Adsorption of an amine drug onto microcrystalline cellulose and silicified microcrystalline cellulose samples

The adsorption of a model amine drug (tacrine hydrochloride) from aqueous solution onto 21 microcrystalline cellulose (MCC) based samples has been investigated. The MCC source (manufacturer) affected adsorption. The adsorption appeared to be fully reversible. Adsorption was reduced by the use of high-density grade MCC, high-energy milling, and silicification. Adsorption of the model drug was not affected by the particle size of the MCC. Significant variations of the adsorption characteristics between batches of certain MCC products were found. The primary mode of adsorption was by ion exchange.     

微晶纤维素的制备及性质研究

分别用HCl和H2SO4处理从棉纤维和稻秆中提取的纤维素，制备得到微晶纤维素。研究了酸处理对微晶纤维素的聚合度、结晶度、体积密度和热稳定性的影响．X射线衍射结果表明，纤维素微晶化后仍保持原来的晶型和晶区和非晶区两相共存的微细结构。扫描电子显微镜测试结果表明，不同原料，酸处理后所得产物的形态不同．     

Weight and weight uniformity of hard gelatin capsules filled with microcrystalline cellulose and silicified microcrystalline cellulose

The objective of this study was to investigate the weight and weight uniformity of hard gelatin capsules filled with microcrystalline cellulose (MCC) and silicified microcrystalline cellulose (SMCC) powdered formulations. A tamping-type encapsulation apparatus was used to fill the capsules. The four formulations that were tested included MCC alone, MCC blended with fumed silica, SMCC, and high-density SMCC (SMCC-HD). The mean capsule weight and the average variation in mean capsule weight of each formulation were determined. Both SMCC products exhibited better flow than the MCC alone, with SMCC-HD being the freest flowing of the powders investigated. Capsules filled with the SMCC products had higher fill weights than those containing the MCC powders. The SMCC-containing capsules exhibited the lowest variation in weight, although these findings were not significantly different from either of the MCC-containing capsules. Significantly higher weight variations were found in capsules filled with SMCC-HD. A relationship between Carr's compressibility index and capsule weight variation was found, with more compressible materials producing more uniformly filled capsules. No relationship could be established between powder flow and capsule weight uniformity. These findings suggest that powder flow may not be a critical parameter in ensuring capsule weight uniformity when the encapsulation equipment utilizes a tamping-type filling system.     

Effect of amount and composition of granulation liquid on mixing, extrusion and spheronization

Avicel RC 581 is regarded as an excellent excipient in formulations for extrusion (1). The CMC-Na in this microcrystalline cellulose improves the binding properties and the plasticity. In this study Avicel RC 581 was mixed in various ratios with theophylline. These mixtures were granulated with either water or water/ethanol (60/40) mixtures in a Collette high shear mixer. The power consumption during mixing was recorded as a function of the amount of granulation liquid. From the mixtures obtained in this way the plasticity / viscosity was determined before extrusion. Measurement of the plasticity / viscosity was carried out in an apparatus similar to the one described by Alleva et a1 (2). Extrusion was done using a Fuji Paudal extruder (EXD-60); the power consumption during extrusion was recorded.

The influence of the amount and composition of the granulation liquid on the various power consumptions and on plasticity / viscosity will be discussed, as well as the spheronization behaviour of the extruded pellets.     

Preparing of pellets by extrusion/spheronization using different types of equipment and process conditions

Introduction: The focus of this work was to produce matrix pellets made by extrusion/ spheronization using two types of equipment. The aim was to accomplish the laboratory-scale I process that has been already optimized and accepted with another type of equipment (laboratory-scale II).

Methods: A matrix pellet formulation consisting of MCC, Eudragit NE 30D and diclofenac sodium was used in the two types of equipment. Physico-chemical parameters and the dissolution profiles of the pellets in phosphate buffer pH 6.8 were compared.

Results: Pellets from both processes were similar in shape and tensile strength. They differed in particle size and dissolution profile. This may be contributed to different spheronization conditions.     

Effect of microcrystalline cellulose grade and process variables on pellets prepared by extrusion-spheronization

This study evaluated the effects of spheronizer load and speed on the size, circularity, microporosity, compressibility, and friability of pellets prepared by extrusion-spheronization of wet microcrystalline cellulose (MCC) masses with a water content shown by mixer torque rheometry to ensure maximum consistency. Two MCC grades with different mean particle size were used. Both gave pellets with good particle size, sphericity, and compressibility, under a wide range of spheronization conditions. Modification of pellet properties of interest (including size and porosity) was possible by adjustment of spheronization conditions and MCC grade; in particular, pellet porosity was greater with MCC of larger particle size.     

