Method for producing a nanoemulsion with encapsulated natural antioxidants for preserving fresh and

专利摘要:
The present invention relates to a method for producing a nanoemulsion comprising encapsulated natural antioxidants on a nanometre scale, disclosing the formulation of said product and the application thereof for the preservation of different natural food products or derivatives such as fresh or minimally processed fruit, vegetables and cereals and juices. The formulation comprises four main steps: a) the isolation of natural antioxidants from fruit, vegetable and cereal waste, b) encapsulation of the natural antioxidants, c) formation of the nanoemulsion with natural antioxidants, d) freeze-drying of the nanoemulsion formed. In this sense, the subject matter of the invention is the design of a method for producing nanoemulsions with a high antioxidant power from fruit and/or vegetable and/or cereal waste, efficiently encapsulated, and easy to process lacking organic chemical additives in the end product, which help to preserve and/or enhance the nutritional and organoleptic properties of fresh and minimally processed products, for humans and animals, with food or neutraceutical grade. The key aspect of the invention is a thin, nanometre-size layer on the food, which prevents gas and fluid exchange with the environment, enhanced with selected antioxidants, the role of which is similar to an enzyme that slows down or inhibits the biochemical decomposition and oxidation reactions of the food. This provides fresh and minimally processed foods with a longer shelf life and means that the organoleptic quality of foods to be frozen improves upon thawing.
公开号:ES2764899A2
申请号:ES202090007
申请日:2017-08-23
公开日:2020-06-04
发明作者:Ramos Miguel Enrique Jesús Malnati；Du-Pont Melissa Ximena Adriazola；Morales Daniel Ali Oviedo
申请人:Malnati Ramos Miguel Enrique Jesus；
IPC主号:

专利说明:

[0002] PROCESS TO OBTAIN A NANOEMULSION WITH ENCAPSULATED NATURAL ANTIOXIDANTS FOR THE CONSERVATION OF FRESH AND MINIMALLY PROCESSED FOODS, AND THE NANOEMULSION SO OBTAINED
[0004] TECHNICAL FIELD
[0006] The present invention corresponds to methods of optimal extraction and encapsulation within a nanoemulsified matrix, especially applicable to the preservation of fruits, vegetables, fresh cereals, juices and minimally processed foods directed at humans or animals; it further comprises optimized formulation and encapsulation.
[0008] This invention is comprised in the technical field of nanotechnology and food industries, bioindustry, biotechnology and agroindustrial derivatives.
[0010] STATE OF THE ART
[0012] Edible coatings are dispersed emulsions consisting of homogenization of non-miscible substances, which can be categorized into three different types, a) oil: water (O / W) b) water: oil (W / O) c) multi-emulsion (W / O / W or O / W / O), which each depends on the element to be dispersed on the majority matrix. These are commonly used to preserve the shelf life of foods, through polysaccharides with microbial power such as chitosan, which conserves the shelf life of fruits and vegetables in post-harvest, or other foods such as eggs, legumes or even cereals, by increasing the antimicrobial capacity of these fresh products.
[0014] Currently, the research, development and innovation of edible films in the field of the preservation of foods such as fruits and vegetables is being developed increasingly due to the climate change that afflicts all countries in the world and the imminent deterioration that food presents in general due to exposure to environmental conditions. In addition, the desire of logistics and agro-industrial companies to conserve with methods that use less and less energy, compared to current techniques such as freezing and conservation with a controlled atmosphere, encourages this type of product. Fortunately, technology evolved and edible coatings became They developed at a smaller particle level, at the micrometer scale, which allowed better application on the food surface and greater thermodynamic stability over time, compared to normal droplet size emulsions. However, the use of chemical surfactants to achieve spontaneous formation of these microemulsions became a problem, since the products became toxic. For this reason, the nanotechnology of emulsions was effectively developed, which led to providing them with kinetic stability, thanks to homogenization processes at high speeds and pressures, thereby reducing the use of surfactants to a minimum.
[0016] Thus, nanoemulsions are stable compositions, molecularly composed mainly of a water-oil mixture, so that the internal particles are in a nanometric range between 20 - 500nm. These nanometric mixtures are characterized and considered the best means to facilitate the transport, release and absorption of functional active agents such as antioxidants, antimicrobials or even nutraceuticals (Cardoso & Jiménez, 2015); They also exhibit low sensory perception, which is why they have various uses in sectors such as pharmaceuticals, cosmetics, medicine or even food. However, the world trend was directed towards the use of natural or organic products that suppose to be free of inputs harmful to health, or an approach related to superfoods, which influenced the development of products with active agents extracted from natural compounds, thus the trend made that edible coatings intended for food were enriched with essential oils of aromatic vegetables such as oregano, rosemary, cinnamon and other antioxidants, which contain phenolic compounds that give these additional characteristics competent to the preservation of foods with additional nutritional properties , required by the market.
[0018] The functional active agents extracted in industrial processes can be polyphenols, terpenes, glycosics or alkaloids, this depends on the raw material used. For example, polyphenols are abundant in fruits, in the form of phenolic compounds; while terpenes in the essential oil of aromatic herbs. Flavonoids are phenolic compounds characterized by representing an important source of antioxidants that help reduce the oxidative stress of lipids, proteins and nucleic acids due to the surrounding oxygen in the environment (Cerón, Higuita & Cardona, 2010). However, scientific advances in food biotechnology contributed to the reuse of various active agents, such as flavonoids, present in residues with great antioxidant potential, which are found in the shells and seeds of various fruits. Therefore, countries with Great biodiversity, like Peru, must take advantage of the agro-industrial remnants to transform them and produce additives made from antioxidants that can make various food products functional, that is, that nourishes and prevents diseases, in a way that is commercially viable, and sustainable with the environment. ambient. In addition, natural phenolic compounds are increasingly accepted by industries, and global institutions such as the FAO (Food and Agriculture Organization of the United Nations) that requires safe food, free of bacterial contamination and toxicity caused by commonly used synthetic additives. in the food industry (Conte et al, 2007); However, phenolic compounds present the technical problem of volatility and sensitivity due to their chemical composition, which represented a problem to be able to conserve them effectively. Furthermore, the use of inorganic chemical inputs for the extraction and concentration stages damages the edible condition of the product. In this way, technologies such as nanofiltration of compounds and encapsulation were developed to conserve active compounds, at different particle sizes of volatile compounds, such as antioxidants or other products such as omegas, vitamins, proteins and others, which contribute to maintaining and / or improve the nutritional and organoleptic characteristics over time of minimally processed foods.
