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.     

Application of Caseinate Modified with Maillard Reaction for Improving Physicochemical Properties of High Load Flaxseed Oil Microcapsules

High-load flaxseed oil microcapsule is prepared with the Maillard reaction products (MRPs) of sodium caseinate and isomaltooligosaccharide as wall material. It is found that the emulsifying activity index and emulsion stability index of MRPs are increased by 31.32% and 34.11% respectively at the appropriate degree of graft (26.30%) compared with the mixture of sodium caseinate and isomaltooligosaccharide. Smaller droplet size and lower polydispersity index can be achieved in the flaxseed oil emulsions coated by MRPs, due to the change of sodium caseinate molecular weight and spatial structure. The microencapsulation efficiency of the microcapsules coated by MRPs is highly improved up to 98.22% at oil load of 58.43%, compared with the control group. Furthermore, MRPs as coating material can protect flaxseed oil against lipid oxidation at 50 °C for 4 weeks. More importantly, the smooth, round, and compact external surface structures of microcapsule powder support its physical necessity for industrial usage. Due to its high microencapsulation efficiency and good oxidation stability, MRPs formed with sodium caseinate and isomaltooligosaccharide show great application potential in preparing high load oil microcapsule. Practical Applications : Findings in this research could be utilized for developing microencapsulation loaded with higher concentration of flaxseed oil, a rich source of α-linoleic acid and lignans. Application of MRPs (Maillard reaction products) formed through interaction between sodium caseinate and isomaltooligosaccharide by heating improved both its physicochemical properties and oxidative stability. It is a novel approach for developing microcapsule with higher percentages of oils with better oxidative stability.     

Production of Microencapsulated Crawfish (Procambarus clarkii) Astaxanthin in Oil by Spray Drying Technology

In this study, an emulsion prepared with flaxseed oil containing crawfish astaxanthin, sodium caseinate, lactose, and water was spray dried to produce microencapsulated flaxseed oil containing crawfish astaxanthin powder (MCA). Production rate and energy used to produce MCA were estimated. Physicochemical properties and storage stability of MCA were determined. The energy required to spray dry the microencapsulated flaxseed oil containing astaxanthin was 2.36 × 10⁴ kJ/kg of emulsion. The microencapsulation efficiency for MCA was 86.06%, which indicated that more oil was encapsulated than on the particles’ surfaces. The particle size of MCA ranged from 6 to 100 µm. The astaxanthin concentration in MCA was 13.76 μg/g powder and alpha-linolenic acid (ALA) was the predominant fatty acid (53%) in MCA. Degradation of astaxanthin in MCA followed first-order reaction kinetics and could be well described by the Arrhenius equation. The astaxanthin in MCA was more stable when the powder was stored at 5°C than at 25 or 40°C.     

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.     

Sodium Humate as a Promising Coating Material for Microencapsulation of Beauveria bassiana Conidia Through Spray Drying

Microencapsulation of Beauveria bassiana (Bb) conidia with sodium humate (SH) was undertaken successfully through spray drying at a high inlet air temperature of 175°C with corresponding outlet air temperature of 86.5 ± 1.3°C using 0.2% SH. The obtained product was a free-flowing, dark-brown powder containing microcapsules of Bb conidia coated with sodium humate (Bb-SH). These microcapsules measured 2.47–3.57 µm and possessed an uneven, fluffy surface. The colony-forming units (CFU) of Bb-SH microcapsules spray-dried at 175°C were 21.54 LCFUg^?1, on par with 21.59 LCFUg^?1 for Bb conidial powder not subjected to spray drying. Bb-SH microcapsules resulted in a high mortality of 93.0% against six-day-old Helicoverpa armigera larvae within five days after treatment. Bb-SH microcapsules readily dispersed in water, releasing sodium humate from the conidial surface. Germination of conidia was not affected by sodium humate as visualized by scanning electron microscopy of the cuticular surface of treated larvae. Bb-SH microcapsules showed good viability (21.11 LCFUg^?1) at the end of six months of storage at room temperature (～30°). Thus, sodium humate is a promising biopolymer for encapsulation of Bb conidia for extended shelf-life at room temperature.     

