Analysis of Microencapsulation Ability of Essential Oils during Spray Drying

Results of preliminary investigations of the preservation of elemi (E) and peppermint (M) oils in a maltodextrin microcapsule during spray drying of emulsion in a laboratory dryer are discussed. The ratio of maltodextrin to water in the emulsion was 30:70, and the content of each oil 10, 20, and 30 wt·% in relation to maltodextrin. Product quality and results of the process were estimated on the basis of microscopic features of the powder (the shape and size of microparticles) and its density, moisture content and water vapor sorptivity. The efficiency of encapsulation was estimated by specifying the content of essential oil in the product. The compositions of initial oils and the oils contained in the emulsion, inside and on the capsule surface were compared. The positive results of this study justify the necessity of further research and provide a perspective for developing novel technologies.     

Microencapsulation of extra‐virgin olive oil by spray‐drying: Influence of wall material and olive quality

Encapsulation is a process by which small particles of core products are packaged within a wall material to form microcapsules. One common technique to produce encapsulated products is spray‐drying which involves the conversion of liquid oils in the form of an emulsion into dry powders. Emulsification conditions, wall components, and spray‐drying parameters have been optimized for the microencapsulation of different extra‐virgin olive oils. To achieve this goal, the influences of emulsion conditions have been evaluated for different wall components such as proteins (sodium caseinate and gelatin), hydrocolloids (Arabic gum), and hydrolyzed starches (starch, lactose, and maltodextrin). In addition, for each of the tested conditions the ratio of wall solid‐to‐oil and spray‐drying parameters were as well optimized. The microencapsulation effectiveness was determined based on process yield and the ratio between free and encapsulated oil (microencapsulation efficiency). Highest encapsulation yields were achieved when gelatin, Arabic gum and maltodextrin and sodium caseinate and maltodextrin were used as encapsulation agents and the ratio of wall solid‐to‐oil was 1:4 and 1:2, respectively. Under these conditions, 53% of oil was encapsulated. The influence of olive oil quality in the microencapsulation process was evaluated in terms of fatty acids profile alteration after the microencapsulation process.     

Measuring Salinity in crude oils: Evaluation of methods and an improved procedure

In this work, a novel procedure is developed to determine the amount of salt for crude oils in which the available laboratory techniques are unable to provide accurate salt content values. The technique is based on measuring the salinity of the wash water that is vigorously mixed with the crude oil (forming an emulsion) and then separating it from the water-in-oil emulsion by irradiating microwave energy during few minutes. This three step process involves the emulsification of the wash water exempt of salt in crude oil, followed by the recovery of the water by microwave heating and, finally, the analysis of the salt content using the classical Mohr’s method titration procedure. The novel technique presented here was able to provide reliable information about the salt content on Brazilian crude oils, in a rapid manner, without need of unsafe time-consuming solvent extraction procedures.     

Preparation of microcapsules of W/O/W emulsions containing a polysaccharide in the outer aqueous phase by spray‐drying

A water‐in‐oil‐in‐water (W/O/W) multiple emulsion containing a hydrophilic substance, 1,3,6,8‐pyrenetetrasulfonic acid tetrasodium salt (PTSA), and a wall material in its inner and outer aqueous phases, respectively, was prepared by a two‐step emulsification using a rotor/stator homogenizer, and was further homogenized with a high‐pressure homogenizer. Maltodextrin or gum arabic were used as wall materials, and olive oil was used as the oily phase. The high encapsulation efficiency for PTSA (>0.9) was realized. The emulsion was spray‐dried to produce microcapsules of W/O/W type. The efficiencies of the microcapsules prepared with maltodextrin and gum arabic were 0.82 and 0.67, respectively. Stability of the microcapsules was examined at 37 °C and 12%, 33% and 75% relative humidity. Microcapsules prepared with maltodextrin were more stable than those prepared with gum arabic.     

