Spherical Granules Research Articles

Effect of Agaricus bisporus polysaccharide flour and inulin on the antioxidant and structural properties of gluten-free breads

Enrichment of gluten-free bread (GFB) with mushroom polysaccharide and prebiotic is necessary to enhance its organoleptic and health attributes. This work investigated the enrichment effect of the GFB with Agaricus bisporus polysaccharide (ABP) flour and inulin. Volatile compounds, as well as the antioxidant and structural properties of the fortified GFB were evaluated. Sweet potato-glutinous rice flour was fortified with ABP flour and the same with inulin at different levels (3, 6 and 9%), besides a constant percentage of xanthan gum (0.5%) was added to all the blends. Addition of ABP flour resulted in higher levels of volatile compounds compared to inulin addition and the control. ABP flour formulation (F3) had the highest total phenolic content (19.05 mg GAE/g), reducing power (5.31 mg/mL, EC50 value), DPPH (6.85 mg/mL, EC50 value), ABTS (8.86 mg/mL, EC50 value) radical-scavenging activities, and β-carotene bleaching (13.22 mg/mL, EC50 value). Conversely, the control and inulin formulation (F1) showed the lowest levels of these activities. The micrographs of the ABP flour formulations showed polyhedral, aggregated, and some spherical granules, whereas inulin formulations revealed spherical granules bound together with deformed granules. FTIR spectroscopy confirmed the presence of the amide I band and both α- and β-glycosidic linkages. The current findings exhibited that ABP flour and inulin had good attributes to improve the antioxidant activity of GFB and modify its structural characteristics.

Managing Properties of Alumina Based Granules Prepared by Disk (Dished) Molding

Alumina-based spherical granules were prepared by disk granulation. Products of gibbsite thermoactivation in various reactors were used as the initial materials. In the course of molding, combustible additives (starch, carbon, wood meal) were added to the thermoactivated gibbsite powder, and NaOH (10 %), C2H5OH (15 %), Н3ВО3(6 %) to the wetting solution (H2O). With the product of centrifugal thermoactivation of hydrargillite, the prepared granules were stronger at the larger average size of pores; addition of NaOH, C2H5OH and H3BO3led to an increase in the specific surface area and micropore proportion but had different effects on the mechanical strength of the granules. Introduction of combustible additives (wood meal, activated carbon) affected only slightly the specific surface area, favored an increase in the total pore volume and mesopore volume, resulted in a decrease in bulk density and mechanical strength of the granules. Conditions were determined for preparation of a highly effective strong dessicant with large specific surface area (up to 340 m2/g) and average pore diameter up to 3.4 nm. Conditions were determined for preparation of strong ultramacroporous granules that are highly active to the Klaus process.

Mechanisms of Forming Hollow Microspheres from Solid Granules

Problems in fabrication of large-size hollow microspheres with specific properties and ideal geometric parameters for inertial confinement fusion and other applications require profound knowledge of their formation processes. In this work, we analyze experimentally and analytically the formation of hollow microspheres from solid spherical granules by high-temperature foaming and formulate the conditions for fabrication of microcapsules with high parameters in high-temperature processes.

Development of Novel Functional Formulations Based on Pharmaceutical Technologies

After 32 years as a researcher in a pharmaceutical company, the author has served as a professor in the Development of Pharmaceutical Engineering and Drug Delivery Science at University of Shizuoka for the past 11 years. The research I was involved in can be categorized into four main items. First, the crystal transformation of clarithromycin (CAM) was focused on to develop the CAM high-loaded sustained release and gastro-floating formulations. Furthermore, the stabilization mechanism of CAM in the gastro-intestinal tract was clarified to elucidate gel formation under conditions of low pH. Second, the development of novel dosage regimens and optimization of formulation design were carried out using powder technology. In this category, a wax matrix formulation for taste masking, highly drug-loaded fine globular granules using a multi-functional rotor processor, and orally disintegrating tablets treated with microwave or high-pressure carbon dioxide were our targets. The third category was the manufacture of dispersion systems including lipid nanoparticles and cubosomes in order to improve the bioavailability and stability of poorly water-soluble drugs. The fourth category was the development and application of novel physical testing methods including investigation of the internal structure of fine granules using microtomography with synchrotron X-ray radiation, dissolution of spherical granules under non-sink conditions, mathematical models to analyze the dissolution behavior of metastable crystals or amorphous drugs and prediction of the available surface area of tablets during dissolution process.