[0020] In the state of the art there are invention patents related to the production of nanoemulsions aimed at food preservation in general, which use extensive and inaccurate homogenization processes at high speeds and pressures, or by mechanical fragmentation with the use of chemical surfactants, whereby fine-grain water-oil emulsions below 100 nanometers (nm) are obtained; Also patent applications such as EP728460 or EP1016453 use surfactants or chemical polyols to stabilize the emulsion and obtain the desired particle size. Patent US20140205722A1 mentions the composition of a complex solid lipid nanoparticle that preserves fruits, vegetables, seeds and / or cereals for long periods of time from a lipid base consisting of waxes, and additional inputs such as proteins, antioxidants and materials film formers. There are also patents such as KR20140115427 and KR20160005182A that propose nanoemulsions, which do not mention the efficient extraction processes of their active compounds, and present inaccurate processes that compete with antioxidant solutions of curcumin and cinnamon oil due to their antimicrobial functional principle, they are obtained from through a mixture between emulsifier and water, followed by a mixture with the oil and the agent antimicrobial, to finally mix both products by high pressures. Finally, patent CN104997129 proposes extensive processes of a food additive using vegetable compounds, for this the input with the active compound (Larix tree) is pulverized and extracted by ultrasound using ethanol as a chemical solvent at 60-70 ° C for 30-50 minutes, then it is concentrated with chemical additives such as sulfuric acid to finally centrifuge and crystallize.
[0022] Regarding the extraction of antioxidant compounds, methods with organic solvents or hydrothermal treatments with recirculation are used. The patent W02004009206A1 is a phenolic compound extraction procedure that uses reactors at temperatures between 180 ° -240 ° C for times up to 30 minutes in reaction and then let cool for hours and remove the filtered liquid fraction, which does not preserve the antioxidant characteristics given the temperatures used, it is neither efficient. Patent ES2198286T3 is a new process to obtain natural antioxidants that consists of extraction with organic solvents at temperatures up to 100 ° C with rapid cooling, evaporation of the organic solvent, distillation of the solution and drying in a fluidized bed, this means too many extensive processes and the use of chemicals to make the final product.
[0024] Patent US2016262438 mentions a phenol extraction method, which is based on the concentration of antioxidant juice up to a Brix degree of 25 °, to then undergo adsorption processes with resins and ethanol as solvent, finally concentrated on rotavapor to spray With the Spray Dryer method, this demands extensive, complex processes that demand high costs for prolonged processes. Lastly, patent CN104305468 is an extensive method that uses chemicals for the preparation of sesame antioxidant, which consists of drying the seeds, carrying out a "degreasing" process with n-hexane and extraction with high concentration ethanol by a span of 1 day, to finally concentrate on rotavapor In the state of the art, the use of nanofiltration technology aimed at the concentration and purification of antioxidant solutions has not been recorded, patent ES2294696T3 shows a method that includes several stages of nanofiltration of albumin solutions to achieve the desired purity and concentration.
[0026] Regarding the encapsulation techniques of active compounds, they are used in very diverse fields, from pharmaceuticals to agrochemistry. The techniques used are competent to the use of polymeric materials to wrap involved active agents, followed by techniques to obtain increasingly smaller particle size capsules, resulting from spray drying processes, supercritical fluid or, in exceptional cases, solvent freeze-drying processes. Patent ES2213572T3 is a complex, but industrially viable procedure for microencapsulating water-soluble substances, which involves mixing the substance with biodegradable polymers and a chemical solvent to homogenize the sample under ideal conditions for the formation of the microparticle, which solidifies through the removal of this solvent. The patent ES2268073T3 is a procedure for microencapsulating agricultural active agents, for which they mix chemical materials with a high melting point and another with a normal melting point, which are heated to become liquid and through interfacial polymerization processes become a solid state microcapsule This assumes that the microencapsulated antioxidant may deteriorate due to excess heat exposure.
[0028] For its part, the following non-patent document has been identified, which we also cite as antecedent: Memories of the XXXIV National Meeting and III International Congress of AMIDIQ. Mazatlán, Sinaloa, Mexico. May 7-10, 2013. M. G. Michel Barba, et al. Effect of microfluidization processing parameters on the physicochemical properties of nanoemulsions (gum arabic - linseed oil). pages: 2738 - 2743. ISBN: 978-607-95593-1-1. This publication describes a method for making a microemulsion from linseed oil and gum arabic. A colloidal dispersion is formed from dissolved and filtered gum arabic. The emulsion sample is prepared with 3% w / w dispersed phase in gum arabic: linseed oil equal to 2: 1. Thus a coarse emulsion is formed where linseed oil is added dropwise to the colloidal dispersion of gum arabic, using a high cut disperser, at 5000 RPM for 10 minutes at a temperature of 20 ° C. This thick emulsion was then homogenized in a microfluidizer, in triplicate. Deionized water was used for all the work. However, this process differs in terms of the temperature, time and rpm parameters used during the process.
