Particle Size Distribution Of Granules Research Articles

Influence of drought stress and growth temperature during kernel development on physical and chemical starch characteristics of malting barley

AbstractBackground and ObjectivesStarch is the main component of malting barley (Hordeum vulgare L.), and its physical and chemical characteristics are particularly important in further processing in the beverage industry. This study investigates how the parameters (i) growing temperature (high/low) and (ii) water deficit (drought stress) during grain filling affect starch characteristics by cultivating nine different commonly used malting barley varieties in greenhouses under defined conditions. Particle size distribution of the starch granules, their phase transition characteristics (DSC), the pasting temperature (RVA), and the amylose/amylopectin (AM/AP) ratio were examined to assess starch characteristics.FindingsTwo‐way ANOVA analyses revealed that drought stress during the grain‐filling phase resulted in significantly smaller starch granules, lower onset, peak, and endset temperatures (DSC), and increased pasting temperature (PT) while not affecting the AM/AP ratio. High growth temperature during grain filling resulted in significantly higher onset, peak, and endset temperatures (DSC), lower phase transition enthalpies, significantly higher PTs, and lower AM/AP ratios.ConclusionsGrowth temperature during kernel development affected starch phase transition characteristics the most, while water availability was significantly associated with starch granule sizes.Significance and NoveltyClimate change is increasing the events and severity of heat and drought in Europe. Agricultural practices and modern barley varieties must be adapted to these requirements to maintain processability for food production.

In-line particle size measurement during granule fluidization using convolutional neural network-aided process imaging

This paper presents a machine learning-based image analysis method to monitor the particle size distribution of fluidized granules. The key components of the direct imaging system are a rigid fiber-optic endoscope, a light source and a high-speed camera, which allow for real-time monitoring of the granules. The system was implemented into a custom-made 3D-printed device that could reproduce the particle movement characteristic in a fluidized-bed granulator. The suitability of the method was evaluated by determining the particle size distribution (PSD) of various granule mixtures within the 100–2000 μm size range. The convolutional neural network-based software was able to successfully detect the granules that were in focus despite the dense flow of the particles. The volumetric PSDs were compared with off-line reference measurements obtained by dynamic image analysis and laser diffraction. Similar trends were observed across the PSDs acquired with all three methods. The results of this study demonstrate the feasibility of performing real‐time particle size analysis using machine vision as an in-line process analytical technology (PAT) tool.

A novel dry granule preparation technology and comparison of granule properties with conventional wet system for ceramic tiles production

The ceramic tile manufacturing process uses a lot of energy, mainly thermal energy, and to a lesser extent electric energy. Total energy costs account for between 50% and 55% of average direct manufacturing costs. Fossil fuel combustion, such as natural gas combustion, produces carbon dioxide emission. Therefore, energy consumption and emissions issues are vitally important for both environmental effects and process costs in ceramic tile manufacturing. The wet process of granule production systems including wet grinding and spray drying is widely used for the production of granules. Although there is high energy consumption for the water evaporation in the spray dryer, it ensures to produce high quality tile for many years. In this study, important granule properties were introduced for a novel dry granule production system. In the successful application of a dry granulation system, the conformity of produced granules is vitally important such as particle size distribution, bulk density, flow properties, and moisture of granules and conformity for the pressing process. This paper includes the comparative studies for properties of granules produced in spray dryer and new dry granule preparation systems and the full results of the industrial trials with these granules. The cost comparison of both granule production systems was also made for the same raw material usage. The natural gas consumption and water consumption were reduced respectively from 46 to 15 m3/ton and from 540 to 95 liters/ton in the new dry granulation system while electricity consumption and maintenance costs remain almost the same in both systems.

