Effect of emulsifier type on physicochemical properties of water‐in‐oil emulsions for confectionery applications

In a first step of designing tailored confectionery masses using water‐in‐oil emulsions, a parameter screening on emulsion rheology and stability was carried out. The experimental set‐up included cocoa butter as continuous phase and the variation of the disperse phase (water, or 50% sucrose in water), two volume fraction levels and the type of emulsifier (lecithin, polyglycerol polyricinoleate (PGPR), ammonium phosphatide (YN) and blends of lecithin or YN with PGPR). Emulsions were characterised by microscopy, laser diffraction, analytical centrifugation and shear rheology. Results show multimodal droplet size distributions in lecithin‐ or YN‐stabilised emulsions, and droplets which tend to form aggregates and an internal network responsible for shear thinning. PGPR emulsions are characterised by monomodal droplet size distributions and smaller droplets without networking tendency. They exhibit Newtonian flow behaviour and a much higher stability against phase separation. In emulsifier blends, PGPR is mainly responsible for the modulation of physical properties of the emulsions.     

Effect of oil content and processing conditions on the thermal behaviour and physicochemical stability of oil-in-water emulsions

The destabilisation mechanism of oil-in-water (o/w) emulsions was studied as a function of oil content (20% and 40% o/w), homogenisation conditions and crystallisation temperatures (10, 5, 0, −5 and −10 °C). A mixture of anhydrous milk fat and soya bean oil was used as the lipid phase and whey protein isolate (2 wt%) as emulsifier. Crystallisation and melting behaviours were analysed using differential scanning calorimetry. Physicochemical stability was measured with a vertical scan macroscopic analyser. Emulsions with 20% oil were found to be less stable than those with 40% oil. For 20% o/w emulsions, the crystallisation was delayed and inhibited in emulsions with smaller droplets and promoted in emulsions with larger droplets when compared with 40% o/w emulsions. Depending on the droplet sizes in the emulsion, the formation of lipid crystals (in combination with the emulsifier) either stabilises (small droplets) or destabilises (big droplets) the emulsion.     

Combined effects of milk fat globule membrane polar lipids and protein concentrate on the stability of oil-in-water emulsions

Milk fat globule membrane (MFGM) material isolated from reconstituted buttermilk by microfiltration (i.e., whole MFGM) contains two major fractions, namely proteins (consisting mainly of MFGM-specific proteins and serum proteins) and lipids (original membrane polar lipids and contaminating triglycerides from the globule core). In this study, MFGM proteins and polar lipid (PL) concentrate were separated from whole MFGM material using solvent extraction. The particle size distribution, stability, surface protein and polar lipid load of oil-in-water emulsions prepared with protein or PL concentrate, individually or in combination, at various concentrations were examined. At low emulsifier concentrations (<2.3%), there was an interacting effect between proteins and PLs on the droplet size. The phase separation of emulsions prepared with a combination of 0.3% proteins and 0.3% PLs was similar to that of emulsions containing 0.3% proteins. The proteins were more preferentially adsorbed at the emulsion droplet surface compared with PLs.     

Effects of water-soluble soybean polysaccharide on rheological properties,stability and lipid digestibility of oil-in-water emulsion during in vitro gastrointestinal digestion

Water-soluble soybean polysaccharide (SSPS) is a naturally occurring emulsifier. SSPS was used as the sole emulsifier to stabilize an oil-in-water (O/W) emulsion. The effects were investigated of different SSPS concentrations (3–20% (w/w)) on the lipid digestibility, rheological properties and stability of O/W emulsions during in vitro digestion model. The droplet size of the emulsions tended to increase during the oral phase because the emulsions were unstable and droplets coalesced, except with a SSPS concentration of 20% (w/w). The presence of SSPS markedly reduced the free fatty acid (FFA) content after its stabilized O/W emulsion passed through in vitro gastrointestinal digestion. The amount of FFA significantly decreased as the concentration of SSPS increased due to SSPS stabilization film on oil droplet surface and high viscous system. SSPS may be an attractive alternative ingredient to control the lipid digestibility of emulsions for various food products.     