Effect of microencapsulation and spray drying on oxidative stability of flaxseed oil and its release behavior under simulated gastrointestinal conditions

Flaxseed oil is one of the richest sources of omega-3 fatty acid (α-linolenic acid, ALA). It contains high amounts of polyunsaturated fatty acids, making it extremely susceptible to oxidation. In the present study, flaxseed oil was stabilized using microencapsulation followed by spray drying and studied for its oxidative stability in terms of peroxide value (PV), thiobarbituric acid, and p-anisidine value at room temperature (35 ± 1°C) and low temperature (4–7°C) storage for 6 months. Results revealed that the developed flaxseed oil powder was stable throughout the storage period and PV remained below to the maximum permissible limit (≤5 mEq/kg oil) prescribed by the Codex Alimentarius Commission. The fatty acids profile measured by gas–liquid chromatography indicated a 14.28–15.13% decrease in ALA content in flaxseed oil as a result of microencapsulation and storage at room temperature. In vitro digestion behavior of microcapsules showed 4.39 ± 0.53 to 19.87 ± 0.47% release of flaxseed oil under simulated gastric continued, whereas under gastrointestinal conditions it was 20.00 ± 3.66 to 59.99 ± 9.29%.     

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.     

Spray drying of babassu coconut milk using different carrier agents

The objective of this work was to optimize the spray drying of babassu coconut milk, an oil-in-water emulsion extracted from babassu kernels, using maltodextrin 10DE and modified starch as the carrier agents. Two central composite rotatable designs were used to verify the effect of the inlet air temperature and carrier agent concentration on process performance (process yield and outlet air temperature) and the physicochemical properties of the powder (moisture content, water activity, hygroscopicity, and lipid oxidation). Powders obtained under optimized conditions (25% maltodextrin concentration and 188°C, and a modified starch concentration of 20% and 170°C) were evaluated according to their morphology, particle size distribution, bulk and absolute densities, porosity, wettability, and thermal analysis.     

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.     

Physicochemical and nutraceutical properties of barley grass powder microencapsulated by spray drying

ABSTRACT

Barley grass (Triticum aestivum L.) is popular, commonly known as a nutritional supplement in China. To obtain the highest chlorophyll and flavonoid content as well as other physicochemical characteristics, spray drying from barley grass juice was carried out for two different maltodextrin concentrations (10 and 20%, dried basis) and four different inlet air temperatures (140, 150, 160, and 170°C). After drying, color, water activity, odor, taste, density, particle size, glass transition temperature, and chlorophyll and flavonoid contents of the dried product were measured. Highest contents of flavonoid (5.66?mg/kg) and chlorophyll (7.29?mg/kg) were obtained under 150°C inlet air temperature, 10% maltodextrin concentration, at a feed flow rate of 1.8?L/h for the drying. Corresponding particle size was 19.58–13.33?µm. The glass transition temperature (T_g) increased with the increasing of maltodextrin concentration; and two max T_g of powder obtained from 10 and 20% maltodextrin concentration were 74.4 and 77.4°C, respectively. Retention of taste and flavor were highest with 20% maltodextrin. High inlet air temperature was contributed to the large discrepancy of odor and taste substances. The best color (lightness L*?=?64.44 and greenness b*?=??11.53) was obtained at 150°C inlet air temperature and 10% maltodextrin concentration. Both maltodextrin concentrations resulted in poor flowability of the dried product (C_I?≤?32.51).     

