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    • 专利摘要:
    Method for obtaining extracts comprising hydroxycinnamic compounds from plant residues. A method for obtaining an extract comprising hydroxycinnamic acids, characterized in that the method uses one or more vegetable residues as a starting material in the preparation of vegetable food products, and comprises: a) selecting at least one residue of at least one plant species, b ) extract the hydroxycinnamic acids present in the residue, c) separate the main liquid phase comprising the compounds extracted from the solids, d) clarify the liquid phase obtained in step c), and e) concentrate the clarified liquid phase. As well as the extract obtained by said obtaining method, and the formulations comprising this extract. (Machine-translation by Google Translate, not legally binding)
    公开号:ES2569132A1
    申请号:ES201531951
    申请日:2015-12-31
    公开日:2016-05-06
    发明作者:José Antonio Novejarque Conde；José Vicente PONS RAGA
    申请人:Signes-Costa Minana Miguel；
    IPC主号:
    专利说明:

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    METHOD FOR OBTAINING EXTRACTS THAT INCLUDE HYDROXYCINAMIC COMPOUNDS FROM VEGETABLE WASTE
    TECHNICAL SECTOR
    The present patent application describes a method for obtaining extracts comprising hydroxycinmic acids such as ferulic, caffeic, p-coumaric or chlorogenic acid, from the waste generated in the commercial valuation of different plant species, in particular high plants economic interest, thus giving added value to this waste and obtaining products with reduced production costs.
    Additionally, the present patent application refers to the use of extracts obtained, alone or in combination with each other, in food, cosmetic or pharmaceutical applications.
    BACKGROUND
    The industrial revolution and the improvement of processes achieved throughout the twentieth century and up to the present, has resulted in the food industry in a great improvement of food preservation and the prolongation of their half-life, thus guaranteeing a better and greater availability of food and, therefore, a higher quality of life for a large percentage of the population, particularly in the western world.
    In parallel in the world of cosmetics and pharmacy, with the empowerment of the industry and the development of the synthesis of compounds in order to have a greater supply capacity and reach a greater number of population, those products from the plants were In oblivion
    Through the purification of food, heat treatments and the addition of additives obtained mostly by synthetic means, greater food preservation was achieved. However, the application of these processes also had negative consequences, in particular, the loss of minor components whose biological function was neglected or diminished, with the food industry concentrating only on macro constituents, that is, lipids, proteins and carbohydrates. On the other hand, in
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    Pharmaceutical and cosmetic industries developed, more than new molecules, molecules derived from those already known, modified in order to enhance their effects. However, compounds from natural sources were not considered, among other factors, because they were expensive.
    The plant world is characterized by being permanently exposed to the environment and, therefore, subject to the inclemency of it, the action and effects of solar radiation, the aggressions of changing environments, such as droughts, sunstroke, pathogen attacks , insects and predators, etc. Given its nature, the flight of plants to other areas is not feasible, and their survival depends on the ability to dispose or generate protective elements that allow them to withstand such circumstances. Therefore, practically all plant species have compounds or families of compounds with protective properties. Recent studies have shown that these compounds, currently known as Generic Phytochemicals, although not essential nutrients, are also useful for humans.
    The list of phytochemical compounds is very extensive, and among them the following groups stand out: terpenoids (isoprenoids), phenolic compounds, glucosinolates, betalains, chlorophylls, other organic acids and protease inhibitors. Among the phenolic compounds can be found natural monophenols, polyphenols or aromatic acids.
    The presence of phytochemical compounds in food depends on the state of preservation and the treatment to which these foods have been subjected.
    On the other hand, today's society is characterized by having acquired insane and unbalanced dietary habits, this being an important factor in the development of diseases such as obesity, diabetes, hypertension, cardiovascular problems, stroke, and various types of cancer. Various epidemiological and biochemical studies have shown that regular intake of natural foods is associated with the improvement of these conditions or diseases, as well! with those conditions linked to aging. The protection provided by fruits and vegetables has been attributed to the presence of antioxidant vitamins (groups C, E and provitamins A), although the latest studies indicate as responsible for these actions to phenolic compounds, very present in compound plants. (Garcia-Salas, Patricia et al., "Phenolic-Compound-Extraction Systems for Fruit and Vegetable Samples", Molecules 2010, 15, 8813-8826)
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    These phenolic compounds are widely distributed in plants and contribute to the organoleptic and nutritious quality of fruits and vegetables. In particular, they contribute to its color, taste, aroma, smell and are responsible for its astringency and bitterness. The degree of maturity and exposure to light of fruits and vegetables affect the content of phenolic compounds and, therefore, the quality and effects they produce. The chemistry of the phenolic compounds is very complex due to their great capacity to react with other compounds and with themselves, so they constitute a very complex group with strong synergistic actions, so that the effects detected are generally due to all the Phenolic compounds present in a product. Because of these characteristics, these phenolic compounds are referred to collectively as "polyphenolic compounds."