The simulated in vitro infant gastrointestinal digestion of droplets covered with milk fat globule membrane polar lipids concentrate

Milk fat globule membrane polar lipids (MPL) are increasingly used as the surface-active components for emulsions in many infant food products. However, the precise effect of the emulsifier MPL on the digestion of lipids during gastrointestinal digestion has not been elucidated. This study investigated the lipid digestion of droplets covered with MPL with different sizes in a simulated in vitro infant gastrointestinal digestion assay. The well-used surface-active component casein was used as a control. Four types of emulsions were formulated: small and large droplets covered with MPL concentrate (MPL-S and MPL-L, with volumetric means of 0.35 ± 0.01 and 4.04 ± 0.01 μm, respectively), and small and large droplets covered with casein (CN-S and CN-L, with volumetric means of 0.44 ± 0.01 and 4.09 ± 0.03 μm, respectively). The emulsions were subjected to in vitro gastrointestinal digestion using a semidynamic model mimicking infant digestion. Through the determination of particle size evolution, zeta-potential, and microstructure of emulsions, the lipid droplets covered with MPL were found to be more stable than that of the CN-S and CN-L during gastrointestinal digestion. Moreover, although CN-S and CN-L showed a higher initial lipolysis rate at the beginning of gastric digestion, droplets covered by MPL exhibited a significantly higher amount of free fatty acid release during later digestion. The amount of free fatty acid release of the emulsions in both gastric and intestinal digestion could be generally classified as MPL-S ≥ MPL-L > CN-S > CN-L. Our study highlights the crucial role of MPL in the efficient digestion of emulsions and brings new insight for the design of infant food products.     

Emulsification by the phase inversion temperature method: the role of self-bodying agents and the influence of oil polarity

Oil-in-water emulsions stabilized with nonionic emulsifiers change to water-in-oil emulsions as the temperature rises when the hydrophilic and lipophilic properties of the mixed emulsifier are just balanced. Preparation above the phase inversion temperature followed by rapid cooling yields emulsions that exhibit very fine droplet size and extreme long-term stability. Cosmetic emulsions were prepared by this phase inversion temperature (PIT) method using typical raw materials such as polar oils, e.g. decyl oleate, 2-octyl dodecanol or isopropyl myristate, and nonionic emulsifiers, e.g. ceteareth-12 or polyoxyethylene eicosyl/docosyl ether combined with cetostearyl alcohol as a co-emulsifier. The phase inversion temperature was measured as a function of the oil polarity and the concentration of mixed emulsifier. The relationship between phase inversion temperature, droplet size and emulsion stability was investigated. In addition, self-bodying agents such as cetostearyl alcohol or monoglycerides were added to these thin, fine disperse emulsions to adjust the consistency. The influence of these ingredients on phase inversion temperature, droplet size, yield value and emulsion stability was studied.     

Preparation and Characterization of Water/Oil/Water Emulsions Stabilized by Polyglycerol Polyricinoleate and Whey Protein Isolate

ABSTRACT: In this study we tried to prepare stable water-in-oil-in-water (W/O/W) emulsions using polyglycerol polyricinoleate (PGPR) as a hydrophobic emulsifier and whey protein isolate (WPI) as a hydrophilic emulsifier. At first, water-in-oil (W/O) emulsions was prepared, and then 40 wt% of this W/O emulsion was homogenized with 60 wt% aqueous solution of different WPI contents (2, 4, and 6 wt% WPI) using a high-pressure homogenizer (14 and 22 MPa) to produce W/O/W emulsions. The mean size of final W/O/W droplets ranged from 3.3 to 9.9 μm in diameter depending on the concentrations of PGPR and WPI. It was shown that most of the W/O/W droplets were small (<5 μm) in size but a small population of large oil droplets (d > 20 μm) was also occasionally observed. W/O/W emulsions prepared at the homogenization pressure of 22 MPa had a larger mean droplet size than that prepared at 14 MPa, and showed a microstructure consisting of mainly approximately 6 to 7-μm droplets. When a water-soluble dye PTSA as a model ingredient was loaded in the inner water phase, all W/O/W emulsions showed a high encapsulation efficiency of the dye (>90%) in the inner water phase. Even after 2 wk of storage, >90% of the encapsulated dye still remained in the inner water phase; however, severe droplet aggregation was observed at relatively high PGPR and WPI concentrations.     

