A process for preparing a totum or filtrate that allows for the stabilization of fresh plant material.

The described process integrates fresh plant material with fat at room temperature to create a totum or filtrate, addressing the degradation issues in existing methods by maintaining biological activities and reducing energy costs, thereby enhancing the value of plant materials.

FR3110342B1Active Publication Date: 2025-04-25ID4FEED
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Patent Information

Application Number
FR2020005403
Authority / Receiving Office
FR · FR
Patent Type
Patents
Current Assignee / Owner
Filing Date
2020-05-21
Publication Date
2025-04-25
Estimated Expiration
2040-05-21

AI Technical Summary

Technical Problem

Existing methods for preparing plant materials result in significant loss and degradation of active compounds due to drying and storage processes, which are costly in energy and time, and do not effectively preserve the biological and chemical properties of fresh plant materials.

Method used

A process involving the immediate integration of fresh plant material with a fat at room temperature, including grinding and dehydration steps to create a totum or filtrate, maintaining biological activities by minimizing oxidation and degradation.

Benefits of technology

The process effectively stabilizes the metabolic wealth of plant matter, reducing energy costs and preserving biological properties, while allowing for easy implementation and adaptation to various plant materials, thus enhancing the value of co-products.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to a process for preparing a totum, which is a mixture of plant material with a solid or liquid fat. The invention is characterized in that it comprises the following steps, according to which: a. fresh plant material, comprising at least 10% water by weight of its total weight before or after loss on drying, taken alone or in mixtures, whole or in part, is brought into contact with the fat, selected from a hydrogenated or non-hydrogenated oil or fat, at a temperature between 50°C and 180°C; b. the plant material-fat mixture is then ground at said temperature between 50°C and 180°C; and c. a solid or liquid totum at room temperature, with a water concentration less than or equal to 4% by weight of the total weight of the totum, is recovered. The invention also relates to the totum or filtrate thus obtained and their uses. Figure 2
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Description

Title of the invention: Process for preparing a totum or a filtrate allowing the stabilization of fresh plant material Technical field

[0001] The present invention relates to a process for preparing a solid or liquid totum or filtrate at room temperature, from fresh plant material and fatty material, as well as the water-depleted totum or the liquid or solid filtrate capable of being obtained according to said process, and their uses.

[0002] A totum can be defined as a mixture of at least one plant material with at least one fat that is solid or liquid at room temperature. The totum thus comprises active compounds or metabolites, in particular extracted from the plant material and which can be partly transferred into the fat and partly into the plant residue.

[0003] Natural active compounds or metabolites are molecules originating from a plant material or part of a plant material, the biological and technological activities of which have been demonstrated and described in the literature. These natural active compounds may be in pure form or contained in extracts in which the residue and solvent are separated. The interest of these active compounds may be established in the context of food and / or well-being and / or human or animal health. Their use as additives may encompass different objectives, such as in particular: - improving health (antioxidant, anti-inflammatory, antimicrobial compounds in particular, alkaloids and polyphenols); - improving palatability (compounds increasing palatability such as aromatic compounds, terpenes or pigments such as carotenoids or chlorophylls); and - contribution to nutrition (nutrients such as proteins, amino acids, vitamins, trace elements, etc.).

[0004] Natural metabolites of plant origin to which it is possible to attribute biological activities of interest in human or animal food and health can belong to different families of molecules. They are mainly secondary metabolites, which, unlike primary metabolites, are directly non-essential to the nutrition, growth and development of the plant (Verpoorte, 2000, Secondary metabolism, In Metabolic engineering of plant secondary metabolism (p. 1-29), Springer, Dordrecht). These are compounds whose biosynthetic pathways are quite specific to a taxonomic group and which generally participate in the mechanisms of interaction between the plant and its environment (defense, resistance and responses to abiotic and biotic stresses, symbioses, allelopathy, etc.).

[0005] There are different families of secondary metabolites of interest in food and animal health.