    Under the term polyphenol include more than 8000 compounds with a great structural diversity, although all of them have at least one aromatic ring with one or more 15 hydroxyl groups. Polyphenols can be divided into different classes depending on their basic structure; The main families are indicated in the following table:
     Carbon Number  Basic structure Class
     AC  <vJ ^ OH Simple phenols
     Benzoquinones
     0 O) 1 p  C ^ co ° h Benzoic Acid
     Ca-C2  Orr0 "- '- / 0 Acetophenones
     / = XOOH  Phenylacetic Acid
     Ca-C3    Cinnamic Acid
    image 1
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    Phenylpropene
    Coumarins
    Chrome
    C6-C4
    OR
    OR
    Naphthoquinones
    C6-C1-C6
    image4
    Xanthones
    C6-C2-C6
    image5
    image6
    Stilbenes
    Anthraquinones
    C6-C3-C6
    image7
    Flavonoids
    C6-C4-C6
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    Lignans, Noeolignans
    (C6-Cl) n
    Heterogeneous polymers composed of phenolic acids and simple sugars
    Hydrolysable Tannins
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    (C6-C2) n
    Highly linked aromatic polymers
    Lignins
    Polyphenolic compounds have been assigned anticarcinogenic, anti-inflammatory, antibacterial, regulatory activities of enzymatic activities and as potent antioxidants.
    Among the polyphenolic acids, two main groups stand out: those derived from benzoic acid (C6-C1) and those derived from cinnamic acid (C6-C3). These compounds appear predominantly, respectively, as hydroxybenzoic acids and hydroxycinmic acids, both in their free and conjugated form.
    Hydroxycinmic acids are considered structural and functional constituents of plant cell walls. Additionally, they are bioactive ingredients of the diet. Recent studies show its effects as preventive or therapeutic agents in certain diseases related to oxidative stress, such as atherosclerosis, inflammations or cancer, as well as important cardioprotective, anti-obesity and antidiabetic effects. Additionally, hydroxycinmic acids have very positive synergistic effects in many modern diseases. On the other hand, different studies show the dependence between the antioxidant capacity of hydroxycinmic acids and the position of hydroxyl groups in the structure, in particular, the presence of hydroxyl groups in the aromatic structure of these compounds results in a greater antioxidant capacity. .
    The family of hydroxycinmic acids is very extensive, which can be divided into 4 main subgroups: aglycones, esters, oligomeric forms and conjugates with co-enzyme A.
    In turn, the aglicons can be selected from the group consisting of cinnamic acid (the precursor of this family), monohydroxycinmic acids such as p-coumaric acid, o-coumaric acid and m-coumaric acid; dihydroxycinnamic acids such as caffeic acid (3,4-dihydroxycinnamic acid), umbellic acid (2,4-dihydroxycinnamic acid), 2,3-dihydroxycinnamic acid, 2,5-dihydroxycinmic acid and 3,5-dihydroxycinmic acid; trihydroxycinnamic acids such as 3,4,5-trihydroxycinnamic acid and 3,4,6-trihydroxycinnamic acid; O-methylated forms such as ferulic acid, 5-hydroxyiferulic acid and synaptic acid; and others such as Plicatin A and Plicatin B.
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    On the other hand, the subgroup of esters can be selected from the group consisting of glucoside type esters, tartaric acid esters, other caffeic acid esters and coffeeoyl phenylethanoid glycosides (GPGs), Caffeoyl phenylethanoid glycoside. In turn, glycoside-type esters can be selected from the group consisting of esters of caffeic acid with cyclic and glucosides. More specifically, the esters of caffeic acid with cyclics can be selected from the group consisting of esters of qulnic acid such as chlorogenic acid (3-caffeoylquinic acid), cryptochlorogenic acid (4-O-caffeinoquinic acid), neochlorogenic acid (acid 5-O-caffeinoquinic), cyanarine (1,5-dicaphenoquinic acid), 3,4-dicaphenoxyulic acid and 3,5-dicafeoylqulnic acid; and esters of shiklmico acid such as finger acid (3-O-caffeoylshiklmico acid). On the other hand, the glucosides can be selected from the group consisting of ferulic acid glucoside, p-coumaric acid glucoside and 1-sinapoyl-D-glucose.
    The esters of tartaric acid can be selected from the group consisting of caffeic acid, cyclic acid (dicafeoyltartaric acid), coutaric acid, fertile acid and glutathic conjugated coffee acid (reaction product of the grape). The other esters with caffeic acid can be selected from the group consisting of caffeilyl acid, ethyl caffeine, methyl caffeine, phenethyl ester of caffeic acid (CAPE according to its acronym in English, Caffeic acid phenethyl ester) and rosmarlenic acid (acid ester lactic with 3,4-dihydroxyphenyl).