Application of unsupervised and supervised learning to a material attribute database of tablets produced at two different granulation scales

The purpose of this study is to demonstrate the usefulness of machine learning (ML) for analyzing a material attribute database from tablets produced at different granulation scales. High shear wet granulators (scale 30 g and 1000 g) were used and data were collected according to the design of experiments at different scales. In total, 38 different tablets were prepared, and the tensile strength (TS) and dissolution rate after 10 min (DS10) were measured. In addition, 15 material attributes (MAs) related to particle size distribution, bulk density, elasticity, plasticity, surface properties, and moisture content of granules were evaluated. By using unsupervised learning including principal component analysis and hierarchical cluster analysis, the regions of tablets produced at each scale were visualized. Subsequently, supervised learning with feature selection including partial least squares regression with variable importance in projection and elastic net were applied. The constructed models could predict the TS and DS10 from the MAs and the compression force with high accuracy (R2= 0.777 and 0.748, respectively), independent of scale. In addition, important factors were successfully identified. ML can be used for better understanding of similarity/dissimilarity between scales, for constructing predictive models of critical quality attributes, and for determining critical factors.

Continuous manufacturing of vitamin D3 and iron enriched granules by means of a novel twin-screw dry granulation process

A multi-disciplinary approach involving continuous manufacturing (CM) of thermally stable food supplements containing vitamin D3 (VitD3) and iron (Fe ++ ) via a single-step twin-screw granulation (TSG) process was tested in this work. Two selected excipients, namely Neusilin® US2 and corn starch, were used in the work. The particle size distribution and morphology of pre-mixed and post-extruded granules were investigated with a laser diffraction particle size analyzer, sieve analysis, scanning electron microscopy and energy dispersive X-ray (SEM-EDX), X-ray powder diffraction (PXRD), and polarized light microscopy (PLM). The thermal stability of the granules was assessed through differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). The SEM visualized a good distribution of all ingredients without the forming of any crystals on the extrudate surface, indicating good mixing during the high shear granulation inside the extruder barrel. The FT-IR analysis demonstrates that characteristic vibration peaks of VitD3 were present in all physical mixtures as well as the extruded granules, indicating that VitD3 was stable in the formulations despite the high shear mixing during the TSG. The mean volumetric diameter (Dv50) of the formulation containing Neusilin increased significantly ( P < 0.05) to 90.8-μm when compared with neat Neusilin (71.3-μm) and VitD3 (33.8 μm) confirming granulation, however, no improvement was observed for the corn starch blend. In addition, the calculated Hausner ratio (HR) and Carr's index (CI) suggest similar inter-particulate friction of VitD3 and Neusilin, whereas corn starch showed a difference. The surface elemental analysis confirmed the presence of Fe ++ with a homogenous distribution of the metal in the granules. Overall, for the first time, the blend of VitD3 and iron has been prepared using the CM platform, which has great potential for the intervention of VitD3 and iron deficiencies. • Twin screw dry granulation is employed to develop vitamin D3 and iron granules. • Neusilin and corn starch are used as excipients for the blend. • Particle size distributions and morphology confirm the formation of granules. • Vitamin D3 remained almost constant in the TSG process.

Process parameter optimization for the preparation of soap granules by Comil

A conical screen mill is commonly used to reduce particle size and produce granules of the required particle size. In the present work, an experimental study was designed to explore the use of a comil for the milling of soft solids. As a helpful example for research on soft solids, soap noodles were selected for optimizing the milling parameters such as impeller speed and type, screen type and size, and design of the milling cycle. A preferable combination of the comil parameters was the one generating a minuscule percentage of fines as also the one causing no damage or softening of the structure whatsoever due to agitation or temperature. The study involves comparing the particle sizes statistically and computing different parameters for designing the process. The particle size distribution of the soap granules obtained from the comil affects the soap bar's hardness and friability when punched. Hence, it was deduced that, for soft solids like soap noodles, comil can be helpful in particle size reduction, provided the parameters are optimized according to the mechanical properties of the material. Finally, this work presents a novel application to the comil equipment and gives a new processing technique for soap noodles.

Combined Effect of Nitrogen Fertilizer Application and High Temperature on Grain Quality Properties of Cooked Rice.