Stability and Oil Migration of Oil‐in‐Water Emulsions Emulsified by Phase‐Separating Biopolymer Mixtures

Oil‐in‐water (O/W) emulsions with varying concentration of oil phase, medium‐chain triglyceride (MCT), were prepared using phase‐separating gum arabic (GA)/sugar beet pectin (SBP) mixture as an emulsifier. Stability of the emulsions including emulsion phase separation, droplet size change, and oil migration were investigated by means of visual observation, droplet size analysis, oil partition analysis, backscattering of light, and interfacial tension measurement. It was found that in the emulsions prepared with 4.0% GA/1.0% SBP, when the concentration of MCT was greater than 2.0%, emulsion phase separation was not observed and the emulsions were stable with droplet size unchanged during storage. This result proves the emulsification ability of phase‐separating biopolymer mixtures and their potential usage as emulsifiers to prepare O/W emulsion. However, when the concentration of MCT was equal or less than 2.0%, emulsion phase separation occurred after preparation resulting in an upper SBP‐rich phase and a lower GA‐rich phase. The droplet size increased in the upper phase whereas decreased slightly in the lower phase with time, compared to the freshly prepared emulsions. During storage, the oil droplets exhibited a complex migration process: first moving to the SBP‐rich phase, then to the GA‐rich phase and finally gathering at the interface between the two phases. The mechanisms of the emulsion stability and oil migration in the phase‐separated emulsions were discussed.     

Physical stability of emulsion encapsulated in alginate microgel particles by the impinging aerosol technique

Emulsion filled alginate microgel particles can be applied as carrier systems for lipophilic actives in pharmaceutical and food formulations. In this study, the effects of oil concentration, emulsifier type and oil droplet size on the physical stability of emulsions encapsulated in calcium alginate microgel particles (20–80 μm) produced by a continuous impinging aerosol technique were studied. Oil emulsions emulsified by using either sodium caseinate (SCN) or Tween 80 were encapsulated at different oil concentrations (32.55, 66.66 and 76.68% w/w of total solids content). The emulsions were analysed before and after encapsulation for changes in emulsion size distribution during storage, and compared to unencapsulated emulsions. The size distribution of encapsulated fine emulsion (mean size ~ 0.20 μm) shifted to a larger size distribution range during encapsulation possibly due to the contraction effect of the microgel particles. Coarse emulsion droplets (mean size ~ 18 μm) underwent a size reduction during encapsulation due to the shearing effect of the atomizing nozzle. However, no further size changes in the encapsulated emulsion were detected over four weeks. The type of emulsifier used and emulsion concentration did not significantly affect the emulsion stability. The results suggest that the rigid gel matrix is an effective method for stabilising lipid emulsions and can be used as a carrier for functional ingredients.     

Viscosity change in oil/water food emulsions prepared using a membrane emulsification system

This paper reports viscosity measurements of oil/water (O/W) monodispersed emulsions of different droplet diameters obtained in a membrane emulsification system. Hydrophilic microporous glass membranes of different pore diameters were used to prepare O/W emulsions. The results showed that the droplet diameter of the emulsions varied with the average pore diameter of the membrane. The average droplet diameter was found to be about five times greater than the average membrane pore diameter. A correlation was found for the relationship between the average droplet diameter and the emulsion viscosity. As the dispersed droplet size became smaller, the total surface area of the droplets increased. Therefore, the emulsion viscosity and the relative viscosity increased. Few studies have reported the viscosity of O/W emulsions with droplet diameter of 5 μm or more and an oil phase concentration of 10 vol% or less. In the present study a correlation between the droplet diameter and the emulsion viscosity was statistically established. ©     

Droplet Size and Coalescence Stability of Whey Protein Stabilized Milkfat Peanut Oil Emulsions

Droplet diameter and the polydispersity of droplet size tended to decrease with increased proportion of peanut oil. Macromolecular additives affected droplet size. Xanthan gum or sodium carboxymethyl-cellulose (Na-CMC) produced smaller droplets than the controls, but the average diameter was independent of the composition of the dispersed phase. At 50°C the coalescence stability of these emulsions qualitatively correlated with the initial droplet diameter. Xanthan gum and Na-CMC, despite increasing continuous phase viscosity, gave lower stability than controls, primarily the result of flocculation of droplets due to depletion of the highly hydrophilic macromolecule from the intervening region between approaching droplets. At 25°C, stability increased as solid butter oil content of the dispersed phase increased.     

