Superfine Marigold Powder Improves the Quality of Sponge Cake: Lutein Fortification, Texture, and Sensory Properties.

This study aimed to investigate and optimize the quality and sensory properties of baked products with lutein-enriched marigold flower powder (MP). Lutein-enriched marigold flowers produced via hydroponic methods using LED lights were used as a functional material in sponge cakes to increase lutein content. MP particles were divided into coarse (Dv50 = 315 µm), fine (Dv50 = 119 µm), and superfine MP (Dv50 = 10 µm) fractions and added to the sponge cake after being designated to control (sponge cake prepared without MP), coarse MPS (sponge cake prepared with coarse MP), fine MPS (sponge cake prepared with fine MP), and superfine MPS (sponge cake prepared with superfine MP) groups. The sizes and surface properties of superfine MP particles were more homogeneous and smoother than the other samples. As the particle size decreased, the specific volume increased, whereas baking loss, hardness, and chewiness of the sponge cake decreased. Superfine MP and superfine MPS had the highest lutein content. The flavor of marigold and the overall acceptability of sponge cake with superfine MP were 7.90 ± 0.97 and 7.55 ± 0.76, which represents the highest values among the samples. The results of this study have shown that jet milling can contribute to improvements in texture, lutein content, and sensory qualities for baked products with MP.

Comminution of Polymetallic Nodules with a High-Pressure Water Jet.

This paper presents an original method for the comminution of polymetallic nodules in a hydro-jet mill of our own design, having the water jet pressure in the range of 70-200 MPa. The best comminution results are ensured by equipping the mill with a water jet having a diameter dw = 0.7 mm and a comminution-homogenization tube having a diameter dh = 2.4 mm, and by setting a distance s = 10 mm from the outlet of the homogenization tube to the comminuting disc. Particles of concretions comminuted under such conditions are characterized by a fairly regular isometric shape and favorable morphology represented by intense development of the specific surface.

Mechanical Characterization of Pharmaceutical Powders by Nanoindentation and Correlation with Their Behavior during Grinding.

Controlling the size of powder particles is pivotal in the design of many pharmaceutical forms and the related manufacturing processes and plants. One of the most common techniques for particle size reduction in the process industry is powder milling, whose efficiency relates to the mechanical properties of the powder particles themselves. In this work, we first characterize the elastic and plastic responses of different pharmaceutical powders by measuring their Young modulus, the hardness, and the brittleness index via nano-indentation. Subsequently, we analyze the behavior of those powder samples during comminution via jet mill in different process conditions. Finally, the correlation between the single particle mechanical properties and the milling process results is illustrated; the possibility to build a predictive model for powder grindability, based on nano-indentation data, is critically discussed.

Research on the Grinding Energy Density in a Jet Mill.

Raw materials are used in many industrial technologies. The raw material frequently has to be prepared as an intermediate with an appropriate particle size distribution, which requires the use of grinding. In grinding processes, energy consumption is a very important profitability criterion for the applied particular size reduction technology. The paper describes the comminution process that takes place in the jet mill using a modified form of the thermodynamic theory of grinding. In this theory, new material characteristics have been added: the surface and volumetric density of grinding energy. The thermodynamic theory is a combination of the classical Kick's theory and the modified form of Rittinger's theory. The tested physical magnitudes are a measure of the energy consumption of the grinding process. They describe the energy that must be provided in the grinding process to overcome interactions between particles related to the volume and surface of the material. Knowledge of these magnitudes is necessary to model thermomechanical phenomena in the solid state. The paper presents the results of research on comminution in a jet mill, on the basis of which the values of the tested material magnitudes were determined. It is graphically shown how the values of the tested magnitudes depend on the grain size of the ground samples.

Inhalable Hydroxychloroquine Powders for Potential Treatment of COVID-19.

