Spray-dried whey protein/lactose/soybean oil emulsions. 1. Surface composition and particle structure

Emulsions made of whey protein, lactose and soybean oil were spray-dried and the chemical surface composition of the dried powders estimated by electron spectroscopy for chemical analysis. In particular, the ability of whey protein to encapsulate fat was highlighted. Additionally, the structure of the spray-dried powder particles was studied by scanning electron microscopy. The powders were examined after storage in both dry and humid atmospheres (relative humidity 75%, 4 days). It was found that the ability of whey protein to encapsulate soybean oil is rather low compared with sodium caseinate, with a large part of the powder surface covered by fat after spray-drying. After storage in humid atmosphere there is a release of encapsulated oil onto the powder surface in most cases, and an increase in fat coverage. The release offat onto the powder surfaces causes the particle structure to change dramatically for powders containing a critical amount of lactose. Such powders agglomerate and lose structure completely. In comparison, powders containing no lactose storage under humid conditions also cause a release of fat onto the powder; however, in this case particle structure remains intact. Powders containing only a small amount of lactose, up to ~25% of emulsion dry weight, do not exhibit the release of fat onto the powder surfaces after storage under humid conditions and the structure of these powder particles does not change. The presence of lactose in whey protein-stabilized emulsions, however, does not increase fat encapsulation by whey protein, as reported earlier for sodium caseinate-stabilized emulsions that were spray-dried. During spray-drying of whey protein/lactose solutions there is a strong overrepresentation of surface-active whey protein on the powder surface. Whey protein coverage increases even further when the powders are stored under humid conditions, also making them lose structure.     

Invited review: spray-dried dairy and dairy-like emulsions--compositional considerations

Milk constituents [caseins, whey proteins (WP), lactose, and anhydrous milk fat] are used widely in the manufacture of dehydrated dairy and dairy-like emulsions. When sodium caseinate- (NaCas) and WP-stabilized emulsions with an oil-to-protein ratio ranging from 0.25 to 5 are dehydrated, NaCas is a more effective encapsulant than WP because of its superior emulsifying properties and resistance to heat denaturation. Denaturation degree of WP during drying has been associated with increased powder surface fat and larger droplet size after reconstitution. Encapsulation of NaCas-stabilized emulsions improves in the presence of lactose; powder surface fat was reduced from 30 to <5% when lactose was added at a 1:1 ratio to NaCas in an emulsion containing 30% (wt/wt) oil. This has been related to the ability of lactose to form solid-like (or glassy) capsules during sudden dehydration. Encapsulation of WP-stabilized emulsions is not improved by addition of lactose, although there are conflicting reports in the literature. Storage stability of dehydrated dairy-like emulsions is strongly linked to lactose crystallization as release of encapsulated material occurs during storage at high relative humidities (e.g., 75%). The use of alternative carbohydrates as “matrix-forming” materials (such as maltodextrins or gum arabic) improves storage stability but compromises the emulsion droplet size after reconstitution. The composition of the powder surface has been recognized as a key parameter in dehydrated emulsion quality. It is the chemical composition of the powder surface that dictates the behavior of the bulk in terms of wettability, flowability, and stability. Analyses, using electron spectroscopy for chemical analysis of the surface of industrial milk powders and dehydrated emulsions that mimicked the composition of milk, showed that powder surface is covered mainly by fat, even when the fat content is very low (18 and 99% surface fat coverage for skim milk and whole milk powders, respectively). The functional properties of milk constituents during emulsion dehydration are far from being thoroughly understood; future research needs include a) the encapsulation properties of pure micellar casein; b) a deeper understanding of colloidal phenomena (such as changes in the oil-water and air-oil interfaces) that occur before, during, and after dehydration, which ultimately define emulsion stability after drying; and c) reconciliation of the current different views on powder surface composition.     

