Amir Hossein Saberi

Fabrication of vitamin E-enriched nanoemulsions: Factors affecting particle size using spontaneous emulsification

Oil-in-water nanoemulsions are finding increasing use as delivery systems to encapsulate lipophilic bioactive components in functional food, personal care, and pharmaceutical products. We have investigated the influence of system composition and preparation conditions on the particle size of vitamin E acetate (VE)-loaded nanoemulsions prepared by spontaneous emulsification. This method relies on the formation of very fine oil droplets when an oil/surfactant mixture is added to water. The oil-to-emulsion ratio content was kept constant (10 wt.%) while the surfactant-to-emulsion ratio (%SER) was varied (from 2.5 to 10 wt.%). Oil phase composition (vitamin E to medium chain triglyceride ratio) had a major effect on particle size, with the smallest droplets being formed at 8 wt.% VE and 2 wt.% MCT. Surfactant type also had an appreciable impact on particle size, with TWEEN® 80 giving the smallest droplets from a group of food-grade non-ionic surfactants (TWEEN® 20, 40, 60, 80, and 85). Surfactant-to-emulsion ratio also had to be optimized to produce fine droplets, with the smallest droplets being formed at SER=10 wt.%. Particle size could also be reduced by increasing the temperature and stirring speed used when the oil/surfactant mixture was added to water. By optimizing system composition and homogenization conditions we were able to form VE-loaded nanoemulsions with small mean droplet diameters (d<50 nm) and low polydispersity indexes (PDI<0.13). The spontaneous emulsification method therefore has great potential for forming nanoemulsion-based delivery systems for food, personal care, and pharmaceutical applications.

Formation of vitamin D nanoemulsion-based delivery systems by spontaneous emulsification: Factors affecting particle size and stability

Oil-in-water nanoemulsions are particularly suitable for encapsulation of lipophilic nutraceuticals because of their ability to form stable and transparent delivery systems with high oral bioavailability. In this study, the influence of system composition and preparation conditions on the particle size and stability of vitamin D nanoemulsions prepared by spontaneous emulsification (SE) was investigated. SE relies on the formation of small oil droplets when an oil/surfactant mixture is titrated into an aqueous solution. The influence of oil phase composition (vitamin D and MCT), surfactant-to-oil ratio (SOR), surfactant type (Tween 20, 40, 60, 80 and 85), and stirring conditions on the initial particle size of vitamin D nanoemulsions was studied. Nanoemulsions with small droplet diameters (d<200 nm) could be formed using Tween 80 at SOR⩾1 at high stirring speeds (800 rpm). These systems were relatively stable to droplet growth at ambient temperatures (<10% in diameter after 1 month storage), but unstable to heating (T>80°C). The thermal stability of the nanoemulsions could be improved by adding a cosurfactant (sodium dodecyl sulphate (SDS)). The spontaneous emulsification method is simple and inexpensive to carry out and therefore has great potential for forming nanoemulsion-based delivery systems for food, personal care, and pharmaceutical applications.

Effect of glycerol on formation, stability, and properties of vitamin-E enriched nanoemulsions produced using spontaneous emulsification

Oil-in-water nanoemulsions are finding increasing use as delivery systems to encapsulate lipophilic bioactive components in functional food, personal care, and pharmaceutical products. We investigated the influence of a water-soluble cosolvent (glycerol) on the formation, stability, and properties of vitamin E acetate-loaded nanoemulsions (VE-NEs) prepared by spontaneous emulsification. VE-NEs were formed by titration of a mixture of vitamin E acetate, carrier oil (MCT) and non-ionic surfactant (Tween 80) into an aqueous glycerol solution with continuous mixing. Cosolvent concentration had an appreciable effect on the particle size produced, with the smallest mean droplet diameters (d<50 nm) being formed at 40 and 50 wt% glycerol. Nanoemulsions (d<100 nm) containing 10% vitamin E acetate could be produced at relatively low surfactant concentrations (5%) using these high glycerol levels. The turbidity of the NEs decreased at high glycerol concentrations due to the reduction in droplet size and refractive index contrast. The long-term stability of the VE-NEs was strongly influenced by glycerol concentration and storage temperature. VE-NEs containing 40% glycerol were relatively stable to droplet growth when stored at 5 and 20°C, but a rapid increase in droplet size and turbidity occurred during storage at 37°C. Temperature scanning experiments (20-80-20°C) indicated that a steep and irreversible increase in turbidity occurred during heating, which was around 70°C in the absence of glycerol and 60°C in the presence of 40% glycerol. Droplet instability was attributed to an increase in the rate of Ostwald ripening and/or coalescence as the temperature was increased, associated with dehydration of the non-ionic surfactant head-group leading to a reduction in phase inversion temperature. Dilution (100×) of VE-NEs containing glycerol with water considerably improved their stability to droplet growth, especially at high storage temperatures. This study provides important information about the effect of glycerol on the formation, stability and physical properties of VE-enriched NEs suitable for food, personal care, and pharmaceutical products.

