WO2005058476A1 - Proceso de multi-microencapsulación continuo para la mejora de la estabilidad y almacenamiento de ingredientes biológicamente activos - Google Patents
Proceso de multi-microencapsulación continuo para la mejora de la estabilidad y almacenamiento de ingredientes biológicamente activos Download PDFInfo
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- WO2005058476A1 WO2005058476A1 PCT/ES2004/000562 ES2004000562W WO2005058476A1 WO 2005058476 A1 WO2005058476 A1 WO 2005058476A1 ES 2004000562 W ES2004000562 W ES 2004000562W WO 2005058476 A1 WO2005058476 A1 WO 2005058476A1
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- microcapsules
- biologically active
- spp
- omega
- active materials
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- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 150000003648 triterpenes Chemical class 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
- 239000013598 vector Substances 0.000 description 1
- 230000009385 viral infection Effects 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/18—In situ polymerisation with all reactants being present in the same phase
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P25/00—Drugs for disorders of the nervous system
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/16—Interfacial polymerisation
Definitions
- UV ultraviolet light (includes all its wavelengths)
- FA Fatty acid; long chain (more than 6 carbons)
- SFA saturated fatty acid
- UFA unsaturated fatty acid
- MUFA monounsaturated fatty acid (1 unsaturation)
- PUFA polyunsaturated fatty acid (2 or more unsaturations)
- HUFA highly unsaturated fatty acid (4 or more unsaturations )
- w-3 omega-3 unsaturated fatty acid, that is, it has at least one unsaturation in carbon 3, numbering the carbon chain from the opposite end of the carboxylic group.
- w-6 omega-6 unsaturated fatty acid, defined as w-3, except that the first unsaturation (at least one) counted from the hydrocarbon end of the chain is carbon 6 and not 3.
- GMOs Genetically modified organisms.
- the present invention relates to microcapsules and continuous process of water-in-oil microencapsulation in water by in-situ and interfacial polymerization of the emulsion.
- the formulation comprises a continuous aqueous phase having a dispersion of microcapsules containing drops of oil, and wherein inside each drop of the oil phase - optionally containing oil soluble materials - there is a dispersion of water, or aqueous extract or material. water dispersible or water soluble material.
- the oil drops are encapsulated with a polymerizable material of natural origin.
- Such microcapsules are suitable for spray drying processes.
- microcapsules to be used as a dry powder, lyophilized, self-emulsifying powder, gel, cream and any liquid form.
- the active compounds included in the microcapsules are beneficial for health or other biological purposes.
- Such formulations prove to be suitable for incorporation into any kind of food, especially for the production of nutraceuticals, as well as cosmetic products (such as rejuvenating creams, wrinkles, gels, bath and shower consumables and sprays.)
- the preparations are suitable for stabilization. compounds added to food, microbial and nutraceutical culture media, especially those that are easily degradable or oxidizable.
- the field of the present invention corresponds to methods of phonulation and use of biologically active materials, especially in foods, and more specifically in functional or nutraceutical foods; It comprises microencapsulation method, microcapsules produced and application (use) thereof containing certain compounds, some of them described here for the first time.
- microencapsulation The microencapsulation technique is known and used in very different fields (fancy, agrochemicals, dyes, etc.). Different forms of microencapsular compounds are described, so that they are released from controlled sources.
- Fong, W. “Technologies of microencapsulation” in the book “Controlled Relay Systems: Fabrication Technology, 1988 Vol I Editor Dean Hsieh, CRD Press, Florida: In that appointment, it is mentioned that many times the
- SUBSTITUTE SHEET (RULE 26) term microcapsule with other fonnulation sources, such as emulsion, microsphere, liposome, etc.
- the true microcapsules are based on a physical separation of phases by means of a wall (polymer) that occludes inside - the core - the microencapsulated material; They should not be confused with formulations containing materials dispersed in polymers or mixed in polymer matrices. Nor should we confuse microcapsules with simple emulsions. This warning is necessary so as not to confuse the broad state of the art referred to dispersions of this in matrices made of polymers, as well as referred to emulsions of W / O and (W / 0) / W.
- microcapsules A fundamental difference of our invention with respect to practically all microcapsule patents is that we create an emulsion (W / O) that is enclosed by the wall of a microcapsule, and the microcapsules are dispersed or emulsified in W, and also The microcapsules may contain smaller microcapsules in their nucleus, thus creating multi-microcapsules.
- our microcapsules and microencapsulation process are characterized in that the wall is made of a mixture of hydrocolloids that polymerize and crosslink, and their structure is fixed definitely through an increase in temperature; The process takes place without waiting for time between process stages and under continuous agitation. No patent or scientific article presents a microencapsulation method similar to that described here.
- US 6,234,464 describes a method of microencapsulation of FAs, in particular w-3, w-6 or derivatives.
- the microencapsulated core material of the microcapsules is an O / W emulsion; in our invention the core contains a W / O emulsion and also smaller microcapsules;
- each drop of water is protected with a wall; In our invention there are multiple drops of water inside the drops of oil, and not all drops of water are protected with a wall;
- the wall is limited to being formed by two hydrocolloids, also separated into two different layers defined as "inner” and "outer”; In our process it is possible, and convenient, to combine more than two hydrocolloids to form the wall and in addition there is no defined structure of the wall in two (or any number
- SUBSTITUTE SHEET (RULE 26) aqueous phase, which act as stabilizers and prevent their oxidation; (vi) curing of the microcapsules in US 6,234,464 is performed by cooling; while we do it by temperature increase, resulting in our case, a firmer wall; (vii) to remove water from the walls in US 6,234,464, ethanol is used as a substitute for water and drying to obtain a microcapsule powder, while we can obtain microcapsule powder without the intervention of ethanol.
