Modification of molecular conformation of spray-dried whey protein microparticles improving digestibility and release characteristics

This study reports on the preparation of riboflavin-loaded whey protein isolate (WPI) microparticles, using desolvation and then spray drying. Ethanol desolvation led to the exposure of embedded hydrophobic amino acids of WPI to riboflavin, facilitating the formation of riboflavin-WPI complexes. The extent of desolvation and cross-linking influenced the morphology of the spray-dried microparticles, while the moisture content of microparticles decreased with desolvation and increased with crosslinking. The modification of WPI conformation upon desolvation could be retained in the dry state via spray drying. The gastric resistance, release site and release characteristics of microparticles were readily adjusted by varying the ethanol and calcium ion contents from 0 to 50% v/v and from 0 to 2 mM, respectively. The sample prepared from 30% v/v ethanol without calcium crosslinking displayed rapid peptic digestion in less than 30 min. The samples from 30% v/v ethanol at 1 and 2 mM Ca 2+ exhibited excellent gastric resistance and intestinal release

Characterisation of thermal and structural behaviour of lipid blends composed of fish oil and milkfat

The blend of fish oil with a high percentage of long chain poly-unsaturated fatty acids, and milkfat with a high percentage of saturated fatty acids, could potentially demonstrate desirable characteristics from both components, such as increased omega-3 fatty acids and melting point, as well as improved crystallization and oxidative stability. In this study, the effect of various milkfat concentrations on thermal properties and crystalline structure of these blends were analysed to understand parameters determining the overall characteristics of the blend. Blends with different ratios of fish oil: milkfat (9:1, 7:3, 5:5, 3:7, 1:9), as well as pure fish oil and pure milkfat, were investigated at different cooling conditions. The crystallization behaviour in all samples shifted to lower temperature ranges, by increasing the cooling rate from 1 to 32 °C/min. However, the changes in cooling rate did not have significant effect on the melting profile of the samples. Whereas changes in milkfat ratio affect both the crystallization and melting behaviour. New crystallization peaks were observed on DSC spectra between the range of −4 to −13 °C in the blends. Moreover, new melting peaks appeared in two ranges of −1 to −8 °C and 8–9 °C, in the blends. The crystallization and melting behaviour of the blends were similar to those of milkfat when >30% milkfat was used. This was further confirmed via XRD where milkfat demonstrated the dominant polymorphic behaviour. Regarding shape of the crystals, fractal dimension analysis showed a similarity between clusters in blends containing 50% milkfat or higher. Increasing the ratio of milkfat led to an increase in fractal dimension which indicates higher mass-spatial distribution of the crystal networks in the blends. The data showed that adding 30% or more milkfat to pure fish oil resulted in blends demonstrating similar characteristics to milkfat, including thermal, structural, and oxidative stability. This shows the potential of blending a high percentage of docosahexaenoic acid in milk fat to improve their overall stability

Time scale based analysis of in-situ crystal formation in droplet undergoing rapid dehydration

The surface structure of crystalline particles affects the functionality of the particles in drug delivery. Prediction of the final structure of particles that crystallize easily within the spray drying process is of interests for many applications. A theoretical framework was developed for the prediction of crystal structure precipitating on the surface of the particle. This model was based on the dimensionless Damkohler number (Da), to be an indicator of final particle morphology. Timescales of evaporation and reaction were required for calculation of the Damkohler number. The modified evaporation time scale was estimated based on the time that is available for the crystal to precipitate after supersaturation. The reaction time scale was estimated based on the time scale for induction time. Mannitol was produced under different processing conditions in order to validate the theoretical model. Results showed for the high Damkohler numbers, the surface structure of the particle was rough, while smaller Damkohler numbers led to relatively smooth particle surfaces. Additionally, although the beta polymorph was dominant in all of the experiments, alpha polymorph was precipitated in the experiments with a large Damkohler number. The theoretical framework developed will be a useful predictive tool to guide the manipulation of particle crystallization in spray dryers

An accurate account of mass loss during cheese ripening described using the reaction engineering approach (REA)-based model

