 ,3 6 gβ 萘酚 ,3ml甲醇 ,1 5g一水合硫酸氢钠 ,80℃反应5h ,HPLC分析产率达 78 3%。固体催化剂容易过滤分离。     

一水硫酸氢钠催化合成乙二醇单甲醚乙酸酯

以一水硫酸氢钠为催化剂,由乙二醇单甲醚和冰乙酸合成了乙二醇单甲醚乙酸酯。考察了乙二醇单甲醚和冰乙酸摩尔比及催化剂用量对酯化率的影响。适宜反应条件为:乙二醇单甲醚∶冰乙酸∶一水硫酸氢钠=1∶1.75∶0.036(摩尔比),苯作带水剂,回流分水60min,酯化率达90.0%。产品经元素分析和红外光谱表征。     

Assessment of adhesion and autoadhesion forces between particles and surfaces. Part II. The investigation of adhesion phenomena of Salmeterol Xinafoate and lactose monohydrate particles in particle-on-particle and particle-on-surface contact

The centrifuge technique has been used to compare particle-on-particle and particle-on-surface adhesion with Salmeterol Xinafoate particles on single lactose particles or compacted lactose surfaces. The results from particle-on-particle and particle-on-surface adhesion measurements are not equivalent in terms of median adhesion force. The assessment of adhesion using either particle-on-particle or particle-on-surface systems depends on the process on which information is required: e.g. mixing problems are better investigated by applying the particle-on-particle technique, whereas surface transport problems such as powder compaction or flow can be more appropriately studied using particle-on-surface measurements. Taking autoadhesion measurements from the previous study into account, adhesion and autoadhesion forces were found to allow the prediction and choice of mixture components for powder blends. The results suggest that the homogeneity of such a powder blend depends both on thermodynamic properties and on the adhesion and autoadhesion properties of the single components.     

铁离子检测用自组装膜的光谱特性分析

以聚二烯丙基二甲基氯化铵（PDDA）和聚4-苯乙烯基磺酸钠（PSS）为前驱体,以1-亚硝基-2-萘酚-3,6-二磺酸二钠一水合物为铁离子指示剂,根据静电自组装原理,设计制备了对铁离子具有光学敏感性的自组装膜。采用紫外可见分光光度计考察了敏感膜的自组装制备过程,分析了不同指示剂含量的敏感膜与铁离子作用前后的光谱变化规律,并通过扫描探针显微镜对其微观形貌进行了观察,通过敏感膜与铁离子作用前后的特征峰分析,初步确定了敏感膜吸光度变化量与铁离子浓度间的对应关系。     

一水硫酸氢钠催化合成混合二元酸二辛酯

在一水硫酸氢钠催化剂作用下,以异辛醇及生产环己酮的副产混合二元酸为原料,考察了混合二元酸二辛酯合成的工艺条件。结果表明,最佳酯化反应条件为混合二元酸粗品14.6 g,异辛醇40 mL,以15 mL二甲苯作带水剂,催化剂一水硫酸氢钠0.30 g,110～156℃回流反应1.5 h。在该优化条件下,混合二元酸的酯化率达99.64%。催化剂经重结晶后可重复使用。     

固体酸催化蓖麻油制备生物柴油

以一水硫酸氢钠固体酸为催化剂,对蓖麻油酯交换制备生物柴油进行了研究。在反应温度为75℃条件下,考察了醇油摩尔比、催化剂用量(占油质量)及反应时间对酯交换反应的影响。在反应温度为75℃、醇油摩尔比为9∶1、催化剂用量为4%、反应时间为8 h的优化工艺条件下,平均甘油收率达93%,产物中甲酯总含量为95.20%。甲酯和甘油静置分层快,后处理简单,对环境无污染。     

Characterization and selection of suitable grades of lactose as functional fillers for capsule filling: part 1

The purpose of this work is to characterize thermal, physical and mechanical properties of different grades of lactose and better understand the relationships between these properties and capsule filling performance. Eight grades of commercially available lactose were evaluated: Pharmatose 110?M, 125?M, 150?M, 200?M, 350?M (α-lactose monohydrate), AL (anhydrous lactose containing ～80% β-AL), DCL11 (spray dried α-lactose monohydrate containing ～15% amorphous lactose) and DCL15 (granulated α-lactose monohydrate containing ～12% β-AL). In this study, different lactose grades were characterized by thermal, solid state, physical and mechanical properties and later evaluated using principal component analysis (PCA) to assess the inter-relationships among some of these properties. The lactose grades were characterized by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), X-ray diffraction (XRD), moisture sorption/desorption isotherms, particle size distribution; the flow was characterized by Carr Index (CI), critical orifice diameter (COD) and angle of friction. Plug mechanical strength was estimated from its diametric crushing strength. The first and second principal components (PC) captured 47.6% and 27.4% of variation in the physical and mechanical property data, respectively. The PCA plot grouped together 110?M, AL, DCL11 and DCL15 on the one side of plot which possessed superior properties for capsule formulation and these grades were selected for future formulation development studies (part II of this work).     

Dextrose monohydrate as a non-animal sourced alternative diluent in high shear wet granulation tablet formulations

The feasibility of dextrose monohydrate as a non-animal sourced diluent in high shear wet granulation (HSWG) tablet formulations was determined. Impacts of granulation solution amount and addition time, wet massing time, impeller speed, powder and solution binder, and dry milling speed and screen opening size on granule size, friability and density, and tablet solid fraction (SF) and tensile strength (TS) were evaluated. The stability of theophylline tablets TS, disintegration time (DT) and in vitro dissolution were also studied. Following post-granulation drying at 60?°C, dextrose monohydrate lost 9% water and converted into the anhydrate form. Higher granulation solution amounts and faster addition, faster impeller speeds, and solution binder produced larger, denser and stronger (less friable) granules. All granules were compressed into tablets with acceptable TS. Contrary to what is normally observed, denser and larger granules (at ≥21% water level) produced tablets with a higher TS. The TS of the weakest tablets increased the most after storage at both 25?°C/60% RH and 40?°C/75% RH. Tablet DT was higher for stronger granules and after storage. Tablet dissolution profiles for 21% or less water were comparable and did not change on stability. However, the dissolution profile for tablets prepared with 24% water was slower initially and continued to decrease on stability. The results indicate a granulation water amount of not more than 21% is required to achieve acceptable tablet properties. This study clearly demonstrated the utility of dextrose monohydrate as a non-animal sourced diluent in a HSWG tablet formulation.