- microcapsules produced by US 6,234,464 and those described in the present invention also have different properties: thermal, iso protection, controlled emission of the iso, the contents of the microcapsules (US 6,234,464 is limited to FAs), etc.
- infant feeding An important aspect of the invention is the application of our formulation in infant products, since cow's milk lacks certain UFAs that are present in breast milk. On this subject of complementation of products for pregnant women, infants and children there are also
- antioxidants Use of antioxidants, protectors and / or UV blockers and free radical blockers. It is well known that the origin of many diseases, from very different types of cancer to cataracts, is due to oxidation reactions, degradation of DNA chains, all this due to oxidation processes, induced by oxidants, UV light and / or free radicals. There are also many patents that claim the use of natural extracts, antioxidant compounds, etc. (EP 1344516, EP 1064910) to prevent a wide range of diseases. The present invention, unlike all others, shows the particularity that antioxidant compounds preserve their antioxidant capacity thanks to the structure and configuration of the microcapsules or their formulations, and allow these antioxidants to be added to foods with all properties
- the proposed multi-encapsulation process is by continuous multi-microencapsulation, by interfacial and in-situ polymerization, of biologically active materials characterized in that (a) in a first step a water phase containing an initiator of polymerization and, optionally, at least one biologically active material, to an oil phase, optionally containing at least one biologically active material; additionally there is at least one emulsifier in at least one of the two mentioned phases, and there is a biologically active material in at least one of the two phases (b) in a second step an aqueous solution or dispersion containing at least one hydrocolloid is added, which causes an inversion of phases, and at the same time the hydrocolloid begins to deposit and polymerize on the walls of the new drops consisting of a water-in-oil emulsion, also a cross-linking of the polymers (c) in a third step is added an aqueous solution or dispersion
- microcapsules are separated and joined together, eventually enclosing droplets inside larger ones (multi-microencapsulation) (f) when enough time has elapsed for the drops of water in oil to be coated with at least one hydrocolloid. and, at least, a protective colloid, the temperature is increased to strengthen the wall of the aforementioned drops, which are now microcapsules or multi-microcapsules in aqueous suspension (g) optionally the formulation is dried to obtain powder, and it is reformulated by techniques belonging to the state of the art to obtain (or be mixed the microcapsules in) wettable powders, gel, cosmetic or medicinal creams, bath products, microorganism culture media.
- step g) the entire process - optionally except step g) - occurs under continuous agitation.
- SUBSTITUTE SHEET (RULE 26) (a) two different solutions (Fig. 1) la (oil) and Ib (water) are mixed by adding Ib to it, these solutions containing active ingredients and optionally free or sequestered cations to be released afterwards (b) thanks to a food emulsifier that may be in the solution in or in Ib, an emulsion of water droplets (10) is formed in the oil phase (9).
- This step is concluded with the formation of the emulsion le, where in the oil phase (9) the preferably fat-soluble active ingredients are solubilized or dispersed; A water-in-oil emulsion is also formed, with the water droplets (10) preferably containing the water-soluble active ingredients (c), then the solution 2b of at least one hydrocolloid is added - capable of being polymerized and crosslinked, and optionally containing at least one active ingredient, to the emulsion existing in it. (d) then an inversion of phases occurs, and we have dispersed drops (11) that are an emulsion of water (12) in oil, dispersed in the continuous medium (24), that is, water. (e) then, (Fig.
- a solution or dispersion 5a containing at least one hydrocolloid (15), which acts as a protective colloid.
- the solution or dispersion 6a containing the primary emulsifier is added to the emulsion 2a.
- the temperature between 30 ° C and 70 ° C is increased to 60 ° C - 100 ° C
- a food viscosity modifier is optionally added, the formulation can be spray dried, or any form belonging to the state of the art, and collected and form dry powders, self-emulsifying powders, gels, creams or any liquid form that contains them (including a dispersion in oil), as well as can also be lyophilized.
- Preferred Embodiment of the Invention Since one of the preferred embodiments is the use for addition to food is a preferred embodiment, the microcapsules obtained by this process have been successfully tested in terms of resistance
- the hydrocolloid (s) such as the protective colloid (s) can be added together as an initial aqueous solution or dispersion.
- the primary emulsifier and the protective colloid can be chosen from the group of hydrocolloids, as well as the viscosity modifier, since hydrocolloids have all these different types of properties.
- SUBSTITUTE SHEET (RULE 26) ⁇ 5
- the most appropriate group of compounds for the success of a formulation according to the process described corresponds to the group: chitosan, starch, dextrin, cyclodextrin, cellulose, lignin, pectin, agar, alginates, carrageenan, gelatin, guar gum, gum arabic, gelatin, tragacanths, lignosulfonates, Carayá gum, Ceratonia siliqua gum, saponin, xanthan gum, seed gums, galactomananas, arabanogalactans, beta-glucans, inulin, psyllium, acacia gum; in all its isomeric and stereochemical forms, in all its variants with respect to the quantity and proportion of monomers or oligomers constituting the hydrocolloid, in all its variants of presentation, such as metal cation salts or salts of nitrogen or phosphorus or sulfur compounds, as well as of any
- the lipophilic hydrophilic balance is an estimate of the emulsifying power of a compound with emulsifying capacity, varying according to the convenience of forming a W / O emulsion or an O / W emulsion.
- the HLB of the primary emulsifier of the present invention should be between 9 and 16, preferably between 12 and 14.
- the emulsion shown in (10) must have a particle size, determined by a measuring equipment of the Master Sizer type, between 50-500 ⁇ m, preferably between 70-200 ⁇ m.