    Phenylethanoid glycosides of caffeine (CPG) can be selected from the group consisting of equinacoside, calceolarioside A, B, C and F, chiritoside A, B and C, cystanoside A, B, C, D, E, F, G and H , conandroside, myconoside, pauoifloside, plantainoside A, plantamajoside, tubulosiede B, verbascoside such as isoverbascoside and 2'-acetylverbascoside.
    The hydroxycinmic acids included in the subgroup of the oligomeric forms can be selected from the group consisting of dimer, in particular, diferulic acids (DIFA according to its acronym in English, diferulic acids) such as 5,5'-diferulic acid, acid 8- O-4'-diferulic acid, 8,5'-diferulic acid, 8,5'-DIFA (DC), 8,5'-DIFA (BF) and 8,8'-diferulic acid; trimers, in particular, triferulic acids such as 5-5 ', 8'-O-4 "-triferulic acid; and tetramers such as tetraferulic acids.
    Finally, conjugates with coenzyme A can be selected from the group consisting of caffeoyl-coenzyme A, cinnamoyl-coenzyme A and cumaryl-coenzyma A.
    Among the hydroxycinmic acids mentioned above, the most important and significant are caffeic, chlorogenic, ferulic, synaptic and p-coumaric acids; Its chemical structures are presented below. The presence of these compounds and their concentration is used as a therapeutic or biological action indicator studied, although the 5 effects are generally due to the synergistic action of these compounds and other hydroxycinmic derivatives that are usually present in smaller amounts.
    image9
    OCH3
    OH
    HO-C H
    cffeic acid
    ferulic acid

    HOOC-
    OH
    chlorogenic acid
    synaptic acid
    p-cumanco acid
    10 For all the properties noted there has been renewed interest in hydroxycinmic acids in dietary and nutritional applications in the sector of functional nutrition, in the pharmaceutical sector due to its therapeutic effects, and in the cosmetic industry for its antioxidant properties and as UV protectors.
    15 As mentioned above, hydroxycinmic acids are widely distributed in plants. However, its presence occurs in very low proportions in relation to the total mass of the vegetable, so that only a regular and significant consumption of products rich in these compounds allows to guarantee an adequate intake to achieve the desired protective effects.
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    Many of the widely extended crops for food production are of species that possess, in addition to their own nutritional elements, relatively high levels of polyphenol compounds. Most food products of this type are subjected to industrial transformations, in order to improve their half-life and facilitate distribution to a wider segment of the population.
    The beneficial effects of the polyphenolic compounds they possess require regular and significant consumption of significant quantities of the product, since otherwise the necessary doses to obtain are not reached. That is why every day is more frequent reinforcement of products made with selective ingredients that allow to reach the necessary doses more easily; alternatively, other products that complement it with the same effects are incorporated into the diet.
    However, obtaining polyphenolic compounds such as hydroxycinmic acids for the enrichment of other compositions is an expensive process due to the low availability of plant materials suitable for effective extraction, as well as the high price of the product harvested due to at its highest profitability as a base food.
    The industrialization of the production of plant-based foods is focused on the manipulation, conservation and preparation of the part of the plant that is likely to be consumed, so that significant amounts of waste are generated that frequently cause environmental problems and whose use results complicated and inefficient. Depending on the species considered, the amounts of waste generated can vary from 25% to 85%, (MT Torres-Mancera et al. '' Enzymatic Extraction of hydroxycinnamic acids from Coffee Pulp ”, Food Technol. Biotechnol. (2011) 49 (3) 369-373; Gaafar, AA et al., Phenolic Compounds from Artichoke (Cynara scolymus L.) Byproducts and their Antimicrobial Activities, Journal of Biology, Agriculture and Healthcare, Vol. 3, No.12, 2013, 1-7; Usman A. et al., "Effect of Soxhlet and ultrasound assisted extraction on antioxidant activity of pomegranate peel extract", International Journal of Food and Nutritional Sciences (IJFNS), Vol. 3, Iss. 6, Oct -Dec 2014; Sumaya-Martlnez, Ma. T. et al. "Mango Value Network and its wastes based on Nutritional and functional properties." Mexican Journal of Agribusiness. Fifth Time. Year XVI. Volume 30. January- June 2012) being therefore very important volumes.
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    In the industrialization of a product of plant origin, the highest costs correspond to the valuation of the raw material in the field, but the costs associated with the collection, classification, transport and handling of these foods are more important every day. In the method described in this patent application, raw materials generated during the preparation and manipulation of the food product of plant origin are used as raw material. In this way, the main cost factors are absorbed by the food product that is going to be produced, that is, the fruit or vegetables harvested, and the costs associated with the work of collecting and concentrating the residual plant mass, raw material of the method of the present invention, are reduced to the industrial environments where the food is processed.