Effects of process parameters on the physical properties of poly (urea–formaldehyde) microcapsules prepared by a one-step method

The physical properties of microcapsules are strongly influenced by the synthetic conditions used for their preparation. To prepare microcapsules possessing a smooth surface morphology, high mechanical strength, and reduced permeability of the core material, in situ polymerization in an oil-in-water emulsion was performed using poly (urea–formaldehyde) and tetrachloroethylene as the shell and core materials, respectively. The influence of the synthetic conditions, including the initial pH value, concentration of wall material, concentration of NaCl, and heating rate, on the properties of the resulting microcapsules was investigated systematically by an orthogonal factorial design. The physical properties of the microcapsules were characterized using scanning electron microscopy and optical-photographic microscopy. The results showed that the concentration of shell material has a substantial effect on the mechanical strength of the microcapsules. Additionally, a slow heating rate and high initial pH value enhance the preparation of well-defined spherical microcapsules having excellent barrier properties. Finally, a moderate concentration of sodium chloride can remarkably improve the compactness of the capsule wall. The optimum conditions, determined on the basis of utilization of wall material, are as follows: initial pH value: 3.5; concentration of shell material: 3.6 × 10^?2 g/mL; heating rate: 0.5 °C/min; and concentration of sodium chloride: 5.0 × 10^?2 g/mL.     

Microencapsulation of tea tree oil by spray‐drying with methyl cellulose as the emulsifier and wall material together with chitosan/alginate

Amphiphilic methyl cellulose (MC) was used as the emulsifier and the internal wall material to increase the microencapsulation efficiency (ME) of tea tree oil (TTO) and the stability of the emulsion for spray‐drying. The results of microscopy images, zeta potential, and microencapsulation efficiency indicated that the wall material components affected the morphology, stability, and ME of the microcapsules. The microcapsules with the wall materials of MC/chitosan (CTS)/alginate (ALG) were spherical and had higher ME than those with monocomponent or bicomponents of MC, CTS, or ALG, or triple components of MC/ALG/CTS. Spray drying conditions were optimized to find the optimum microencapsulation conditions. The highest ME 89.4% and the highest oil embedding rate (ER) 90.4% were obtained through spray‐dying the emulsion of 0.8 mL TTO embraced by 0.4 g MC, 0.6 g CTS, and 3 g ALG at the drying conditions of inlet air temperature 210 °C, needling frequency 2 s, and pump flow rate 55 r/min. Microencapsulation obviously decreased the release of TTO. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44662.     

Microencapsulation of capsanthin by soybean protein isolate‐chitosan coacervation and microcapsule stability evaluation

Although capsanthin possesses excellent coloring performance and healthcare functions, its application in the food industry is limited due to its susceptibility to humidity, heat, and light. The purpose of this research was to microencapsulate capsanthin by soybean protein isolate (SPI)‐chitosan coacervation and evaluate whether the microencapsulation improved the stability of capsanthin against the adverse conditions mentioned above. The results indicated that the optimum conditions for capsanthin microencapsulation were emulsification speed 10,000 rpm, emulsification temperature 45°C, wall concentration 15 g/L and core to wall ratio 1:2 (w/w). Under these conditions, the droplets in the emulsion were even in size distribution without agglomeration and the microencapsulation efficiency and microencapsulation yield reached 90.46% and 86.69%, respectively. Microencapsulation increased the stability of capsanthin against low/medium moisture, heat, and especially light, but was less effective in protecting capsanthin microcapsules in high moisture. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 39671.     

Volatile Retention and Antifungal Properties of Spray-Dried Microparticles of Lippia sidoides Essential Oil

Spray drying microencapsulation of Lippia sidoides essential oil was investigated. Maltodextrin DE10 and gum arabic at different proportions (4:1, 3:2, 2:3, 0:1 m/m) was used as a carrier. The content of essential oil related to the carrier was 20 and 25% in weight and the emulsions were atomized from 30% up to 60% (m/m) of total solid concentration. Spray dryer inlet temperatures varied from 140 to 160°C and the best thermal efficiency and powder recovery were found at 160°C. Product properties and process performance were assessed on the basis of microscopic features of the powder (shape and size of microparticles), moisture content, and powder recovery. Encapsulation efficiency was estimated through determination of the content of essential oil in the microcapsules. The best encapsulation efficiency was related to experimental parameters as follows: solid content of the encapsulating composition of 50% (m/m), maltodextrin:gum arabic ratio of 0:1 (m/m) and carrier:essential oil ratio of 4:1 (m/m). Antifungal activities of microparticles were evaluated, evidencing their potential as important antifungal agents. The positive findings in this study encourage further research and provide perspectives for the development of phytotherapeutic products from essential oil of Lippia sidoides.     