Synthesis of macroporous silica from solid-stabilised emulsion templates

We have investigated the microstructures of the solid residue left behind after the evaporation of solid-stabilised emulsions. The correlation between the microstructure and the properties and preparation conditions of the emulsions will be thoroughly discussed. The type of microstructure is related to the conditions (oil type, oil content, particle type, particle concentration and emulsion type) of the initial emulsion. Solid residues left after evaporation of oil-in-water emulsions containing volatile oils (relative to water) show a “knobbly” microstructure. When oils with similar or lower vapour pressure to that of water were used, “sponge-like” structures were obtained. For emulsions containing volatile oils, the mean drop diameter is similar to the mean pore diameter, whereas when oils with low vapour pressure are used, the pores are much smaller. Finally, this paper will illustrate that stable toluene-in-water emulsions leave porous microstructures, whereas water-in-toluene emulsions and emulsions close to the phase inversion show sheet-like or “knobbly” structure.     

Susceptibility of water-emulsified extra virgin olive oils to oxidation

The effect of emulsion structure on the susceptibility to oxidation of emulsified olive oils was tested. Olive oil samples were emulsified by adding a certain quantity of water in different ways. The resulting water-in-oil emulsions were then oxidized with UV light. The results revealed that the emulsion structure played a significant role in the oxidation process of emulsified olive oils. A kinetic mechanism is discussed based on the PV determined experimentally. The susceptibility of water-emulsified extra virgin olive oils to oxidation was quantified by means of a dimensionless parameter that displayed a characteristic dependence on the specific surface area of the water dispersed phase.     

Study on Demulsification of Crude Oil Emulsions by Microwave Chemical Method

Abstract

The demulsifying and separating experiments of crude oil emulsion were performed by using the heating method, the thermal chemical method, the microwave radiating method, and the microwave chemical method separately. The water content of this emulsion was 78 v/v%, and the type was water‐in‐oil (w/o). The influence tendencies of the key factors on demulsification effect were explored by changing the heating temperature, the demulsifier amount used and the microwave radiating time in this paper. With the microwave chemical experiments on the self‐made emulsions of different water content, the demulsification rate and separation efficiency were explored. The type of these emulsions were oil‐in‐water (o/w), water‐in‐oil (w/o) and the multiple type, related to the water content scopes which were less than 30 v/v%, more than 70 v/v% and between them, respectively. The separation effect by the microwave chemical method for the high water content crude oil emulsion was better than that of emulsion with lower water content. For the crude oil used in this experiment, the result could be obtained that the separation efficiency was about 95 v/v% under the conditions of 50 ppm of demulsifier, 10 seconds radiation time, and 1 minute settling time for the microwave chemical method.     

Effect of Clarification System on the Conservation of Virgin Olive Oil during Its Storage

The results obtained in this work explain how clarification systems can affect the conservation of virgin olive oils (VOOs) during the storage step. The evolution of the quality and sensory properties during the storage of VOOs clarified by different systems, vertical centrifugal separator (VCS) with minimal water addition and conical bottom settling tank (CBST), is studied at industrial scale for two different crop years. In general, VCS oils show a slight higher moisture and solid impurities content at the end of the storage step due to a higher emulsion grade (because of the emulsion generated) caused by the rotating movement of this clarification system. For the studied clarification systems, no remarkable differences are observed between the oils during their storage for quality indexes. However, these systems show differences regarding oil sensory properties. The VOOs clarified by VCS are characterized by a higher presence of phenol components, higher positive sensory attributes intensity, and higher lipoxygenase (LOX) aldehydes content during their storage. VOOs from CBST show lower phenol content, a higher “non‐LOX” volatiles content, and the presence of sensory defects during storage. Practical Applications: The results obtained in this work are very important in order to provide specific recommendations and scientific support based on objective data to improve VOO quality. As described in this study, the VCS with a minimal water addition can be a better option to produce VOO of improved quality. This clarification system is an efficient and quick operation that reduces the contact between oil and the remaining water and impurities during the storage step. The minimal water addition used in this clarification system allows obtaining VOOs with higher phenol content and positive sensory notes. This leads to prolong VOO shelf‐life and conservation during the storage stage, due to preservation of the quality indexes and minor components with antioxidant activity. Besides, this clarification system reduces the water consumption during oil clarification and generates a lower wastewater volume regarding conventional vertical centrifugation, and therefore can be considered more environmentally friendly.     