Microencapsulation properties of soy protein isolate: Influence of preheating and/or blending with lactose

Properties and storage stability of spray-dried emulsions stabilized by unheated and preheated (95 °C, 15 min) soy protein isolates, alone or in combination with lactose, were investigated. In general, the heat pretreatment greatly improved retention efficiency (RE), redispersion behavior, glass transition temperature (T_g) and thermal stability of the emulsion powders, but accelerated instability of the reconstituted emulsions. Additional blending with lactose further considerably improved the RE and dissolution behavior, but significantly decreased the stability of reconstituted emulsions and T_g. Storage at 75% relative humidity resulted in considerably increased droplet size of reconstituted emulsions, as well as decreased RE, wettability and T_g, especially in the powders containing lactose. Microscopic observations confirmed that the changes in properties and stability of the powders upon storage were closely related to rupture of particle structure, and/or particle agglomeration. These findings provide fundamental understanding for the development of microencapsulated products using soy proteins as the wall materials.     

热处理对大豆分离蛋白稳定乳液包埋特性的影响

本实验通过喷雾干燥前对SPI溶液95℃1 5 min热处理及形成乳液后加入乳糖溶液制备粉末样品,并将部分干粉储存于RH 75%环境中记录其7 d内等温吸湿线,待吸湿稳定后得到湿粉样品,测定原始乳液及干、湿粉末复溶乳液的粒径大小分布,干、湿粉末的水分含量、包埋效率(ME)、溶解速率并用扫描电镜(SEM)观察其微观结构。结果表明热处理和加糖处理能显著提高喷雾干燥SPI稳定乳液的包埋效率,高达98.68%,相对于未经处理的SPI乳液包埋效率高出1倍以上,此外含糖粉末表现出良好的溶解性,但潮湿环境对其溶解性、包埋效率及微观结构有较大影响。     

Behaviour of oil droplets during spray drying of milk-protein-stabilised oil-in-water emulsions

The effects of spray drying on the behaviour of oil droplets in oil-in-water emulsions (12.0%, w/w, maltodextrin; 20.0%, w/w, soya oil) stabilised with either sodium caseinate or whey protein isolate (WPI) were examined as a function of protein concentration (0.5–5.0%, w/w). Spray drying and redispersion caused a shift in the droplet size distribution to larger values for all emulsions made using low protein concentrations (0.5–2.0%, w/w), in comparison with their respective parent emulsions. However, the droplet size distribution was affected only very slightly by spray drying when the protein concentration was above 2.0% (w/w). The effects of maltodextrin concentration (1.0–25.0%, w/w) on the behaviour of WPI-stabilised emulsions (0.5–10.0%, w/w, WPI, 20.0%, w/w, soya oil) were also examined. Emulsions containing low levels of maltodextrin showed marked re-coalescence during spray drying and redispersion even at a WPI concentration of 10.0% (w/w).     

Pea (<Emphasis Type="Italic">Pisum sativum,L.</Emphasis>) Protein Isolate Stabilized Emulsions: A Novel System for Microencapsulation of Lipophilic Ingredients by Spray Drying

Oil-in-water emulsions can be considered as an important delivery system for lipophilic food molecules. In this study, pea protein isolate (PPI) was studied for its emulsifying capacity at various pH values and pH 7 was selected to prepare emulsions for the production of dry microcapsules. Emulsions stabilized by PPI just enough to cover oil droplets were mixed with solutions of starch hydrolysates of various dextrose equivalent (DE) and subsequently spray dried to yield powders with 30 wt% oil. Effects of DE (6, 12, 19, and 28) on feed emulsion properties and on the characteristics of the spray-dried powders were examined. Reconstituted emulsion oil droplet size and stability were affected by DE in all cases. Microencapsulation efficiency of dried emulsions increased significantly with increasing DE. The scanning electron microscope results showed that lower maltodextrins DE microcapsules are shallow and presented rough surfaces or invaginations. However, higher carbohydrates DE microcapsules were circular and uniform showing minimum cracks and dents on the surface confirming these DE to be efficient encapsulating materials. The formation of the drying matrix seems control the destabilization of pea protein-coated oil droplets during spray drying. In systems where the matrix is formed in a uniform manner, the interfacial protein film is less affected by the drying process. Thus the functionalities of pea protein can be protected during drying by using high DE carbohydrates.     