Ambient temperature and nitrogen (N) fertilizer are two of the most important factors that affect rice grain quality. However, less information has been available on the interactive effect of N fertilizer and ambient temperature on grain quality under stressful high temperature (HT). In this article, the effects of panicle N fertilizer, ambient temperature, and their interaction on starch composition, particle size distribution of starch granules, starch physicochemical properties, and storage protein accumulation in milled grains were investigated to clarify the potential role of panicle N fertilizer topdressing in regulating rice grain quality under stressful HT by using a two-factor experiment of three N levels in combination with two temperature regimes. Results showed that appropriate application of panicle N fertilizer could attenuate the adverse effect of HT during grain filling on milling quality and chalky occurrence to some extent, particularly for the effective alleviation of HT-induced decrease in milling quality. However, the topdressing of panicle N fertilizer tended to enhance starch gelatinization enthalpy (ΔH) and its setback viscosity in HT-ripening grains, with the simultaneous decrements in the number and surface area proportions of smaller starch granules under the higher N fertilizer in combination with HT exposure. The effects of higher nitrogen fertilizer and HT exposure on total protein content and gluten composition of grains were additively increased. Hence, the topdressing of panicle N fertilizer exacerbated HT-induced deterioration in cooking and eating quality, rather than alleviating the negative impact of HT exposure on the palatability of cooked rice.

Influence of Formulation Factors, Process Parameters, and Selected Quality Attributes on Carvedilol Release from Roller-Compacted Hypromellose-Based Matrix Tablets.

The importance of roller compaction is recently increasing. This study evaluates the combined effects of formulation factors, process parameters, and selected quality attributes on drug release from roller-compacted hypromellose-based matrix tablets containing carvedilol as a model drug. The influence of selected factors was statistically assessed and good predictive models were developed for various time points of the release profile. The results show that the release profile is mostly affected by the particle size distribution of granules and roll speed. This indicates that the roller compaction process has a major impact on drug release, which is also formulation dependent. A higher d50 and lower d90 value of spatial filtering technique-based particle size distribution results, a lower roll speed, increased hypromellose content, using microcrystalline cellulose as a filler, and higher tablet hardness, resulted in a decrease in the drug release rate. On the other hand, the effect of the roll pressure, size of screen apertures, and d10 values on drug release was insignificant. The significance of the factors was further explained by granule shape, their porosity, and friability evaluation, and by compressibility and compactibility studies of compression mixtures. Additionally, the spatial filtering technique demonstrated to be a promising tool in controlling the roller compaction process.

Effects of particle size distribution of potato starch granules on rheological properties of model dough underwent multiple freezing-thawing cycles

In order to elucidate the mechanism underlying the effect of different-sizes potato starch on dough during freeze–thaw treatment, the rheological properties, moisture distribution, secondary structure, and relative crystallinity of dough were investigated. The results showed that the storage modulus (G′), loss modulus (G″), and complex modulus (|G*|) of dough increased as a result of the freeze–thaw treatment, and the effect was more obvious as the starch granular sizes increased. The higher β -sheet and T22 contents reflected the higher viscoelasticity and freeze–thaw sensitivity, which may be related to the higher degree expansion of amylose. In contrast, dough with small-sized starch had higher intermolecular interactions, and denser structure, lower water migration, showing that this has better resistance and higher stability. The presented mechanisms may contribute to the better understanding of the effects of freeze–thaw process on model dough properties.