- the microcapsules formed (7b) have a particle size of in the range 0.1-100 ⁇ m, preferably in the range 1-30 ⁇ m, more preferably in the range 1-5 ⁇ m. ⁇ 9 This size may vary over time by aggregation processes, which are somewhat desirable, as long as the structure of the formulation is not greatly affected.
- hydrogels A particular type of colloid is hydrogels, so hydrocolloids can be substituted by hydrogels, optionally those based on albumin, alginates, polycarboxylates, poly-L-lactide, starch, and derivatives.
- various mixtures of hydrocolloids or hydrogels can be used, so we can vary the degree of polymerization, the hardness of the walls, their thickness, their electrical properties, their permeability to certain compounds, for obtain the microcapsule with resistance to food processes and the environment in which it will be found (eg in a yogurt) until its final consumption.
- microcapsule wall components are also applicable to viscosity modifiers and emulsifiers used, both initially used to form le (preferably a polysorbate) and for primary emulsifier (preferably a compound based on soy lecithin ).
- the microcapsules can be obtained in the dry state, or also redispersed in other liquid or even solid or solidifiable matrices.
- the external medium may contain compounds that help maintain the microcapsule wall, as regulators of the ionic strength of the solution in which the microcapsules are found, of the osmotic pressure, etc. There may also be, for example, metal cations inside the microcapsules that, once completely fused, help the wall not to be destroyed, as would be the case with calcium ions inside a microcapsule formed with pectins in its wall.
- the active ingredients can be added at any step of the process, even in the food processing phase (mixed with microcapsules) but obviously, the most important thing is that the active and beneficial health materials are inside the microcapsules, either because they come from Ib, 2b, 5a or added at any time during the process.
- one of the embodiments constitutes adding to any type of food compounds beneficial to health, in antioxidant particles and UFAs, it is important to prevent oxidation during the formation of the microcapsules. Under the following process conditions oxidation is greatly reduced: under vacuum, reduced pressure, in the presence of an inert gas, preferably nitrogen or helium, protected from light of any wavelength, under sterile conditions.
- an inert gas preferably nitrogen or helium
- solutions or dispersions are included: (i) based on aqueous extracts, (ii) with an alcohol content not exceeding 40%, being the water residue (iii) of water soluble or dispersible compounds.
- oil phase can be any hydrophobic phase, such as waxes or even complex mixtures such as honey.
- microbiological stabilizer bactericides, fungicides, bacteriostatics, fungistatics, etc.
- An embodiment of the invention consists of a dry formulation of the microcapsules, coated with the microbiological stabilizer.
- microcapsules For certain applications, especially cosmetics, once the microcapsules are dried, they must be reinstated in other media such as gels, oils, alcoholic solutions for perfumes, etc.
- the microcapsules contain aromas to be used in perfumery or to perfume gels and bath creams.
- the microcapsules can be applied to all types of foods, but not limited to the following examples: cereals and derivatives (optionally muesli, cereals for milk), pastries and pastries, sugars and derivatives (optionally chocolates, sweets, nougat, marzipan) , dietary sweets (with low calorie level), in diet and diabetic foods, oils and derivatives, dairy and derivatives, eggs, vegetables, legumes, fruits, tubers and derivatives, edible stems, snacks, snacks, edible roots (optionally licorice), berries and wild products, canned fruits, nuts, meats, sausages, fish, shellfish and crustaceans and their preserves, alcoholic and non-alcoholic beverages, carbonated or non-carbonated drinks, juices, syrups, nectars, spices, condiments, pre-cooked meals, pre-processed foods (frozen bread dough), pizzas, honey.
- cereals and derivatives optionally muesli, cereals for milk
- sugars and derivatives optionally chocolates, sweets, nougat, marzi
- the microcapsules can be used for other purposes, in particular to encapsulate semiochemicals, attractants, repellents, insecticides , sterilizers, herbicides, fungicides, bactericides, viricides (or materials that prevent viral infections), gene vectors (for gene therapy or for purposes of recombinant DNA techniques), aromas, pungent indicators of the presence of odorless, astringent chemical compounds for avoid ingestion of toxic products (preferably ethanol, isopropyl alcohol, hydrogen peroxide, furniture cleaners and other similar products for home use).
- the invention will be carried out to avoid aromas, with the consequent adaptation of the wall materials and other factors, in order to avoid the maximum release of the encapsulated materials.
- microcapsules produced by a continuous microencapsulation process characterized in that (a) they contain active ingredients beneficial to human health; (b) the wall of the microcapsules is composed of a mixture of at least two hydrocolloids, such a polymerized and crosslinked mixture, such hydocolloids are edible; (c) the degree of polymerization, cross-linking and nature of hydrocolloids influences the controlled release of active compounds and protection against oxygen and / or light and / or temperature; (d) the microcapsules contain inside them a water-in-oil emulsion, there are optionally active ingredients in the oil phase, optionally in the water phase or optionally in both phases and in addition, they may contain smaller microcapsules (multi-encapsulation possible up to, at least
- microcapsules produced according to the process described herein may release their content due to at least one factor chosen from the group of: pH, temperature, pressure, ionic strength, osmosis, volatilization, presence of compounds that dissolve the microcapsule wall.
- the microcapsules formed, in an embodiment corresponding to human consumption, must withstand the usual food processes, in particular operations, belonging to the state of the art, concerning protection against microorganisms, harmful and / or unwanted both in the newly formulated formulation.
- microorganisms of the formulation or food to which it is intended these operations being eventually: sterilization, stabilization of microorganisms, pasteurization, UHT, ozonation, UV rays, addition of chemical antimicrobial products (both synthetic and natural), irradiation with gamma rays.
- Microbiological stabilizers can also be added in the industrial process, therefore in one embodiment, inside the microcapsules (optionally in the oil phase, or in the water phase, or both) and / or in the phase containing the microcapsules, a stabilizing material is found in terms of microbiological quality.