Background: Hydroxychloroquine (HCQ) is one of the repurposed drugs proposed for the treatment of coronavirus disease 2019 (COVID-19). However, all the published clinical trials involve oral administration of the drug, although the disease is primarily a respiratory one. Direct inhaled delivery could reduce the side effects associated with oral use and ensure a high concentration of the drug in the lungs. In this study, inhalable HCQ powders were prepared and characterized for potential COVID-19 therapy. Methods: Hydroxychloroquine sulfate (HCQ-sul) was jet milled (JM) followed by conditioning by storage at different relative humidities (43%, 53%, 58%, and 75% RHs) for 7 days. The solid-state properties, including particle morphology and size distribution, crystallinity, and vapor moisture profiles of HCQ-sul samples, were characterized by scanning electron microscopy, laser diffraction, X-ray powder diffraction, differential scanning calorimetry, thermogravimetric analysis, and dynamic water vapor sorption. The aerosol performance of the HCQ-sul powders was assessed using a medium-high resistance Osmohaler coupling to a next-generation impactor (NGI) at a flow rate of 60 L/min. Results: The jet-milled powder showed a volume median diameter of 1.7 µm (span 1.5) and retained the same crystalline form as the raw HCQ-sul. A small amount of amorphous materials was present in the jet-milled HCQ-sul, which was convertible to the stable, crystalline state after conditioning at 53%, 58%, and 75% RH. The recovered fine particle fraction (FPF)recovered and the emitted fine particle fraction (FPFemitted) of the HCQ-sul sample immediately after jet milling and the samples after conditioning at 43%, 53%, and 58% RH were similar at ∼43% and 61%, respectively. In contrast, the sample having conditioned at 75%RH showed lower corresponding values at 33% and 26% respectively, due to the formation of solid bridges caused by excessive moisture. Conclusion: Inhalable crystalline powders of HCQ-sul were successfully prepared, which can be used for clinical testing as a potential inhaled COVID-19 treatment.

Development of High Dose Oseltamivir Phosphate Dry Powder for Inhalation Therapy in Viral Pneumonia.

Oseltamivir phosphate (OP) is an antiviral drug available only as oral therapy for the treatment of influenza and as a potential treatment option when in combination with other medication in the fight against the corona virus disease (COVID-19) pneumonia. In this study, OP was formulated as a dry powder for inhalation, which allows drug targeting to the site of action and potentially reduces the dose, aiming a more efficient therapy. Binary formulations were based on micronized excipient particles acting like diluents, which were blended with the drug OP. Different excipient types, excipient ratios, and excipient size distributions were prepared and examined. To investigate the feasibility of delivering high doses of OP in a single dose, 1:1, 1:3, and 3:1 drug/diluent blending ratios have been prepared. Subsequently, the aerosolization performance was evaluated for all prepared formulations by cascade impaction using a novel medium-resistance capsule-based inhaler (UNI-Haler). Formulations with micronized trehalose showed relatively excellent aerosolization performance with highest fine-particle doses in comparison to examined lactose, mannitol, and glucose under similar conditions. Focusing on the trehalose-based dry-powder inhalers' (DPIs) formulations, a physicochemical characterization of extra micronized grade trehalose in relation to the achieved performance in dispersing OP was performed. Additionally, an early indication of inhaled OP safety on lung cells was noted by the viability MTT assay utilizing Calu-3 cells.

Amplification of Vitamin D2 in the White Button Mushroom (Agaricus bisporus) by UV-B Irradiation and Jet-Milling for Its Potential Use as a Functional Ingredient.

The objective of this study was to amplify vitamin D2 in white button mushrooms using ultraviolet (UV-B) irradiation and to prepare a vitamin D2-fortified superfine mushroom powder through jet milling. Mushrooms irradiated with UV-B for 30 min had a vitamin D2 concentration of 8.19 µg/g, an amount about 400 times greater than that of the control (0.02 µg/g). The vitamin D2-fortified mushrooms were then freeze-dried and conventionally ground or jet-milled to obtain coarse (Dv50 = 231 µm), fine (Dv50 = 106.3 µm), and superfine (Dv50 = 7.1 µm) powders. The vitamin D2 content was retained during the preparation of the powders. The physical characteristics were evaluated by scanning electron microscopy and hydration properties. The superfine powder of vitamin D2-amplified mushrooms was suitable for use as a functional ingredient because its roughness was significantly reduced, and it had a neutral aroma and taste as determined by descriptive analysis.

Characteristics of Bread Made of Various Substitution Ratios of Bran Pulverized by Hammer Mill or Jet Mill.