Effects of process variables on the size, shape, and surface characteristics of microcrystalline cellulose beads prepared in a centrifugal granulator

Preparation of microcrystalline cellulose (MCC) beads with a laboratory-scale centrifugal granulating apparatus was studied, and the pharmaceutical quality of the beads was characterized with respect to the subsequent drug layering. Five process parameters of potential importance, including rotor rotation speed X1, slit air X2, spray air pressure X3, spray air rate X4, and height of nozzle setting X5, were evaluated using a fractional factorial design (FFD 2(5-2)) as the experimental design. The responses evaluated were expected yield, mean size, size distribution, shape characteristics (including roundness, circularity, elongation, rectangularity, and modelx), and friability. All five process parameters studied were found to have an influence on the selected properties of the beads, but the effects of rotor rotation speed, slit air flow rate, and spray air rate were statistically significant (p < .05). The effect of the rotor rotation speed was found to be the most potent on all the responses studied. The results also show some significant interactions between the parameters tested. The most significant interactions were between rotor rotation speed and slit air, rotor rotation speed and spray air, and slit air and spray air.     

Extrudate fracture and spheronisation of microcrystalline cellulose pastes

An experimental study of the ram extrusion and subsequent spheronisation of water-based microcrystalline cellulose (MCC) pastes has been performed. The effects of extrusion velocity, die geometry, and paste water content on the integrity of the extrudate produced were investigated. The apparent severity of extrudate fracture increased with decreasing die length/diameter ratio (L/D), and increasing extrusion velocity. The spacing between the fractures was approximately constant for a given set of process conditions, and increased with increasing émph{L/D} and decreasing extrusion velocity, whilst the flare of the extrudate fracture segment increased with decreasing émph{L/D} and increasing extrusion velocity. Two types of fracture shape were identified, émph{viz}. knuckle-bones and cups, the occurrence of which is explained in terms of the relative extent of the radial and axial strain release at the surface of the extrudate upon exiting the die.The shape and size distributions of the corresponding spheronised pellets were analysed and related to the geometry of the extrudate fracture segments. Severe knuckle-bone fracture gave spherical pellets with a wide size distribution. Visibly smooth extrudates gave non-spherical pellets with an apparently narrow size distribution (as measured by sieving). Extrudates displaying the cup type of fracture generated the best quality pellets in terms of both sphericity and size distribution.     

Preparation and characterization and release properties of Eudragit RS based ibuprofen pellets prepared by extrusion spheronization: effect of binder type and concentration

Objective: The effects of type and concentration of binding agent on properties of Eudragit RS based pellets were studied.

Materials and methods: Pellets containing ibuprofen (60%), Eudragit RS (30%), Avicel (10%) were prepared by extrusion spheronization. PVP K30, PVP K90, HPMC 6cp, HPMC K100LV or HPMC K4M were used as binders in concentrations of 2, 4 or 6% based on the total weight of formulation. The process efficiency, pellet shape, size distribution, crushing strength, elastic modulus and drug release were examined. The effect of curing on pellet properties was also investigated.

Results: The process of extrusion spheronization became difficult with increase in binder viscosity and/or concentration. An increase in binder viscosity and/or concentration resulted in reduction in the yield of pellets, wider particle size distribution and departure from spherical shape especially in the case of HPMC binder. The crushing strength and elastic modulus of pellets decreased with increase in PVPs concentration. However this was not the case for pellets containing HPMCs. Drug release rate increased as the concentration of binder increased. Pellets containing 2%w/w of PVP K30 showed the slowest release rate. For those pellets with brittle nature, curing changed the behavior of pellet under mechanical test to plastic deformation. Yield point and elastic modulus of all formulations decreased after curing. Curing decreased the drug release rate.

Conclusion: Binder type and concentration significantly affected the properties of pellets. For production of sustained release ibuprofen Eudragit RS based pellets lower viscosity binders (PVP K30) with concentrations less than 4%w/w was optimum.     