- the formulation is accompanied by a quality certificate that analyzes the absence of heavy metals, harmful degradation products of biologically active materials, agrochemicals used in the production of biologically active materials and other compounds that They are harmful to health.
- the microcapsules are used to provide nutrients, anabolites, compounds that help identify disease causing microbes (such as selective anabolites or fluorescent or radioactive labeled products), and these compounds may be released by changes. pH in the culture medium (e.g., potato-dextrose agar), by
- SUBSTITUTE SHEET (RULE 26) production of enzymes (from the same microbial culture, eg) or other metabolites (such as alcohol or released enzymes).
- Microcapsules can be added to natural or artificial sweeteners, salt, pepper, spices and condiments in general, so that the addition of the aforementioned condiments to food increases the nutritional value, or health benefit, of food.
- a compound that prevents the oxidative and / or destructive action of ultraviolet rays is suitable.
- a preferred embodiment is one in which materials that are heavily known to scientists and the public are microencapsulated - with a certain level of culture - as very appropriate to maintain health or prevent disease, or even cure disease.
- the inventors choose the group of compounds, (totally or partially mixed or used individually), to be microencapsulated as follows: green tea, black tea, cocoa, red wine or red grapes or pomace of some inks, cider or apple or Apple juice, germ or bran of cereals, cariots or carrots, chili, garlic, radish (especially horseradish).
- the present invention shows a novel method of formulation of many different types of compounds, constituting a complete novelty regarding the state of the art that the compounds are microencapsulated with edible materials of such that they protect the active ingredients from degradation in the processes of the food industry and / or in the kitchen, in a way superior to what is described, thanks to the multi-microcapsule structure that provides a multitude of protective layers to a percentage of the microencapsulated products, thanks to the water-in-oil emulsion inside the microcapsules that allows both hydrophilic and hydrophobic products to be microencapsulated, and that the mixtures of these compounds pennite that some compounds protect other compounds from oxidation, as well as the details and steps of the production process that result in microcapsules that p can be tailored to the microencapsular compounds, in terms of
- SUBSTITUTE SHEET (RULE 26) Optimal protection and adequate release speed.
- chemically similar compounds behave similarly in the process and the microcapsule (e.g., limonene and pinene, both being monoterpenes, should not present much difference to When it comes to encapsulating or when it is released by the microcapsules, even the copaeno -which is a sesquiterpene- will not differ much from the monoterpenes, nor will the limonene oxide, with an additional functional group, present large differences at the time of its microencapsulation according to the process described here, since the functional groups do not have an impact on the formation of the emulsions or the constitution of the wall of the microcapsules drastically.In cases where certain compounds do greatly modify the needs of emulsifiers In particular, the inventors have foreseen these cases, and for this purpose different emulsifiers, polymers, etc., are used.
- flavonoids in general and their derivatives: anthocyanidins, pro-anthocyanidins, oligomer-procyanidin, isoflavones, chalconas, catechin, epicatechin, epicatechin gallate, epigallocatechin, epigallocatechin gallocatechin , eriocitrine, narirutin, rutin, naringin, myrithitrine, hesperidin, myricetin, erythiocythol, fisetin, quercetin, naringenin, luteolin, hesperitin, kaempferol, isorhamnetin, apigenin, rhamnetin, galangina, quercitrin, quercetin, biodynin, gazetin, gazetin, amethe
- amides comprising hydroxycinnamic acids and anthranilic acids (avenanthramides), avenasterol, hydroxycinnamic acids structurally combined with saturated or unsaturated long chain fatty acids, hydroxycinnamic acids structurally combined with alcohols, indoleamines, melatonin, inulin; glutathione (d) terpenoids in general and their derivatives, monoterpenes, diterpenes, sesquiterpenes, triterpenes, tetraterpenes, including carotenoids, alpha-carotene, phytotene, cyclo-artol, beta-carotene, ionone, zeaxanthin, capsantin, astaxanthin, cantaxanthin, violaxanthin, violaxanthin , mutatoxanthin, luteoxanthin, auroxanthin, neoxanthin, apo-carotinal,
- antioxidants commonly used in the food industry such as butylhydroxyanisole, 2,6-di-tert-butylhydroxytoluene, tert-butylhydroquinone, 2,6-di-tert-butylhydroquinone, 2,6-diterbutyl- 4-hydroxymethylphenol, 2,4,5-trihydroxybutyrophenone, tocopherols and their derivatives, [alpha-,
- SUBSTITUTE SHEET (RULE 26) beta-, gamma- and delta-] tocopherol; tocotrienols and their derivatives, [alpha-, beta-, gamma- and delta-] tocotrienols; tocochromanols (f) alpha-lipoic acid; coenzyme Q-10; squalene; phytoestrogens; chlorophyll; vitamins; amino acids, preferably L-arginine, and their corresponding organic polymers such as glutathione, oligopeptides, preferably carnitine and carnosine, peptides, enzymes; enzyme inhibitors, preferably inhibitors of phenolases, oxygenases, lipoxygenases, peroxidases and lipases; (g) as well as minerals, trace elements, especially those that participate in in vivo redox processes such as selenium, zinc and magnesium.
- This list is a non-limiting example of natural sources of active compounds to microencapsular, both for the isolation of compounds, and for aqueous or alcoholic solutions of the aforementioned sources and for dispersions of leaves, stems, roots, fruit flowers, etc. crushed to a certain degree of particle size, as well as lyophilized preparations thereof or pre-processed in any way.