Nanoemulsion-Based Delivery Systems for Polyunsaturated (ω-3) Oils: Formation Using a Spontaneous Emulsification Method

Nanoemulsion-based delivery systems are finding increasing utilization to encapsulate lipophilic bioactive components in food, personal care, cosmetic, and pharmaceutical applications. In this study, a spontaneous emulsification method was used to fabricate nanoemulsions from polyunsaturated (ω-3) oils, that is, fish oil. This low-energy method relies on formation of fine oil droplets when an oil/surfactant mixture is added to an aqueous solution. The influence of surfactant-to-oil ratio (SOR), oil composition (lemon oil and MCT), and cosolvent composition (glycerol, ethanol, propylene glycol, and water) on the formation and stability of the systems was determined. Optically transparent nanoemulsions could be formed by controlling SOR, oil composition, and aqueous phase composition. The spontaneous emulsification method therefore has considerable potential for fabricating nanoemulsion-based delivery systems for incorporating polyunsatured oils into clear food, personal care, and pharmaceutical products.

Stabilization of Vitamin E-Enriched Nanoemulsions: Influence of Post-Homogenization Cosurfactant Addition

Oil-in-water nanoemulsions are being used in the food, beverage, and pharmaceutical industries to encapsulate, protect, and deliver lipophilic bioactive components, such as drugs, vitamins, and nutraceuticals. However, nanoemulsions are thermodynamically unstable systems that breakdown over time. We investigated the influence of posthomogenization cosurfactant addition on the thermal and storage stability of vitamin E acetate nanoemulsions (VE-nanoemulsions) formed from 10% oil phase (VE), 10% surfactant (Tween 80), 20% cosolvent (ethanol), and 60% buffer solution (pH 3). Addition of a nonionic cosurfactant (0.5% Tween 20) caused little change in droplet charge, whereas addition of anionic (0.5% SDS) or cationic (0.5% lauric arginate) cosurfactants caused droplets to be more negative or positive, respectively. Tween 20 addition had little impact on the cloud point of VE-nanoemulsions, but slightly decreased their isothermal storage stability at elevated temperatures (37 °C). Lauric arginate or SDS addition appreciably increased the cloud point, but did not improve storage stability. Indeed, SDS actually decreased the storage stability of the VE-nanoemulsions at elevated temperatures. We discuss these effects in terms of the influence of surfactants on droplet growth through Ostwald ripening and/or coalescence mechanisms. This study provides important information about the effect of cosurfactants on the stability of VE-nanoemulsions suitable for use in pharmaceutical and food products.

Thermal reversibility of vitamin E-enriched emulsion-based delivery systems produced using spontaneous emulsification.

