Echium oil with oxidative stability increased by emulsion preparation in the presence of the phenolic compound sinapic acid followed by dehydration by spray and freeze drying processes.

Echium oil is rich in omega-3, however, is unstable. The objective of this work was the co-encapsulation of echium oil and sinapic acid (SA) by emulsification using Arabic gum as emulsifier/carrier, followed by spray or freeze-drying. Eight treatments (S0, S200, S600 and S1000: particles spray dried with different concentrations of SA; L0, L200, L600 and L1000: particles freeze dried with different concentrations of SA) were analyzed in relation to microscopy, water activity (Aw), hygroscopicity, moisture, solubility, particle size, X-ray diffraction, thermogravimetry and accelerated oxidation. Particles of rounded shape and undefined form were obtained by spray and freeze-drying, besides ideal physicochemical properties for application (values from 0.091 to 0.365, 3.22 to 4.89%, 57 to 68% and 2.32 to 12.42 µm for Aw, moisture, solubility and particle size, respectively). All treatments protected the oil against oxidation, obtaining induction time of 5.31 h for oil and from 7.88 to 12.94 h for treatments. The better protection to oil was obtained with it emulsified and freeze-dried (L600); the encapsulation increased oxidative stability of the oil, besides facilitating its application over the fact the material is in powder form.

Profile and content of isoflavones on flaked and extruded soybeans and okara submitted to different drying methods.

Isoflavones (IFs) are biocompounds found in considerable amounts in soybean grains. However, to originate soybean-based materials, the grains must be subjected to numerous thermal and mechanical treatments, which can impair the IFs content. The influence of these treatments was investigated and a protocol for IFs extraction and quantification is proposed. Sequential extractions were performed on industrially pretreated soybean samples (broken, flakes, and collets), on okara submitted to different drying methods (freeze-drying, forced convection, and under vacuum), and on soybean oils extracted with hexane and ethanol. ß-glucosides levels were decreased by the thermal processes of lamination, expansion, and drying, while the aglycone forms were not affected. Lyophilization was identified as the most viable drying method for the quantification of IFs in okara. Soybean oils extracted with ethanol presented significant amounts of aglycone. Furthermore, two stages of extraction were sufficient for the recovery of the IFs from different matrices.

Encapsulation of Active Pharmaceutical Ingredients in Lipid Micro/Nanoparticles for Oral Administration by Spray-Cooling.

Nanoencapsulation via spray cooling (also known as spray chilling and spray congealing) has been used with the aim to improve the functionality, solubility, and protection of drugs; as well as to reduce hygroscopicity; to modify taste and odor to enable oral administration; and many times to achieve a controlled release profile. It is a relatively simple technology, it does not require the use of low-cost solvents (mostly associated to toxicological risk), and it can be applied for lipid raw materials as excipients of oral pharmaceutical formulations. The objective of this work was to revise and discuss the advances of spray cooling technology, with a greater emphasis on the development of lipid micro/nanoparticles to the load of active pharmaceutical ingredients for oral administration.

Production of a rich-carotenoid colorant from pumpkin peels using oil-in-water emulsion followed by spray drying.

Peels and seeds are byproducts generated during the processing of fruits and vegetables that have been cut off or rejected in the food industry. Pumpkin peels are an example of products that provide valuable nutritional aspects but that have low commercial value. This work aimed at recovering carotenoids from pumpkin peels to produce valuable powders. The pumpkin peel flour was obtained from convective drying and milling processes. Liquid-solid extraction produced the ethanol raw extract with a high carotenoid content. Carotenoid extract and Arabic gum suspensions were mixed in proportions of 1:2, 1:3, or 1:4 w/w. Emulsions produced via Ultra-Turrax (UT) and Ultra-Turrax plus high pressure (UTHP) were evaluated and spray dried. The particles carotenoid concentrations varied from 159.1 to 304.6 µg/g and from 104.3 to 346.2 µg/g for samples primarily produced via UT and UTHP, respectively. UTHP 1:3 particles showed the lowest degradation of carotenoids during 90 days of storage, with a retention index of 79%. The homogenization and spray drying techniques were proven to be suitable steps to preserve the carotenoids recovered from the byproduct studied. Microparticles can be used as a natural dye with potential use in food, pharmaceuticals, and cosmetics.