    In the state of the art, extracts comprising polyphenolic derivatives obtained from plant material are known. For example, US patent application 2004/0097584 A1 describes the stimulation of T lymphocytes from one or more plant extracts containing chlorogenic acid or its functional derivatives, mentioning as plants of origin Echinacea, Ginseng, Green Coffee, Cocoa Green, hawthorn, green tea, artichoke, elderberry, arnica, Phoenix spp, Butia Capitata, dandelion, mixtures of dicotylus and birch. However, this application is based on the entire plant and no extractive process or specific concentration is described.
    On the other hand, patent application US 2011/0237533 A1 describes the production of a new polyphenolic complex that inhibits lipase activity, as well as its use in food and pharmaceutical preparations, but they are obtained by combining them. / reaction of a natural compound rich in flavonoids with others rich in derivatives of caffeic, gallic or chlorogenic acid, and / or derivatives of catechin reacting with polyphenoloxidase.
    In the application WO 98/01143 new uses of artichoke extracts combined with other derivatives of echinacea for the treatment of diseases or as palliative of other treatments or adjuvants in other aggressive treatments are established. However, in this application the source is not specified, that is, which part of the artichoke is used as the starting product, nor the way of obtaining the extracts.
    The application WO 2008/105023 (EP 2131681 B1) describes a process for obtaining purified extracts from the residues of the industrialization of the artichoke.
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    Additionally, this application describes the use of the extract obtained in both food and cosmetics and pharmacy.
    On the other hand, the application WO 2013/088203 A1 describes the obtaining of a concentrate obtained from the washing waters generated with the wet coffee cherry benefit, rich in sugars and with the aim of obtaining a sugar syrup with certain antioxidant properties This patent application focuses on the factors of waste utilization as a way of reducing the environmental cost through the recycling of solids as fertilizers.
    WO 2014/0830032 A1 establishes a process for obtaining pectin from green coffee cherry by extraction and enzymatic treatment.
    Various patents WO 2006/093114 A1 and WO 2011/155505 A1, from 2006 and 2011 respectively, deal with the preparation of chlorogenic acid preparations, without cafelna, from green or roasted coffee beans.
    With CN 103520228 A published in 2014, it is about using raw mango extracts as a basis for the preparation of medications with cardiovascular activity.
    Finally, the CN patent 16344853 A of the year 2005 tries to establish the residue of tobacco production as an alternative source of obtaining chlorogenic acid by extracting the residual material and subsequent purification for obtaining the purified product by means of ultrasonic and microwave techniques and solvents selective.
    The patent CN 103204765 A, tries to obtain simultaneously solanesol and chlorogenic acid with hydroalcoholic extraction and subsequent filtration with ceramic membranes, selective redisolutions and the use of column chromatography.
    DESCRIPTION
    In a first aspect, the present patent application refers to a method for obtaining an extract comprising hydroxycinmic acids, characterized in that the method uses as one raw material one or more plant residues of the preparation of plant food products, and comprises:
    a) select at least one residue of at least one plant species,
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    b) extract the hydroxycinmic acids present in the residue by a technique selected from the group consisting of washing, decoction, maceration, percolation and any combination of the above,
    c) separating the main liquid phase comprising the compounds extracted from solids with a size greater than 2 mm,
    d) clarify the liquid phase obtained in step c), and
    e) concentrate the clarified liquid phase.
    The method described in the present invention allows obtaining an extract comprising hydroxycinmic acids. In particular, the method of the present invention allows obtaining an extract with an enrichment of at least 5 times with respect to the concentration of hydroxycinmic acids present in the residue used as the starting material, where the proportion of the different hydroxycinmic acids will depend to a large extent. of the plant species or species used as the starting product.
    Ace! Thus, the method of obtaining an extract comprising hydroxycinmic acids described in this patent application uses as a raw material a residue from the processing or industrial use of plant food products such as fruits or vegetables. In particular, the raw materials used can be the skins, leaves, stems, bracteas, pulp, wrappers, rejected product and in general the remains of the processing of the vegetal species to consider. Generally, the amount of polyphenolic compounds, in particular hydroxycinmic acids, of these waste materials may vary with respect to the food itself, being in some cases smaller, while in other cases the content of these compounds may be the same or even higher in the material. of residue that in the vegetable, fruit or stem of the plant used as food.
    The choice of the plant species, or the combination of species, is initially conditioned by the activity of interest in the extract obtained. The activity of the compounds called hydroxycinmic acids and their derivatives is every source of new discoveries, since their antioxidant properties and biological activity make them very interesting in many applications. In particular, in the food sector these compounds can improve the taste properties of a food, for example, by acting as flavor enhancers or taste masks; ace! they can also exercise protective functions, for example, as antioxidants, free anti-radicals, etc. On the other hand, in the cosmetics and pharmacy sectors, acids
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    Hydroxycinnamics are interesting because of their ability to boost the immune system, or act as an anticarcinogenic, cardioprotective, anidiabetic, etc.
