Spray-drying Process Research Articles

Optimization of Spray Drying Process of Mangiferin Extract from Mango Leaf (Mangifera indica L.) and Encapsulation for Diabetes Treatment

Optimization of Spray Drying Process of Mangiferin Extract from Mango Leaf (Mangifera indica L.) and Encapsulation for Diabetes Treatment

Investigating the spray drying damage mechanism of baijiu yeast with combined drying process and equipment

Abstract Traditional drying processes used to dry high-quality baijiu yeast-Sporidiobolus johnsonii A do not offer advantages such as high efficiency, high survival rate, and low energy consumption. Therefore, we investigated the damage inactivation mechanism of S. johnsonii A for the spray drying process. Subsequently, the combined drying process and equipment for spray + vacuum-microwave-vibration were designed. The results reveal selective permeability damage and collapse owing to gel and anti-hexagonal phase transitions of the cell membrane, resulting in S. johnsonii A inactivation and massive inactivation at 52 °C with a water content of 0.21 and at 71 °C with a water content of 0.07, respectively. The combined drying process developed in this study successfully dried S. johnsonii A with high efficiency (1.1 h) and excellent quality (85.4 ± 2 %).

Data-Driven Modeling of the Spray Drying Process. Process Monitoring and Prediction of the Particle Size in Pharmaceutical Production.

Spray drying is used in the pharmaceutical industry for particle engineering of amorphous solid dispersions (ASDs). The particle size of the spray-dried (SD) powders is one of their key attributes due to its impact on the downstream processes and the drug product's functional properties. Offline and inline laser diffraction methods can be used to estimate the product's particle size; however, the final release of these ASDs is based on offline instruments. This paper presents a novel data-driven modeling approach for predicting the particle size of SD products. The model-based characterization of the process and the product's particle size, as a critical quality attribute, follows the quality by design principles. The resulting model can be used for online process monitoring, reducing the risks of out-of-specifications products and supporting their real-time release. A Tucker3 model is trained to capture and factorize the deterministic variability of the process. Subsequently, a partial least-squares regression model is calibrated to model the impact that variability in the input material properties, the process parameters, and the spray nozzle have on the products' particle size. This strategy has been calibrated and validated using large scale production data for two intermediate drug products under high sparsity of particle size data. Despite the challenges, high accuracy was obtained in predicting the median particle size (dv50) for release. The 99% confidence interval results in an error of maximum 2.5 μm, which is less than 10% of the allowed range of variation.

Microencapsulation of highly concentrated polyphenolic compounds from purple corn pericarp by spray-drying with various biomacromolecules

Colored corn pericarp contains unusually high amounts of industrially valuable phytochemicals, such as anthocyanins, flavanols, flavonoids, and phenolic acids. Polyphenols were extracted in an aqueous solution and spray-dried to produce microencapsulates using four carrier materials, namely, maltodextrin (MD), gum arabic (GA), methylcellulose (MC), and skim milk powder (SMP) at three concentrations (1, 2, and 3 %, respectively). The encapsulates were evaluated for their polyphenolic contents using spectrophotometric techniques and HPLC analyses, and their antioxidant properties were evaluated using four different assays. The physicochemical properties of encapsulates were analyzed by measuring the zeta potential (ZP), particle size distribution, water solubility index (WSI), water absorption index (WAI), and color parameters. Structural and thermal properties were evaluated using Fourier transform infrared spectroscopy (FTIR), optical profilometry, and differential scanning calorimetry (DSC) analyses. Comparative analysis of structural characteristics, particle size distribution, zeta potential, WSI, WAI, and aw of the samples confirmed the successful formulation of encapsulates. The microencapsulates embedded with 1 % concentrations of MD, MC, GA, or SMP retained polyphenolic compounds and exhibited noteworthy antioxidant properties. The samples encapsulated with GA or MD (1 %) demonstrated superior physicochemical, color, and thermal properties. Comprehensive metabolomic analysis confirmed the presence of 38 phytochemicals in extracts validating the spray-drying process.

Characterization of the Aroma Profile of Ginger Powder Produced by a Split-Stream Spray-Drying Process.