Microfluidic Extractive Crystallization for Spherical Drug/Drug-Excipient Microparticle Production

Granulation is a common manufacturing step for pharmaceutical drug products, which improves powder flowability, compactibility, and ensures tablet content uniformity. Granules of uniform content can conventionally be challenging to obtain due to powder segregation and mixing issues prior to granulation. Spherical crystallization—a method where drug crystals are directly formed into spherical granules—is a promising way to overcome issues with mixing and form granules with uniform content. However, a common challenge of existing quasi emulsion solvent diffusion or solvent extraction methods for spherical crystallization involving miscible solvents in stirred batch vessels is the coarse control over particles sizes, as they are sensitive to multiple scale-up factors (mixing efficiency, impeller and vessel geometry, inlet configuration). This limits the method in terms of content uniformity, which in turn limits the extent to which granules with tunable dissolution profiles can be created. Here, we propose a...

Expression of Maize MADS Transcription Factor ZmES22 Negatively Modulates Starch Accumulation in Rice Endosperm.

As major component in cereals grains, starch has been one of the most important carbohydrate consumed by a majority of world’s population. However, the molecular mechanism for regulation of biosynthesis of starch remains elusive. In the present study, ZmES22, encoding a MADS-type transcription factor, was modestly characterized from maize inbred line B73. ZmES22 exhibited high expression level in endosperm at 10 days after pollination (DAP) and peaked in endosperm at 20 DAP, indicating that ZmES22 was preferentially expressed in maize endosperm during active starch synthesis. Transient expression of ZmES22 in tobacco leaf revealed that ZmES22 protein located in nucleus. No transactivation activity could be detected for ZmES22 protein via yeast one-hybrid assay. Transformation of overexpressing plasmid 35S::ZmES22 into rice remarkedly reduced 1000-grain weight as well as the total starch content, while the soluble sugar was significantly higher in transgenic rice lines. Moreover, overexpressing ZmES22 reduced fractions of long branched starch. Scanning electron microscopy images of transverse sections of rice grains revealed that altered expression of ZmES22 also changed the morphology of starch granule from densely packed, polyhedral starch granules into loosely packed, spherical granules with larger spaces. Furthermore, RNA-seq results indicated that overexpressing ZmES22 could significantly influence mRNA expression levels of numerous key regulatory genes in starch synthesis pathway. Y1H assay illustrated that ZmES22 protein could bind to the promoter region of OsGIF1 and downregulate its mRNA expression during rice grain filling stages. These findings suggest that ZmES22 was a novel regulator during starch synthesis process in rice endosperm.

Reduction of falling number in soft white spring wheat caused by an increased proportion of spherical B-type starch granules

A low falling number (FN) in wheat indicates high α-amylase activity associated with poor end-use quality. We hypothesize starch – the substrate of α-amylase, can directly influence hot flour pasting properties and its susceptibility to α-amylase, which further affects viscosity. We examined the structural characteristics of starch in three soft white spring wheat cultivars grown in Idaho in 2013 (normal FN year) and 2014 (low FN year with pre-harvest rains). Our data surprisingly show that starch in some low FN wheat was not significantly degraded by α-amylase but had developmental changes with an increased proportion of B-type wheat starch. We reconstituted wheat starch and verified that starch with an increase of B-granules has a relatively low viscosity and high susceptibility to wheat α-amylase, which further facilitates the decrease of viscosity. The influence of starch structure and starch-enzyme interaction must be considered while developing a solution to the low FN issue.