    The therapeutic effects mentioned above are a consequence of the synergistic activity of the group of hydroxycinmic acids, and sometimes also in combination with other polyphenolic compounds, which are found in a plant. In fact, it is sometimes beneficial to obtain a combination of extracts from different plants, because better results are obtained by combining the action of the different molecules in each of these extracts. As mentioned above, compounds that act as indicators or markers of the concentration or richness of antioxidant compounds and therefore of the expected action can be identified, being the most commonly used hydroxycinmic acids for this purpose: chlorogenic acid, caffeic acid, ferulic acid and p-coumaric acid. Among these, the most commonly used as a marker is chlorogenic acid, although under this denomination the chlorogenic acid itself and those other compounds with similar functional properties (in general esters of qulnic acid) are generally collected.
    The preferred plant species for use as a raw material in the method of the present invention are those that have hydroxycinmic acids among their major compounds and, additionally, there is at least one industrialization process associated with the exploitation of said plant species and, as a result, residues derived from this industrialization process concentrated at the transformation point can be obtained. In this way, the method described in this patent application allows obtaining an extract comprising hydroxycinmic acids at a reduced cost, while increasing the profitability of the industrialization process of the plant species in question and contributing to eliminating or reduce the environmental impact of said industrialization process, by revaluing the waste obtained in said process.
    These waste materials can be skins, leaves, stems, bracteas, pulp, wrappers, rejected product and, in general, any vegetable waste obtained during the processing of the plant species.
    Consequently, the preferred plant species for use in the method of obtaining an extract comprising hydroxycinmic acids are the artichoke (Cynara scolymus), in which processing is generated more than 75% of remains of bracteas, receptacle leaves and stems; the eggplant (Solanum Melongena) and in general the solanaceas, since you can
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    use the skin, leaves and stems as a starting residue in the method of the invention; green coffee (Coffea arabica) and Maqui (Aristotelia chilensis), whose processing results in berries, cherries, pulp and mucllagos as usable residues in the method of the present invention; the pomegranate (Punica granatum) and the mango (Mangifera indica L.), from which you can take advantage of the skin, bark and pulp; and tobacco (Necotiana tabacum), since the leaves, dust, logs and rejection material obtained in its processing can be used as a starting material in the method of the present invention. Additionally, residues obtained in the processing or industrial use of blueberries, acai, Goyi berry, acerola, noni, pear, mangostan, cabbage, coliarabano, bimi (broccolini), black garlic, mate, celery and can also be used as raw material. the plants of the sage group.
    In order to ensure that plant residues are suitable for use as a raw material in the method of the present invention, they are preferably subjected to a quality control analysis prior to their use. This analysis can include the determination of its activity in water, the state of maturity and conservation of the residual material, the presence of esters free of degradation and contamination.
    The plant residues that constitute the raw materials of the method of the invention are preferably subjected to a pre-treatment prior to step b) to facilitate the extractive process. In particular, this waste can be partially dried to facilitate its manipulation, which can be done naturally, that is, solar drying, or artificial drying by air flow at a temperature not exceeding 75 ° C, preferably below 50 ° C. Preferably, this drying process takes place until the residue reaches a humidity of less than 70%, preferably between 40-50% even more preferably less than 40%, amounts expressed in percentage of water by weight with respect to the total weight of the residue.
    Additionally, in order to improve the contact surface during the extraction process and, consequently, to improve the effectiveness of this process, the pre-treatment may comprise cutting up the plant residues at a particle size of less than 10 cm, preferably between 2 -4 cm, more preferably less than 20 mm and ideally less than 10 mm.
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    For residual materials from the pulping of berries or cherries, these materials are preferably used directly, or they are chopped in wet, that is, in the presence of water, in order to increase the efficiency of the extraction process.
    The extraction of the hydroxycinmic acids is carried out by washing, decoction, maceration and / or percolation of the optionally pre-treated residues as indicated above. This extraction can take place with a pure solvent or with a mixture formed by two solvents selected from the group consisting of water, methanol, ethanol, acetone and ethyl acetate. Preferably, water or a mixture of solvent and water is used in solvent: water proportions that can vary from 20: 1 to 1:20; preferably from 10: 1 to 1:10 and more preferably from 5: 1 to 1: 2. The extraction solutions can be neutral, acidic or basic, by adding an amount between 0 and 5%, preferably between 0 and 2% of a reagent selected from the group consisting of hydrochloric acid (ClH), acetic acid (AcH) , caustic soda (sodium hydroxide: NaOH), ammonia (NH3) and potassium hydroxide (KOH), even calcium or sodium carbonate can be used for the same purpose, and adjusting the final pH between 3-10.