Freeze-dried ginger (Zingiber officinale) is renowned for its high quality, but it is expensive. As an alternative, spray drying can be explored for producing ginger powder. However, sugar rich feed solutions can lead to stickiness development during the process. Adding carrier materials increases costs and labeling. Accordingly, a split-stream spray-drying process was developed, where ginger fibers in their natural composition were reintroduced as a carrier material into the spray-drying process. The inlet and outlet temperatures were set at 220 and 80 °C, respectively, for optimal aroma retention. Using a stir bar sorptive extraction-gas chromatography-mass spectrometry-olfactometry, the results revealed that reintegrating ginger fibers significantly increased the concentration of eight key odorants. Although freeze-dried ginger retains more aroma, the total concentration of twenty-seven odorants in the developed spray-dried ginger was 1.9 times higher compared to frozen ginger.

Archaeosomes for Oral Drug Delivery: From Continuous Microfluidics Production to Powdered Formulations.

Archaeosomes were manufactured from natural archaeal lipids by a microfluidics-assisted single-step production method utilizing a mixture of di- and tetraether lipids extracted from Sulfolobus acidocaldarius. The primary aim of this study was to investigate the exceptional stability of archaeosomes as potential carriers for oral drug delivery, with a focus on powdered formulations. The archaeosomes were negatively charged with a size of approximately 100 nm and a low polydispersity index. To assess their suitability for oral delivery, the archaeosomes were loaded with two model drugs: calcein, a fluorescent compound, and insulin, a peptide hormone. The archaeosomes demonstrated high stability in simulated intestinal fluids, with only 5% of the encapsulated compounds being released after 24 h, regardless of the presence of degrading enzymes or extremely acidic pH values such as those found in the stomach. In a co-culture cell model system mimicking the intestinal barrier, the archaeosomes showed strong adhesion to the cell membranes, facilitating a slow release of contents. The archaeosomes were loaded with insulin in a single-step procedure achieving an encapsulation efficiency of approximately 35%. These particles have been exposed to extreme manufacturing temperatures during freeze-drying and spray-drying processes, demonstrating remarkable resilience under these harsh conditions. The fabrication of stable dry powder formulations of archaeosomes represents a promising advancement toward the development of solid dosage forms for oral delivery of biological drugs.

Amino acids as stabilizers for lysozyme during the spray-drying process and storage

Amino acids (AAs) have been used as excipients in protein formulations both in solid and liquid state products due to their stabilizing effect. However, the mechanisms by which they can stabilize a protein have not been fully elucidated yet. The purpose of this study was to investigate the effect of AAs with distinct physicochemical properties on the stability of a model protein (lysozyme, LZM) during the spray-drying process and subsequent storage. Molecular descriptor based multivariate data analysis was used to select distinct AAs from the group of 20 natural AAs. Then, LZM and the five selected AAs (1:1 wt ratio) were spray-dried (SD). The solid form, residual moisture content (RMC), hygroscopicity, morphology, secondary/tertiary structure and enzymatic activity of LZM were evaluated before and after storage under 40 °C/75 % RH for 30 days. Arginine (Arg), leucine (Leu), glycine (Gly), tryptophan (Trp), aspartic acid (Asp) were selected because of their distinct properties by using principal component analysis (PCA). The SD LZM powders containing Arg, Trp, or Asp were amorphous, while SD LZM powders containing Leu or Gly were crystalline. Recrystallization of Arg, Trp, Asp and polymorph transition of Gly were observed after the storage under accelerated conditions. The morphologies of the SD particles vary upon the different AAs formulated with LZM, implying different drying kinetics of the five model systems. A tertiary structural change of LZM was observed in the SD powder containing Arg, while a decrease in the enzymatic activity of LZM was observed in the powders containing Arg or Asp after the storage. This can be attributed to the extremely basic and acidic conditions that Arg and Asp create, respectively. This study suggests that when AAs are used as stabilizers instead of traditional disaccharides, not only do classic vitrification theory and water replacement theory play a role, but the microenvironmental pH conditions created by basic or acidic AAs in the starting solution or during the storage of solid matter are also crucial for the stability of SD protein products.

Safflower protein as a potential plant protein powder: optimization of extraction and spray-drying process parameters and determination of physicochemical and functional properties.