Osteoinductivity of Porous Biphasic Calcium Phosphate Ceramic Spheres with Nanocrystalline and Their Efficacy in Guiding Bone Regeneration.

Conventional biphasic calcium phosphate (BCP) bioceramics are facing many challenges to meet the demands of regenerative medicine, and their biological properties are limited to a large extent due to the large grain size in comparison with nanocrystalline of natural bone mineral. Herein, this study aimed to fabricate porous BCP ceramic spheres with nanocrystalline (BCP-N) by combining alginate gelatinizing with microwave hybrid sintering methods and investigated their in vitro and in vivo combinational osteogenesis potential. For comparison, spherical BCP granules with microcrystalline (BCP-G) and commercially irregular BCP granules (BAM, BCP-I) were selected as control. The obtained BCP-N with specific nanotopography could well initiate and regulate in vitro biological response, such as degradation, protein adsorption, bone-like apatite formation, cell behaviors, and osteogenic differentiation. In vivo canine intramuscular implantation and rabbit mandible critical-sized bone defect repair further confirmed that nanotopography in BCP-N might be responsible for the stronger osteoinductivity and bone regenerative ability than BCP-G and BCP-I. Collectedly, due to nanotopographic similarities with nature bone apatite, BCP-N has excellent efficacy in guiding bone regeneration and holds great potential to become a potential alternative to standard bone grafts in bone defect filling applications.

Synthesis of Sm–Co nanoparticles by sol–gel method

Sm–Co nanoparticles have promising applications in both scientific and industrial fields. In this paper, Sm–Co single-crystal nanoparticles were prepared using respective metal salts and complexing agents, such as citric acid by Pechini-type sol–gel method. The mixture solution was heated to form a highly viscous gel, and then heated at different temperatures to achieve SmCo-oxide. And then Sm–Co particles were yielded by reductive annealing of the precursors. Phase analysis, microstructural investigation and magnetic properties were performed by X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), Fourier transform infrared (FT-IR) and VSM. TGA trace analysis of the gel determined the heat treatment temperature. XRD results showed that SmCoO3 and Co3O4 were obtained at 800[Formula: see text]C, FT-IR spectrometry analysis also verified the results. In the calcium-thermal reduction process, Sm2O3 and Co were obtained after reductive annealing at 800[Formula: see text]C, meanwhile Sm–Co nanoparticles were formed at 850[Formula: see text]C. FESEM analysis revealed that the Sm–Co nanoparticles were composed in the form of spherical granules and exhibited well distribution with size in the range of 100 nm. The room temperature saturation magnetization and coercivity of the Sm–Co nanoparticles were 49.61 emu/g and 3.53 kOe, respectively.

Prevalence, site of infection, and differentiating oocytes of the cymothoid isopod, Norileca indica (Milne Edwards, 1840) from its infected short mackerel, Rastrelliger brachysoma, in the Upper Gulf of Thailand

Norileca indica, a cymothoid isopod crustacean, is an obligate parasite infecting marine fishes in tropical areas. This study attempted to investigate the prevalence, site of infection and distinct stages of oogenesis of this parasitic isopod obtained from short mackerel (Rastrelliger bachysoma). All N. indica samples were collected and processed through histological techniques. N. indica showed higher prevalence during the dry season than the rainy season and its parasitic infections were more prevalent in the female R. brachysoma (60% prevalence) compared to males. Two distinct sites of N. indica attachment on the host (infection sites) including gill and integument were clearly observed. Interestingly, this isopod preferred to attach more on the integument surface than gill, especially in the female R. brachysoma (55% prevalence). Using histological observation, N. indica exhibited asynchronous development of oocyte in the ovary. The oocytes were enclosed by a thin layer of connective and muscular tissues. Three stages of oogenesis can be identified in the ovary: oogonium, primary oocyte, and secondary oocyte. Oogonium located inside the cyst near the germinal epithelium. A large nucleus of oogonium was surrounded by a weak basophilic cytoplasm. Unlike oogonium, multiple nuclei (2 - 3 nuclei) surrounded by basophilic cytoplasm was a key characteristic of the primary oocyte. The secondary oocyte contained spherical yolk granules with multiple layers of follicular cells, which might function to support yolk uptake into the ooplasm. In addition, early embryonic development of N. indica was also observed in this study. Taken together, this finding highlights parasitic prevalence and infection sites of N. indica in short mackerel, as well as a better resolution of its oogenesis, early development and reproductive cycle.