Reducing carotenoid loss during storage by co-encapsulation of pequi and buriti oils in oil-in-water emulsions followed by freeze-drying: Use of heated and unheated whey protein isolates as emulsifiers.

Buriti and pequi oils are rich in carotenoids and beneficial to human health; however, carotenoid oxidation during storage causes color loss in foods, making it difficult to use these oils in food products. This research aimed to encapsulate pequi oil and co-encapsulate pequi and buriti oils by emulsification using whey protein isolate (WPI) as an emulsifier in two forms, natural (unheated) and heated, followed by freeze-drying. The emulsions were studied by droplet size under different stress conditions, instability index, and rheology. The freeze-dried (FD) samples were studied after accelerated oxidation and the total carotenoid retention was determined; for the reconstituted FD, the zeta potential and droplet size were recorded after storage at 37 °C for 30 days. The emulsions were stable in all conditions, with average droplet sizes between 0.88 ± 0.03 and 2.33 ± 0.02 µm, and formulations with heated WPI presented the lowest instability index values. The FD's zeta potential values ranged from -50 ± 3 to -32 ± 3 mV. The co-encapsulated oils presented higher carotenoid retention (50 ± 1 and 48 ± 1%) than the free oils (31 ± 2%) after 30 days. The oxidative stability indexes were 51 ± 4 and 46 ± 3 for the co-encapsulated oils with unheated and heated WPI, respectively, and 20.5 ± 0.1 h for the free oils. FD formulations with 1:3 ratio of oil: aqueous phase and heated or unheated WPI showed the best carotenoid retention and oxidative stability, indicating that FD oil emulsions have potential as next-generation bioactive compound carriers.

Sugarcane Juice with Co-encapsulated Bifidobacterium animalis subsp. lactis BLC1 and Proanthocyanidin-Rich Cinnamon Extract.

Bioactive compounds are sensitive to many factors, and they can alter the sensory characteristics of foods. Microencapsulation could be a tool to provide protection and allow the addition of bioactives in new matrices, such as sugarcane juice. This study focused on producing and evaluating the potential function of probiotics and proanthocyanidin-rich cinnamon extract (PRCE), both in free and encapsulated forms when added to sugarcane juice. The pure sugarcane juice treatment T1 was compared with other sugarcane juices to which bioactive compounds had been added; T2, a non-encapsulated Bifidobacterium animalis subsp. lactis (BLC1); T3, a non-encapsulated BLC1 and PRCE; T4, BLC1 microcapsules; and T5, with BLC1 and PRCE microcapsules. The samples were morphologically, physicochemically, rheologically, and sensorially characterized. Samples were also evaluated regarding the viability of BLC1 during the juice's storage at 4 °C. It was possible to produce probiotic sugarcane juice with non-encapsulated BLC1, but not with the addition of free PRCE, which in its free form reduced the viability of this microorganism to < 1 log CFU/mL after 7 days. The microcapsules were effective to protect BLC1 during juice storage and to maintain high contents of phenolic and proanthocyanidin compounds, although the products containing these had their viscosity altered and were less accepted than either the control or those with non-encapsulated BLC1.

Improving stability of vitamin B12 (Cyanocobalamin) using microencapsulation by spray chilling technique.