[0030] Therefore, it is necessary to have a process to obtain nanoemulsions with a high antioxidant power from residues of fruits and / or vegetables and / or cereals, efficiently encapsulated, and easy to process without organic chemical additives in the final product, which contribute to preserving and / or improve nutritional characteristics and organoleptic in fresh and minimally processed foods, aimed at humans and animals, with food grade.
[0032] BRIEF DESCRIPTION OF THE INVENTION
[0034] More and more products are required that contribute to the preservation of food and other natural products, which do not include elements, substances, synthetic or artificial derivatives and which in turn have nutraceutical properties, are easy to obtain and friendly to the environment. , reducing the environmental impact of the industry that uses plant inputs, such as fruits, vegetables and cereals and discards organic material remains.
[0036] A solution to the described problem is proposed in the present patent application.
[0038] The invention comprises a method for obtaining a preservative suspension, hereinafter nanoemulsion, which contains encapsulated active agents on a nanometric scale; The formulation of said product and its application for the conservation of different products or natural food derivatives such as fresh or minimally processed fruits, vegetables and cereals and juices are disclosed.
[0040] In this sense, the object of the invention is the elaboration of a method to obtain nanoemulsions with a high antioxidant power from residues of fruits and / or vegetables and / or cereals, efficiently encapsulated, and easy to process without organic or grade chemical additives. in the final product, which contribute to preserving and / or improving the nutritional and organoleptic characteristics in fresh or minimally processed products, aimed at humans and animals, with food and nutraceutical grade.
[0042] The core aspect of the invention consists of a layer of fine nanometric dimensions on the food, which prevents the gas and fluid exchange with the environment, enhanced with selected antioxidants, whose function is similar to an enzyme that delays or inhibits biochemical reactions decomposition and oxidation of food. This allows fresh and minimally processed foods to have a longer shelf life and foods that are intended for freezing to improve their organoleptic quality when thawed.
[0043] DETAILED DESCRIPTION OF THE INVENTION
[0045] As a solution to the aforementioned technical problem, the present invention was developed, which proposes a novel formulation of a dispersed system such as a nanoemulsion powered with edible natural antioxidants extracted from fruit and / or vegetable and / or cereal residues, the encapsulation and cryodesiccation processes of the nanoemulsion, and this finished product that ensures stability, prolonged and effective action over time on fresh and minimally processed foods that have been protected with this product, such as fruits, vegetables and cereals.
[0047] The object of the invention is the process for obtaining a nanoemulsion with natural antioxidants, which comprise the following steps a) efficient obtaining of natural antioxidants, b) encapsulation of natural antioxidants, c) formation of the nanoemulsion with natural antioxidants, d) cryodesiccation of the nanoemulsion formed.
[0049] The efficient obtaining of natural antioxidants from residues of fruits, vegetables and cereals, comprises the following processes:
[0050] - Selection, washing and disinfecting of the peels and seeds of the residues of the selected fruits, vegetables or cereals.
[0051] - Dehydration of the disinfected raw material, which can be carried out in a conventional oven at 30-60 ° C for about 2-6 hours with hot air at reflux, or by lyophilization at temperatures between -30 to -50 ° C and a pressure absolute vacuum of at least 0.04 mbar, for 10-15 hours, depending on the sensitivity of the antioxidant component of the fruit, vegetable or cereal.
[0052] - Extraction with polar solvents, such as ultra pure water, of the dehydrated residues with active potential obtained in the previous stage, with a degree of humidity between 2-20%, which can be carried out by means of assisted extraction with microwave waves at a power of between 100 - 400 W for 5-40 minutes, or ultrasound with a vibration power between 20 - 60 kHz, for 10 - 40 minutes, at a temperature between 30 -60 ° C, depending on the sensitivity of the antioxidant component of the fruit, vegetable or cereal.
[0053] - Partial concentration of the antioxidant extract with the simple distillation method in a rotary evaporator under vacuum between 0.5 - 15 inHg at 20-60 ° C for 10-95 minutes until achieving a concentration between 10-50%.
[0054] - Tangential nanofiltration of the concentrated antioxidant solution at a pH between 6 -10.5, in two sequential filters with nanopores between 10 - 100 nm and a minimum surface area of 0.01 m2, at the same temperature as the previous process, through which the solution pumped at pressures between 0.5 - 1 bar.
[0056] For its part, the encapsulation of natural antioxidants includes the following processes:
[0057] - Mixed at a speed between 500-2000 RPM, at a temperature between 20 - 60 ° C for 1-3 hours of concentrated antioxidant extracts in a 1: 1 ratio mixture with polysaccharides such as maltodextrin and gum arabic, or a direct ratio of modified corn or cassava starch, in an amount that replaces the percentage of soluble solids measured with refractometry techniques, of the selected antioxidant solution.
[0058] - Homogenized at a speed between 8000 - 15000 RPM for about 1 -15 minutes to encapsulate the active compounds with the biopolymers and thus protect them from damage by submission to the environment, from the formation of a microemulsion with a material wall that will make such protection. The resulting antioxidant microemulsion is temporarily stored under refrigeration at a temperature of 5-15 ° C.
[0060] The formation of the nanoemulsion with natural antioxidants, comprises the following steps:
[0061] - Dilution of alginic acid in drinking water, at a temperature between 50-70 ° C, with constant movement for 1-3 hours at 500-1500 RPM.
[0062] - Homogenization at a speed of 8000 - 15000 RPM for about 1-15 minutes of the alginic acid in solution with the rest of the components: oleaginous matrix, polysorbate, glycerol and the antioxidant microemulsion.
[0063] - Microfluidization at high pressures of 100 - 200 MPa for 3-5 cycles, with which the fluid nanoemulsion was obtained, boosted with natural antioxidants from residues of fruits and / or vegetables and / or cereals.
[0065] Finally, the cryodesiccation of the nanoemulsion obtained in the preceding stage comprises the concentration of the nanoemulsion by cryodesiccation methods such as the lyophilization process subjected to vacuum pressures of at least 0.04 mbar and temperatures between -10 to -50 ° C. , which give it a powdery, low-volume appearance.
[0066] An advantage of the present invention is that the concentration is reduced to less than 2 hours and without using inorganic chemical solvents, in order to increase the naturalness of the product, the food grade and the efficiency of the process by 20-40 %.
[0068] Another advantage of the invention is that it is not composed of proteins of any kind and the oil matrix that is used is a combination of saturated and monounsaturated fatty acids that have molecular stability due to the reduced number of double bonds in their molecules, such as oil. coconut, canola, almonds, avocado or peanuts that provide the desired permeability and oxidative stability to the nanoemulsion, in addition to oleic acid that provides a functional characteristic to the final product.
[0070] Another advantage of the invention is that the refractometry method used in the encapsulation contributes to reducing the lyophilisate time by 20-30%.
[0072] Another advantage of the invention is that the final product that corresponds to a concentrated nanoemulsion in powder, which decreases its volume by more than 100% compared to the fluid nanoemulsion, contributes to improving the logistical processes of the product, also the product when rehydrated will maintain all its properties and particle size. Finally, an advantage of the product applied over minimally processed foods such as fruits, vegetables and cereals, is that the storage conditions will be superior, avoiding long freezing chains and a controlled atmosphere, since the colloidal suspension cover will preserve the food. under refrigeration conditions, given the permeable principle and its enrichment with active agents from the residues of fruits, vegetables or cereals.
[0074] An objective of the invention is to obtain antioxidants of high phenolic concentration, from residues of various fruits, vegetables or cereals, characterized by being a formula rich in antioxidant functional active compounds.
[0076] Another object of the invention is to obtain a composition comprising:
[0077] a) 0.5 - 10% Alginic Acid, preferably sodium or potassium alginate from natural sources, food grade
[0078] b) 0.1 - 10% Oil matrix with saturated and / or monounsaturated fatty acids as major compounds
[0079] c) 0.1 - 1% Polysorbates, preferably polyoxyethylene sorbitan monolaurate or food grade polyoxyethylene sorbitan monosterate
[0080] d) 0.5 - 10% Glycerol, preferably rosin glycerol esters from natural plant sources, food grade
[0081] e) 0.2 - 40% Antioxidant Microemulsion
[0083] An alternative to the invention is a formulation intended to maintain the shelf life of cut fruits under refrigerated conditions. The solution is composed of the presented formulation, replacing glycerol and polysorbate with an amount of 1-5% of calcium ascorbate or a 1: 1 combination of ascorbic acid and citric acid.
[0085] Another alternative of the invention involves a microemulsified matrix, no longer on a nanometric scale, that contains correctly encapsulated antioxidants, and has the same field of action aimed at food preservation, since it involves the entire procedure described, except for the microfluidization process, which is responsible for taking the emulsion to a nanometric scale.
[0087] Another alternative of the invention, directed as an input for use in organic agriculture, consists of a formulation that lacks polysorbate, since according to the Equivalence Programs of different regulatory entities in the world, the chemical parameters evaluated are primarily trace amounts of quaternary ammonium according to ISO 17025.
[0089] Another alternative of the invention, directed as an input to preserve the quality of natural fruit juices, also excludes the use of polysorbates in its formulation, since it generates an undesirable increase in the viscosity of the final product by up to 50%.