    The temperature of the extraction process can vary between 15 ° C and 95 ° C, preferably between 20 ° C and 65 ° C, the contact times may vary between 15 minutes and 5 hours, preferably between 1 and 2 hours. Optionally, techniques of MAE (microwave) or with greater frequency of UAE (ultrasound) can be used using ultrasonic frequency between 20 and 40 kHz, and intensity between 10-30 W / cm2, optionally with pulses programmed with cycles of up to 10- 6 sec and contact times less than 1 hour.
    After the extraction process, the solution is subjected to a roughing process in order to separate the main liquid phase comprising the compounds extracted from the solids with a size larger than 2 mm, to make this separation a vibrating screen can be used or a basket centrifuge with porosity equal to or greater than 2 mm.
    The solids separated in this stage c) can be subjected to a second extractive stage, preferably with the same conditions as the first one carried out in stage b) of the method described in this patent application. Once this second extraction is finished, the secondary liquid phase is separated from the solids with a size greater than 2 mm, for which a vibrating screen or a basket centrifuge with porosity equal to or greater than 2 mm can also be used, and mixed the secondary liquid phase with the main fraction obtained above.
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    The liquids obtained after step c) of roughing can be cooled to a max. of 43 ° C, if necessary, and subsequently subjected to clarification by means of, for example, the use of centrifuges of aita efficacy, ultracentrifugation or filtration with polymeric paper or membranes or not and preferably tangential filtration.
    The filtered solution can be concentrated by vacuum evaporators, either simple boilers or preferably vacuum evaporation systems of descending or ascending film, with or without the aid of agitation and at temperatures below 70 ° C, preferably below 45 ° C.
    This step of concentration continues until obtaining an extract comprising hydroxycinmic acids, preferably as major components, until obtaining the concentration required for the final application of the extract; preferably varying from 50% by weight of solids with respect to the total weight of the concentrated extract, to dryness. In those starting materials that comprise a high sugar content, the final concentration of the extract is preferably established so that it provides a minimum of 66 ° Brix in sugars.
    The extract obtained by the method described in this patent application can be used directly in liquid form, or it can be dried to form powder, for example using spray drying techniques. If so, it is preferred to add maltodextrins prior to the drying stage to improve its texture and stability of the powder obtained.
    In most applications the quality obtained by the extraction method described in this patent application is sufficient and allows a broad spectrum of use. However, for some particular applications, a higher degree of purity or concentration of hydroxycinmic acids may be required, in this case it is possible to understand the dry concentration of the extract in step e), the redisolution of the concentrate obtained in ethyl acetate, the subsequent concentration of hydroxycinmic acids through the use of macroporous chromatographic resins, and elution with alcoholic alcohol at a richness of 55-65% and after adjusting the pH to 3-3.5 using hydrochloric or acetic acid, which allows a more selective extraction, filtering of the solution obtained and crystallization of its components leaving it static for 12 hours. Until reaching room temperature.
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    The present invention also relates to extracts comprising hydroxycinmic acids, preferably in an amount at least 5 times greater than their concentration in the residue used as the starting material. In particular, this extract may comprise as major components one or more hydroxycinmic acids selected from the group consisting of caffeic acid, chlorogenic acid, ferulic acid, synaptic acid and p-coumaric acid.
    Additionally, these extracts may comprise other active ingredients such as amino acids, vitamins, minerals and phytochemical compounds chosen depending on the final application of the extract. These active ingredients can be derived from the vegetable residue used as a starting product in the method of the invention, or they can be added later in some of the steps of the method described in this patent application.
    Additionally, the present invention also relates to the use of extracts obtained by the method described in this patent application in the food, pharmaceutical or cosmetic industry. In particular, they can be used in the food sector to improve the taste properties of a food, for example, acting as flavor enhancers or taste masks; ace! they can also exert protective functions of the food, for example, as antioxidants, free anti-radicals, etc. On the other hand, in the cosmetics and pharmacy sectors, the extracts obtained by the method of the present invention can be used to boost the immune system, or to act as an anticarcinogenic, cardioprotective or antidiabetic.
    The present invention also relates to a formulation, in particular a food, cosmetic or pharmaceutical formulation, comprising the extract obtained by the method described in this patent application. This formulation may additionally comprise other active ingredients such as, for example, amino acids, vitamins, minerals and phytochemical compounds chosen depending on the final application of the formulation.
    This pharmaceutical formulation can be a product designed to be applied in orthomolecular medicine, that is, special products dedicated to cell rehabilitation, providing the necessary nutrients for the body. Orthomolecular medicine originated with the French biologist Louis de Brouwer, doctor of medicine and molecular biologist, international consultant for Health and Oncology at the UN and UNESCO. The
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    Orthomolecular fundamentals are based on the work of four exemplary scientists: Alvert Szent Gyorgi, Otto Warburg, Everett Storey and Linus Pauling, who share 7 Novel awards.