The Role of Water in Protection Against Thermal Deterioration of Liquid Margarine

The thermal stability of liquid margarine and vegetable oils was investigated by measuring the oxidative stability index (OSI) at temperatures ranging from 90 to 180 °C, whereas total polar compounds (TPC) and tocopherols (vitamin E) were measured during heating at 180 °C in frying trays. Results showed that the OSI of liquid margarine was in the same range as the OSI of vegetable oils at lower temperatures, but at 160 and 180 °C, liquid margarine had significantly higher thermal stability, close to that observed for hard margarine and butter. The increased stability was confirmed by lower levels of TPC and a smaller relative reduction in vitamin E content during heating. Variations between different vegetable oils could partly be explained by differences in degree of saturation and level of vitamin E, with high oleic sunflower oil being the most stable oil at all temperatures. The water in liquid margarine vaporized within 1.5 min at 160 °C, and it is hypothesized that volatile pro‐oxidants are removed with the water, inducing a delay in deterioration. The results indicate a role for water in preventing lipid oxidation and decomposition in fat emulsion products at 160–180 °C, suggesting that liquid margarine, low in saturated fat, may be the healthier and preferable alternative for pan‐frying compared to other liquid vegetable oils.     

蓖麻油聚氨酯-丙烯酸酯复合乳液的合成

采用甲基丙烯酸甲酯（MMA）与蓖麻油水性聚氨酯乳液共聚反应制备聚氨酯丙烯酸酯（PUA）复合乳液,研究了蓖麻油水性聚氨酯性能、MMA添加量、引发剂种类和聚合温度对PUA复合乳液及涂膜性能的影响,并应用傅里叶红外光谱（FTIR）测定反应产物的结构.研究发现,用外观半透明或微透明的PU-M分散液制备的PUA乳液及涂膜性能优良.油溶性引发剂（AIBN）比水溶性引发剂（K₂S₂O₈）更适合本体系的乳液聚合.随着MMA含量增大,PUA复合乳液胶粒粒径增大,黏度减小,涂膜光泽度下降,机械性能变好,耐水性增加.合适的MMA含量为体系总固含量的20%～30%.提出了PUA复合乳液胶粒形成及粒径长大机理.     

用均匀设计的方法进行阳离子型重油乳化剂的研究

采用均匀设计与调优软件进行了重油乳化剂配方实验方案的设计和实验结果的优化。通过两次优化设计的方法 ,较快地取得了最佳配方。实验结果表明 ,阳离子表面活性剂与阴离子表面活性剂复配容易生成不具有表面活性的物质 ,故不宜一同使用。阳离子表面活性剂与非离子表面活性剂复配制得的乳化剂性能较好。乳化剂最佳配方为氯化十八烷基二甲基苄基铵 70mg,聚氧乙烯失水山梨醇单月桂酸酯 7mg ,失水山梨醇单硬脂酸酯 7mg ,乳酸乙酯 36mg(共占乳化油总质量的 0 12 % )。可使燕山石油化工公司产运动黏度ν10 0 =12 0mm2 /s的重油在油水质量比为 70∶30时形成的油包水型乳化重油在 80℃下稳定 3d(72h)以上 ,常温下稳定 1a以上。不同重油乳化稳定性的差别较大。     

Influence of Oil Load and Maltodextrin Concentration on Properties of Tuna Oil Microcapsules Encapsulated in Two-Layer Membrane

The two layers of tuna oil-in-water emulsions containing different oil loads (5–10 wt%) and maltodextrin concentrations (10–20 wt%) were stabilized by a lecithin–chitosan membrane. The liquid emulsions were then spray dried at an inlet air temperature of 180 ± 2°C and an outlet air temperature of 85 ± 5°C. The characteristics of liquid emulsion (creaming and mean droplet size) and spray-dried microcapsules (moisture content, water activity, color, morphology, glass transition temperature, and encapsulation efficiency) were measured. The results suggest that two-layer oil-in-water emulsions are an effective system to produce high oil-loaded microcapsules, which may lead to its wide application for use in food products.     

Reducing Oil Losses in Alkali Refining

Neutralization is an important step in the chemical refining of edible oils. Free fatty acids (FFA) are generally removed in neutralization as sodium soaps but neutral oil is also entrapped in the emulsion and removed with the soap during centrifugation. Thus, alkali neutralization causes a major loss of neutral oil in the chemical refining of edible oils. The effects of demulsifiers (NaCl, KCl, Na₂SO₄ and tannic acid) on reducing alkali refining losses of refined palm, soybean, and sunflower oils (used as model oils) incorporated with FFA from rice bran oil were investigated. Adding small amounts of demulsifiers to the alkali neutralization step significantly reduced neutral oil loss of these model oils. All demulsifiers except for tannic acid had similar effects on refining losses in all oil model systems. The optimum demulsifier content was 1.0 % (w/w of oil).     