Use of machine learning in prediction of granule particle size distribution and tablet tensile strength in commercial pharmaceutical manufacturing

In the manufacturing of pharmaceutical Oral Solid Dosage (OSD) forms, Particle Size Distribution (PSD) and Tensile Strength (TS) are common in-process tests that are controlled in order to achieve the quality targets of the end-product. The Quality by Design (QbD) concept elaborates process understanding and sufficient controls. However, for older pharmaceutical products upscaled to commercial phase with Quality by Testing (QbT) approach, the knowhow of the product-specific critical parameters is often limited. In this study, two predictive machine learning (ML) models were used for a commercial tablet product, for which historical data of raw materials, production, in-process controls and condition monitoring were available. With the aforementioned data, the aim was to predict the PSD and the TS that indicate the product quality. The feature importance was used to evaluate the parameter importance for the PSD and the TS. Partial dependence, in turn, was used to estimate the parameter impact on the predicted TS. The study illustrates the capability of the ML models to bring additional value for commercial products through the enhanced product-related knowhow.

Implementation of spatial filtering technique in monitoring roller compaction process

This study investigates the use of the spatial filtering technique (SFT11spatial filtering technique) to monitor the particle size distribution (PSD22particle size distribution) of granules obtained by roller compaction. In the first part of the study, the influence of the selected process and formulation parameters on the PSD2 of granules is monitored at-line using SFT1. The correlation between the PSD2 obtained by SFT1, sieve analysis, laser diffraction, and dynamic image analysis was satisfactory. The same trend was observed with all methods; however, SFT1 proved to be especially advantageous for monitoring the PSD2 of irregularly shaped granules obtained by roller compaction. Another aim of this study was to investigate the suitability of using the SFT1 method as a potential process analytical technology (PAT33process analytical technology) tool for monitoring and predicting the PSD2 of granules obtained by roller compaction. The SFT1 model for d10 was poor due to less precise detection of smaller particles by SFT; nevertheless, the models for d50 (R2 = 0.93) and d90 (R2 = 0.93) were very good. The at-line models were further tested in real time on samples collected during the milling of ribbons. The correlation between the predicted and achieved values was good; however, it was time and formulation dependent.

Tablet Quality-Prediction Model Using Quality Material Attributes: Toward Flexible Switching Between Batch and Continuous Granulation

The purpose of the study was to develop a model to predict the critical quality attribute (CQA) of tablets during continuous and batch manufacturing using only critical material attributes (CMAs). Experiments were performed using ethenzamide as the active pharmaceutical ingredient processed with batch and continuous high-shear granulators. The disintegration time of tablets was defined as the CQA, and the particle-size distribution of granules and tablet hardness were defined as the CMAs. We first investigated the influence of granulation conditions on particle-size distribution during batch and continuous granulation. We then proceeded to construct the CQA estimation model by producing tables using batch and continuous granulation. The results indicated the similarity of the granulation mechanisms, as observed by the bimodality of the distributions and the significant causal factors. Principal component analysis revealed that the CQA was influenced strongly by the particle-size distribution and that the CMA–CQA correlations were similar for both processes. Finally, a model based on partial least-squares regression could be developed that could reasonably estimate the CQA using CMAs without involving any process parameters. This approach of using process-independent CQA prediction could enable flexible switching between batch and continuous manufacturing during a product life cycle, thus offering new possibilities for efficient life cycle management.

РАССЕВ ПОРОШКОВ В АДДИТИВНОМ И ГРАНУЛЬНОМ ПРОИЗВОДСТВАХ (обзор)

Considers the features of powders obtained by various methods, their technological properties in relation to additive and granular manufacturing. The sequence of operations upon receipt of metal powder compositions is presented. The factors affecting the process of vibration sieving of metal powders and granules are described. The features and advantages of vibratory sieving on horizontally arranged circular sieves using ultrasonic cleaning to obtain specified trajectories of motion are shown. Criteria for evaluating the sieving efficiency are given and explanations are given for determining the particle size distribution of powders and granules.

Controlled-Release Fine Particles Prepared by Melt Adsorption for Orally Disintegrating Tablets.