Influence of fermented and unfermented Agaricus bisporus polysaccharide flours on the antioxidant and structural properties of composite gluten-free cookies

Products fermented by probiotics are consumed worldwide and play important roles in human nutrition and health. In this study, the effects of fermented and unfermented Agaricus bisporus polysaccharide (FABP and UABP) flours on the structural and antioxidant properties of composite gluten-free (CGF) doughs and cookies were investigated. The extracted Agaricus bisporus polysaccharide flour was subjected to fermentation by Lactobacillus plantarum at 37 °C for 72 h. Incorporation of both FABP flour and UABP flour resulted in larger interconnected structures in doughs, with smoother surfaces being observed compared to the control. Moreover, FABP flour formulations showed higher total phenolic content (20.07–28.12 mg GAE/g, dwb), ABTS radical scavenging activity (82.17–86.82%) and β-carotene bleaching (68.80–83.72%), and UABP flour formulations had greater reducing power (0.61–0.83) and DPPH radical scavenging activity (78.66–91.22%), whereas less antioxidant activity was found in the control. Aggregated spherical granules were observed in all micrographs of CGF cookie formulations, and the control showed both individual and aggregated spherical granules. Several protein bands (20.1, 21.1, 32.0 and 33.1 kDa) with higher intensities were detected in all CGF cookie formulations compared to the control. Overall, the inclusion of mushroom polysaccharide flours could enhance the antioxidant attributes and alter structural characteristics of CGF cookies.

Numerical modelling of flow field within a packed bed of granular material

Computational domain discretization is the pre-processing stage in CFD analysis and it highly contributes to reducing the level of solution error as well as increasing the numerical stability of a model. The discretization of domain representing a packed bed of granular material is a demanding task due to the topology of the model consisting of spherical granules contacting tangentially and narrow regions in the direct vicinity of the contact point. Therefore the aim of the carried out research is to define guidelines to effectively discretize the computational domain representing the packed bed of granular material and validate it using Particle Image Velocimetry (PIV). Two methods of contact point representation between granules (contact point extension, granule radius reduction) and two mesh types (tetrahedral, polyhedral) are examined within the paper. Differences between the analyzed cases are discussed and compared to experimental research results. The obtained results prove that the applied method significantly affects the calculated porosity but does not affect the flow field considerably. Polyhedral mesh turned out to be preferable as the numerical model converges within substantially lower number of iterations and the obtained results are not as affected by the numerical diffusion as in the case of tetrahedral mesh.

Controlled energy dispersion in two-dimensional decorated granular crystals

The present study describes a way to control the dispersion of an impulse in a two-dimensional square granular crystal with tapered beads. The control is through the redirection of the characteristic load transfer path by controlling the shape of the scattering of wavefront. The main goal is to contribute to the development of appropriately designed granular media to mitigate impacts. The crystal is constituted of spherical granules with a wide range of radii. Interstitial particles are strategically positioned to allow a large number of collisions per unit area. The waves are produced by a striker that collides against the crystal. We analyze how material combinations, number of layers, tapering parameter, and disorder affect the decay of the wave amplitude. Our studies suggest that $\ensuremath{\sim}90%$ impulse attenuation can be accomplished using a system thickness of 5 grains.