Influence of interfacial composition on oxidative stability of oil-in-water emulsions stabilized by biopolymer emulsifiers

The objective of this research was to evaluate the influence of storage pH (3 and 7) and biopolymer emulsifier type (Whey protein isolate (WPI), Modified starch (MS) and Gum arabic (GA)) on the physical and oxidative stability of rice bran oil-in-water emulsions. All three emulsifiers formed small emulsion droplets (d₃₂ < 0.5 μm) when used at sufficiently high levels: 0.45%, 1% and 10% for WPI, MS and GA, respectively. The droplets were relatively stable to droplet growth throughout storage (d₃₂ < 0.6 μm after 20 days), although there was some evidence of droplet aggregation particularly in the MS-stabilized emulsions. The electrical charge on the biopolymer-coated lipid droplets depended on pH and biopolymer type: −13 and −27 mV at pH 3 and 7 for GA; −2 and −3 mV at pH 3 and 7 for MS; +37 and −38 mV at pH 3 and 7 for WPI. The oxidative stability of the emulsions was monitored by measuring peroxide (primary products) and hexanal (secondary products) formation during storage at 37 °C, for up to 20 days, in the presence of a pro-oxidant (iron/EDTA). Rice bran oil emulsions containing MS- and WPI-coated lipid droplets were relatively stable to lipid oxidation, but those containing GA-coated droplets were highly unstable to oxidation at both pH 3 and 7. The results are interpreted in terms of the impact of the electrical characteristics of the biopolymers on the ability of cationic iron ions to interact with emulsified lipids. These results have important implications for utilizing rice bran oil, and other oxidatively unstable oils, in commercial food and beverage products.     

Impact of iron encapsulation within the interior aqueous phase of water-in-oil-in-water emulsions on lipid oxidation

Iron (Fe³⁺) was encapsulated within the internal aqueous phase of water-in-oil-in-water (W/O/W) emulsions, and then the impact of this iron on the oxidative stability of fish oil droplets was examined. There was no significant change in lipid droplet diameter in the W/O/W emulsions during 7 days storage, suggesting that the emulsions were stable to lipid droplet flocculation and coalescence, and internal water diffusion/expulsion. The initial iron encapsulation (4 mg/100 g emulsion) within the internal aqueous phase of the water-in-oil (W/O) emulsions was high (>99.75%), although, a small amount leaked out over 7 days storage (≈10 μg/100 g emulsion). When W/O/W emulsions were mixed with fish oil droplets the thiobarbituric acid-reactive substances (TBARS) formed decreased (compared to fish oil droplets alone) by an amount that depended on iron concentration and location, i.e., no added iron < iron in external aqueous phase < iron in internal aqueous phase. These differences were attributed to the impact of W/O droplets on the concentration and location of iron and lipid oxidation reaction products within the system.     

Droplet Size and Emulsifier Type Affect Crystallization and Melting of Hydrocarbon-in-Water Emulsions

Differential scanning calorimetry was used to monitor crystallization and melting of 20 wt% n-hexadecane oil-in-water emulsions. The temperature at which droplet crystallization occurred depended on type of emulsifier used to stabilize the droplets: sodium caseinate, whey protein isolate, Tween 20. 40. 60 and 80 or sodium dodecyl sulfate. Emulsifiers with hydrocarbon; ails close in structure to n-hexadecane promdted crystallization at higher temperatures, which suggested that emulsifier molecules at the interface acted as nucleation sites for oil. Smaller droplets crystallized at a slower rate than larger droplets. Droplet size and emulsifier type had no appreciable effect on melting behavior of the droplets.     

Impact of salt and lipid type on in vitro digestion of emulsified lipids

This study examined the effects of oil type and NaCl addition on the micro-structural changes that occur to emulsified lipids as they pass through a model gastrointestinal tract (GIT). Oil-in-water emulsions stabilized by a non-ionic surfactant (Tween 20) were prepared using different kinds of lipids (3% soybean oil, corn oil, olive oil or lard). The emulsified lipids were passed through an in vitro digestion model that simulated the composition (pH, minerals, surface active components, and enzymes) of the human GIT. Prior to digestion, emulsified lipid droplets appear to be bridging flocculation in 1% NaCl added emulsified lipids, moreover lipid droplets of 1% NaCl added emulsified lipids seems to be more disrupted than no NaCl added emulsified lipids. Mean particle size prepared with lard was smaller than those of other emulsified lipids. Free fatty acid contents increased after in vitro digestion in all emulsified lipids. Especially, free fatty acid content of emulsified lipid made from lard and olive oil were significantly higher than those of other emulsions after in vitro digestion.     