[0091] The invention represents an improvement in the state of the art, since a simple method with a unique composition that improves production efficiency, with a higher percentage of antioxidant and functional nanoemulsion, in addition to maintaining naturalness and food grade, is proposed, through techniques that do not use organic chemical additives such as ethanol, methanol or hexane, nor temperatures above 60 ° C for the extraction, concentration and encapsulation processes, which helps to keep the polyphenols present in antioxidants intact natural extracted from residues of fruits, vegetables and cereals.
[0092] The invention also supposes, an effective method to efficiently encapsulate active compounds such as proteins, fatty acids, vitamins and minerals, which have been correctly extracted from fruits, vegetables or cereals and are desired to be preserved over time, using emulsions that efficiently encapsulate the agent. active.
[0094] BRIEF DESCRIPTION OF THE FIGURES
[0096] Figure 1. Flow diagram of the process of the invention in which its four main stages are detailed.
[0098] EXAMPLE OF PREFERRED EMBODIMENT OF THE INVENTION
[0100] A. Procedure for obtaining the nanoemulsion with encapsulated natural antioxidants
[0102] An nanoemulsion preparation of the invention, by way of example, involves the selection, washing and disinfection of the peel and peel of the mango fruit Mangifera indica L. with 100 ppm of sodium hypochlorite diluted in ozonated water; it is then dehydrated with a tray freeze dryer at an approximate temperature of -40 ° C and an absolute vacuum pressure of at least 0.04 mbar, for 12 hours. Once the dehydration is complete, the degree of humidity of the raw material is measured and it is extracted with polar solvents by means of assisted extraction with microwave waves at a power that oscillates 200 W for 20 minutes; the antioxidant extract is then partially concentrated with the simple distillation method in a rotary evaporator under vacuum between 0.5 - 15 inHg at 40 ° C for 60 minutes until achieving a concentration of at least 15%, to pass through tangential nanofiltration of the concentrated antioxidant solution in two sequential filters with 50 nm nanopores and a minimum surface area of 0.01 m2, at the same temperature as the previous process, through which the pumped solution passes at pressures between 0.5 bar. In a separate process, the antioxidant extracts concentrated are mixed at a speed of 500 RPM, at 25 ° C for 2 hours, in a mixture in direct proportion to the percentage of brix degrees of the concentrate, of modified corn starch; homogenized in an industrial mixer at a speed of 12000 RPM for about 5 minutes to encapsulate the active compounds, the resulting antioxidant microemulsion is temporarily stored in refrigeration at a temperature of 5-15 ° C.
[0103] Alginic acid is diluted in ozonated water at 50 ° C, with constant movement for 1 hour and homogenized with the rest of the inputs: oil matrix, polysorbate, glycerol and the antioxidant microemulsion. Then, the microfluidization process is carried out at high pressures of 100 MPa for 3 cycles, with which the fluid nanoemulsion was obtained, boosted with natural antioxidants from fruit and / or vegetable residues. Finally, the nanoemulsion obtained in the previous stage was cryo-dried at vacuum pressures of at least 0.04 mbar and temperatures of -40 ° C, which give it a fine grain size solid appearance.
[0105] B. Application of the nanoemulsion with encapsulated natural antioxidants on selected foods
[0107] The fruits and vegetables that were the object of the experimentation (mango, avocado, tangerine, strawberry and asparagus) were selected considering characteristics of optimum quality, that is to say, of uniform sizes, shapes, colors and absent from mechanical or phytosanitary damage after harvest, maturity in the state of Pinton. , washed and disinfected with 100 ppm of sodium hypochlorite; then the fluid nanoemulsion was applied in the form of a spray for 5 minutes and a drying-draining of another 5 minutes was carried out, at room temperature of 25 ± 2 ° C on harmless grids; The food was immediately packed in containers recommended by the CODEX Alimentarium. After finishing the application protocol of the nanoemulsion of the invention, accelerated tests - controlled in triplicate, were carried out every 7 and 14 days under a temperature of 25 ± 2 ° C and relative humidity of 80 - 90%, with the exception of the strawberry and asparagus that was refrigerated at 10 ± 2 ° C, all tests at the same concentration of the product. The samples were experimental batches of 1 Kg of Mangifera indica L. mango, Persea americana avocado , Citrus reticulata mandarin, Fragaria vesca L. strawberry and Asparagus officinalis asparagus . The variables measured were weight differential, brix degree differential and hedonic scale, from a Sensory Evaluation test, where it was evaluated on a scale of 1 to 5, with 5 being the scale of best acceptance according to the taste of the product, before a panel of previously trained tasters of 15 people. The results show that the experimental samples coated with the invention show a remarkable improvement with respect to the control samples without any treatment, since these at 8-12 days, depending on the fruit, were in a state of putrefaction. It should be noted that the tests were carried out at extreme temperatures, thus, samples at refrigeration temperatures between 5 - 10 ° C increase their quality by at least 50%, which is beneficial for the sector. agroindustrial, which manages even freezing temperatures and even controlled atmospheres to maintain the quality of the food product.
[0108] Day zero
[0112] Day 7
[0116] Day 14
[0122] Biochemical food degradation, largely caused by oxidative processes, is the main non-microbial factor, where formed free radicals initiate spoilage reactions that act mainly on lipids and proteins (Barefoot, Rizzo, Rossetti, Negri, Paéz , Costabel and Taverna, 2010), which can be countered with the invention that contains correctly encapsulated antioxidants.