Effects of granulation process variables on the physical properties of dosage forms by combination of experimental design and principal component analysis

The current study was to understand how process variables of high shear wet granulations affect physical properties of granules and tablets. The knowledge gained was intended to be used for Quality-by-Design based process design and optimization. The variables were selected based on the risk assessment as impeller speed, liquid addition rate, and wet massing time. Formulation compositions were kept constant to minimize their influence on granules properties. Multiple linear regression models were built providing understanding of the impact of each variable on granule hardness, Carr's index, tablet tensile strength, surface mean diameter of granules, and compression behavior. The experimental results showed that the impact of impeller speed was more dominant compared to wet massing time and water addition rate. The results also revealed that quality of granules and tablets could be optimized by adjusting specific process variables (impeller speed 1193 rpm, water spray rate 3.7 ml/min, and wet massing time 2.84 min). Overall desirability was 0.84 suggesting that the response values were closer to the target one. The SEM image of granules showed that spherical and smooth granules produced at higher impeller speed, whereas rough and irregular shape granules at lower speed. Moreover, multivariate data analysis demonstrated that impeller speed and massing time had strong correlation with the granule and tablet properties. In overall, the combined experimental design and principal component analysis approach allowed to better understand the correlation between process variables and granules and tablet attributes.

High-shear granulation of high-molecular weight hypromellose: effects of scale-up and process parameters on flow and compaction properties

Context: Knowledge of the effects of high-shear granulation process parameters and scale-up on the properties of the produced granules is essential for formulators who face challenges regarding poor flow and compaction during development of modified release tablets based on high-molecular weight hypromellose (hydroxypropylmethylcellulose (HPMC)) polymers. Almost none of the existing studies deal with realistic industrial formulation.Objective: The aim was to investigate the effects of scale-up and critical process parameters (CPPs) of high-shear granulation on the quality attributes of the granules, particularly in terms of the flow and compaction, using a realistic industrial formulation based on HPMC K100M polymer.Methods: The flow properties were determined using flow time, Carr index, tablet mass, and crushing strength variations. The compaction properties were quantified using the ‘out-of-die’ Heckel and modified Walker models, as well as the tensile strength profile and elastic recovery. High-shear granulation was performed at different scales: 4 L, 300 L, and 600 L.Results and conclusion: The scale itself had larger effects on the granule properties than the CPPs, which demonstrated high robustness of formulation on the individual scale level. Nevertheless, to achieve the desired flow and compaction, the values of the CPPs need to be precisely selected to fine-tune the process conditions. The best flow was achieved at high volumes of water addition, where larger and more spherical granules were obtained. The CPPs showed negligible influence on the compaction with no practical implications, however, the volume of water addition volume was identified as having the largest effects on compaction.

Preparation of spherical porous hydroxyapatite granules as support materials for microorganisms

Preparation of spherical porous hydroxyapatite granules as support materials for microorganisms

Processing of sintered and CVD coated SiC/CNFs thin composite tubes

Silicon carbide (SiC) and its composite powders dispersed with 1–3 wt% carbon nano-fibres (CNFs) were spray freeze granulated to produce spherical granules with uniform composition. Powders were shaped to thin dense tubes for use in a harsh environment by cold isostatic pressing followed by pressureless sintering at 2150 °C for 1 h in argon and SiC coating by chemical vapour deposition (CVD) technique. The physical, microstructural and thermo - mechanical properties of the composite tubes were evaluated and compared with bare SiC tubes. Good dispersibility of CNFs and sintering additives in the matrix by spray freeze granulation processing technique resulted in more than 98.5% theoretical density of the composite tubes with superior mechanical properties. SEM & EBSD analysis show grains are platy and equiaxed in nature with many CNFs trapped at the triple points hindering the SiC grain growth which is also confirmed by TEM analysis. The thermal conductivity value of the composite was also found higher than bare SiC at all temperatures when measured up to 1000 °C due to uniform distribution of CNFs in the matrix.