[0006] First of all, alkaloids (generally alkaline compounds containing at least one nitrogen atom). These are compounds which generally have significant biological activity, in particular an action on the central and / or peripheral nervous system (stimulant or depressant), in particular as anesthetics, as hypertensives or antihypertensives, as antimalarials or even as anticancers.

[0007] Alkaloids are generally grouped according to their nucleus (non-heterocyclic, derived from indole, pyrrole, pyridine, tropane, etc.). Among the alkaloids, we find well-known molecules such as caffeine, morphine, piperine, nicotine, atropine, scopolamine and quinine.

[0008] Capsaicinoids, including capsaicin and dihydrocapsaicin, can represent up to 90% of total capsaicinoids. These are the active components of chili peppers that belong to the benzylamine alkaloid group. Consuming capsaicin activates TRPV1 receptors, which trigger a burning sensation. It also stimulates the production of two hormones, adrenaline and noradrenaline, and therefore has therapeutic value given its anti-inflammatory, antioxidant, and analgesic properties (Zimmer et al., 2012, Antioxidant and anti-inflammatory properties of Capsicum baccatum: from traditional use to scientific approach. Journal of Ethnopharmacology, 139(1), 228-233).

[0009] Then the carotenoid type pigments (yellow, orange or red tetraterpenes), including carotenes, composed solely of carbon and hydrogen and xanthophylls, which also have oxygen atoms.

[0010] Chlorophylls (a, b, cl, c2 and d) are pigments present in all green plants (terrestrial and aquatic). Chlorophyll a (C55H72O5MgN4) remains the form mainly found in plant leaves.

[0011] Anthocyanins are water-soluble pigments (oxygenated glycosides) that range from red to blue.

[0012] Curcuminoids (orange pigments from the rhizome of Curcuma longa), have been shown to significantly decrease concentrations of C-reactive protein, an important factor in inflammation (Sahebkar, Are Curcuminoids Effective C-Reactive Protein-Lowering Agents in Clinical Practice? Evidence from a Meta-Analysis, Phytother Res, 2013 Aug 7).

[0013] Flavonoids can range from red to ultraviolet color depending on the pH and correspond to two aromatic cycles linked by three carbons.

[0014] These different classes of pigments mainly have effects of regulating inflammation, protection against light and also act as as antioxidants (powerful anti-free radicals) (Stahl and Sies, Bioactivity and protective effects of natural carotenoids. Biochimica et Biophysica Acta (BBA)-Molecular Basis ofDisease, 1740(2), 101-107).

[0015] The interest in their use in animal feed is in particular to couple their antioxidant activities with their participation in improving the visual quality (coloring and appearance) of the product formulation, as well as in the coloring and preservation of animal products (flesh, eggs).

[0016] Terpenes are also interesting secondary metabolites. They are volatile compounds whose structure corresponds to an aromatic cycle and which possess hydroxyl and terpenoid groups. They are at the origin of the aromatic properties of certain plants depending on their taxonomy. According to the literature, there are approximately 25,000 different terpene structures.

[0017] Added to this are the properties of another family which are essential components of essential oils: phenols.

[0018] Phenols are the metabolites that give essential oils their very characteristic odor and biological activities.

[0019] For example, oregano essential oil is composed mainly of thymol (monoterpenoid phenol) and its isomer, carvacrol and y-terpinene, the presence of which gives the essential oil its antioxidant and antimicrobial properties.

[0020] Natural compounds of plant origin have very wide applications in the fields of cosmetics and perfumery, but also in human and animal health and nutrition. Prior art

[0021] Obtaining them generally involves first harvesting, drying, storing and packaging the raw plant material.

[0022] The drying phase is a critical phase for any plant metabolite (Mediani et al., 2014, Effects of different drying methods and storage time on free radical scavenging activity and total phenolic content of Cosmos caudatus, Antioxidants, 3(2), 358-370).