Prediction of Thermohydric History of Whey Protein Concentrate Droplets during Spray Drying

In this study, we analyzed heat and mass transfer phenomena occurring during spray drying of a whey protein concentrate at pilot scale. Conservation equations were written for both liquid droplets and humid air. Predicted results were then compared with experimental data: particle final moisture content, outlet air temperature, and humidity. The good adequacy found between experimental and predicted data allowed us to use the predicted values as a good indicator of thermohydric history followed by a droplet during drying. These results can also be used to help to find optimal process settings during production of spray-dried powders with specific properties.     

Microencapsulating Properties of Whey Protein Concentrate 75

ABSTRACT Emulsions containing various levels of soya oil dispersed in solutions of whey protein concentrate (WPC) 75 (5% w/v) were spray-dried to yield powders with oil contents ranging from 20% to 75% (w/w). The effect of homogenizing pressure and oil/protein ratio on oil globule size distributions and protein load of the emulsions and the microencapsulation efficiency (ME) and redispersion behavior of the powders were examined. Emulsion oil droplet size decreased with increasing homogenization pressure but was not affected by oil/protein ratio. Emulsion protein load and ME of the powders were negatively correlated with increasing oil/protein ratio. Powders with an oil/protein ratio < 0.75 were least susceptible to destabilization during spray-drying.     

Effects of feed composition,protein denaturation and storage of milk serum protein/lactose powders on lactosylation

During whey powder production, the feed is subjected to several heat treatments which can cause lactosylation of proteins. In this study, lactosylation of whey proteins was evaluated in spray-dried powders before and after storage by varying the native protein fraction as well as the serum protein/lactose ratio in the powders. The lactosylation of native α-lactalbumin and β-lactoglobulin in the powders before storage was not affected to a large extent by the protein denaturation or if the feed had been heat treated in a high or low lactose environment. After storage (relative humidity of 23.5%, 30 °C, 25 days), the kinetic of lactosylation tended to increase with increasing native protein fraction and bulk protein content in the powders. An explanation could be that proteins dissolved in the lactose glassy structure might have a lower reactivity, while proteins present in the protein glassy structure with dissolved lactose may display higher lactosylation reactivity.     

Influence of homogenisation conditions and drying method on physicochemical properties of dehydrated emulsions containing different solid components

Dehydrated o/w emulsions containing sodium caseinate and lactose (sample 1), and gelatine, sucrose and maltodextrin (DE 10) (sample 2) were used to study the influence of homogenisation conditions – homogenisation pressure (15 and 70 MPa) and number of passes (1 and 2) – and the drying method – spray‐drying vs. freeze‐drying – on physicochemical parameters, including oil microencapsulation efficiency (ME), oil droplet size in reconstituted emulsions, water activity, glass transition temperature, powder bulk density and time for emulsion reconstitution in water. Results showed that small and uniform oil droplets attained with increased homogenisation pressure were not sufficient for high oil encapsulation. The permeability of the solid wall to the extraction solvent appeared to be the dominant factor, and this may increase with homogenisation pressure. With the exception of oil droplet size in sample 1 and ME in sample 2, the drying method exerted larger changes in the physicochemical parameters studied than the homogenisation pressure. For sample 2, significant changes in the ME were not observed between the freeze‐dried and spray‐dried samples, even though a great emulsion destabilisation was observed in the reconstituted emulsion of the latter.     