Influence of droplet size on the efficacy of oil-in-water emulsions loaded with phenolic antimicrobials

In this study we investigated the effect of droplet size on the antimicrobial activity of emulsions containing two essential oil compounds that are known for their antimicrobial effectiveness: carvacrol and eugenol. Coarse emulsions were prepared by blending a triacylglyceride (Miglyol 812N) containing various concentrations of carvacrol or eugenol (5, 15, 30, 50 wt%) at an oil droplet mass fraction of 10 wt% with an aqueous phase containing 2 wt% Tween 80(?). Premixes were then further dispersed using a high shear blender, a high pressure homogenizer at different pressures or an ultrasonicator to produce droplets with a variety of mean diameters. Microscopy and light scattering storage stability studies over 10 days indicated that manufactured emulsions were stable, i.e. that no aggregation, creaming or other destabilization mechanisms occurred and droplet size distributions remained unchanged. The antimicrobial activity of emulsions was assessed against two model microorganisms, the Gram negative Escherichia coli C 600 and the Gram positive Listeria innocua, by determining growth over time behavior. The analysis yielded the unexpected result that emulsions with larger droplet sizes were more effective at inhibiting growth and inactivating cells than smaller ones. For example, emulsions with a mean oil droplet size of 3000 nm at a concentration of 800 ppm carvacrol completely inhibited L. innocua, while for 80 nm emulsions, only a delay of growth could be observed. Measurements of the concentration of the antimicrobial compounds in the aqueous phase indicated that concentrations of eugenol and carvacrol decreased with decreasing oil droplet sizes. Determination of interfacial tension further showed that eugenol and carvacrol are preferentially located in the oil-water interfaces. Theoretical calculations of Tween 80(?) concentrations needed to saturate interfaces suggested that in small emulsions for the given formulation less Tween 80(?) micelles are present in the aqueous phase. We therefore attribute the fact that antimicrobial nanoemulsions are less active than macroemulsions due to an increased sequestering of antimicrobials in emulsion interfaces and a decreased solubilization in excess Tween 80(?) micelles.     

Characterisation of O/W emulsions encapsulating ergocalciferol using onion skin waste saponins: insights on formulation and release properties

The study was conducted to produce ergocalciferol (Vit-D₂) loaded oil-in-water (O/W) emulsions utilising the onion skin waste saponins (OSW) as a natural emulsifier and almond oil as carrier oil. The impact of different formulations upon the digestibility of lipids, LCT (long-chain triglycerides) or MCT (medium-chain triglycerides), and bioaccessibility of Vit-D₂ was analysed. The mean particle size diameter of almond oil-based O/W emulsions was decreased with increasing homogenisation pressure and emulsifier concentration. During 120 mins of digestion in small intestinal fluids (SIF), almond oil in high-lipid emulsions (5% w/w) was not fully digested, resulting in a lower bioaccessibility of ergocalciferol than low-lipid samples. Almond oil emulsions with larger particle size have a slower rate of lipid digestion than the smaller size particles, but the release rate of free fatty acids was constant throughout the digestion process. Moreover, almond oil emulsions showed similar Vit-D₂ bioaccessibility to the oil-based emulsions but were much higher than MCTs.     

Effect of modified Acacia gum (SUPER GUM™) on the stabilization of coconut o/w emulsions

Two modified Acacia gums, the already tested SUPER GUM? EM2 and the new EM10, were used as combined emulsifiers and stabilizers in coconut oil model emulsions. The properties of gum solutions as well as those of the emulsions were examined. The gum solutions were completely mechanically stable during high-pressure homogenization; therefore, the gum could be added to the emulsion prior to high-pressure treatment. The emulsions were prepared by a small-scale rotor-stator process and by high-pressure homogenization, respectively. Droplet size, stability and rheological properties of the emulsions were examined. As expected, the high-pressure process was very effective. The emulsions made with both modified gums had a droplet size below 1 μm and were completely stable for at least 7 weeks at up to 30 °C. The new SUPER GUM? EM10 was more efficient as an emulsifier than EM2; the droplet size distribution was more homogenous. All emulsions proved to be low-viscous and nearly Newtonian liquids. It can be concluded that the emulsion stability was mainly a result of the excellent emulsifying properties and not of an additional thickening effect of the gums. The modified Acacia gums can be recommended as an emulsifier and stabilizer for application in different food products, preferably in low-viscous emulsions such as coconut milk drinks or other beverages.     

球磨-酯化复合改性槟榔芋淀粉对Pickering乳液形成的影响

为了提高淀粉颗粒的乳化能力,以球磨-酯化复合改性槟榔芋淀粉为颗粒乳化剂,大豆油为油相,制备水包油型Pickering乳液.采用激光粒度仪、研究级正置显微镜、流变仪等对Pickering乳液外观、液滴粒径、显微形态及动态流变特性进行表征,考察淀粉颗粒质量浓度(1、5、10、20、30 mg/mL)和油相体积分数(10％、...