Vitamin-B12 or cyanocobalamin is an essential micronutrient, so it must be supplied by diet. However, vitamin-B12 is found just in foods derived from animals and it is sensitive of many factors. Due to the unrelenting increase of people with deficiency in vitamin-B12 and easy degradation of this vitamin when subjected to adverse conditions, the aim of this research was to produce solid lipid microparticles (SLM) loaded with vitamin-B12 using the spray chilling technique. It was produced 6 SLM (with 0.1 and 1% vitamin and 0, 2.5 and 5% of lecithin) that were analyzed for optical and scanning electron microscopy, size and particles size distribution, water activity, instrumental color, X-ray diffraction, yield and encapsulation efficiency, release profile, besides free and encapsulated vitamin stability for 120 days. It was reported that the SLM presented a spherical shape and smooth surfaces, medium size values varying from 13.28 to 26.99 µm. The yield and encapsulation efficiency values within the range of 80.7 to 99.7% and from 76.7 to 101.1%, respectively. The encapsulation promoted better protection of vitamin-B12 (>91.1% for all formulations after 120 days of storage) when compared to the free one (75.2%). In addition, it was observed a good effect of the presence of soya lecithin in formulations; it promoted a more controlled release of vitamin-B12 in fluids and also shown better stability results. The spray chilling encapsulation technique proved to be a promising alternative, since it protected vitamin-B12 without the necessity of using high temperatures or organic solvents to encapsulate it, besides having a low cost.

Production and characterization of solid lipid microparticles loaded with guaraná (Paullinia cupana) seed extract.

Guaraná is a native fruit of the Amazon rainforest, which presents high levels of phenolic compounds. However, these bioactive compounds may be unstable in food processing and gastrointestinal conditions. Thus, this work aimed to characterize guaraná seed extract (GSE) followed by microencapsulation using a spray-chilling method and with vegetable fat as carrier, as well as to evaluate the particles. Phenolic-rich GSE was produced using 50% (w/w) hydroalcoholic solution and dehydrated by spray drying and lyophilization. Powdered GSE was characterized in relation to its inhibitory activity on digestive enzymes. Solid lipid microparticles (SLM) were evaluated for the retention of bioactive compounds and the release profile of phenolic compounds in simulated gastrointestinal conditions. Powdered GSE showed anti-obesity potential due to the high inhibitory activity of lipase. Regarding the retention of phenolic compounds, at least 75% were detected after 90 days at 25 °C in SLM. Moreover, SLM loaded with 7.5% GSE released approximately 99% of phenolic compounds in simulated gastrointestinal conditions. These results show the efficiency of spray chilling for protection and release of phenolic compounds from GSE, allowing future application in food.

Microencapsulation of lactase by W/O/W emulsion followed by complex coacervation: Effects of enzyme source, addition of potassium and core to shell ratio on encapsulation efficiency, stability and kinetics of release.

This study evaluated the technological viability of the formation of lactase microcapsules by coacervation (gelatin/gum arabic) containing potassium ions (cofactor). The impacts of the encapsulation and the cofactor on the enzyme properties obtained from Aspergillus oryzae and Kluyveromyces lactis were evaluated as a function of different pH values, temperatures, and storage times. The best microcapsules formed by coacervation showed good functional properties, such as low water activity (≤ 0.4) and particle size (≤ 93.52 µm), as well as high encapsulation efficiency (≥ 98.67%). The potassium ions were capable of reducing the flexibility of the polypeptide backbone, thereby increasing the stability of the enzyme. The microcapsules were also capable of increasing the stability of the enzyme under unfavorable pH values, high temperatures and during storage. An in vitro experiment showed that microcapsules were effective in the retention of about 90% of the enzyme in simulated gastric fluid, but as much as 95% of the enzyme can be released from the capsules in simulated intestinal fluid. The released enzyme retained 83% and 66% of the total enzymatic activity for the capsules produced with lactase from Kluyveromyces lactis and A. oryzae, respectively. These results are promising and demonstrated that these microcapsules are a promising technology to protect and deliver bioactive proteins during storage and delivery in the GI tract.

Immobilization of ß-galactosidase by complexation: Effect of interaction on the properties of the enzyme.