Cheese ripening is an important step in cheese making for modifying surface and curd properties. Due to physical, chemical and biological changes, mass loss usually occurs during the process. Although these changes are essential for developing the texture and flavour of cheese, mass loss decreases product yields. A reliable mathematical model is used to quantify mass loss during cheese ripening so that the processing conditions can be fine-tuned to achieve the desirable throughput. In this study, for the first time, the reaction engineering approach (REA)-based model is applied to model the cheese ripening. The study shows that the REA-based model is accurate to model cheese ripening of Camembert and French smear cheese. In addition, the REA is able to model the cheese ripening under time-varying environmental conditions. For this purpose, the equilibrium activation energy is evaluated according to the corresponding humidity and temperature in each period, while the same relative activation energy for ripening under constant environmental conditions is implemented. The REA is a simple yet effective approach to model the simultaneous heat and mass transfer process accompanied by chemical and biological reactions. Considering its effectiveness, the REA can be applied in industrial settings for predicting mass loss during cheese ripening

The role of the intermediate stage of drying on particle in-situ crystallization in spray dryers

In-situ crystallization of particles in spray drying has several advantages particularly for product quality modification in the pharmaceutical industry. This process was investigated in a counter current spray dryer using lactose as a model material by manipulation of the local humidity within the drying chamber. Sample collection and humidity injection at different location of the dryer were carried out to better understand the mechanism of particle formation and solidification which are essential components of in-situ crystallization. They revealed that particle formation can be delayed by local humidity elevation. Differential scanning calorimetry and XRD of the yields showed that humidity manipulation was capable to produce semi crystalline lactose of up to 90% crystallinity. The results confirmed that there is a critical period for crystallization such that extending this period would significantly increase the degree of crystallization. Comparison on different requirements of crystallization indicated that extending the time for nucleation and the growth at the critical period via humidity manipulation has the most significant effect on the in-situ crystallization process

Enhancing the stability of protein-polysaccharides emulsions via Maillard reaction for better oil encapsulation in spray-dried powders by pH adjustment

Lipid oxidation remains a major problem faced by the dairy industry. The bio-active ingredient (oil/milkfat) can be shielded by encapsulation within a secondary material. Emulsion stability is one of the main requirements for the production of oil/fat microcapsules with low levels of free surface fat and better encapsulation efficiency. This study focused on the use of sodium caseinate (NaCas)-lactose complex; conjugated via the Maillard reaction, as encapsulating materials, and investigated the effect of pH on the stability of protein-polysaccharide oil-in-water (O/W) emulsions. Subsequently, the properties of spray dried oil microcapsules, including encapsulation efficiency, insolubility, wettability, and microstructure, were analysed. The results demonstrated that better NaCas-lactose interactions were achieved at pH 11, with enhanced adsorption of the conjugates at the oil droplet particles and subsequently better emulsifying properties and stability. Additionally, a better oil entrapment (95.2 ± 3.7%) by the cross-linked protein and lactose was achieved when the pH of NaCas-lactose mixture was adjusted to 11 as compared to a pH of 7.5 (73.1 ± 2%). The outcome showed that it was possible to achieve stable microcapsules with oil loading as high as 80%, and with similar functional properties as those with 40% oil loading

Identification of regions in a spray dryer susceptible to forced agglomeration by CFD simulations

Agglomeration during spray drying improves the rehydration and flow properties of produced powders. However, tools for predicting agglomeration are rare. In this work a rigorous mapping approach incorporating number density and stickiness state of particles was developed for CFD simulations, which identifies different zones prone to coalescence and agglomeration inside a spray dryer. This approach was found to be quick, informative, reasonably accurate and resource efficient, as it bypasses the modelling of collision phenomena. The predictions were validated with experimental data of particle size distribution and SEM analyses of the powder morphology performed on samples produced in a lab-scale counter current spray dryer with varying two-nozzle- configurations. For the investigated dryer, the optimum nozzle configuration to achieve effective agglomeration was successfully identified and configurations yielding size enlargement dominated by coalescence could be distinguished. The developed method is generic and hence can be applied to find suitable location and angle for multiple atomization as well as fine returns in industrial practice to achieve controlled agglomeration. This study forms the fundament of a rigorous CFD model for agglomeration, which along with the findings from this study will allow the agglomeration phenomenon to be better understood and thus attain more efficient design, scale-up and operation of spray dryers