[0023] It has been shown that a very significant loss of the active molecules contained in the plant (evaporation, degradation, metabolization) was observed during this drying step, consequently reducing the biological activity potential of the plant (antioxidants, antimicrobials for example) (Lim and Murtijaya, 2007, Antioxidant properties of Phyllanthus amarus extracts as affected by different drying methods, LWT-Food Science and Technology, 40(9), 1664-1669; Al-Farsi et al., 2005, Comparison of antioxidant activity, anthocyanins, carotenoids, and phenolics of three native fresh and sun-dried date (Phoenix dactylifera L.) varieties grown in Oman, Journal of agricultural and food chemistry, 53(19), 7592-7599).

[0024] The degradation of certain molecules can also create degradation products that are toxic to cells (O'Brien et al., 2008, Aldehyde sources, metabolism, molecular toxicity mechanisms, and possible effects on human health, Critical reviews in toxicology, 35(7), 609-662).

[0025] For plant materials containing a large quantity of sugars, the interaction of the latter with certain amino acids can also be feared during heating (pH-, water content-dependent) and produce the synthesis of new molecules modifying the aroma and the biological potential.

[0026] Certain drying techniques have been developed to avoid the degradation and loss of thermolabile molecules, or those whose hydrolysis or oxidation can be very rapid. This is the case of low-temperature drying (30-38°C) or freeze-drying, which uses a specific state of water, sublimation, to dehydrate a product after freezing (Oikawa et al., 2011, Effects of freeze-drying of samples on metabolite levels in metabolome analyses, Journal of separation science, 34(24), 3561-3567; Adams, 1991, Freeze-drying of biological materials, Drying technology, 9(4), 891-925).

[0027] Nevertheless, even using these gentler drying processes, it has been shown by a freeze-dried plant / fresh plant comparison that a significant portion of the plant's metabolites was lost (Oikawa et al., 2011, Effects of freeze-drying of samples on metabolite levels in metabolome analyses, Journal of separation science, 34(24), 3561-3567).

[0028] These methods are costly in terms of energy, time, and economically unprofitable for businesses. However, the main interest in drying plant materials lies in the possibility of storing and preserving these dehydrated plants. Removing water from the plant therefore remains essential in its conservation, the stabilization of its chemical content and the preservation of its biological activities over the long term (Mediani et al., 2014, Effects of different drying methods and storage time on free radical scavenging activity and total phenolic content of Cosmos caudatus, An-tioxidants, 3(2), 358-370).

[0029] It has also been demonstrated that during storage and in a manner very dependent on storage conditions, the chemical profile of a fresh fruit or a fresh plant (carotenoids, polyphenols, vitamins, etc.) could be strongly affected and reduced in quantitative and qualitative terms, the molecules not being subject to degradation in the same way (Yamauchi and Watada, 1991, Regulated chlorophyll degradation in spinach leaves during storage, Journal of the American Society for Horticultural Science, 116(1), 58-62; Vishnu Prasanna et al., 2000, Effect of storage temperature on ripening and quality of custard apple (Annona squamosa L.) fruits, The Journal of Hor- Cultural Science and Biotechnology, 75(5), 546-550).

[0030] Among the extraction processes used, notably using water as a solvent, we can cite hydrodistillation or steam distillation, cold maceration, hot digestion, decoction, leaching, percolation under pressure or cold, or even infusion.

[0031] Another common extraction method is to use volatile organic solvents such as petroleum ether, hexane, ethyl ether, acetone, carbon dioxide, benzene or toluene.

[0032] Concerning the extraction in particular of fresh plant matter in a fat, the process classically used since Antiquity consists of hot enfleurage. Enfleurage is a process aimed at integrating the aromas of a fresh plant into an oil or fat by maceration. The fat can be heated upstream of the process and the plant is infused in the latter. At the end of the process, the plant is separated from the enfleured fat by filtration. This process mainly concerns aromatic flowers or herbs.

[0033] However, the plant material is not crushed during the enfleurage process and the water from the plant material is not removed.

[0034] Technical problem

[0035] Generally speaking, there is a need to develop a process for preparing a stabilized plant material which makes it possible to integrate the fresh plant, for example immediately after harvesting and thus to avoid transport and handling constraints, and to preserve the chemical and biological properties of the plant while avoiding the degradation of the active molecules.