In the present work, we aimed to explore the molecular binding between alginate and ß-galactosidase, as well as the effect of this interaction on the activity retention, thermal stability, and kinetic properties of the enzyme. The impact of pH and enzyme/alginate ratio on physicochemical properties (turbidity, morphology, particle size distribution, ζ-potential, FTIR, and isothermal titration calorimetry) was also evaluated. The ratio of biopolymers and pH of the system directly affected the critical pH of complex formation; however, a low alginate concentration (0.1 wt%) could achieve an electrical charge equivalence at pH 3.4 with 93.72% of yield. The binding between ß-galactosidase and alginate was an equilibrium between enthalpic and entropic contributions, which promoted changes in the structure of the enzyme. Nevertheless, this conformational modification was reversible after the dissociation of the complex, which allowed the enzyme to regain its activity. These findings will likely broaden functional applications of enzyme immobilization.

Enhancing stability of echium seed oil and beta-sitosterol by their coencapsulation by complex coacervation using different combinations of wall materials and crosslinkers.

Intake of omega-3 fatty acids and phytosterols aids in the reduction of cholesterol and serum triglycerides. However, both fatty acids and phytosterols are susceptible to oxidation. This work coencapsulated echium oil (source of stearidonic and alpha-linolenic fatty acids) and beta-sitosterol (phytosterol) by complex coacervation using different combinations of wall materials, and sinapic acid (SA) and transglutaminase as crosslinkers. High encapsulation yields were obtained (29-93% for SA; 68-100% for the mixture of oil and phytosterols) and retention of 49-99% and 16% for encapsulated and free SA, at 30 days-storage. Treatment with gelatin-arabic gum and 0.075 g SA/g gelatin showed the best results: 0.07 mg MDA/g capsule, and retention of 96, 90 and 74% for alpha-linolenic, stearidonic acid and beta-sitosterol at 30 days of storage, respectively. Thus, coencapsulation of echium oil and phytosterol using SA as the crosslinker was possible, obtaining effective vehicles for protection and application of these compounds in foods.

Effect of microencapsulated Jabuticaba (Myrciaria cauliflora) extract on quality and storage stability of mortadella sausage.

The aim of the present study was to add microencapsulated Jabuticaba aqueous extract (MJE) to mortadella as a natural dye and to evaluate its possible antioxidant and antimicrobial activity during refrigeration. Anthocyanins in the extract were quantified and identified. Three treatments of mortadella were prepared: without dye (Control), with cochineal carmine (Carmine) and with the addition of 2% MJE. We determined the chemical composition of mortadella, along with pH, instrumental color, lipid oxidation, microbiological characteristics (Escherichia coli, Staphylococcus aureus, Salmonella, sulphite-reducing Clostridium, aerobic mesophiles, aerobic psychrotrophics and lactic acid bacteria) and sensory acceptance during storage at 4 °C for 56 days. MJE showed high content of anthocyanins, with prevalence of cyanidin-3-glucoside. MJE improved sensory acceptance of texture and flavor of mortadella (P < 0.05), but we observed a slight decrease in color and aroma attributes (P < 0.05). Lipid oxidation of mortadella was not influenced by MJE or cochineal carmine. MJE also displayed a minor effect on physicochemical and microbiological characteristics during storage. As MJE did not alter most of mortadella sausage's evaluated characteristics, it could be used as a natural dye in order to make better use of agro industry waste and to create a meat product enriched with natural antioxidants.

Improving oxidative stability of echium oil emulsions fabricated by Microfluidics: Effect of ionic gelation and phenolic compounds.

Echium oil is rich in omega-3 fatty acids, which are important because of their benefits to human health; it is, however, unstable. The objective of this work was the coencapsulation of echium oil and quercetin or sinapic acid by microfluidic and ionic gelation techniques. The treatments were analyzed utilizing optical and scanning electron microscopy, encapsulation yield, particle size, thermogravimetry, Fourier transform infrared spectroscopy, stability under stress conditions, and oil oxidative/phenolic compound stability for 30days at 40°C. High encapsulation yield values were obtained (91-97% and 77-90% for the phenolic compounds and oil) and the encapsulated oil was almost seven times more stable than the non-encapsulated oil (0.34 vs 2.42mgMDA/kg oil for encapsulated and non-encapsulated oil, respectively). Encapsulation was shown to promote oxidative stability, allowing new vehicles for the application of these compounds in food without the use of solvents and high temperature.