Reduction of surface fat formation on spray-dried milk powders through emulsion stabilization with λ-carrageenan

The appearance of surface fat during the atomization process in spray drying of milk particles often impairs the functional powder properties. To investigate a possible approach that could minimise the surface fat formation, the interaction between a whole milk model emulsion and λ-carrageenan at various concentrations was studied, as well as how it influences the atomization behaviour and the resulting particle characteristics. Carrageenan can stabilize emulsions in the presence of milk protein by adsorption on the milk fat globule membranes. If too little or too much of the polysaccharide was added, bridging flocculation or depletion flocculation, respectively, occurred inside the emulsions. The best stability and minimal fat globule size were obtained for a carrageenan content of 0.3% w/w. Rheological investigation indicated that the extensional viscosity can be an important factor influencing the emulsion disintegration behaviour during atomization. The λ-carrageenan stabilized emulsions featured a significantly increased extensional viscosity and a better fat encapsulation in the corresponding spray-dried particles, promoting solubility and oxidative stability. Surface fat extraction showed that the most stable emulsion lead to particles with the least amount of surface fat. Though the surface of these particles was still covered by fat according to spectroscopic analysis, this surface fat layer was very thin in comparison to carrageenan-free powder as observed by confocal microscopy. Yet, the addition of carrageenan was also found to have one adverse effect on the intended powder properties, as the strengthened emulsion network translated into denser particles and thus a deterioration of the powder's reconstitution behaviour

Improvement of rheological and functional properties of milk protein concentrate by hydrodynamic cavitation

Spray drying at higher solids concentrations improves drying efficiency, and reduces the overall energy cost of milk powder production. As the performance of the evaporator prior to spray drying is limited by viscosity, several methods can be employed to reduce feed viscosity such as thermal pre-treatment or ultrasound. The method employed in this study was hydrodynamic cavitation (HC) on milk protein concentrate (MPC80). Rheological properties of the protein milk were observed to improve, with a reduction in viscosity by 20% and 56% upon the application of a cavitation rotor speed of 25 Hz and 50 Hz, respectively, due to the breakdown in protein gel structure and hence a decrease in the elastic modulus of the proteins. While HC did not adversely affect solubility, with the powders having on average a solubility of 97.5% at a reconstitution temperature of 50 °C, both bulk and tapped density increased when the emulsion was subjected to HC, owing to a reduction in particle size. This study therefore suggests the potential of using HC for a more efficient drying of high solids milk, while maintaining and/or improving the physicochemical properties of powders

A practical CFD modeling approach to estimate outlet boundary conditions of industrial multistage spray dryers: Inert particle flow field investigation

Industrial multistage spray drying systems often have limited in situ process measurements to provide sufficient information for computational fluid dynamics (CFD) simulations of the primary drying chamber. In this case study on the spray dryer at Davis Dairy Plant (South Dakota State University), uncertainties were encountered in specifying the outlet boundary conditions of the spray drying chamber with two outlets: the side outlet and the bottom outlet leading to the second stage external vibrating bed. Using the available data on the vacuum pressure of the chamber, a numerical framework was introduced to approximate suitable outlet boundary conditions for the drying chamber. The procedure involved analyzing the ratio of the airflow rate between the two outlets and using a pseudo-tracer inert particle injection analysis. The goal of this approach was to determine a suitable range of outlet vacuum pressure that will lead to realistic particle movement behaviors during the actual plant operation. The protocol developed here will be a useful tool for CFD modeling of large scale multistage spray drying systems. Abbreviations: ARC: Australian Research Council; CFD: Computational Fluid Dynamics; FFT: Fast Fourier Transform; MCC: Micellar Casein Concentrate; PRESTO: Pressure Staggering Option; SDSU: South Dakota State University; SIMPLE: Semi − Impilicit Method for Pressure Linked Equations; WPC: Whey Protein Concentrate