    Likewise, the present patent application also refers to the extract obtained by the procedure described, or a formulation comprising said extract, for use in medicine. In particular, to use in the treatment or prevention of a disease that requires boosting the immune system, or to treat or prevent cancer, cardiovascular disease or diabetes.
    These formulations can be obtained by mixing and homogenizing the different ingredients that comprise them in suitable facilities for this. Particularly in cleanrooms that comply with GMP standards, DIN EN ISO 16644-1.
    In some embodiments of the present invention, the formulation can be obtained by a supercritical fluid system and process, to obtain a quality and purity of the final components that meet particular needs required by certain.
    Mixing and homogenization of the different ingredients in the formulation can be done by applying ultrasound. Preferably, for a time interval of 16 to 60 minutes, at a temperature between 14 and 33 ° C.
    Once all the ingredients have been mixed and homogenized, the quality controls that guarantee the quality of the product are generally carried out. Preferably, these controls include: determining the interaction between the components of the formulation (existence of synergism); pH control, redox potential and environmental factors such as light, air, etc; Determine the TROLOX / DPPH / ORAC / FRAF Indices, rule out the possible interaction of the extract with the container that will contain the formulation.
    Examples
    Example 1: Obtaining an extract comprising hydroxycinmic acids from artichoke leaves
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    For the realization of this example, gills and basal leaves of the artichoke were selected as raw material. The extraction of hydroxycinmic acids was carried out at 75 ° C, by recirculation of water. Subsequently, the main liquid phase of the solids with a size greater than 2 mm was separated and a second extractive stage was carried out from the separated solids, at 75 ° C and by means of water recirculation. After the extraction, the solids with a size greater than 2 mm were separated and the extracted liquid phase was combined with the main liquid phase obtained after the first extractive stage.
    Next, the mixture of liquid phases extracted by conventional filtration was clarified using a filter press, and concentrated in vacuo to obtain a 50% w / w solution of solids. This concentration stage was carried out at a maximum temperature of 70 ° C and using vacuum (less 50 mbar). In this way, an extract with a minimum richness of 4.5% chlorogenic acid was obtained.
    For those applications that require a dry product, the concentrated extract obtained in the previous stage can be dried in a vacuum tray oven.
    Example 2: Water Cell Repair Bano Gel 54.4%
    Surfactants 40%
    Thickeners 3%
    Conservative 0.1%
    Perfume 0.7%
    Active ingredients 0.8%
    (*) Extract comprising 1% hydroxycinmic acids
    Example 3: Anti-aging Serum energize you Water 87.95%
    1% thickener
    3% glycerin
    Conservative 0.05%
    Distilled water of orange blossom 3%
    Active ingredients 3%
    (*) Extract comprising 2% hydroxycinmic acids
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    Example 4: Tomato Drink Tomato juice 95.90%
    1% lemon juice
    0.7% Tabasco
    Celery Salt 0.4%
    (*) Extract comprising 2% hydroxycinmic acids
    Example 5: Soluble coffee with and without caffeine
    Dry Coffee Extract 98.90% (obtained by atomization or lyophilization)
    Vitamins E and B1 (Thiamine) 0.4%
    400mg magnesium
    (*) Extract comprising 0.7% hydroxycinmic acids
    Soluble coffee with caffeine contains> 0.3%, and soluble coffee without caffeine (decaffeinated) contains <0.3%, in both cases with a maximum of 5% humidity.
    Example 6: Food supplement in capsules Two vegetable capsules provide:
    Vehicles (microcrystalline cellulose-vegetable magnesium stearate)
    Vegetable capsule of hydroxypropyl methyl cellulose Plant extracts and healthy active ingredients
    Vegetable powder base (boldo extract, ginko biloba extract, spirulina seaweed) 60mg
    Vegetable antioxidants / (*) Extract comprising 100mg hydroxycinmic acids
    Tocopherol Blend 21mg
    Zinc 7mg
    Riboflavin 5mg
    Copper 1000 micrograms
    Selenium 50 micrograms
    (*) The extract used in examples 2 to 6 was obtained following the method described in example 1.
    权利要求:
    Claims (14)
    [1]
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    1. - A method for obtaining an extract comprising hydroxycinmic acids, characterized in that the method uses as raw material one or more plant residues from the preparation of plant food products, and comprises:
    a) select at least one residue of at least one plant species,
    b) extracting the hydroxycinmic acids present in the residue by means of a technique selected from the group consisting of washing, decoction, maceration, percolation and any combination of the above,
    c) separating the main liquid phase comprising the compounds extracted from solids with a size greater than 2 mm,
    d) clarify the liquid phase obtained in step c), and
    e) concentrate the clarified liquid phase.