Melt adsorption is a manufacturing method that offers precise control of particle size distribution of granules and circumvents the disadvantages of conventional melt granulation. However, drug release from particles adsorbed with hydrophobic materials has not been fully investigated, and there are missing details as to whether particles manufactured by this technique can be applied to orally disintegrating tablets (ODT). In this report, we aimed to optimize process parameters and formulation to manufacture ODT containing melt adsorption-particles with the specific characteristic of sustained release. Melt adsorption particles containing Neusilin US2 as the adsorbent were prepared by using various waxes to determine the most suitable material for controlled release formulation. Glycerol fatty acid ester (Poem TR-FB: TR-FB) was the optimal wax examined because of its drug release pattern and tabletability. We then optimized manufacturing conditions by examining granulation time, disintegrant amount per tablet and compression force on the tablet for ODT that meet the criteria of controlled drug release, tensile strength and disintegration of the tablet. Multiple regression analysis revealed the effect of process parameters on tablet properties and drug release with increasing the granulation time affording sustained release of the drug. The analysis also showed that a high compression force crushed the granules coated by TR-FB, which impaired sustained drug release. From the regression model the optimal manufacturing conditions were determined, and the tablet prepared under these conditions concurred with the predicted values and met all criteria. This new technique should contribute to the development of ODT to improve medication adherence.

Influence of granulation temperature on particle size distribution of granules in twin-screw granulation (TSG)

This study investigated an influence of granulation temperature during twin-screw granulation (TSG) on particle size distributions (PSDs). The influence of the granulation temperature on granule size distributions varied, depending on the liquid to solid (L/S) ratio, the kind of binders, the method of binder addition, and the filler material. The PSD of granules was broad and bimodal at a barrel temperature of 30 °C. Granules size distributions became narrow and second height decreased at high barrel temperature. While the L/S ratio had an effect on the sharpness of granule size distributions, this effect was minor compared to the granulation temperature. Granule size distributions were influenced by binder addition methods. When the binder was added as solution, PSD became broad. In formulations using lactose as filler, PSD became broad and bimodal at 90 °C. Much lactose was dissolved in granulation solution at high temperature, because the solubility of lactose rises significantly with the solution temperature leading to higher effective L/S ratio in the granulator. Hence, granulation was proceeded and large granules were formed. From these results, the granulation temperature is one of important parameters to obtain mono-modal PSD in TSG.

Wet-granulation process: phenomenological analysis and process parameters optimization

Wet granulation is a size-enlargement process applied in many industrial fields, such as pharmaceutical, nutraceutical, zootecnichal, to improve flowability and compressibility properties of powders. In this work analysis of the particle size distribution (PSD) of granules was performed to understand the phenomena involved during the granulation process and to optimize the operating conditions. Hydroxypropyl methylcellulose (HPMC) granules were produced spraying distilled water as liquid binder on powders in a low-shear granulator. The experimental campaign was planned using the full factorial design statistical technique varying two factors (impeller rotation speed and binder flow rate), each at three intensities. PSDs of HPMC granules at different granulation times were obtained by an ad hoc dynamic image analysis device based on the free falling particle scheme. PSD measurements showed that wet granules size depends on the simultaneous presence of nucleation, agglomeration and breakage phenomena. The process parameters optimization was carried out using response surface methodology (RSM) and using the granulation yield (% w/w of wet granules within the size range 2000–10,000 μm) as the main variable of interest.

Experimental and mathematical simulation study on the effect of granule particle size distribution on partial nitrification in aerobic granular reactor

The granules in the aerobic granular sludge reactor usually follow certain particle size distribution. In the previous studies, the average granule diameter was usually assumed in the model simulations. In this study, the impact of granule particle size distribution on the partial nitrification in the aerobic granular reactor was examined both in experiment and mathematical simulation. Both experimental and simulation results showed high NOB (nitrite oxidizing bacteria) presence in the small granules under conditions in which the NOB could be outcompeted in the large granules. The presence of NOB in the small granules reduced the nitrite accumulation. The simulation results indicated that NOB was preferentially presented in granules small than 50 μm. The results could be used to improve the operation of granule reactor for partial nitrification, by removing small granules (less than 50 μm) to outcompete NOB selectively. By including a wide particle size spectrum in the biofilm model, the study provided a quantitative tool for modelling granule sludge reactors.