Preparation of lipid aspirin sustained-release pellets by solvent-free extrusion/spheronization and an investigation of their stability

A novel solvent-free extrusion/spheronization technique was investigated for preparing stable aspirin sustained-release pellets. Lipids as binders and the matrix in this technique were extruded below their melting points, and spheronized in a thermomechanical process. Four types of lipids (adeps solidus, Compritol(?) 888 ATO, Precirol(?) ATO5 and Compritol(?) HD5 ATO) and their admixture in different ratios were used to obtain spherical and extended-release pellets. Pellets containing 80% aspirin, 15% adeps solidus and 5% Compritol(?) 888 ATO had the best spherical geometry and met the dissolution requirements of aspirin extended-release tablets in USP 31. Storage stability studies showed that the content of free salicylic acid increased sharply in the traditional pellets produced by wet extrusion/spheronization, from 1.91 to 7.84%, whereas there was little increase in the lipid pellets (from 0.48 to 1.08%). The dissolution rate from the optimal pellets (F11) stored at 26°C did not change, but became faster at 40°C/RH75% after 5 months. Powder X-ray diffraction, scanning electron microscopy (SEM) and differential scanning calorimetry were used to investigate the physical properties of the pellets during stability testing. The increase in the rate of drug release from aged pellets (40°C/RH75%) may result from the partially melted adeps solidus observed in SEM photographs. This study suggests that it is possible to prepare sustained-release pellets by solvent-free extrusion/spheronization using an appropriate mixture of lipids with high stability. In particular, this novel technique is excellent for hygroscopic drugs.     

Effects of grinding with microcrystalline cellulose and cyclodextrins on the ketoprofen physicochemical properties

Ground mixtures of ketoprofen (KETO) with native crystalline β-cyclodextrin, amorphous statistically substituted methyl-β-cyclodextrin, and microcrystalline cellulose were investigated for both solid phase characterization (differential scanning calorimetry (DSC) powder X-ray diffractometry, and infrared (IR) spectrometry) and dissolution properties (dispersed amount and rotating disk methods) to evaluate the role of the carrier on the performance of the final product. The effects of different grinding conditions, partial sample dehydration, and 1 year storage at room temperature were also investigated. The results pointed out the importance of the carrier nature on the efficiency of the cogrinding process. Both cyclodextrins were much more effective than was microcrystalline cellulose, even though no true inclusion complex formation occurred by mechanochemical activation. The best results were obtained from ground mixtures with methyl-β-cyclodextrin, which showed the best amorphizing and solubilizing power toward the drug and permitted an increase of approximately 100 times its intrinsic dissolution rate constant, in comparison with the approximate 10 times increase obtained from ground mixtures with β-cyclodextrin.     

In-situ thermoset polyurethane coating of glass beads dispersed in polystyrene by reactive extrusion

The condensation reaction between hydroxyl terminated polybutadiene and an uritonimine modified 4, 4 diphenylmethane diisocyanate (liquid MDI) was carried out by reactive extrusion in the presence of propyl trietoxy amino silane treated glass-beads and polystyrene. Reactants were selected having a surface tension favoring the glass bead coating using the spreading coefficient concept. FTIR, SEC (size exclusion chromatography) and rheological analysis of the resultant material showed that condensation reaction had occurred leading to crosslinked Polyurethane located principally around the glass beads.     

海藻酸钠/纤维素水凝胶球的制备与应用

利用基于p H值反转的落球法制备出不同质量分数的纤维素和海藻酸钠复合水凝胶球,并采用扫描电子显微镜(SEM)和傅里叶变换红外光谱(FTIR)对凝胶样品的形貌和化学态进行表征。结果表明海藻酸钠含量≤50%时凝胶球可以保持稳定的球形结构,内部为纤维链交叉聚集的三维网络多孔结构。复合凝胶球对亚甲基蓝、金胺O和臧红T等阳离子染料有着良好的吸附效果,含有50%海藻酸钠凝胶球对亚甲基蓝的吸附量为163.36 mg/g,吸附过程满足准二阶动力学方程,经过5次吸附脱附实验后仍然保持初始81%的吸附量。因此,该复合凝胶球可以作为一种低成本的生物吸附剂用于染料处理领域。     

Structure and superparamagnetic behaviour of magnetite nanoparticles in cellulose beads

Superparamagnetic magnetite nanoparticles were obtained starting from a mixture of iron(II) and iron(III) solutions in a preset total iron concentration from 0.04 to 0.8 mol l⁻¹ with ammonia at 25 and 70 °C. The regeneration of cellulose from viscose produces micrometrical spherical cellulose beads in which synthetic magnetite were embedded. The characterization of cellulose-magnetite beads by X-ray diffraction, Scanning and Transmission Electron Microscopy and magnetic measurement is reported. X-ray diffraction patterns indicate that the higher is the total iron concentration and temperature the higher is the crystal size of the magnetite obtained. Transmission Electron Microscopy studies of cellulose-magnetite beads revealed the distribution of magnetite nanoparticles inside pores of hundred nanometers. Magnetite as well as the cellulose-magnetite composites exhibit superparamagnetic characteristics. Field cooling and zero field cooling magnetic susceptibility measurements confirm the superparamagnetic behaviour and the blocking temperature for the magnetite with a mean size of 12.5 nm, which is 200 K.     