The physicochemical and antioxidant properties of dough and bread were measured in wheat flours substituted with two types of bran (HMB: bran pulverized by a hammer mill and JMB: bran pulverized by a jet mill) at various ratios (0%, 5%, 10%, 15%, 20%, and 25%) of substitution. The particle size of hammer mill bran (HMB) (119.71 µm) was larger than that of jet mill bran (JMB) (25.78 µm). Wheat flours substituted with HMB contained more total dietary fiber than those with JMB. A significant increase of water absorption and dough development time in Mixolab® analysis was observed depending on the level of HMB or JMB substitution. The breads made with HMB or JMB (5% or 10%) showed a higher specific volume and lower crumb hardness than the control bread. However, breads made with ≥15% HMB or JMB had a decreased specific volume and increased crumb hardness. Overall, breads made with wheat flour substituted with 5%-10% HMB or JMB were of a higher bread quality and had more antioxidant properties.

Development of an Excipient-Free Peptide Dry Powder Inhalation for the Treatment of Pulmonary Fibrosis.

The caveolin scaffolding domain peptide (CSP) is being developed for the therapeutic intervention of a lethal lung disease, idiopathic pulmonary fibrosis. While direct respiratory delivery of CSP7 (a 7-mer fragment of CSP) is considered an effective route, proper formulation and processing of the peptide are required. First, air-jet milling technology was performed in order to micronize the neat peptide powder. Next, the fine particles were subjected to a stability study with physical and chemical characterizations. In addition, the in vivo efficacy of processed CSP7 powder was evaluated in an animal model of lung fibrosis. The results revealed that, with jet milling, the particle size of CSP7 was reduced to a mass median aerodynamic diameter of 1.58 ± 0.1 µm and 93.3 ± 3.3% fine particle fraction, optimal for deep lung delivery. A statistically significant reduction of collagen was observed in diseased lung tissues of mice that received CSP7 powder for inhalation. The particles remained chemically and physically stable after micronization and during storage. This work demonstrated that jet milling is effective in the manufacturing of a stable, excipient-free CSP7 inhalation powder for the treatment of pulmonary fibrosis.

Preparation of a new high-performance calcium-based desulfurizer using a steam jet mill.

Dry flue gas desulfurization is an increasingly attractive technique in SO2 emission control. However, the low efficiency in dry desulphurization is the bottleneck of this technology. To find a high-performance desulfurizer is an urgent task. This research utilized a steam jet mill digestion to prepare a desulfurizer at steam temperature of 220 ℃ and pressure of 0.45 MPa, and compared this product with the conventional digestion desulfurizer. Our results show that the digestion in steam jet mill can transform all the calcium oxide into calcium hydroxide. The calcium hydroxide had good fluidity and with honeycomb morphological characteristics. The experiments of dry flue gas desulfurization demonstrated that under the relative humidity of 15, 30 and 45%, the total dead times were 340, 640 and 720 min, the working time for keeping a 100% desulfurization efficiency were 120, 420 and 580 min, and the total sulfur fixation were 124.05, 274.58 and 332.09 mg. Compared with the desulfurizer by conventional dry digestion, the desulfurizer prepared in this research had a significantly superior performance. This experiment provides a new method for high-performance desulfurizer via quicklime digestion, which is an important step in pushing forward the application of dry flue gas desulfurization.

Tailoring Physical and Sensory Properties of Tofu by the Addition of Jet-Milled, Superfine, Defatted Soybean Flour.

The use of defatted soybean flour (DSF) in food as a source of dietary fiber has been limited due to its rough texture and bitter taste. Our previous work indicates that superfine DSF prepared by jet milling could overcome these problems, as it positively affected physical and sensory properties. Therefore, differently sized DSFs were incorporated in tofu, and their impacts on physical and sensory properties were investigated in this study. Coarse DSF (Dv50 = 341.0 µm), fine DSF (Dv50 = 105.3 µm), and superfine DSF (Dv50 = 5.1 µm) were prepared by conventional sifting and jet milling. Tofu was made with a 5% addition of differently sized DSFs and without DSF (control tofu). The quality of tofu was evaluated by scanning electron microscopy, color measurement, texture profile analysis, and quantitative descriptive analysis. The tofu made with coarse and fine DSF showed negative changes in its physical and organoleptic qualities, such as reduced yields, a less pure color, a harder texture, and a rougher mouthfeel. However, the tofu made with superfine DSF showed only minimal changes in its qualities compared to the control. Therefore, superfine DSF is a promising fiber supplement that does not change the physical and sensory properties in the making of high-quality tofu.