Proposing Novel Encapsulating Matrices for Spray-Dried Ginger Essential Oil from the Whey Protein Isolate-Inulin/Maltodextrin Blends

The aim of this study was to evaluate the effects of the blending of whey protein isolate (WPI) with maltodextrin (MD) and inulin (IN) biopolymers as encapsulating matrices for spray-dried ginger essential oil. Encapsulation was performed by ultrasound-assisted emulsification and using spray drying, and the stability parameters of the emulsion (with or without ultrasound-assisted) were evaluated. The influence of these different wall material systems was investigated based on various functional properties of microparticles such as stability of the emulsion, encapsulation efficiency, reconstitution properties, chemical profile, microparticle stability, morphology, particle size distribution, and crystallinity. Higher viscosity values were obtained for the emulsions prepared with WPI and IN which had the apparent viscosity increased by the ultrasound-assisted emulsification process. Creaming index values indicated that ultrasound-assisted emulsions had higher stability. The composition of the wall materials did not affect the solubility and the moisture content of the particles. The wettability property of the powders was improved by the addition of IN. The lowest level of water adsorption under conditions of high relative humidity was also observed in microparticles containing IN. The partial replacement of WPI by MD significantly affected the efficiency of encapsulation. Moreover, MD led to high thermal microparticle stability. Larger particles were observed in the powders prepared with WPI. The powders obtained from WPI, WPI:IN, and WPI:MD treatments exhibited amorphous structures and did not have any cracks on the surface. The findings of this study indicate that IN and MD together with WPI proved to be good alternative secondary wall materials for spray-dried ginger oil.     

Droplet characterization and stability of soybean oil/palm kernel olein O/W emulsions with the presence of selected polysaccharides

Droplet characteristics, flow properties and stability of egg yolk-stabilized oil-in-water (O/W) emulsions as affected by the presence of xanthan gum (XG), carboxymethyl cellulose (CMC), guar gum (GG), locust bean gum (LBG) and gum Arabic (AG) were studied. The dispersed phase (40%) of the emulsions was based on soybean oil/palm kernel olein blend (70:30) that partially crystallized during extended storage at 5 °C. In freshly prepared emulsions, the presence of XG, CMC, GG and LBG had significantly decreased the droplet mean diameters. XG, LBG, GG and CMC emulsions exhibited a shear-thinning behavior but AG emulsion exhibited a Bingham plastic behavior and control (without gum) emulsion almost exhibited a Newtonian behavior. Both control and AG emulsions exhibited a severe phase separation after storage (30 days, 5 °C). The microstructure of stored XG emulsion showed the presence of partially coalesced droplets, explaining a large increase in its droplet mean diameters. Increases in droplet mean diameters and decreases in flow properties found for stored GG and LBG emulsions were attributed to droplet coalescence. Nevertheless, the occurrence of droplet coalescence in these emulsions was considered to be small as no free oil could be separated under centrifugation force. Increases in flow properties and excellent stability towards phase separation found for stored CMC emulsion suggested that CMC could retard partial coalescence. Thus, the results support the ability of CMC, GG and LBG in reducing partial coalescence either by providing a sufficiently thick continuous phase or by acting as a protective coating for oil droplets.     

Fat properties during homogenization, spray-drying, and storage affect the physical properties of dairy powders

Changes in fat properties were studied before, during, and after the drying process (including during storage) to determine the consequences on powder physical properties. Several methods were combined to characterize changes in fat structure and thermal properties as well as the physical properties of powders. Emulsion droplet size and droplet aggregation depended on the homogenizing pressures and were also affected by spray atomization. Aggregation was usually greater after spray atomization, resulting in greater viscosities. These processes did not have the same consequences on the stability of fat in the powders. The quantification of free fat is a pertinent indicator of fat instability in the powders. Confocal laser scanning microscopy permitted the characterization of the structure of fat in situ in the powders. Powders from unhomogenized emulsions showed greater free fat content. Surface fat was always overrepresented, regardless of the composition and process parameters. Differential scanning calorimetry melting experiments showed that fat was partially crystallized in situ in the powders stored at 20°C, and that it was unstable on a molecular scale. Thermal profiles were also related to the supramolecular structure of fat in the powder particle matrix. Powder physical properties depended on both composition and process conditions. The free fat content seemed to have a greater influence than surface fat on powder physical properties, except for wettability. This study clearly showed that an understanding of fat behavior is essential for controlling and improving the physical properties of fat-filled dairy powders and their overall quality.     