The Effect of Dryer Inlet and Outlet Air Temperatures and Protectant Solids on the Survival of Lactococcus lactis during Spray Drying

The influence of spray-drying conditions, inlet air temperature (130°C to 200°C), outlet air temperature (38°C to 65°C), drying medium (air and nitrogen) and milk-derived protectants (10%, 15%, and 25% lactose; 5% and 10% sodium caseinate; 10%, 25%, and 35% lactose:sodium caseinate (Lac:NaCas, 3:1)) on the survival of Lactococcus lactis ssp. cremoris was studied using a laboratory-scale spray dryer. An inlet air temperature of 130°C and 65°C as the outlet air temperature maintained high survival of the bacteria without sacrificing low moisture content. Inlet air temperature, previously considered to have no significant effect, was shown to play an important role in the survival of bacteria during spray drying. A mixture of Lac:NaCas (3:1) showed a better protective effect on the survival of bacteria than lactose and sodium caseinate individually, and this effect increased with increasing amount of protectant. The results were generalized by substituting whey protein isolate for sodium caseinate. Finally, the positive effect of elimination of oxygen was demonstrated both by replacing air with nitrogen and adding ascorbic acid as an oxygen scavenger to improve survival of the bacteria. Adding an oxygen scavenger would be a better candidate for industrial application considering the potential high cost of manufacturing if nitrogen was used as the atomization and/or drying medium.     

A New Technique for Spray-Dried Encapsulation of Lycopene

A new technique for lycopene microencapsulation by spray drying using dehumidified air as the drying medium was developed and the optimum operating conditions for encapsulation efficiency were determined. A pilot-scale spray dryer was employed for the spray-drying process. The modification made to the original design consisted of connecting the dryer inlet air intake to an absorption air dryer. The dextrose equivalent (DE) of maltodextrin, ratio of core to wall material, feed temperature, inlet air temperature, drying air flow rate, and compressed air flow rate were the factors investigated with respect to encapsulation efficiency. The resulting microcapsules were evaluated in terms of moisture content, bulk density, rehydration ability, lycopene isomerization, and storage stability. The optimum operating conditions were found to be as follows: ratio of core to wall material, 1:3.3; feed temperature, 52°C; inlet air temperature, 147°C. Under these conditions, the maximum encapsulation efficiency was about 93%. The use of dehumidified air was proven to be an effective way of increasing lycopene encapsulation efficiency.     

Spray Drying and Process Optimization of Unclarified Pomegranate (Punica granatum) Juice

In this study, production of pomegranate juice powder using a spray dryer was investigated. To prevent stickiness, maltodextrin dextrose equivalent 6 (DE6) was used as a drying agent. While feed flow rate, feed temperature, and air flow rate were kept constant, air inlet temperature (110–140°C), percentage maltodextrin (MD; maltodextrin dry solids/100 g feed mixture dry solids; 39.08–64.12%), and feed mixture concentration (19.61–44.11 °Brix) were chosen as the independent variables. Product properties investigated included moisture content, hygroscopicity, anthocyanin content, color change, solubility, bulk density, total phenolics content, antioxidant capacity, and sensory properties. The products were produced with high yield (86%) and high antioxidant activity (77%). MD and drying temperature were found to be the most important variables in production of pomegranate juice powders. Because total color change (ΔE), bulk density, antioxidant capacity, and powder yield were affected strongly by the independent variables, these parameters were used in optimization of the process. The optimum temperature, feed mixture concentration, and percentage maltodextrin were 100°C, 30.8 °Brix, and 53.5% MD, respectively. This study revealed that by applying these optimal conditions, pomegranate juice powder with a 55% dry solids yield, 9.78 total color change, 0.35 g/mL bulk density, and 57.8% antioxidant capacity were produced.     