The research about sustainable and alternative plant protein sources has accelerated with the increasing need for protein. Safflower meal has a potential to be used in protein production due to its high protein content. This research aimed to produce an alternative plant-based protein powder using safflower meal. Both extraction and spray-drying parameters of safflower protein powder production were optimized using response surface methodology to achieve maximum yield. Moreover, the physicochemical and functional properties of safflower protein were determined and compared with those of commercial protein powders (soy, sunflower, pea, fava bean, and rice). The optimum extraction conditions were found to be 33.06:1 mL-1 g solvent-to-meal ratio, pH 11.00, 23.34 °C extraction temperature, and 30.86 min extraction time, which were achieved with a protein yield response of 75.21%. The highest powder yield (51.28%) was recorded for drying conditions of inlet air temperature of 160.11 °C, aspiration rate of 54.17 m3 h-1, and feed flow rate of 16.01 mL min-1. According to the amino acid profile of safflower protein, the glutamic acid content (14 475 mg (100 g)-1) was highest, while the methionine content (96 mg (100 g)-1) was lowest. Moreover, safflower protein can be regarded as a high-quality protein due to its high essential amino acid ratio (41.55%). The experiments showed that safflower protein had high solubility and good foam and emulsifying properties. Safflower protein could be a nutritional and functional protein source for the food industry. © 2024 Society of Chemical Industry.

Stabilization of antioxidant thyme-leaves extract (Thymus vulgaris) within biopolymers and its application in functional bread formulation

The aim of this study was to stabilize the antioxidant compounds of thyme (Thymus vulgaris) extract by spray-drying process and MD, WPC and MD-WPC carriers at different temperatures (120 and 150°С). Then, the optimal encapsulated sample was used in different ratios (1, 2, 3 and 5% w/w) to fortify pan-breads. The highest production yield (∼68 %) was obtained in the extract encapsulated with MD-WPC at 150°С. The values of moisture (3.2–4.1 %) and water activity (0.28–0.33) indicated the microbial stability of the powders. The functional characteristics of the particles (solubility and wettability) were affected by the composition and nature of the carriers. Also, the use of WPC led to an increase in physical stability, encapsulation efficiency (∼84 %), TPC (4.4 mgGAE/g) and antioxidant activity (∼77 %). The results of SEM and staining of the samples respectively indicated the effect of the process parameters on the morphology and the placement of the phenolic compounds within carrier's matrix. The physicochemical, textural characteristics, color indices (crumb and crust) and antioxidant activity of fortified breads were affected by the ratio of added free and spray-dried extract. The evaluation of sensory indices (color, texture, chewiness, taste and overall acceptance) indicated the ability to fortify bread with 3 % spray-dried extract.

Spray-drying and rehydration on β-carotene encapsulated Pickering emulsion with chitosan and seaweed polyphenol

The spray-drying process to generate microcapsules from Pickering emulsions needs high temperatures, leading to instability of emulsions and degradation of encapsulated thermosensitive compounds (β-carotene). However, these effects may be attenuated by the introduction of seaweed polyphenols into the emulsion interfacial layers, although the effects underlying this protective mechanism have not been explored. This study evaluates the effects of spray-drying/rehydration on the morphology, encapsulation efficiency, redispersibility, and stability of β-carotene loaded Pickering emulsions stabilized by chitosan (PESC) and Pickering emulsions stabilized by chitosan/seaweed polyphenols (PESCSP). The encapsulation efficiency of β-carotene in PESCSP microcapsules (61.13 %) was higher than PESC (53.91 %). Rehydrated PESCSP exhibited more regular droplet size distribution, higher stability, stronger 3D network morphology, and lower redispersibility index (1.5) compared to rehydrated PESC. Analyses of interfacial layers of emulsions revealed that chitosan covalently bound fatty acids at their hydrophobic side. Polyphenols were linked to chitosan at the hydrophilic side of emulsions through hydrogen bonds, providing 3D network between droplets and antioxidant activities to inhibit the degradation of β-carotene. This study emphasized the role of polyphenols in the interfacial layers of Pickering emulsions for the development of efficient delivery systems and protection of β-carotene and other thermosensitive bioactive compounds during spray-drying and rehydration.