The influence of food emulsifiers on fat and sugar dispersions in oils. III. Water content,purity of oils

The influence of water on the interactions between fat and sugar crystals dispersed in triglyceride (vegetable) oils was qualitatively estimated from sedimentation and rheological experiments. The experiments were performed both with and without food emulsifiers (monoglycerides and lecithins) present in the oil. The effects of minor natural oil components (nontriglycerides) on the interactions and on emulsifier adsorption to the crystals were examined by comparing a commercial refined oil and a chromatographically purified oil. The results show that water generally increases the adhesion between fat and sugar crystals in oils and also increases the surface activity of the oil-soluble food emulsifiers. Minor oil components give a small increase in the adhesion between fat and sugar crystals in oils, but do not influence the adsorption of food emulsifiers in any systematic way.     

Making homogeneous and fine droplet O/W emulsions using nonionic surfactants

In many emulsion systems, creaming occurs during the first stage of emulsion breakdown. To reduce the rate of creaming, emulsions having small and uniform droplets are desirable. In this work, types and HLB of nonionic surfactants, emulsification methods, and combinations of oils and nonionic surfactants were investigated in order to make stable and homogeneous emulsions. Emulsification was attained by dissolving the surfactants in the oil phases. The addition speed and volume of water to the oil phases were important factors affecting the emulsion droplet size. The change of the solute state in the process of emulsification was observed stage by stage, and the mechanism of emulsification was elucidated. Homogeneous emulsions were formed in the HLB region, showing liquid crystalline and gel phases in the emulsifying process. The addition speed of water to the oil phase was very important in forming the liquid crystalline and gel phases. Polyoxyethylene(n)sorbitan monostearate could emulsify three kinds of oils (hydrocarbon, fatty acid ester and triglyceride). Polyoxyethylene(n)alkyl ether could emulsify hydrocarbon and fatty acid ester. Polyoxyethylene(n)-monostearate could emulsify only hydrocarbon. Surfactants with proper HLB which were soluble in the oil phase and in the presence of a very small amount of water formed a stable emulsion. The solubility state of oil and surfactant was the key to making a fine emulsion.     

共轭亚油酸粉末化微胶囊的制备

研究了喷雾干燥法制备共轭亚油酸微胶囊的工艺参数及配比条件。结果表明,最佳的工艺参数及配比条件为:乳液80℃热处理60 m in,乳化剂蔗糖酯加入量为水液的1%~1.5%,大豆分离蛋白与麦芽糊精质量比为1∶4,壁材中玉米糖浆含量38.5%,固形物含量16.7%,共轭亚油酸理论含量16%左右,进风温度130~150℃,进料流量(2.5~3.5)×150 mL/h,进料温度35℃,进风流量1.1 m3/m in左右,喷嘴压力180 kPa。制备出的共轭亚油酸微胶囊有较好的产品质量。     

Synthesis of a Series of Anionic Surfactants Derived from NP and their Properties as Emulsifiers for Reducing Viscosity of Highly Viscous Oil via Formation of O/W Emulsions

A series of alkyl phenol polyoxyethylene glycidyl ether (NP-n-O) and alkyl phenol polyoxyethylene ether hydroxypropyl sulfonate (NP-n-S) surfactants was synthesized to explore emulsification viscosity reduction. The optimum sulfonation conditions were obtained through orthogonal experiments, the ratio of alkyl phenol polyoxyethylene glycidyl ether and sodium bisulfite 1:1.5, 100 °C, and 6 h. The effects of concentrations of the synthesized surfactants, pH values, emulsifying temperature (40 and 60 °C) and water content on emulsification viscosity reduction and the stability of the emulsion to Venezuela’s Orinoco heavy oil were investigated. The water diversion ratio of emulsion at the reservoir temperature (55 °C) in 30 days was taken as an index, the results show that under the conditions of a temperature of 40 °C, an oil/water ratio of 7:3 and a surfactant NP-4-S concentration of 0.5 %, emulsions can be formed with a viscosity reduction rate reaching up to 99.69 % and with a water diversion ratio in 30 days reaching 9.38 %; while at 60 °C and an oil/water ratio of 7:3, at an NP-4-S concentration of 1 %, the viscosity reduction rate can reach 99.55 % and water diversion ratio is merely 4.23 % in 30 days. The mixture of NP-n-S, xanthan gum and cocamidopropyl dimethylamine oxide (CAO-30) at suitable concentration can greatly improve the emulsification viscosity reduction and emulsion stability, which gives an emulsion viscosity rate of over 98 %. Moreover, the emulsion can be stable for at least 30 days without water emerging.     