[0036] In view of the above, a problem which the present invention proposes to solve consists in developing a new process for preparing a totum or a solid or liquid filtrate at room temperature from fresh plant material and a fatty substance, easy and quick to implement and making it possible to preserve all the metabolic richness of the plant material and to avoid any degradation by oxidation of the fragile molecules. The extracted natural active compounds are contained in a complex whole and act in synergy with each other, thus increasing the biological potential of the totum.

[0037] Benefits provided

[0038] The advantage of said method according to the invention is to use the fresh plant material, whole or in part, for example from the field, directly in the method according to the invention and to grind it, dry it, and stabilize it in the fatty material while retaining the maximum of its biological activities (little metabolic change).

[0039] Integrating the fresh plant immediately after harvesting presents a major advantage for those skilled in the art in terms of handling, transport but also in terms of preservation of the biological properties of plant matter, in particular a plant.

[0040] The process makes it possible to stabilize by dehydration, block the access of oxygen to the active molecules (oxidation) by grinding the plant directly in the fat, the latter surrounding the fine plant particles and providing the fresh plant matter with a fat with antimicrobial properties in order to prevent the degradation of the active ingredients. In addition to the biological advantage (increase in the biological and chemical potential of the product), stabilization via this process has an energy advantage because it is an “all-in-one” process.

[0041] Said process can also be used to stabilize co / by-products from manufacturing in other sectors quickly at the factory outlet. Said process thus also fits into the problem of recovering co / by-products. Indeed, these by- or co-products are products removed by companies which are not or cannot necessarily be stored in optimal conditions, the companies not being compliant for this purpose. The financial burden due to the removal of co / by-products from the company (transport, destruction) is also greatly reduced or even eliminated. The idea is therefore to preferentially implement the process directly at the factory outlet in order to stabilize the co / by-products as quickly as possible and preserve them in good conditions, and thus be able to recover them subsequently.The totum or filtrate from the co / by-products obtained by the process constitutes an optimized stable state in order to store them and enhance their chemical richness.

[0042] In addition to the advantages in terms of no cleaning of different machines, the energy cost is lower than the successive use of several specific tools in that said process is an all-in-one grinding, dehydration, mixing, extraction, formulation treatment.

[0043] Finally, this process is very simple to implement and adaptable (duration of the process, temperature, application or not of vacuum, grinding, adapted to the initial water content of the plant, its lignin composition, its chemical fragility, etc.).

[0044] Technical solution

[0045] The solution to this problem posed has as its first object a process for preparing a totum which is a mixture of a vegetable material with a solid or liquid fatty material, characterized in that it comprises the following steps according to which: (a) the plant material is fresh and comprises at least 10% water by mass of water relative to its total mass (mass / mass) before or after loss on drying, taken alone or as a mixture, whole or in part, is brought into contact, preferably with stirring, with the fat chosen from a fat and a hydrogenated or non-hydrogenated oil, at a temperature between 50°C and 180°C; (b) the vegetable matter - fat mixture thus obtained is then ground at a temperature between 50°C and 180°C; (c) the ground material obtained at the end of step (b) is heated, preferably with stirring, to a temperature between 50°C and 180°C to dehydrate the mixture; and (d) a solid or liquid totum at room temperature comprising a water content less than or equal to 4% by mass of the total mass of the totum is recovered.

[0046] Its second object is a solid or liquid totum or filtrate at room temperature capable of being obtained by the process according to the invention.

[0047] Its third object is the use of a totum or filtrate according to the invention, for the preparation of a food or cosmetic composition.

[0048] Finally, it has as its fourth and final object a composition comprising a totum or filtrate according to the invention, for its pharmaceutical, nutraceutical or animal health use. Brief description of the drawings

[0049] The invention and the advantages resulting therefrom will be better understood upon reading the description and the non-limiting embodiments which follow, with regard to the appended figures in which:

[0050] [Fig.l] represents the different stages (mixing, grinding, dehydration) of the process according to the invention for preparing a totum or a filtrate allowing the stabilization of fresh plant material.