[0124] For this reason, the experimental results obtained for the asparagus can be extrapolated to cereals, since the asparagus, representative of the vegetables, has similar proportions in terms of essential amino acids, which reflects the protein similarity between both classes of food. .
[0126] Table: Amino Acid Content in Representative Cereals and Asparagus
[0130] 1Source: FAO (2013), Dietary protein quality evaluation in human nutrition 2Source: Alimentos.org.es (s / n), Amino acids from Asparagus
[0131] 3 Source: Ayala, G. (2014), Contribution of Andean crops to human nutrition
[0133] On the other hand, samples of minimally processed foods and juices were evaluated in experimental batches in triplicate of 500 g of peeled and cut Malus Communis apple, and 500 mL of Musa paradisiaca banana juice with a minimum of 15-20% fruit, under conditions controlled 20 ± 2 ° C and relative humidity 70%. It was measured using the hedonic scale, based on a Sensory Evaluation test, where it was evaluated on a scale of 1 to 5, with 5 being the scale of best acceptance, sensory criteria such as taste, smell and sight, before a panel of tasters previously trained 15 people, and pH to analyze the degree of acidity that the fruit is taking. The experimental samples show a considerable improvement with respect to the control samples without any treatment and the pH ranges remain within the standard of the fruit.
[0134] Day zero
[0136]
[0139] Day 5
[0147] C. Quality Parameters of Nanoemulsion with encapsulated natural antioxidants
[0149] Encapsulation efficiency
[0150] This is measured as a percentage, it was performed through a relationship between the output and input of the efficient encapsulation process, taking an average of the tests performed with a standard deviation that shows the uncertainty of the repetitions in each run. It was considered to evaluate the best results obtained from the present invention, with respect to the best result stated in patent KR20160005182A.
[0152] Encapsulation efficiency comparison table (%)
[0157] The results show that patent KR20160005182A at a concentration of 1.6% cinnamon oil, an encapsulation efficiency of 77.87% was obtained, while with the invention patent filed, the antioxidant at a concentration of 1.5% had a yield of 81.32%.
[0159] Acute toxicity
[0160] It is the ability of a substance to be lethal in low doses in humans (SINIA, 2017). The nanoemulsion mentioned in the invention was subjected to the oral LD50 ingestion toxicity test according to the OECD test 423, which consisted of a single dose to laboratory rats administering 2000 mg / kg of body weight, being observed for 14 days, lapse time that did not induce toxic damage and had an LD50 greater than 2000 mg / kg of body weight, so the final product can be considered not classifiable as toxic or low intrinsic toxicity.
[0162] Measurement of nanoemulsion particle size
[0163] It was measured on a Mastersizer laser analyzer (<100nm to> 2mm). The colloidal sample is placed in the optical bank of the measuring instrument, where a light beam illuminates the particles and the measurement is generated from various angles, scattering light throughout the sample. The invention has an average particle size between 90-100 nm, at the 90th percentile.
[0165] Measurement of the zeta potential (mV)
[0166] The nanoemulsion is a measure of the electrical potential on the interfacial surface of the suspensions, this is measured in electrophoretic cells with two electrodes connected to an energy source (Kosegarten & Jiménez, 2012), it is associated with the pH value, since this associates the charge of the particles. A zetameter was used as the nanoemulsion measurement instrument in the invention, which yielded a value between -20 mV to -40 mV, depending on the concentrations of the inputs, and the pH was around 6.5 to 10, which shows a Adequate stability within the allowed range <-30mV. The KR20160005182A patent has zeta potentials of around 0.5 to almost 6 mV, which can sense a high degree of dissociation.
[0168] Sanitary microbiological analysis
[0169] Of the nanoemulsions applied in minimally processed foods, it was carried out considering the growth of microorganisms such as aerobic mesophiles over time, under temperature conditions between 15-30 ° C. Colony count to 30 ° C using the surface seeding technique resulted in 14 days, in mangoes, avocados, mandarins (shelf at 30 ° C); and 10 days in strawberries and camu - camu (shelf at 15 ° C), favorable treatments that were in a ratio between 450 - 600 CFU / g of total aerobes. This indicator shows an improvement between 200 and 250% compared to the same fruits compared to the white that does not have any coating.
[0171] Sensory analysis
[0172] It is an experimental method that analyzes the organoleptic characteristics of a product, from a panel of judges who perceive and qualify according to their criteria. The analysis of fresh mangoes coated with the nanoemulsion enriched with antioxidant residues of the mango was carried out in triplicate and with a panel composed of 15 trained judges. The results of the aforementioned test had an average score from 1 to 5, of 5.0 points, which shows a slight improvement in the taste of the product since the mango without application (control) obtained a rating of 4.8, due to the fruity aroma is enhanced. The results become more interesting when, after 14 days, the mango with the coating presents an average score of 3.9 points, while the sample controls a score of 0.0 due to its level of decomposition.