In Vitro Evaluation of Nasogastric Tube Delivery Performance of Esomeprazole Magnesium Delayed-Release Capsules

Enteral feeding tubes are used to deliver food or drugs to patients who cannot swallow. To deliver delayed-release drugs that are formulated as enteric coated granules to these patients via feeding tubes requires that they be suspended in water before administration. Importantly, the suspension of enteric granules in water of varying pH can cause damage to the enteric coating and affect the bioavailability of the drug. Here, analytical methods for testing acid resistance stability and particle size distribution (PSD) of esomeprazole granules were used to monitor the integrity of the granule enteric coating after water pretreatment and delivery through an oral syringe and nasogastric (NG) tube. Granules from esomeprazole magnesium delayed-release capsules were transferred to an oral syringe, suspended in water, and delivered on the bench through an NG tube. Subsequently, acid resistance stability (i.e., the amount of drug released after 2-h acid dissolution) was determined via high-performance liquid chromatography, and the PSD were measured with a laser diffraction system. All the granules demonstrated acid resistance stability when the granules were delivered immediately (0 min incubation) through the oral syringe and NG tube. In contrast, some granules demonstrated significant drug release during acid exposure after a 15-min incubation period which mimics a possible delay in delivery of the drug from the syringe by the caregiver. A bimodal PSD was observed with these granules, which was attributed to debris from damaged enteric coating and particle agglomeration. The methods developed in this study could be used to distinguish batches with suboptimal product quality for delivery using NG tubes and to confirm the substitutability of generic drug products for this alternative route of administration.

Particle size distribution of wheat starch granules in relation to baking properties of frozen dough

The impact of freezing on the wheat starches with different particle size was studied using a range of characterization methods including X-ray diffraction, differential scanning calorimetry, the Rapid Visco Analyser and a reconstitution dough system. Wheat starches were fractionated into A- and B-type granules, and then subjected to freezing/thawing treatment for 3 cycles. The freezing treatment did not cause apparent damage on A-type granular surface but induced cracked structure on B-type granules. It facilitated materials such as amylose, proteins, and lipids leaching from starch granule and an increase in gelatinization temperatures, melting enthalpy, and pasting viscosities. A smaller bread specific volume was obtained from freezing-treated B-granules while the crumb firmness significantly increased (p>0.05). No marked differences were observed in the counterparts of A-granules after freezing treatment. It seemed that the B-type granules were more sensitive to the freezing/thawing treatment, thus facilitating structural transformations from dough to bread. Results indicated that the deterioration in frozen bread quality derived from starch could be minimized by increasing the A-granules content.

The Effects of Soaking on Rice Granules for &lt;i&gt;Bedak sejuk &lt;/i&gt;Production

Bedak sejuk, is a traditional cosmetic product that still being used and fond by many women in Malaysia. It is produced by the traditional methods that passed from generation to generation. Rice grains were soaked in water at least for three months or until it fully dissolved. The aim of the study is to determine the effects of soaking on rice granules for bedak sejuk production. Local rice grains (Indica) were soaked in water at ratio of 1:1 (w/v) in a container with lid for 42 days and the water were changed at 14 days interval. The soaking process was a series of batch process. A growth profile of microbial in the fermented supernatant showed that the lag phase started on day 3 of soaking process and the exponential phase started on day 8 of soaking process. The final pH value of fermented supernatant was 4.04 while the final titratable acidity which is expressed as lactic acid was 0.62 mg mL-1. Reducing sugar increased while total starch decreased during the soaking process. For particle size distribution of rice granules, there is no clear differences in the size distribution but there is slight changes of weight fraction of the rice granules. The analysis of fermented supernatant suggests that natural fermentation occurred during the soaking process while the analysis of rice granules suggests that hydrolysis of rice starch occurred during the natural fermentation process.