Effect of process conditions on the microencapsulation of coffee oil by spray drying

Microencapsulation is a good alternative to transform liquid food flavourings, such as coffee oil, into stable and free-flowing powders. Thus the aim of this study was to evaluate the influence of process conditions on the microencapsulation of coffee oil by spray drying, using gum Arabic as encapsulating agent. The effect of total solid content (10–30%), oil concentration with respect to total solids (10–30%) and inlet air temperature (150–190 °C) on the encapsulation efficiency, oil retention, moisture content and powder hygroscopicity were evaluated by a complete 2³ central composite rotatable design. Both encapsulation efficiency and oil retention were negatively influenced by oil concentration and inlet air temperature, and positively affected by total solid content, which could be related to the emulsion viscosity and droplet size. Particles produced at the optimized process conditions (30% of total solids, 15% of oil with respect to total solids and inlet air temperature of 170 °C) were evaluated for oxidative stability and showed to be stable during storage at 25 °C, but not at 60 °C. At this temperature, pure oil presented higher lipid oxidation than encapsulated, confirming the protective effect of microencapsulation on the oxidative stability of this product.     

Estimation of Micellization Parameters of SDS in the Presence of Some Electrolytes for Emulsion Polymerization Systems

The critical micelle concentration and the effective degree of dissociation of micelles (α) of sodium dodecyl sulfate, which is the most extensively used surfactant in emulsion polymerization systems, were determined in the presence of various amounts of sodium carbonate and potassium persulfate, and some monomers, such as methyl methacrylate, butyl acrylate, and styrene by means of the conductometric procedure at 25 °C. In addition, the other micellization parameters, such as aggregation number and number of counter-ions per micelle, were computed directly from the obtained conductivity measurements data. The effect of the combination of sodium carbonate and potassium persulfate, on the critical micelle concentration of the sodium dodecyl sulfate solutions was studied at 60 °C (emulsion reaction temperature). The empirical formulations derived provide an easy way to estimate the critical micelle concentration and the effective degree of dissociation of micelles of a system at a given electrolyte and monomer concentration.     

Microencapsulation of water‐soluble herbicide by interfacial reaction. I. Characterization of microencapsulation

A new microencapsulation was established in which small microcapsules with a hydrophilic polymeric wall could be fabricated, capsulizing the water‐soluble content. The new microencapsulation is based on an emulsion interfacial reaction technique that combines the characteristics of an interfacial reaction and conventional emulsion processes. In this technique, hydrophilic polymers [poly(vinyl alcohol) and chitosan] were used as the wall material of the microcapsules. The microencapsulation process was composed mainly of the following steps: preparation of a water/oil (w/o) emulsion 1 containing hydrophilic polymers and a water‐soluble core material and w/o emulsion 2 containing a water‐soluble crosslinking agent and catalyst; the formation of microcapsules by mixing emulsion 1 and emulsion 2; and washing and drying the formed microcapsules. In the new technique an insoluble polymer film was formed easily by the fast crosslinking reaction on the surface of tiny emulsified polymer solution particles in contact with the emulsified crosslinking agent solution particles under mixing with high speed agitation. Thereby, small stable microcapsules were formed. The emphasis in this study was on the establishment of the microencapsulation process by which microcapsules were formed and controlled. The microencapsulation was characterized by analysis of the size distribution of microcapsules fabricated with process conditions. The clarification of the effect of the preparation conditions was also made on the morphology and diameter of the microcapsules. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 78: 1645–1655, 2000