阿拉伯胶/乳清蛋白乳液的干燥行为特性的研究

为了研究液滴/颗粒在喷雾干燥过程中的干燥机理,本实验制备以阿拉伯胶和乳清蛋白为壁材的乳液,采用单液滴干燥技术(single droplet drying,SDD)模拟喷雾干燥环境,对单个液滴/颗粒的干燥过程进行分析,探究气流温度和壁材种类对液滴/颗粒干燥行为和所得颗粒性质的影响。结果表明:气流温度为130 ℃时所得颗粒形态最大,110 ℃次之,90 ℃下所得颗粒最小,气流温度高会促进表壳快速形成,进而抑制颗粒收缩,故所得颗粒较大。此外,增大气流温度有利于提高液滴/颗粒的干燥速率。与阿拉伯胶乳液相比,乳清蛋白乳液液滴降速干燥阶段出现早,所得颗粒收缩程度较小。研究结果表明干燥气流温度和壁材种类对表壳形成过程和颗粒形态有显著的影响。     

碱热改性米渣谷蛋白对W/O/W型双重乳液稳定性的影响

目的：实现米渣谷蛋白在乳浊体系中的应用。方法：选取碱热改性米渣谷蛋白和span80,采用一步乳化法制备W/O/W型双重乳液,并考察蛋白浓度对双重乳液稳定性的影响。结果：当蛋白质量分数从0.5%升高至2.5%时,乳液大粒径峰消失,显微结构中液滴的双重结构增强,表观黏度及黏弹性提高,离心稳定性和贮藏稳定性增强。当蛋白质量分数为2.5%时,离心后乳清析出指数从37.21%降至10.56%,分层时间从6 h延长至96 h。蛋白质与span80形成复合膜共同稳定油水界面,形成中间态液滴,当界面蛋白足以形成刚性界面膜时,液滴从中间态转为稳定的双重结构;当蛋白质量分数为3.0%时,双重乳液发生絮凝使大粒径峰重新出现,稳定性下降,离心后乳清析出指数为16.48%,制备后96 h左右分层,过剩的蛋白质一部分参与内相液滴的构建,另一部分单独形成O/W型液滴吸附于大体积液滴外侧。结论：一步乳化法下,蛋白质量分数为2.5%时,可制得稳定双重乳液。     

Effects of using whey and maltodextrin in white cheese powder production on free fatty acid content,nonenzymatic browning and oxidation degree during storage

Use of maltodextrin and whey improves the physical properties of spray-dried cheese powder and, as cheese replacers, they decrease the raw material costs. However, it is necessary to evaluate their effects on the chemical quality and sensory properties of the product. Three powders, control (CON), whey-added cheese powder (WACP), and maltodextrin-added cheese powder (MACP) were produced to determine free fatty acid (FFA) content, degree of nonenzymatic browning, oxidation, and sensory (flavour) changes during 12 months' storage. In the emulsion preparation and drying process, total volatile FFAs decreased up to 9% and 53.5%, respectively, with higher decrease in CON than in WACP or MACP. Although whey increased oxidation degree of powder, oxidised flavour could not be perceived until the ninth month of storage. Maltodextrin slightly decreased cheese flavour and overall impression scores. There was no difference detected in the powders for scorched flavour.     

Effects of Co-spray Drying of Surfactants with High Solids Milk on Milk Powder Wettability

Dairy industries often spray lecithin, a food-grade surfactant, to spray-dried whole milk powders while fluidisation to produce instant powders. Though adding surfactant to milk feed was often reported to improve the wettability of dried powders, this approach was not favourably used. The present study investigated the effects of surfactant addition into high solids milk feed before drying on the wettability of whole milk particles. Adding either 0.1 wt.% Tween 80 or 0.1 wt.% lecithin to un-concentrated whole milk led to a significant wettability improvement of spray-dried powders. At higher feed solids levels of 23 and 33 wt.%, the wetting process of pure milk powders was comparatively rapid, but the surfactant-added powders showed similar wettability to the pure milk powders. The development of powder wettability as drying progressed was investigated using single droplet-drying technique for 32 and 43 wt.% whole milk in the presence and absence with surfactants. The technique captured an advanced shell formation during drying of higher solids milk. The wettability of surface shells formed by surfactant-added milk was similar to those formed by pure milk throughout drying, from initial shell formation to final drying stage. By contrast, coating surfactants on the outer layer of particles being dried could substantially improve wettability. The rapid shell formation and the slow material diffusion owing to the high medium viscosity were considered the main factors limiting the migration of surfactant molecules towards droplet surface during drying.     