The influence of temperature scanning and isothermal storage conditions on turbidity, particle size, and thermal reversibility of vitamin E-enriched emulsions produced by spontaneous emulsification was examined. Initially, the mini-emulsions formed were optically transparent and contained small droplets (d ≈ 44 nm). When heated (20-90 °C), emulsions exhibited a complex turbidity-temperature profile with a phase inversion temperature (PIT) at ≈ 75-80 °C. Temperature scanning rate had a major influence on emulsion thermal reversibility. Slow heating (0.5 °C/min) above the PIT followed by quench cooling (≈ 67 °C min(-1)) to 30 °C did not appreciably increase turbidity or droplet diameter (d ≈ 50 nm), suggesting these systems were thermo-reversible. However, slow heating to temperatures below the PIT followed by rapid cooling appreciably increased droplet size and turbidity (thermo-irreversible). Cooling rate also affected emulsion thermo-reversibility: the turbidity and droplet size after heating above the PIT decreased with increasing cooling rate.

Effect of salts on formation and stability of vitamin E-enriched mini-emulsions produced by spontaneous emulsification.

Emulsion-based delivery systems are being utilized to incorporate lipophilic bioactive components into various food, personal care, and pharmaceutical products. This study examined the influence of inorganic salts (NaCl and CaCl2) on the formation, stability, and properties of vitamin E-enriched emulsions prepared by spontaneous emulsification. These emulsions were simply formed by titration of a mixture of vitamin E acetate (VE), carrier oil (MCT), and nonionic surfactant (Tween 80) into an aqueous salt solution with continuous stirring. Salt type and concentration (0-1 N NaCl or 0-0.5 N CaCl2) did not have a significant influence on the initial droplet size of the emulsions. On the other hand, the isothermal and thermal stabilities of the emulsions depended strongly on salt levels. The cloud point of the emulsions decreased with increasing salt concentration, which was attributed to accelerated droplet coalescence in the presence of salts. Dilution (2-6 times) of the emulsions with water appreciably improved their thermal stability by increasing their cloud point, which was mainly attributed to the decrease in aqueous phase salt levels. The isothermal storage stability of the emulsions also depended on salt concentration; however, increasing the salt concentration decreased the rate of droplet growth, which was the opposite of its effect on thermal stability. Potential physicochemical mechanisms for these effects are discussed in terms of the influence of salt ions on van der Waals and electrostatic interactions. This study provides important information about the effect of inorganic salts on the formation and stability of vitamin E emulsions suitable for use in food, personal care, and pharmaceutical products.

Tuneable stability of nanoemulsions fabricated using spontaneous emulsification by biopolymer electrostatic deposition

Nanoemulsions can be formed spontaneously from surfactant-oil-water systems using low energy methods. In this work, we showed that the droplets in oil-in-water nanoemulsions fabricated by spontaneous emulsification could be coated with an anionic biopolymer (beet pectin) using electrostatic deposition. Nanoemulsions were formed by titrating oil (medium chain triglycerides) and surfactant (polyoxyethylene sorbitan monostearate+lauric arginate) mixtures into an aqueous solution (10 mM citrate buffer, pH 4). Lauric arginate was used to generate a positive charge on the droplet surfaces, thereby enabling subsequent electrostatic deposition of anionic pectin. Extensive droplet aggregation occurred when intermediate pectin concentrations were used due to bridging flocculation. However, stable anionic pectin-coated lipid droplets could be formed at high pectin concentrations. These results demonstrate the possibility of tailoring the functionality of lipid nanodroplets produced by spontaneous emulsification.

Influence of surfactant type and thermal cycling on formation and stability of flavor oil emulsions fabricated by spontaneous emulsification

Food-grade emulsions can be fabricated using simple and inexpensive low-energy homogenization methods. In this study, we examined the influence of surfactant type (Tween 40, 60, and 80), oil phase composition (limonene-to-medium chain triglyceride ratio), and temperature (25 to 95°C) on the formation and stability of flavor oil-in-water emulsions (10wt% oil, 15wt% surfactant, pH3) fabricated using spontaneous emulsification. Transparent emulsion-based delivery systems containing ultrafine droplets (d<40nm) could be formed at room temperature at certain limonene contents for all three surfactants. When these emulsions were heated and then cooled, appreciable droplet growth occurred at lower limonene levels (<60% limonene) leading to cloudiness, but ultrafine droplets were still present at higher limonene concentrations (80% limonene) leading to optical clarity. These results were attributed to the influence of oil phase composition and surfactant type on the phase inversion behavior of the surfactant-oil-water systems.