Physical and textural properties of biscuits containing jet milled rye and barley flour.

The biscuit-making performance of flour depends on both its botanical source and particle size. Several quality parameters of biscuits produced by partial replacement of wheat flour by barley and rye flours at 0, 10, 20, 30 and 40% were measured. Moreover, in order to investigate the effect of particle size, a commercial and two jet milled finer samples of both rye and barley flours were used. For most of the composite flours, the level of substitution was not statistically significant for the weight and the spread ratio of the biscuits. Biscuits with composite flours were softer and darker than the control biscuit (100% wheat flour). In addition, their total phenolics content and antioxidant activity were greater. Among composite flour biscuits, the finer barley flour biscuits were harder than those with the commercial flour. Moreover, as rye flour is darker than wheat and barley flours, rye biscuits were the darker of all. Porosity, bulk and true densities were affected by the particle size of the substitute flours.

Steam jet mill-a prospective solution to industrial exhaust steam and solid waste.

Bulk industrial solid wastes occupy a lot of our resources and release large amounts of toxic and hazardous substances to the surrounding environment, demanding innovative strategies for grinding, classification, collection, and recycling for economically ultrafine powder. A new technology for grinding, classification, collection, and recycling solid waste is proposed, using the superheated steam produced from the industrial exhaust steam to disperse, grind, classify, and collect the industrial solid waste. A large-scale steam jet mill was designed to operate at an inlet steam temperature 230-300 °C and an inlet pressure of 0.2-0.6 MPa. A kind of industrial solid waste fluidized-bed combustion ashes was used to grinding tests at different steam temperatures and inlet pressures. The total process for grinding, classification, and collection is drying. Two kinds of particle sizes are obtained. One particle size is d50 = 4.785 µm, and another particle size is d50 = 8.999 µm. For particle size d50 = 8.999 µm, the inlet temperature is 296 °C and an inlet pressure is 0.54 MPa for the grinding chamber. The steam flow is 21.7 t/h. The yield of superfine powder is 73 t/h. The power consumption is 3.76 kW h/t. The obtained superfine powder meets the national standard S95 slag. On the basis of these results, a reproducible and sustainable industrial ecological protocol using steam produced by industrial exhaust heat coupled to solid waste recycling is proposed, providing an efficient, large-scale, low-cost, promising, and green method for both solid waste recovery and industrial exhaust heat reutilization.

Properties of flour films as affected by the flour's source and particle size.

Wheat (W) and rye flour (R, R1 and R2) films were developed. The rye flours used differed in their particle size. R1 and R2 resulted from jet milling of the R flour at two different feed rates. The mean particle size of W, R, R1 and R2 flours was 173.87, 100.91, 54.59 and 35.66 µm, respectively. Glycerol was used as plasticizer at concentrations of 0.5, 0.7 and 1 g/g of flour. Films made from mixtures of flours (50:50 w/w) were also studied in the presence of 0.7 g glycerol/g of flour. Colour, moisture content, solubility, thickness, viscosity, microstructure and mechanical properties were assessed. In most cases the films were homogeneous. Film moisture content, thickness, opacity and mechanical properties were correlated to glycerol concentration. Particle size was found important for the mechanical properties. Wheat films were lighter ([L*] ≈ 49) and less opaque (135). For both single and composite films, moisture content varied from 24 to 35%, solubility from 43.5-58%, opacity from 135 to 371, thickness from 0.66-0.72 mm and mechanical strength from 0.68-1.7 MPa. All film-forming solutions exhibited shear thinning behaviour. Wheat flour dominated most of the studied properties in composite films. Rye films were more opaque, with relatively high solubility but greater mechanical strength.

A review of co-milling techniques for the production of high dose dry powder inhaler formulation.