    [2]
    2. - The method for obtaining an extract according to claim 1, wherein the vegetable waste used as raw material comes from the processing or industrial use of plant food products.
    [3]
    3. - The method for obtaining an extract according to claim 2, wherein the vegetable residue used as raw material is selected from the group consisting of skins, leaves, stems, bracteas, pulp, wrappings and rejected product.
    [4]
    4. - The method for obtaining an extract according to any one of claims 1 to 3, wherein the plant residue is from one or more species selected from the group consisting of artichoke (Cynara scolymus), eggplant (Solanum melongena), green coffee ( Coffea arabica), Maqui (Aristotelia chilensis), pomegranate (Punica granatum), mango (Mangifera indica L.), tabacco (Nicotiana tabacum) and any combination of the above.
    [5]
    5. - The method for obtaining an extract according to any one of claims 1 to 4, which comprises an additional stage of pre-treatment of the plant residue before step b) of extraction.
    [6]
    6. - The method of obtaining an extract according to claim 5, wherein the pre-treatment comprises drying the vegetable residue to a humidity below 70%.
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    [7]
    7. - The method of obtaining an extract according to any one of claims 5 to 6, wherein the pre-treatment comprises cutting the vegetable residue at a size of less than 10 cm.
    [8]
    8. - The method for obtaining an extract according to any one of claims 1 to 7, wherein the extraction step takes place in water or in a solvent / water mixture, wherein the solvent is selected from the group consisting of methanol, ethanol, acetone and ethyl acetate.
    [9]
    9. - The method of obtaining an extract according to any one of claims 1 to 5, wherein the extraction step takes place between 15 ° C and 95 ° C.
    [10]
    10. - The method for obtaining an extract according to any one of claims 1 to 9, wherein the solids separated in step c) are subjected to a second extraction under the same conditions of the extraction performed in step b), is separated the secondary liquid phase of the solids with a size greater than 2 mm, and this secondary liquid phase is mixed with the main liquid phase obtained above.
    [11]
    11. - The method for obtaining an extract according to any one of claims 1 to 10, comprising an additional stage f) wherein the concentrated liquid of step e) is transformed into powder by a spray drying technique.
    [12]
    12. - Extract comprising hydroxycinmic acids obtained by the method described in any one of claims 1 to 11.
    [13]
    13. - A formulation comprising the extract comprising hydroxycinmic acids described in claim 12
    [14]
    14. - Formulation according to claim 13 which additionally comprises one or more active ingredients selected from the group consisting of amino acids, vitamins, minerals and phytochemical compounds.
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    同族专利:
    公开号 | 公开日
    US20190000787A1|2019-01-03|
    ES2569132B1|2017-02-15|
    EP3398453A1|2018-11-07|
    WO2017114992A1|2017-07-06|
    MX2018008077A|2018-08-23|
    EP3398453A4|2019-08-21|
    BR112018013345A2|2018-12-11|
    US10736862B2|2020-08-11|
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    CN103204765B|2013-01-30|2014-03-05|湖南中烟工业有限责任公司|Method for extracting solanesol and chlorogenic acid from discard tobacco leaves|
    CN103520228B|2013-06-11|2016-06-29|浙江大学|Fructus Mangifera Indicae crude extract is preparing medicine and the food applications of prevention and cure of cardiovascular disease|
    CN104418741B|2013-08-30|2016-03-16|中国科学院烟台海岸带研究所|A kind of method of chlorogenic acid extracting and purifying from leaf of canada potato|
    法律状态:
    2016-08-31| PC2A| Transfer of patent|Owner name: MARIA VICTORIA MARTIN LAGUARDA Effective date: 20160825 |
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    优先权:
    申请号 | 申请日 | 专利标题
    ES201531951A|ES2569132B1|2015-12-31|2015-12-31|Method for obtaining extracts comprising hydroxycinmic compounds from plant residues|ES201531951A| ES2569132B1|2015-12-31|2015-12-31|Method for obtaining extracts comprising hydroxycinmic compounds from plant residues|
    US16/066,931| US10736862B2|2015-12-31|2016-12-28|Method for producing extracts containing hydroxycinnamic compounds from vegetable waste products|
    PCT/ES2016/070941| WO2017114992A1|2015-12-31|2016-12-28|Method for producing extracts containing hydroxycinnamic compounds from vegetable waste products|
    MX2018008077A| MX2018008077A|2015-12-31|2016-12-28|Method for producing extracts containing hydroxycinnamic compounds from vegetable waste products.|
    EP16881315.2A| EP3398453A4|2015-12-31|2016-12-28|Method for producing extracts containing hydroxycinnamic compounds from vegetable waste products|
    BR112018013345-0A| BR112018013345A2|2015-12-31|2016-12-28|method for obtaining an extract comprising hydroxycinnamic acids, extract and formulation|
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