- the list referred to is: Medicago sativa, Pimenal officinalis, Hibiscus abelmoschus, Angelica archangelica, Galipea officinalis, Pimpinella anisum, Foetida splint, Asafetida splint, Melissa officinalis, Myroxylon pereirae, Ocimum basilicum, Pimenta acris, Citrus aurantium bermium, Citrus aurantus bermium, Citrus aurantus bermium, Citrus aurantus bermium, Citrus aurantium berdantium, Citrus aurantium berdantus bermium , Citrus aurantium amara, Piper nigrum, Prunus spinosa, Aniba rosaeodora, Camellia oleifera, Camelia sinensis, Carum carvi, Elettaria cardamomum, Ceratonia siliqua, Daucus carota, Dacu
- SUBSTITUTE SHEET (RULE 26) Chimaphila umbellate, P ⁇ nica granatum, Pelargonium spp., Pelargonium graveolens, Rosmarinus officinalis, Crocus sativus, Salvia app., Salvia officinalis, Mentha spicata, Mentha viridis, Satureia hortensis, Satureja hortensis, Origanum majorana, Tamarmistaraculaula draculataula, Tamarindula indicaus Thea sinensis, Thymus vulgaris, Polianthes tuberosa, Turmeric longa, Prunus serótina, Thymus serpillum, Satureja Montana, Cananga odorata, Turmeric zedoaria, Plantago major, Adansonia digitata, Ananas comosus, Artocarpus altilis, Carica papalentum, Lycopersicon sp.
- SUBSTITUTE SHEET (RULE 26) ⁇ 42-45
- Another issue that concerns a considerable part of the population in developed countries is the consumption of probiotic organisms, understood as such, to organisms that by products of their metabolism or by their presence in the organism, protect against certain infections. (especially Candidasis), reduce levels of cholesterol and glycerides, and help in digestion processes and diseases of the digestive system, mainly.
- probiotic organisms are generally introduced into yogurts and dairy products, but by means of the present invention, we have found that it is possible to microencapsulate bacteria, fungi and yeasts alive, remaining alive after microencapsulation and after usual processes in the food industry, such as homogenization pasteurization and even certain types of baking, as well as homemade cooking.
- Probiotic organisms are preferably chosen (but not limited to) from the groups: (a) probiotic bacteria, optionally lactic acid bacteria and more preferably chosen from the group of: Lactobacillus casei., L. acidophillus, L. rhamnosus, L Paracasei, L. gasseri, L. fermentum, L. plantarum, L. salivarius, L. crispatus, L. bulgaricus, L. fermentum, L. reuteri, Bifidobacterium infantis, B. bifidum, Streptococcus termophilus, S. bovis, Enterococcus durans, E.
- probiotic bacteria optionally lactic acid bacteria and more preferably chosen from the group of: Lactobacillus casei., L. acidophillus, L. rhamnosus, L Paracasei, L. gasseri, L. fermentum, L. plantarum, L. salivarius, L. crispatus, L. bulgaricus, L. fermentum, L.
- probiotic yeasts preferably chosen from the group of: Saccharomyces cerevisiae, Kluyveromyces marxianus, Rhodotorula rubra, Sporobolomyces puniceus, Aureobasidium pullulans, Leucosporidium scotti.
- probiotic fungi preferably those fungi present in, or coincident with, or from, cheeses.
- the inventors consider that the combined use of UFAs with sphingolipids, and more especially with cerebrosides, is recommended for adequate or improved development, of cerebral cortex and other places (eg, retina) where there is a neuronal development preferential. Moreover, it is important in fetuses, children or people with neuronal problems.
- Rj is an ester of an omega-3 fatty acid or an omega-6 fatty acid or a w- fatty acid
- R 2 is an ester of an omega-3 fatty acid or an omega-6 fatty acid
- R 3 is an ester of an omega-3 fatty acid or of an omega-6 fatty acid or of a w-9 fatty acid.
- R 4 is an ester of an omega-3 fatty acid or an omega-fatty acid. 6 or a w-9 fatty acid or a covalently linked oligosaccharide
- One of the embodiments consists of a microencapsulation process characterized in that at least one of the biologically active materials present in the phnulation preferably consists of at least one unsaturated long chain fatty acid (at least 6 carbons), in any configuration isomeric and / or stereochemical, as well as derivatives thereof (preferably) esters, ethers, glycerides, phospholipids, sphingolipids and more preferably, diglycerides, triglycerides, phospholipids, compounds (A) and / or (B ) - steradionic, eicosapentaenoic, docosahexaenoic, docosapentaenoic, conjugated linoleic, linolenic, gamma-linoleic, alpha-linoleic, dihomogamma-linoleic, arachidonic and / or oleic.
- the fatty acids are preferably chosen from the group of acids: oleic, stereadionic, eicosapentaenoic, docosahexaenoic, docosapentaenoic, linoleic, linolenic, gamma-linoleic, alpha-linoleic, dihomogamma-linoleic, arachidonic.
- fatty acids may be conjugated with other compounds that subsequently release them under conditions of the stomach or digestive system or enzymatic processes in the liver, so, according to this invention, fatty acids may be conjugated, maintaining or not. keeping all or part of the unsaturations intact, with glycerides -more preferably, diglyceride esters and triglyceride esters-; phospholipids; sphingolipids; myelin; amines; amides; ethers; sugars, oligosaccharides, polysaccharides; Nitrogenous, phosphorus, oxygenated, sulfurized or substituted aromatic heterocycles.
- sources that also proportions w-3 are of: (a) plant origin: more preferably of families: Boraginaceae, especially (Borago spp. And especially Borago officinalis); Linaceae (Linum usitatissimum, Linum arvense, Linum sativum); Onograceae (Oenothera biennis); Grossulariaceae (Ribes nigrum), Zea Mais, Gossypium hirsutum, Carthamus tinctorius, Glycine max.