Drug delivery by inhalation offers several advantages compared to other dosage forms, including rapid clinical onset, high bioavailability, and minimal systemic side effects. Drug delivery to the lung can be achieved as liquid suspensions or solutions in nebulizers and pressurized metered-dose inhalers (pMDI), or as dry powders in dry powder inhalers (DPIs). Compared to other delivery systems, DPIs are, in many cases, considered the most convenient as they are breath actuated and do not require the use of propellants. Currently, the delivery of low drug doses for the treatment of lung conditions such as asthma and chronic obstructive pulmonary disease are well established, with numerous commercial products available on the market. The delivery of low doses can be achieved from either standard carrier- or aggregate-based formulations, which are unsuitable in the delivery of high doses due to particle segregation associated with carrier active site saturation and the cohesiveness of micronized aggregates which have poor flow and de-agglomeration properties. High-dose delivery is required for the treatment of lung infection (i.e. antibiotics) and in the emerging application of drug delivery for the management of systemic conditions (i.e. diabetes). Therefore, there is a demand for new methods for production of high-dose dry powder formulations. This paper presents a review of co-mill processing, for the production of high-efficiency inhalation therapies, including the jet mill, mechanofusion, or ball mill methodologies. We investigate the different techniques, additives, and drugs studied, and impact on performance in DPI systems.

Co-milled API-lactose systems for inhalation therapy: impact of magnesium stearate on physico-chemical stability and aerosolization performance.

CONTEXT: Particle micronization for inhalation can impart surface disorder (amorphism) of crystalline structures. This can lead to stability issues upon storage at elevated humidity from recrystallization of the amorphous state, which can subsequently affect the aerosol performance of the dry powder formulation. OBJECTIVE: The aim of this study was to investigate the impact of an additive, magnesium stearate (MGST), on the stability and aerosol performance of co-milled active pharmaceutical ingredient (API) with lactose. METHODS: Blends of API-lactose with/without MGST were prepared and co-milled by the jet-mill apparatus. Samples were stored at 50% relative humidity (RH) and 75% RH for 1, 5, and 15 d. Analysis of changes in particle size, agglomerate structure/strength, moisture sorption, and aerosol performance were analyzed by laser diffraction, scanning electron microscopy (SEM), dynamic vapor sorption (DVS), and in-vitro aerodynamic size assessment by impaction. RESULTS: Co-milled formulation with MGST (5% w/w) led to a reduction in agglomerate size and strength after storage at elevated humidity compared with co-milled formulation without MGST, as observed from SEM and laser diffraction. Hysteresis in the sorption/desorption isotherm was observed in the co-milled sample without MGST, which was likely due to the recrystallization of the amorphous regions of micronized lactose. Deterioration in aerosol performance after storage at elevated humidity was greater for the co-milled samples without MGST, compared with co-milled with MGST. CONCLUSION: MGST has been shown to have a significant impact on co-milled dry powder stability after storage at elevated humidity in terms of physico-chemical properties and aerosol performance.

Investigation into the Manufacture and Properties of Inhalable High-Dose Dry Powders Produced by Comilling API and Lactose with Magnesium Stearate.

The aim of the study was to understand the impact of different concentrations of the additive material, magnesium stearate (MGST), and the active pharmaceutical ingredient (API), respectively, on the physicochemical properties and aerosol performance of comilled formulations for high-dose delivery. Initially, blends of API/lactose with different concentrations of MGST (1-7.5% w/w) were prepared and comilled by the jet-mill apparatus. The optimal concentration of MGST in comilled formulations was investigated, specifically for agglomerate structure and strength, particle size, uniformity of content, surface coverage, and aerosol performance. Secondly, comilled formulations with different API (1-40% w/w) concentrations were prepared and similarly analyzed. Comilled 5% MGST (w/w) formulation resulted in a significant improvement in in vitro aerosol performance due to the reduction in agglomerate size and strength compared to the formulation comilled without MGST. Higher concentrations of MGST (7.5% w/w) led to reduction in aerosol performance likely due to excessive surface coverage of the micronized particles by MGST, which led to failure in uniformity of content and an increase in agglomerate strength and size. Generally, comilled formulations with higher concentrations of API increased the agglomerate strength and size, which subsequently caused a reduction in aerosol performance. High-dose delivery was achieved at API concentration of >20% (w/w). The study provided a platform for the investigation of aerosol performance and physicochemical properties of other API and additive materials in comilled formulations for the emerging field of high-dose delivery by dry powder inhalation.