Development of functional yogurt containing free and encapsulated echium oil, phytosterol and sinapic acid.

The consumption of omega-3 fatty acids and phytosterol promotes the reduction of cholesterol and triacylglycerol levels. However, such compounds are susceptible to oxidation, which hampers their application. The objective of this work was to coencapsulate echium oil, phytosterols and sinapic acid (crosslinker/antioxidant), and incorporate the obtained microcapsules into yogurt. The microcapsules were evaluated for particle size, accelerated oxidation by Rancimat, and simulation of gastric/intestinal release. The yogurts were assessed for morphology, pH, titratable acidity, color, rheology and sensory analysis. The microcapsules (13-42µm) promoted protection against oil oxidation (induction time of 54.96h). The yogurt containing microcapsules, presented a pH range from 3.89 to 4.17 and titratable acidity range from 0.798 to 0.826%, with good sensorial acceptance. It was possible to apply the microcapsules in yogurt, without compromising the rheological properties and physicochemical stability of the product.

Evaluation of the release profile, stability and antioxidant activity of a proanthocyanidin-rich cinnamon (Cinnamomum zeylanicum) extract co-encapsulated with α-tocopherol by spray chilling.

Cinnamon has many health improving compounds such as proanthocyanidins, which also have potential for the prevention of damages caused by diabetes. Similarly, α-tocopherol is a natural antioxidant with important role on protection of fatty acids in membranes and lipoproteins. However, the addition of antioxidants in food may result in interaction with food matrix, low stability and unpleasant taste. In the present study, a proanthocyanidin-rich cinnamon extract (PRCE) (Cinnamomum zeylanicum) was co-encapsulated with α-tocopherol into solid lipid microparticles (SLMs) by spray chilling. The microparticles were characterized with regard to the physical and chemical properties, morphology, proanthocyanidin stability and release profile. SLMs were spherical with an average diameter of ca. 80µm. Proanthocyanidins were highly stable in SLMs stored for up to 90days at 5, 25 and 37°C. Moreover, SLMs gradually released proanthocyanidins in simulated gastrointestinal fluids by a diffusional process, following a Korsmeyer-Peppas kinetic. Analyses of the antioxidant compounds indicated that PRCE components exhibited a higher scavenging capacity against reactive oxygen species (ROS) and reactive nitrogen species (RNS). Thus, the SLMs produced in the present study have potential for application in the development of new functional foods and nutraceuticals, also providing an alternative for the controlled release of proanthocyanidins and α-tocopherol into the intestine.

Microcapsules loaded with the probiotic Lactobacillus paracasei BGP-1 produced by co-extrusion technology using alginate/shellac as wall material: Characterization and evaluation of drying processes.

Microcapsules containing Lactobacillus paracasei BGP-1 were produced by co-extrusion technology using alginate and alginate-shellac blend as wall materials. Sunflower oil and coconut fat were used as vehicles to incorporate BGP-1 into the microcapsules. The microcapsules were evaluated with regard the particle size, morphology, water activity and survival of probiotics after 60days of storage at room temperature. Fluidized bed and lyophilization were used to dry the microcapsules and the effect of these processes on probiotic viability was also evaluated. Next, dried microcapsules were exposed to simulated gastrointestinal fluids to verify the survival of BGP-1. Microcapsules dried by fluidized bed had spherical shape and robust structures, whereas lyophilized microcapsules had porous and fragile structures. Dried microcapsules presented a medium size of 0.71-0.86mm and aw ranging from 0.14 to 0.36, depending on the drying process. When comparing the effects of drying processes on BGP-1 viability, the fluidized bed was less aggressive than lyophilization. The alginate-shellac blend combined with coconut fat as core effectively protected the encapsulated probiotic under simulated gastrointestinal conditions. Thus, the production of microcapsules by co-extrusion followed by drying using the fluidized bed is a promising strategy for protection of probiotic cells.