Optimization of spray drying for lulo (Solanum quitoense Lam.) pulp using response surface methodology

Lulo (Solanum quitoense Lam.) is an exotic fruit with high potential in international markets due to its intense aromatic characteristics and its content of nutritional and bioactive compounds. However, it is highly perishable, which backslashes its potential for international exportation. Despite the drying processes affect the nutritional and sensory characteristics, fruit powders obtained by spray drying are promising products for the food, cosmetic, and pharmaceutical industries. This work was conducted aiming to optimize the spray-drying process of lulo pulp. A Box-Behnken design with response surface methodology was used, in which the factors evaluated were inlet air temperature (160 - 220 °C), maltodextrin concentration (15-35%), and whey protein concentration (WPC) (1-5% w/w). The feed rate and air velocity were kept constant at 4 mL/min and 9 m/s, respectively. The optimization resulted in an inlet air temperature of 205.6 °C, 35% maltodextrin, and 1.96% WPC. Under these conditions, the mathematical model estimated a powder yield of 62.8%, a moisture content of 2.3 %, a bulk density of 0.49 g/mL, a solubility of 91.9 %, and an ascorbic acid content of 120.8 mg/100 g powder. The optimal process conditions and the mixture of encapsulants (MD and WPC) allow for obtaining lulo powder with adequate yield and quality characteristics.

Enhanced viability and membrane lipid stability of cholesterol-lowering probiotics through spray drying encapsulation with whey protein isolate-coconut oil complex

This study assessed the effect of whey protein isolate (WPI) and its coconut oil complexes (CO-WPI) on the viability of Limosilactobacillus reuteri KUB-AC5 during spray drying and storage. Varied CO concentrations (0%, 4%, and 8%, w/w) and spray drying temperatures (110 °C and 130 °C) influenced secondary structures, free sulfhydryl groups, disulfide bonds, and DPPH• and ABTS•+ scavenging activities of WPI. Throughout the spray drying and storage processes, CO-WPI effectively reduced lipid peroxidation in the probiotic membranes, as detected by advanced 1H-nuclear magnetic resonance, compared to WPI alone. Microencapsulation in 4CO-WPI at 110 °C provided the highest cell viability during drying (1.34 × 1011 CFU g−1), coupled with the highest cholesterol assimilation (58.43%). After 12 months at 4 °C, viability remained high (5.57 × 1010 CFU g−1). This study demonstrated CO-WPI's potential in reducing oxidative damage and improving probiotic survival, highlighting its efficacy as a microencapsulant in spray drying.

Comparing different single milk droplet drying process with spray drying process

Spray drying is currently the main method of industrial milk production because of its high drying speed and high process control accuracy. By controlling the parameters of spray drying process to control the characteristics of the milk powder is well researched. However, the drying mechanism in spray dryer is still not very clear. Methods of measuring single droplet drying kinetics are widely used instead of directly modelling spray drying kinetics. In this study, single droplet drying methods including sessile drying, filament hanging drying, and levitator drying in room temperature are used to compare and simulate the drying kinetics in spray dryer. Experiments show that the droplets in levitator are more spherical, but the final dry particles tend to be more donut-like due to the compression of the upper and bottom sides by the ultrasonic waves. In the filament hanging drying, the droplets are only suspended on the filament by friction. Due to gravity, the shape of the droplets and dried particles is non-sphere droplet shape. In sessile drying, the droplet is half-sphere shape, and the contact area is not changing because of capillary force. By comparison, the final particle morphologies of these are significantly different from those in the spray dryer, therefore, explore the characteristics of spray-dried droplets by monitoring the drying characteristics of single droplets may not suitable on some situation especially on multi-component materials.

Optimization of spray-drying process for the microencapsulation of L. Plantarum (MCC 2974) in ultrasound hydrated finger millet milk.