- plant origin more preferably of families: Boraginaceae, especially (Borago spp. And especially Borago officinalis); Linaceae (Linum usitatissimum, Linum arvense, Linum sativum); Onograceae (Oenothera biennis); Grossulariaceae (Ribes nigrum), Zea Mais, Gossypium hirsutum, Carthamus tinctorius,
- families Graciliariceae (Gracilaria spp); Gigartinaceae (Iridaea spp.); Kallymeniaceae (Callopyllis variegata); Durvillaceae (Durvillaea antartica); Solieriace
- SUBSTITUTE SHEET (RULE 26) australis); Pomadasyidae; Sco ⁇ aenidae; Serranidae; Cyprinidae; Monacanthidae; Centrolophidae; Ophidiidae; Sco ⁇ aenidae; Coryphaenidae; Chanfferhydae; Sciaenidae; Aplodactylidae; Carangidae (Trachurus symetricus mu ⁇ hyi); Bothidae (Paralichthys microps); Mugilidae; Clupeidae; Priacathidae; Merlucciidae (Merluccius gayi gayi, Merluccius australis); Macruronidae (Macruronus magellanicus); Gadidae (Micromesistius australis); Girellidae; Trachichthyidae; Carangid
- (d) of microbial origin most preferably: Saccharomices cerevisiae, Escherichia coli, Schizochytrium spp., Thraustochytrium aureum, Thraustochytrium roseum, Thraustochytrium striatum, Mortiriella spp., Phytium spp., Aspergillus spp. Aspergillus nidulans, Aspergillus sydowi, Fusarium spp., Fusarium equiseti, Fusarium oxysporum
- An embodiment of the invention is a microencapsulated phonulation intended to increase neuronal development, especially of the brain and more especially in fetuses, newborns, infants and children characterized in that there is at least one compound characterized by the B and / or phonules TO.
- Another embodiment is a microencapsulated phonulation intended to increase the potential intelligence in fetuses and infants breastfeeding - through the consumption of breast milk with an appropriate food vehicle in which the microencapsulated phonulation is added - in formulations of milk for infants and children, characterized in that it contains omega-3 and omega-6 fatty acids in a proportion between 0.5 and 10.0, preferably between 1.4 and 5.7 and also contains cerebrosides in a percentage between 0.005% and 1% or / and optionally compounds A and / or B.
- omega-3 and omega-6 fatty acids in a proportion between 0.5 and 10.0, preferably between 1.4 and 5.7
- cerebrosides in a percentage between 0.005% and 1% or / and optionally compounds A and / or B.
- There is a sea of combinations of ratios between omega-3 and omega-6 which do not have a firm scientific basis, and many scientific articles differ in the recommendations.
- there are patents that cover all imaginable ranges of combinations The inventors of the present invention adopt
- SUBSTITUTE SHEET (RULE 26) compound A or B as well as the method of providing the consumer with UFAs in the absence of bad odors or degradation products of the UFAs.
- the inventors have verified that in an industrial process used to manufacture milk with w-3 acids, 50% of the original w-3 is lost during homogenization and pasteurization. With our microcapsules, at the industrial level, in the worst case tested at the industrial level (pilot plant) we obtain a maximum loss of w-3 of 7%.
- a microencapsulated formulation for use in infant formulas characterized in that optionally any omega-6 fatty acid is dispensed with and, independently, optionally gamma linolenic acid is added in a proportion of 1.25%; or a microencapsulated formulation for use in infant formulas, according to claim 25, characterized in that optionally any omega-3 fatty acid is dispensed with and, independently, optionally gamma linolenic acid is added in a proportion of 1.25%.
- a microencapsulated formulation intended to increase the development of the cerebral cortex and intelligence, characterized in that it contains omega-3 and omega-6 fatty acids in a proportion between 0.5 and 10.0, preferably between 1.4 and 5.7 and also contains cerebrosides in a percentage between 0.005% and 1% and optionally compounds A and / or B.
- the inventors have formulated a refreshing beverage containing a microcapsule formulation, produced according to claim 1, characterized in that said beverage contains microcapsules, and these in turn contain in their oil phase omega-6 and / or omega acids -3, optionally with antioxidants added in the aqueous discontinuous phase of the microcapsule or in the continuous hydrophobic phase of the microcapsule or in both, and the beverage contains aromas or extracts of: grape, pineapple and at least some citrus, preferably between the group of tangerine, orange, tangerine, lemon, lime, and omega-3 and / or omega-6 fatty acids remain stable in the drink, once the entire industrial process is finished (including usual microbiological stabilization processes such as pasteurization), when less for a month (loss of omega-3 less than 7,.%).
- microcapsules produced according to any suitable combination of the preceding claims characterized in that (a) the microcapsules contain omega-3 acids from a commercial formulation based on edible flax oil; (b) the oil phase contains flax oil and an emulsifier based on soybean compounds (c) the water phase contains a mixture of different hydrocoloid subclasses of the alginate and / or gum arabic and / or kappa-carrageenan type and / or guar gum, in addition to a primary HLB food emulsifier between 10 and 14, and a food viscosity modifier (d) and the pH of the microcapsule phonulation is in the range of 3-6, the size in the 50th percentile of the newly produced microcapsules is in the range 1-10 ⁇ m
- SUBSTITUTE SHEET (RULE 26) because the fruits of the juice are chosen from the group: citrus, pineapple, grape and because it contains (all data referring to 150 mL of juice) omega-3 in the range 20-200 mg, omega-6 in the range 10-100 mg and w-9 in the range 5-50 mg; with an omega-3 / omega-6 ratio of about 3/1.