Effect of different polysaccharides and crosslinkers on echium oil microcapsules.

Microencapsulation by complex coacervation using gelatin and arabic gum (AG) as wall materials and transglutaminase for crosslinking is commonly used. However, AG is only produced in a few countries and transglutaminase is expensive. This work aimed to evaluate the encapsulation of echium oil by complex coacervation using gelatin and cashew gum (CG) as wall materials and sinapic acid (S) as crosslinker. Treatments were analyzed in relation to morphology, particle size, circularity, accelerated oxidation and submitted to different stress conditions. Rounded microcapsules were obtained for treatments with AG (45.45µm) and microcapsules of undefined format were obtained for treatments with CG (22.06µm). The S incorporation for 12h improved the oil stability by three fold compared to oil encapsulated without crosslinkers. Treatments with CG and S were resistant to different stress conditions similar to treatments with AG and transglutaminase, making this an alternative for delivery/application of compounds in food products.

Development of solid lipid microparticles loaded with a proanthocyanidin-rich cinnamon extract (Cinnamomum zeylanicum): Potential for increasing antioxidant content in functional foods for diabetic population.

Cinnamon proanthocyanidins play an important role on the attenuation of complications associated to diabetes, but the daily ingestion of these compounds is not always satisfactory due to several aspects such as low stability and unpleasant taste. Thus, in the present study, a proanthocyanidin-rich cinnamon extract (Cinnamomum zeylanicum) was incorporated into solid lipid microparticles (SLMs) by spray chilling technique using vegetable fat as carrier. The microparticles were characterized with regard to their physical and chemical properties, morphology, proanthocyanidin stability and sensory properties. SLMs were spherical with a unimodal size distribution between 60 and 130µm, and proanthocyanidins were highly stable in SLM stored for up to 90days at 5, 25 and 37°C. Moreover, SLMs were able to mask the bitter taste and astringent sensation of proanthocyanidins and other polyphenols from cinnamon extract. Taken together, these results show the potential of SLM loaded with cinnamon proanthocyanidins for improving functional properties in new foods.

Protection of echium oil by microencapsulation with phenolic compounds.

The consumption of omega-3 enables the reduction of cardiovascular disease risk; however they are unstable. The aim of this work was to encapsulate echium oil (Echium plantagineum L.), a rich source of omega-3 fatty acids, with phenolic compounds (sinapic acid and rutin) by double emulsion followed by complex coacervation or by complex coacervation with sinapic acid in the capsule wall. Analyses of morphology, particle size, circularity, water activity, moisture, Fourier transform infrared spectroscopy, thermogravimetry, process yield, accelerated oxidation and identification and quantification of fatty acids present in the encapsulated oil were performed. Samples presented values of encapsulation process yield of phenolics and oil in the range of 39-80% and 73-99%, respectively. Moreover, all samples protected the oil against oxidation, obtaining induction time (accelerated oxidation) of 5h for pure oil and values in the range from 10 to 18h for samples. Thus, better protection to the oil was possible with sinapic acid applied in the capsule wall, which enhances its protection against lipid oxidation.

Microencapsulation of xylitol by double emulsion followed by complex coacervation.

The objective of this study was to produce and characterise xylitol microcapsules for use in foods, in order to prolong the sweetness and cooling effect provided by this ingredient. Complex coacervation was employed as the microencapsulation method. A preliminary double emulsion step was performed due to the hydrophilicity of xylitol. The microcapsules obtained were characterised in terms of particle size and morphology (optical, confocal and scanning electron microscopy), solubility, sorption isotherms, FTIR, encapsulation efficiency and release study. The microcapsules of xylitol showed desirable characteristics for use in foods, such as a particle size below 109 µm, low solubility and complete encapsulation of the core by the wall material. The encapsulation efficiency ranged from 31% to 71%, being higher in treatments with higher concentrations of polymers. Release of over 70% of the microencapsulated xylitol in artificial saliva occurred within 20 min.