Spray drying process was optimized for the development of probiotic finger millet milk powder. The independent parameters considered were inlet air temperature, maltodextrin content, and feed rate depending upon the preliminary trials. The major dependent quality parameters considered in the current work were moisture content, water activity, powder yield, encapsulation efficiency, and viability reduction. The desirability function was considered as a basis for the optimization of spray drying process. At the optimum process conditions of 151.68 °C of inlet air temperature, 100mL/h of feed rate, and 29.32% of maltodextrin content, probiotic finger millet milk powder with 43.81% of powder yield and 84.97% of higher encapsulation efficiency could be achieved. The SEM analysis of the spray-dried powder confirmed the proper encapsulation of viable cells in the powder matrix. XRD analysis showed the amorphous powder structure suitable for other food applications. The promising results could be further utilized to produce non-dairy probiotic finger millet milk powder.

Synthesis of 3D ternary microspheres comprising MXene-CNT-MoSe2via a facile spray-drying process for high-performance K-ion battery anode

This study presents a novel spray-drying method for fabricating three-dimensional (3D) porous composite microspheres (p-MX/CNT@MoSe2) as anodes for potassium-ion batteries (KIBs). These microspheres exhibited a well-defined porous structure formed by decomposition of latex beads and consisted of uniform MoSe2 sheets on a conductive MXene substrate and carbon nanotube (CNT) backbone. The precursor microspheres were synthesized from an aqueous solution containing MXene nanosheets, CNTs, latex beads, and molybdenum salts via spray-drying. The microspheres were homogeneously integrated into a 3D structure, establishing strong interactions. Single-step heat treatment under an inert atmosphere decomposed the latex beads, generating numerous pores, enhancing electrolyte permeation, and facilitating potassium-ion transport. The close MXene-CNT association enhanced the electronic conductivity and mitigated MoSe2 volume fluctuations during cycling. This architecture offers exceptional benefits, including efficient ion and electron transport, reduced potassium-ion diffusion distances, and excellent tolerance to volume changes. Electrochemical tests revealed the remarkable electrochemical performance of p-MX/CNT@MoSe2, with a specific capacity of 272 mA h g−1 at 0.5 A/g after 600 cycles and an outstanding rate capability, providing 225 mA h g−1 at a high 2.0 A/g current density. This study highlights the importance of rational design and synthesis for advancing next-generation electrode materials and sustainable energy storage solutions.

Introducing an Efficient and Eco-Friendly Spray-Drying Process for the Synthesis of NCM Precursor for Lithium-ion Batteries

<p>Ni-rich cathode is one of the promising candidates for high-energy lithium-ion battery applications. Due to its specific capacity, easy industrialization, and good circulation ability, Ni-rich cathode materials have been widely used for lithium-ion batteries. However, due to the limitation of the co-precipitation method, including sewage pollution, and the instability of the long production cycles, developing a new efficient and environmentally friendly synthetic approach is critical. In this study, the Ni<sub>0.91</sub>Co<sub>0.06</sub>Mn<sub>0.03</sub>CO<sub>3</sub> precursor powder was successfully synthesized by an efficient spray-drying method using carbonate compounds as a raw material. This Ni<sub>0.91</sub>Co<sub>0.06</sub>Mn<sub>0.03</sub>CO<sub>3</sub> precursor was calcined by mixing with LiOH·H<sub>2</sub>O (5 wt% excess) at 480°C for 5 hours and then sintered at two different temperatures (780°C/800°C) for 15 hours under an oxygen atmosphere to complete the cathode active material preparation, which is a key component of lithium-ion batteries. As a result, LiNi<sub>0.91</sub>Co<sub>0.06</sub>Mn<sub>0.03</sub>O<sub>2</sub> cathode active material powders were obtained successfully via a simple sintering process on the Ni<sub>0.91</sub>Co<sub>0.06</sub>Mn<sub>0.03</sub>CO<sub>3</sub> precursor powder. Furthermore, the obtained LiNi<sub>0.91</sub>Co<sub>0.06</sub>Mn<sub>0.03</sub>O<sub>2</sub> cathode active material powders were characterized. Overall, the material sintered at 780°C shows superior electrochemical performance by delivering a discharge capacity of 190.76mAh/g at 1<sup>st</sup> cycle (0.1 C) and excellent capacity retention of 66.80% even after 50 cycles.</p>

Encapsulation and characterization of soy protein-based ω-3 medium- and long- chain triacylglycerols microencapsulated with diverse homogenization techniques for improving oxidation stability