THE MICROHARDNESS OF THE ADDITIVE PRODUCTS OF THE ELECTRICAL DISCHARGE MACHINING OF COBALT POWDERS

The main requirement for powders for additive 3d technologies is the spherical shape of the particles. Such particles are most compact in a certain volume and provide "fluidity" of the powder composition in the material supply systems with minimal resistance. In addition, the powder must contain a minimum amount of dissolved gas. The microstructure of the powder should be uniform and fine (with a uniform distribution of phase components). Based on the features of methods for producing spherical powders to obtain spherical granules of regulated grain, the technology of electroerosion dispersion, characterized by relatively low energy costs and environmental cleanliness of the process, is proposed. The main advantage of the proposed technology is the use of waste as raw materials, which is much cheaper than the pure components used in traditional technologies. In addition, this technology is powder, which allows powder-alloys. To develop technologies for the reuse of electrical erosion powders and to evaluate the effectiveness of their use, complex theoretical and experimental studies are required. The aim of this work to study the microhardness of the additive products of the electrical discharge machining of cobalt powders. For the proposed studies selected waste cobalt alloy brand CHMS "CELLET". Butyl alcohol (butanol-1) was used as a working liquid. To obtain the cobalt powders used for the installation of AED dielectric materials. Dispersion parameters: voltage 100 V, capacity 48 UF, pulse repetition rate 120 Hz. According to the results of the research, it was experimentally established that the microhardness of additive products obtained from electroerosion powders with an average particle size of 52.5 µm is 5.7 GPA.

Physicochemical Properties of C-Type Starch from Root Tuber of Apios fortunei in Comparison with Maize, Potato, and Pea Starches.

The dry root tuber of Apios fortunei contained about 75% starch, indicating that it is an important starch resource. Starch displayed spherical, polygonal, and ellipsoidal granules with central hila. Granule sizes ranged from 3 to 30 μm with a 9.6 μm volume-weighted mean diameter. The starch had 35% apparent amylose content and exhibited CA-type crystalline structure with 25.9% relative crystallinity. The short-range ordered degree in the granule external region was approximately 0.65, and the lamellar thickness was approximately 9.6 nm. The swelling power and water solubility began to increase from 70 °C and reached 28.7 g/g and 10.8% at 95 °C. Starch had typical bimodal thermal curve in water with gelatinization temperatures from 61.8 to 83.9 °C. The 7% (w/w) starch-water slurry had peak, hot, breakdown, final, and setback viscosities of 1689, 1420, 269, 2103, and 683 mPa s, respectively. Rapidly digestible starch, slowly digestible starch, and resistant starch were 6.04%, 10.96%, and 83.00% in native starch; 83.16%, 15.23%, and 1.61% in gelatinized starch; and 78.13%, 17.88%, and 3.99% in retrograded starch, respectively. The above physicochemical properties of A. fortunei starch were compared with those of maize A-type starch, potato B-type starch, and pea C-type starch. The hierarchical cluster analysis based on starch structural and functional property parameters showed that A. fortunei and pea starches had similar physicochemical properties and were more related to maize starch than potato starch.

Porosity variation within a porous bed composed of multisized grains

We capture the interfacial region of randomly packed porous layers composed of multi-sized spherical or arbitrarily-shaped granules using X-ray computed tomography to explore the porosity-depth variation below a porous media interface. In the case of uni-sized spherical beads, we found in our previous study that the porosity varies from 1 to it's bulk value within a depth of the order of one grain diameter. In this study, we show that for the multi-sized spherical and randomly-shaped granules the porosity reaches it's bulk value within a depth equal to a multiple of the median diameter of the mixture. All multiplication factors for the samples examined here were between 2.6 and 3.8 and mimicked the experimental data with reasonable precision. A direct consequence of this observation is that the diffusion coefficient below the interface can not be considered as a constant. The effect of depth-dependent porosity on the the diffusion coefficient below the porous media interface was examined. It was found that the difference between a constant and a depth-dependent diffusion coefficient in the porous layer is significant and reaches up to 65% for sandy sediment (φb = 0.35) and 20% for highly porous media (φb = 0.90) immediately below the interface. This finding is of great significant when no experimental data of porosity as a function of depth is available. Such situations arise frequently in heat and mass transfer exchanges across fluid-porous or solid wall-porous boundaries.