- microcapsules that are destroyed at low pHs (such as present in the human stomach) or are resistant to low pHs (and may pass through the stomach - suitable for certain hormones such as insulin - and the wall being broken by increasing the pH in the intestine), as well as walls that are attacked by certain enzymes (e.g., using starch on the wall, the amylases destroy the wall), or by pressure when chewed in the mouth, or when gelled in the presence of saliva, releasing an aroma (or eg menthol) very quickly.
- the microcapsules can be designed for the particular conditions of each animal to which they are to be administered (e.g., the pig has abundant amylases in the mouth, unlike the man , and a microcapsule formed with starch would be appropriate to give a taste to the food pleasing to the pig to increase the food intake and therefore its weight, and the benefit to the farmer).
- microcapsules and formulations are compatible and desirable for foods in which the active ingredients come from agriculture (which includes agricultural and fish farming) "biological” and / or “ecological", since this falls in line with a Healthy eating without the intervention of chemicals foreign to nature. Obviously, in this embodiment, as in many others already mentioned, all the materials used must be allowed for feeding.
- the formulation employs for obtaining active ingredients, genetically modified organisms (GMOs), hybrid plant varieties or obtained by human selection, as well as cultures. Microbiological selected by any technique. This embodiment is possible but not desired because consumers in general tend to avoid GMOs.
- the microcapsules produced according to our processes may be included in medicinal formulations, be they in combination with active ingredients not present in the microcapsules or the active ingredients present in the microcapsules or microcapsule formulation being the only active ingredients of the medicinal preparation, including under the term medicinal preparation also contrast materials in radiology, seeds for oncological radiotherapy, thermotherapy or light irradiation therapy of any wavelength.
- contrasts for radiological studies are very suitable used in combination with microcapsules that admit passage through the digestive tract without being degraded, and
- SUBSTITUTE SHEET (RULE 26) then be excreted, for medical purposes (detection of bleeding by materials from microcapsules sensitive to blood plasma enzymes, for example) ⁇ 76-78 Since many of the active ingredients beneficial to health are labile, especially oxidation, An embodiment of the invention is to keep the capsules separated from the food or beverage until a few moments before the final consumption, optionally with a receptacle which, when pressed, releases the formulation, preferably dry, to the food or drink.
- Example 1 In this example we describe the active ingredients used to make a convenient formulation for application to orange juice.
- the oil phase weighs in a bottle, homogenizes in an ultrasonic bath? Does the water phase weigh in a bottle, homogenize in an ultrasonic bath? W / the emulsion Or put the oil then the water phase in the reactor, does the emulsion with stirrer at 7350 ,m, 25 min emulsion? (W / 0) / W adds the alginate solution, stirrer at 350 ⁇ m at 35 ° C
- Example 12 In the present embodiment, we show the release of microcapsules at a certain pH. Microcapsules broken in stomach pH, while the microcapsules remain intact in yogurt, which is also acidic (but not as extremely acidic as the stomach). The objective of the present example should prove the rate of microencapsulated riboflavin release (according to the present invention) presented in a probiotic yogurt. Yogurt has been prepared (20 kg) in a traditional, handmade, way, using an "internal" fermentation culture maintained from the latest yogurt production.
- composition of the formulation (the percentage with respect to total active ingredients) is: -Riboflavine 100 ⁇ G yogurt / kg (less than 0.1% of the total active ingredients) -Casectobacillus casei 10% (the solution in the water of a culture with 500 colonies per cm2) -Oativa sativa extract 90% Fonnulation has been prepared following the general encapsulation procedure, with alginates such as cross-linked hydrocolloid and a mixture of Ceratonia siliqua gum and Arbabic hydrocolloids as a protector. A non-ecpasulated matter has been included in the experiment to show the differences, and also a blank sample.
- the rate of release in the non-encapsulated matter is, as expected, higher.
- the average released amount of Vitamin B2 is 46.8% [say, 40-50% of the compensated sample]; after 60 min., 47.2 ⁇ G / kg [is said, a conversion of the compensated sample of ca. 65-75%].
- White showed no release (the liquid chromatographic gas peak) of Riboflavin.
- B results in yogurt means - Formulation GAT 032541 does not release any vitamin B2, while in yogurt, for at least one and a fortnight.
- the non-encapsulated sample showed a slight release of 0.021 ⁇ g / G after 30 min., And 0.032 ⁇ g / G after 60 min. Blank samples showed no noticeable change in Vitamin B2 content.
- Example 13 One of the innovative aspects of the present invention is its ability to keep the active ingredients fixed for the longest time with respect to the state in the microencapsulation of the art and even any other method of formulation. This obviously does not require fixed active ingredients (E. G. the minerals). We have tested the ability of
- SUBSTITUTE SHEET (RULE 26) storage when the active ingredients remain the same.
- the encapsulation process is basically like the one presented in example 1, with the exception that the secondary wall is fused with xanthan gum (from Fluka), the emulsifier is So ⁇ enol® 3767 (1%) and the viscosity modifier It is Glycosperse® (1%), the source of W-3 and W-6 adipose acids were fish oil (Clupea harengus).
- Example 14 The major problem associated with new revealing formulations is the difficulty of inferring the true results of past fonnulations. As many components (and quantities) can be present in a microencapsulation, the number of experiments needed for a good statistical validation is enormously high. We have overcome this problem with the state of the art statistical techniques associated with experimental design. We have used a folded Plackett-Bunnan experimental design (we are interested only in the main factors, and not in interactions for the purpose of this analysis), with 3 central points and an acceptable level of degrees of freedom error (19).
- Acclndex we have developed, for a series of experiments, a table that gives, for each Particle Size (and the other variables) a value between 0 and 1.
- the " density "(not the true meaning of density) can have the value 0, because outside a defined range, density is not considered;
- the acceptability index depends on the limitations of the other variables (for example, if the degree of unreacted polymers are higher than 40%, we give the acceptability indexes a value of 0, no matter the value of the rest of the parameters).