淀粉/微晶纤维素填充聚氨酯泡沫塑料的制备与力学性能

利用模塑成型方法,在聚氨酯泡沫塑料中引入了淀粉和微晶纤维素两种易于生物降解的填料,制备了不同淀粉和微晶纤维素填充量的聚氨酯泡沫塑料,并研究了填料种类和用量对聚氨酯泡沫塑料力学性能的影响.确定了填料在聚氨酯泡沫塑料中的最大填充量,并发现填料的加入使得硬质聚氨酯泡沫塑料(RPUF)的冲击强度下降,当两种填料含量为40份时,RPUF的压缩强度均达到最大值;使得半硬质聚氨酯泡沫塑料(SRPUF)的拉伸强度升高;当两种填料含量为30份时,SRPUF的拉伸强度均达到最大值;淀粉和微晶纤维素含量分别为20份和10份时,两种SRPUF的断裂伸长率达到最大值.     

Low frequency dielectric spectroscopy characterization of microcrystalline cellulose, tablets and paper

Cellulose fibres and particles in the form of powder, tablets and paper sheets have been investigated by very low frequency dielectric spectroscopy using a novel form of dielectric cell, in which two planar electrodes have been mounted in fixed positions at right angles. The broad pattern of response obtained from the samples is independent of the structural form of the cellulose sample, a loss peak in the 0.1–100 Hz range, and at lower frequencies a dispersion process which is dominated by an imperfect charge transport. Moisture has a significant influence on the rate of charge transport. In dry samples the dipolar loss peak was not evident but as the moisture content increased it appeared. Using a humidity normalizing technique the dielectric response for microcrystalline cellulose has been characterized over the equivalent of 14 decades in frequency. It has also been shown that there is a linear response between the capacitance and the density of microcrystalline cellulose samples. The consolidation of powder into tablets is discussed with respect of the observations of changes in capacitance, loss peak frequency and imperfect charge transport efficiency. Furthermore it was found possible to investigate differences between the dipolar relaxation rate “in” and “out” of the plane of paper in the stack. The relaxation time for dipoles “out” of the paper plane is 7 to 8 times longer than for dipoles “in” the paper plane. This revised version was published online in November 2006 with corrections to the Cover Date.     

Steel fibre reinforced concrete. The effect on fibre orientation of compaction by vibration

In the study of steel fibre reinforced concretes and mortars, it has often been assumed that the fibres are randomly distributed in three dimensions in the test specimens. It is shown herein, that this assumption is unlikely to be correct if the specimens are compacted by external vibration.     

微晶纤维素基复合材料的制备及其对亚甲基蓝的催化降解性能

以微晶纤维素(MCC)为原料,通过在其表面负载纳米氧化铜颗粒(CuO NPs),添加3-氯丙基三甲氧基硅烷(CPTES)与二乙醇胺(DEA)进行接枝反应制备CuO NPs@MCC–Si–N(OH)₂复合材料。探讨了DEA添加量对CuO NPs@MCC–Si–N(OH)₂性能的影响,表征并分析了改性微晶纤维素红外光谱、晶体结构、表面形貌和热稳定性。结果表明,CuO NPs可成功负载在MCC表面,硅烷偶联剂可提高复合材料的分散性与接枝胺基的能力,进而增强其催化活性,使硼氢化钠(NaBH₄)与亚甲基蓝(MB)氧化还原反应效率增加,快速降解MB染色剂。通过优化发现DEA用量为20wt%时制得的CuO NPs@MCC–Si–N(OH)₂催化效果最佳,CuO NPs@MCC–Si–N(OH)₂和NaBH₄的用量分别为30 mg和10 mg,处理30 mL 3 mmol/L MB溶液5 min后,MB去除率可达99.71%,五次循环性测试后,去除率为93.24%。      

Eco-friendly hybrid pigments made of cellulose and iron oxides

The controlled hydrolysis of FeC2O4 in the presence of vegetable cellulose fibres was investigated to produce a pallet of cellulose/iron oxide hybrid colored materials. Distinct iron oxide phases have been deposited at the cellulose fibres surfaces by varying the relative amount of FeC2O4 and NaOH, here used as starting materials, by performing the synthesis in hydrothermal conditions. This is a new chemical strategy for the production of a number of hybrid materials whose coloristic properties have been evaluated aiming their potential use as novel pigments for polymer based products.