Effect of spray freeze drying on the structural modification and rehydration characteristics of micellar casein powders

Micellar casein (MC) is usually spray-dried into powder form for transportation and storage. However, the micellar structure maintained by colloidal calcium phosphate (CCP) and hydrophobic forces leads to poor rehydration ability of MC powders, which limits its potential applications. Here, spray freeze drying (SFD) with controlled droplet size was used to produce MC powders. Their effects on the structure of MC and the subsequent rehydration characteristics including wetting, dispersion and dissolution were investigated. The results showed SFD powders obtained from smaller droplet size caused more than 50% of serum Ca²⁺ and PO₄³⁻ to release from the micellar structure. These powder particles exhibited extremely high porosity (92%) and spherical morphology, which thus greatly shortened their wetting time. Furthermore, the smallest droplets during SFD were believed to produce the MC powders with the quickest dispersion and best solubility, as over 80% of the solids could be completely dissolved in just 15 min.     

Microencapsulation properties of protein isolates from three selected Phaseolus legumes in comparison with soy protein isolate

The spray-drying microencapsulation properties of protein isolates from three selected Phaseolus legumes (kidney, red and mung beans; KPI, RPI and MPI), at a specific concentration (6 g/100 mL) and oil/protein ratio (1:1, w/w) were compared with soy protein isolate (SPI). The oil retention efficiency (RE), redispersion and dissolution behavior, as well as microstructure of the spray-dried powders were characterized. The influence of storage at 75% relative humidity for 7 days on these characteristics was also evaluated. The results indicated that the microencapsulation properties (except RE in the KPI case) of the three protein isolates were considerably poorer than SPI, though their emulsifying ability was even superior. The microencapsulating properties of these protein isolates were largely associated with their interfacial properties, especially the interfacial protein concentration. Among the three protein isolates, the spray-dried powders with KPI exhibited highest RE but least redispersion and/or dissolution behavior. The storage resulted in a severe loss of RE and ability to be redispersed and/or dissoluted, with much higher extent observed for the KPI powder. These results suggest that appropriate modifications, especially in interfacial properties, should be conducted on these proteins to warrant their application as wall materials in spray-drying microencapsulation.     

Modifications in stability and structure of whey protein-coated o/w emulsions by interacting chitosan and gum arabic mixed dispersions

The influence of chitosan and gum arabic mixtures on the behaviour of o/w emulsions has been investigated at pH = 3.0. The emulsion behaviour, properties and microstructure were found to be greatly dependent on the precise gum arabic to chitosan ratio. Mixing of gum arabic with chitosan leads to the formation of coacervates of a size dependent on their ratio. Incorporation of low gum arabic to chitosan weight ratios into whey protein-coated emulsions causes depletion flocculation and gravity-induced phase separation. Increasing the polysaccharide weight ratio further, a droplet network with a rather high viscosity (at low shear stress) is generated, which prevents or even inhibits phase separation. At even higher gum arabic to chitosan ratios, the emulsion droplets were immobilised into clusters of an insoluble ternary matrix. Although the emulsion droplet charge had the same sign as that of the coacervates, clusters of oil droplets in a ternary matrix were generated. A mechanism to explain the behaviour of the whey protein-stabilised o/w emulsions is described on the basis of confocal and phase contrast microscopic observations, rheological data, zeta potential measurements, particle size analysis and visual assessment of the macroscopic phase separation events.