- the constant appraises that justifies the weight of each value, they have developed
- Fig. 10 to 12 are characteristics of our formulation. It indicates that the dimishes of the formulation of progressively microencapsulated its internal stratum due to the applied force (the scissors emphasis), but after a period of time (force) while the cohesive forces that maintain the macromolecular structure of the fixed phonulation break (namely, up to the peak shown). Note that the microcapsules do not break, but the structure that keeps the microcapsules dispersed, withoud precipitation, coacervation or no deformation of the formulation. When the macromolecular cohesive forces (mainly electrostatic forces) are low (Fig.
- microorganism the reference of brands to all kinds of living beings also referred to as “microbes”, namely living beings of the lowest degree of evolution.
- the Tennino also includes a not clearly classified organic structures (he did not consider living beings by many scientists) as viruses, viroids, mycoplasmas, etc.
- Groceries include both solid and liquid, namely beverages (alcoholic and non-alcoholic, sodas, juices, dairy products, etc.). Groceries O also refer to those used in livestock production, and when they appropriate, for, the microorganism's production.
- organic foods both refer to those foods that are produced without the help of anyone synthesized (in other words, the human produced, for example including with the help of microbes) chemical substances, other than those used for centuries to produce food Or also, this term includes those foods that are produced under a restricted number of chemicals that may be involved in the production of food and / or livestock. Sometimes, this second type of food production is called “organic food.”
- food grade means that "it is edible”, this conception may legally differ from country to country.
- unit microcapsule refers to a microcapsule that does not contain any other smaller microcapsule within it.
- the Tennino "agriculture” includes plant production and animal production, and edibles derived from it.
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Abstract
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Priority Applications (11)
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MXPA06006735 MX295630B (es) | 2003-12-18 | 2004-12-17 | Proceso de multi-microencapsulacion continuo para la mejora de la estabilidad y almacenamiento de ingredientes biologicamente activos. |
CA2550615A CA2550615C (en) | 2003-12-18 | 2004-12-17 | Continuous multi-microencapsulation process for improving the stability and storage life of biologically active ingredients |
JP2006544472A JP5500705B2 (ja) | 2003-12-18 | 2004-12-17 | 生物学的有効成分の安定性及び貯蔵寿命を向上させるための連続的マルチマイクロカプセル封入方法 |
BRPI0417767A BRPI0417767B1 (pt) | 2003-12-18 | 2004-12-17 | processo contínuo de multi-microencapsulação para melhorar a estabilidade e o armazenamento de ingredientes biologicamente ativos |
ES04805105.6T ES2630627T3 (es) | 2003-12-18 | 2004-12-17 | Proceso de multi-microencapsulación continuo para la mejora de la estabilidad y almacenamiento de ingredientes biológicamente activos |
AU2004298792A AU2004298792B2 (en) | 2003-12-18 | 2004-12-17 | Continuous multi-microencapsulation process for improving the stability and storage life of biologically active ingredients |
EP04805105.6A EP1702675B1 (en) | 2003-12-18 | 2004-12-17 | Continuous multi-microencapsulation process for improving the stability and storage life of biologically active ingredients |
US10/596,556 US8168225B2 (en) | 2003-12-18 | 2004-12-17 | Continuous multi-microencapsulation process for improving the stability and storage life of biologically active ingredients |
CUP2006000128A CU24194B1 (es) | 2003-12-18 | 2006-06-19 | Proceso del multi-microencapsulación continuo para la mejora de la estabilidad y almacenamiento de ingredientes biológicamente activos |
US12/885,108 US8911783B2 (en) | 2003-12-18 | 2010-09-17 | Continuous multi-microencapsulation process for improving the stability and storage life of biologically active ingredients |
US12/885,165 US8685446B2 (en) | 2003-12-18 | 2010-09-17 | Continuous multi-microencapsulation process for improving the stability and storage life of biologically active ingredients |
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US12/885,165 Division US8685446B2 (en) | 2003-12-18 | 2010-09-17 | Continuous multi-microencapsulation process for improving the stability and storage life of biologically active ingredients |
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Also Published As
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AU2004298792A1 (en) | 2005-06-30 |
CU20060128A7 (es) | 2013-05-31 |
EP1702675B1 (en) | 2016-09-21 |
CU24194B1 (es) | 2016-09-30 |
JP2007521135A (ja) | 2007-08-02 |
CN1917946A (zh) | 2007-02-21 |
ZA200604896B (en) | 2007-10-31 |
CR8511A (es) | 2006-11-10 |
JP5500705B2 (ja) | 2014-05-21 |
US20110064817A1 (en) | 2011-03-17 |
MXPA06006735A (es) | 2007-02-16 |
BRPI0417767B1 (pt) | 2016-02-16 |
ECSP066708A (es) | 2006-10-31 |
US20070077308A1 (en) | 2007-04-05 |
US8911783B2 (en) | 2014-12-16 |
US8168225B2 (en) | 2012-05-01 |
EP1702675A1 (en) | 2006-09-20 |
ES2235642B2 (es) | 2006-03-01 |
AU2004298792B2 (en) | 2010-07-15 |
BRPI0417767A (pt) | 2007-04-17 |
MX295630B (es) | 2012-02-07 |
CA2550615C (en) | 2012-11-27 |
CA2550615A1 (en) | 2005-06-30 |
ES2235642A1 (es) | 2005-07-01 |
US8685446B2 (en) | 2014-04-01 |
US20080102132A2 (en) | 2008-05-01 |
CN100566812C (zh) | 2009-12-09 |
US20110064778A1 (en) | 2011-03-17 |
PL1702675T3 (pl) | 2017-03-31 |
ES2630627T3 (es) | 2017-08-22 |
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