Influence of jet milling and particle size on the composition, physicochemical and mechanical properties of barley and rye flours.

Finer barley and rye flours were produced by jet milling at two feed rates. The effect of reduced particle size on composition and several physicochemical and mechanical properties of all flours were evaluated. Moisture content decreased as the size of the granules decreased. Differences on ash and protein contents were observed. Jet milling increased the amount of damaged starch in both rye and barley flours. True density increased with decreased particle size whereas porosity and bulk density increased. The solvent retention capacity profile was also affected by jet milling. Barley was richer in phenolics and had greater antioxidant activity than rye. Regarding colour, both rye and barley flours when subjected to jet milling became brighter, whereas their yellowness was not altered significantly. The minimum gelation concentration for all flours was 16%w/v. Barley flour gels were stronger, firmer and more elastic than the rye ones.

Effects of Jet-Milled Defatted Soy Flour on the Physicochemical and Sensorial Properties of Hamburger Patties.

We investigated the physicochemical and sensorial properties of hamburger patties made with three different defatted soybean flour (DSF) preparations which differed in particle size. Coarse (Dv50=259.3±0.6 µm), fine (Dv50=91.5±0.5 µm), and superfine (Dv50=3.7±0.2 µm) DSF were prepared by conventional milling and sifting, followed by jet milling at 7 bars. Hamburger patties containing 5% of each DSF were prepared for a property analysis. The hamburger patties made with 5% superfine DSF showed the lowest cooking loss among the treatment groups (p<0.05). The patties with superfine DSF also retained the texture profile values of the control patties in terms of hardness, gumminess, springiness, and chewiness, while the addition of coarse and fine DSF increased the hardness and chewiness significantly (p<0.05). The sensorial results of quantitative descriptive analysis (QDA) indicate that the patties containing superfine DSF were softer and tenderer than the controls (p<0.05). Although the overall acceptability of the patties made with coarse and fine DSF was poor, the overall acceptability of the superfine DSF patty was the same as that of the control patty. These results suggest that superfine DSF is an excellent food material that can supply dietary fiber, while maintaining the physical characteristics and texture of hamburger patty.

Btk Inhibitor RN983 Delivered by Dry Powder Nose-only Aerosol Inhalation Inhibits Bronchoconstriction and Pulmonary Inflammation in the Ovalbumin Allergic Mouse Model of Asthma.

BACKGROUND: In allergen-induced asthma, activated mast cells start the lung inflammatory process with degranulation, cytokine synthesis, and mediator release. Bruton's tyrosine kinase (Btk) activity is required for the mast cell activation during IgE-mediated secretion. METHODS: This study characterized a novel inhaled Btk inhibitor RN983 in vitro and in ovalbumin allergic mouse models of the early (EAR) and late (LAR) asthmatic response. RESULTS: RN983 potently, selectively, and reversibly inhibited the Btk enzyme. RN983 displayed functional activities in human cell-based assays in multiple cell types, inhibiting IgG production in B-cells with an IC50 of 2.5 ± 0.7 nM and PGD2 production from mast cells with an IC50 of 8.3 ± 1.1 nM. RN983 displayed similar functional activities in the allergic mouse model of asthma when delivered as a dry powder aerosol by nose-only inhalation. RN983 was less potent at inhibiting bronchoconstriction (IC50(RN983) = 59 µg/kg) than the ß-agonist salbutamol (IC50(salbutamol) = 15 µg/kg) in the mouse model of the EAR. RN983 was more potent at inhibiting the antigen induced increase in pulmonary inflammation (IC50(RN983) = <3 µg/kg) than the inhaled corticosteroid budesonide (IC50(budesonide) = 27 µg/kg) in the mouse model of the LAR. CONCLUSIONS: Inhalation of aerosolized RN983 may be effective as a stand-alone asthma therapy or used in combination with inhaled steroids and ß-agonists in severe asthmatics due to its potent inhibition of mast cell activation.