Recently, MLCTs have attracted considerable attention as a potential alternative to traditional oils due to their suppressive effect on fat accumulation and insulin sensitivity. In this study, the microcapsules of MLCTs with superior performance were fabricated through different homogenization processes to overcome the limitations of ω-3 medium- and long- chain triacylglycerols (MLCTs), including poor stability and prone oxidation. Additionally, the impact of various homogenization techniques, namely, high-pressure, ultrasound, and cavitation jet, on the particle structure, encapsulation efficiency, and oxidation stability of microcapsules (MLCTs) was investigated. The MLCTs microcapsules fabricated through high-pressure homogenization had a smaller particle size of 295.12 nm, lower PDI of 0.24, and a higher zeta-potential absolute value of 32.65, which significantly improved their dispersion and encapsulation efficiency, reaching 94.56 % after the spray-drying process. Furthermore, the low moisture content and superior storage stability of MLCTs microcapsules have the potential to serve as carriers of liposoluble actives.

Optimization of Spray Drying Process Parameters for the Production of Cranberry Flavoured Oat Milk Powder Using Response Surface Methodology

Optimization of Spray Drying Process Parameters for the Production of Cranberry Flavoured Oat Milk Powder Using Response Surface Methodology

Research on optimization of spray drying conditions, characteristics of anthocyanins extracted from Hibiscus sabdariffa L. flower, and application to marshmallows.

Anthocyanin, a main-colored bioactive compound found in Hibiscus sabdariffa L., is well-known for a varied range of applications as food additives in foodstuff, and natural colorants in food, pharmaceutical, and printing industries. The study aimed to find out the suitable conditions for the spray-drying process to obtain anthocyanin powder from the extract as well as characterized the powder. In addition, the obtained powder was applied to marshmallows and determined the acceptability of appearance, quality, and scavenging capacity of the candy. The carrier of maltodextrin and gum arabic was selected for spray-drying, which had optimal conditions at 144°C and 7 mL/min, resulting in 100.22 mg/g anthocyanin content with an encapsulation efficiency of 93.87%. The obtained anthocyanin has appropriate moisture of 5.14%, quite appropriate bulk density, and tapped density, it also was high solubility, and poor flowability but easy compression. The shape of the particle by SEM analysis was low particle size (2-10 μm), wrinkled, unequal spherical size, rough surfaces with indentations, and slight cracks. The X-ray diffraction (XRD) spectrum of the sample had very low crystallinity and diffuse wide peaks revealing that anthocyanin still exists inside maltodextrin particles. The FT-IR spectrum had oscillations of characteristic groups of anthocyanin structure. Marshmallow samples added 5% anthocyanin powder gained high acceptability of appearance and maintained the scavenging capacity (DPPH) with an IC50 value of 7368.31 ppm after a month of storage.

Electrocatalytic Barrier Comprising Polar SnO2 Quantum Dots Anchored Within Porous Carbon Microspheres Prepared by Spray Drying Process for Li–S Batteries

Hypothesis: Porous carbon microspheres (PCMs) with embedded tin di‐oxide (SnO2) quantum dots (QDs) (P‐SnO2@PCMs) are synthesized and employed as polysulfide barriers to enrich the electrochemical properties.Experiments: This composite structure is prepared by spray drying procedure and followed by heat‐treatment, resulting in well‐arranged macropores with a diameter of 59 nm generated by the polystyrene (PS) nanobeads (ϕ = 150 nm) decomposition. P‐SnO2@PCMs is functioned as an electrocatalytic interlayer and offer advantages such as reduced diffusion length for charged particles that guarantees immediate transfer, improved electrode wetting due to efficient electrolyte infiltration, and accommodation of large volume fluctuations during the redox reactions. Furthermore, the incorporation of polar SnO2 QDs within the microspheres allows for efficient chemical confinement and alteration of trapped polysulfide species due to catalytic activity, leading to an extensive use of the active material.Findings: Advancing from the nanostructural eminence, lithium–sulfur (Li–S) cells paired with P‐SnO2@PCMs‐coated separator and conventional sulfur electrode showed outstanding rate performance (321 mA h g−1 at 2.0 C) and prolonged cyclic steadiness at 0.1 C. This innovative synthesis strategy provides valuable insights for developing novel nanostructures applicable to various rechargeable devices.