权利要求:
Claims (16)
[1]
1. A process to obtain a nanoemulsion formulation with encapsulated natural antioxidants for the preservation of fruits, vegetables and minimally processed foods, characterized in that it comprises the following stages:
to. extraction of natural antioxidants from residues of fruits, vegetables or cereals; where the extraction is carried out with pure water with a partial concentration of the antioxidant extract with the vacuum distillation method between 0.5 - 15 inHg at 20-60 ° C for 10 - 95 minutes until achieving a concentration between 10-50% and with subsequent tangential nanofiltration of the solution;
b. encapsulation of natural antioxidants;
c. formation of the nanoemulsion with natural antioxidants; and
d. cryodesiccation of the nanoemulsion formed.
[2]
2. The process for obtaining a nanoemulsion formulation with encapsulated natural antioxidants for the preservation of fruits, vegetables and minimally processed foods according to claim 1, characterized in that the extraction of natural antioxidants comprises the following steps:
to. sorting, washing and disinfecting peels and / or seeds of selected fruit, vegetable or cereal residues;
b. dehydration of the obtained in the previous stage in a conventional oven at a temperature of 30 - 60 ° C for 2 - 6 hours with hot air at reflux, or by lyophilization at a temperature of -30 - -50 ° C and a pressure of absolute vacuum of 0.04 mbar for 10 - 15 hours, up to a humidity of 2 - 40%;
c. extraction with pure water, of what was obtained in the previous stage, assisted by microwaves at a power of 100 - 400 W for 5 - 40 minutes, or ultrasound with a power of vibration of 20 - 60 kHz, for 10 - 40 minutes at a temperature 30-60 ° C;
d. partial concentration of the antioxidant extract with the simple distillation method in a rotavapor under vacuum between 0.5 - 15 inHg at 20-60 ° C for 10-95 minutes until achieving a concentration between 10-50%;
and. Tangential nanofiltration of the solution from the previous step, at a pH of 6 - 10.5, in two sequential filters with nanopores of 10 - 100 nm and a minimum surface area of 0.01 m2, at a temperature of 30 - 60 ° C, the solution is pumped at a pressure of 0.5 - 1 bar.
[3]
3. The process to obtain a nanoemulsion formulation with encapsulated natural antioxidants for the preservation of fruits, vegetables and minimally processed foods according to claim 1, characterized in that the encapsulation of the natural antioxidants comprises the following steps:
to. What is obtained in the extraction of the natural antioxidant is mixed in a 1: 1 ratio with polysaccharides such as maltodextrin and gum arabic, or a direct proportion of cornstarch or cassava, in an amount that replaces the percentage of soluble solids measured with refractometry techniques. , of the selected antioxidant solution; mixing is carried out at a speed of 500-2000 RPM, at a temperature between 20-60 ° C for 1-3 hours; and
b. homogenized at 8000 - 1500 RPM for 1-15 minutes, to obtain the encapsulation, which is temporarily stored at a temperature of 5 - 15 ° C.
[4]
4. The process for obtaining a nanoemulsion formulation with encapsulated natural antioxidants for the preservation of fruits, vegetables and minimally processed foods, according to claim 1, characterized in that the formation of the nanoemulsion with natural antioxidants comprises the following stages:
to. dilution of alginic acid in drinking water, at a temperature of 50 - 70 ° C, with constant movement of 500 - 1500 RPM, for 1 - 3 hours;
b. homogenization at a speed of 8000-15000 RPM, for 1-15 minutes of the alginic acid in a solution with the oleaginous matrix, polysorbate, glycerol and the antioxidant microemulsion; and
c. microfluidization at high pressures of 100-200 MPa, for 3-5 cycles.
[5]
5. The process for obtaining a nanoemulsion formulation with encapsulated natural antioxidants for the preservation of fruits, vegetables and minimally processed foods according to claim 1, where the cryodesiccation of the nanoemulsion obtained comprises the concentration of the nanoemulsion by cryodesiccation methods.
[6]
6. The process to obtain a nanoemulsion formulation with encapsulated natural antioxidants for the preservation of fruits, vegetables and minimally processed foods according to claim 5, where cryodesiccation is carried out by lyophilization, with a vacuum pressure of 0.04 mbar and a temperature of -10 to -50 ° C.
[7]
7. The process to obtain a nanoemulsion formulation with encapsulated natural antioxidants for the preservation of fruits, vegetables and minimally processed foods according to claim 1, characterized in that the encapsulated natural antioxidants come from residues of fruits, vegetables and / or cereals in different combinations, where the formulation obtained is a functional formula.
[8]
8. The process to obtain a nanoemulsion formulation with encapsulated natural antioxidants for the preservation of fruits, vegetables and minimally processed foods according to claim 4, characterized in that the oleaginous matrix is a combination of saturated and monounsaturated fatty acids, such as oil coconut, canola, almonds, avocado or peanuts.
[9]
9. The process for obtaining a nanoemulsion formulation with encapsulated natural antioxidants for the preservation of fruits, vegetables and minimally processed foods according to claim 4, characterized in that the formulation replaces glycerol and polysorbate with a quantity of 1-5 % calcium ascorbate or a 1: 1 combination of ascorbic acid and citric acid, where the food to preserve is a fruit cut under refrigeration conditions.
[10]
10. The process for obtaining a microemulsified matrix according to claim 4, characterized in that it involves the entire described procedure, except for the microfluidization process.
[11]
11. The process to obtain a nanoemulsion formulation with encapsulated natural antioxidants for the conservation of fruits, vegetables and minimally processed foods according to claim 1 characterized by encapsulating active compounds such as proteins, fatty acids, vitamins and minerals, which have been extracted from fruits, vegetables or cereals.
[12]
12. A nanoemulsion obtained by the process according to claims 1 to 11 characterized in that it has the following formulation:
to. 5 - 40% of antioxidants extracted from residues of fruit, vegetables or cereals; b. 0.5 - 10% alginic acid, preferably sodium or potassium alginate from natural sources, food grade;
c. 0.1 - 10% of oleaginous matrix with saturated and / or monounsaturated fatty acids as major compounds;
d. 0.1-1% polysorbates, preferably polyoxyethylene sorbitan mannolaurate or food grade polyoxyethylene sorbitan monosterate; and
and. 0.5 - 10% Liquid Glycerol or Rosin Glycerol Asters from natural plant sources, food grade.
[13]
13. The nanoemulsion according to claim 12, characterized in that it does not comprise proteins or biopolymers in the formulation.
[14]
14. The nanoemulsion according to claim 12, characterized in that it does not present chemical solvents in its formulation and shows low toxicity, where the nanoemulsion is food grade.
[15]
15. The nanoemulsion according to claim 12, characterized in that it consists of a concentrated powder nanoemulsion that, upon rehydration, maintains all the properties and particle size as well as the fluid nanoemulsion.
[16]
16. The nanoemulsion according to claim 12, characterized in that it does not present the polysorbates in its formulation, where the nanoemulsion consists of an input for organic agriculture or to preserve the quality of natural fruit juices.

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同族专利:

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公开号 | 公开日

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CN111278288A|2020-06-12|

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MX2019012322A|2020-02-13|

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BR112020003962A2|2020-09-01|

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ES2764899R1|2021-06-03|

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WO2019039947A1|2019-02-28|

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ES2764899B2|2021-12-23|

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ZA202001793B|2021-03-31|

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US20200329743A1|2020-10-22|

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CO2020003210A2|2020-04-13|

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PCT/PE2017/000014|WO2019039947A1|2017-08-23|2017-08-23|Method for producing a nanoemulsion with encapsulated natural antioxidants for preserving fresh and minimally processed foods, and the nanoemulsion thus produced|

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