Effects of Surfactant Headgroups on Oil-in-Water Emulsion Droplet Formation: An Experimental and Simulation Study

Nonpolar oils such as kerosene and diesel oil are common collectors in coal flotation. Surfactants are usually added to the pulp to emulsify the oil collectors. The present study used dodecane as the oil collector and anionic sodium dodecyl sulfonate (SDS) and nonionic tetraethylene glycol monododecyl ether (C₁₂EO) with different headgroups and identical chain alkyls to investigate the effect of the surfactant headgroups on oil-in-water emulsion droplet formation. The morphology and stability of dodecane emulsions were determined experimentally. Density functional theory (DFT) and molecular dynamics (MD) simulations were used to explain the microscopic mechanism. The results of DFT indicated a larger interaction between SDS and the water molecules than that between C₁₂EO and water molecules. The results obtained by MD suggested that the SDS headgroup exhibited a loose arrangement and a relatively large gap size, thereby weakening the interaction between SDS and water molecules at the dodecane/water interface. In contrast, the headgroups of C₁₂EO were bent and interwoven with others to form a tight reticulation at the interface. According to the simulation results, the ability of the surfactant to form dodecane-in-water emulsion droplets depends on the arrangement of the surfactants at the oil–water interface rather than on the interaction strength between the headgroups of the surfactants and water molecules. The presented microscopic mechanism of the surfactant headgroup formation of oil-in-water emulsion droplets offers surfactant selection and design references.     

Effect of oil type on stability of high internal phase water-in-oil emulsions with super-cooled internal phase

This study considered the stability and rheology of a type of high internal phase water-in-oil emulsions (W/O) emulsion. The aqueous phase of the emulsions is a super-cooled inorganic salt solution. The oil phase is a mixture of industrial grade oils and stabilizer. Instability of these systems manifests as crystallization of the metastable dispersed droplets with time. This work focused on the effects of oil polarity and oil viscosity on the stability of these emulsions. Ten types of industrial oils, covering the viscosity range 1.4–53.2?cP, and with varying polarity, were used in combination with polymeric poly(isobutylene) succinic anhydride (PIBSA) and sorbitan monooleate (SMO)-based surfactants. The effect of oil relative polarity on rheological parameters of the emulsion was evident mainly in the emulsions stabilized using polymeric surfactant, whereas the oil viscosity did not show any significant effect. The optimum stability of the emulsions stabilized with SMO was achieved using high polar oils with a viscosity of 3?±?0.5?cP. However, when using the PIBSA surfactant, the best emulsion stability was achieved with low polar, high viscosity oils.     

Chemical Stability of the Lipid Phase in Concentrated Beverage Emulsions Colored with Natural β-Carotene

The aim of this study was to examine the oxidation of selected plant oils in concentrated beverage emulsions colored with natural β-carotene. Carotenoid preparations obtained from carrots were dissolved in cold-pressed linseed oil, refined canola oil, and refined palm olein. Oxidative stability of the lipids was examined with and without addition of the pigment to the oil/water (O/W) emulsion. Carotenoid/lipid hydro peroxide (LOOH) concentration was evaluated using two different methods: LOOH + Fe²⁺ reaction connected with a colored complex of ammonium thiocyanate determined with the help of a spectrophotometer, and LOOH determined with the help of a chemiluminometer. It was shown that oxidation rate of lipids in the O/W emulsions strongly depended on chemical composition of the lipid fraction (type of oil used). Presence of the carotenoid pigment increased the rate. Therefore, if a carotenoid-containing emulsion is to be stable, it should be based on oils of a high oxidative stability.