[0051] [Fig. 2] represents the different stages (mixing, grinding, dehydration) of a particular embodiment of the process according to the invention for preparing a totum or a filtrate allowing the stabilization of fresh plant material, in which the supply of fresh plant material is done in two stages.

[0052] [Fig.3] shows a photo of a totum obtained by the process according to the invention using a fresh Habanero pepper and glycerol monolaurate.

[0053] [Fig.4] represents the quantification of the carotenoids identified in the samples of fresh Habanero pepper, oven-dried at 100°C and dehydrated according to the method according to the invention implemented in the context of Example 5.

[0054] [Fig. 5] more particularly represents the absolute quantification of different carotenoids of interest in animal nutrition / health (lutein; beta-carotene and zeaxanthin) identified in the samples of fresh Habanero pepper, oven-dried at 100°C and dehydrated according to the process according to the invention implemented in the context of Example 5.

[0055] [Fig.6] represents the absolute quantification of capsaicin identified in the samples of Habanero pepper and red pepper, respectively fresh, oven-dried at 100°C and dehydrated according to the method according to the invention implemented in the context of Example 5. Description of the embodiments

[0056] The invention relates to a process for preparing a solid or liquid totum or filtrate at room temperature from fresh plant material and fatty material.

[0057] Fresh plant matter means a living organism forming part of the plant kingdom, including aquatic plants, whole or in part, comprising at least 10% water by mass of water relative to its total mass (mass / mass) before or after loss on drying, preferably at least 69% (mass / mass), more preferably at least 79% (mass / mass).

[0058] In contrast, a dry matter generally has a water content which is at most of the order of 5% (mass / mass).

[0059] The fresh plant material, taken alone or in mixture, in whole or in part, used in the process according to the invention is preferably chosen from fruits, whole plants, aerial parts of plants, roots, bulbs, tubers, seeds such as grape or citrus seeds, skins such as pomegranate or citrus skin, pulps, macerates, cakes, or any other by-product of plant material such as residues of pressed plants or fruits.

[0060] The fresh plant material, taken alone or in mixture, in whole or in part, used in the process according to the invention is more preferably chosen from wormwood, yarrow, garlic, wild garlic, artemisia, artichoke, pink berry, goji berry, burdock, basil, coffee, chamomile, cinnamon, blackcurrant, lemon, lemongrass, hemp, coriander, turmeric, cypress, eucalyptus, fenugreek, ash, juniper, clove, ginseng, ginger, pomegranate, hibiscus, hops, bay leaf, lavender, lemon grass, alfalfa, flax, mint, peppermint, mallow, lemon balm, mustard, white mustard, walnut, hazelnut, orange, oregano, nettle, onion, paprika, pansy, pepper, chili, pine, dandelion, pepper, rosemary, grape, savory, sage, wild thyme, marigold, tansy, tea, thyme, clover, goldenrod, even more preferably peppers and chilies of the genus Capsicum annuum et frutescens, chilies of the genus Capsicum chinense, garlic, ginger, grapes, thyme, paprika,more preferably still peppers and chilies of the genus Capsicum annuum, frutescens and chilies of the genus Capsicum chinense such as Habanero, Bhut Jolokia, Carolina Reaper, Trinidad Scorpion, bird's eye / Thai chilies.,

[0061] Fresh plant material can generally only be kept as is for a short time, for example a maximum of a few hours, after harvesting or recovery for by-products, otherwise it will degrade and lose a large part and sometimes all of its active metabolites of interest and the associated biological activities.

[0062] Advantageously, the plant material will be placed in the fat directly after harvesting or recovery, or at least as quickly as possible, for example 12 hours, and will preferably be used within 3 hours, in order to preserve all the active metabolites of interest.

[0063] The fat used in the process according to the invention is chosen from a hydrogenated or non-hydrogenated fat or oil, taken alone or as a mixture.

[0064] According to one embodiment, insofar as obtaining a solid totum at room temperature is desired, the fatty material used is preferably a fat.

[0065] According to another embodiment, to the extent that obtaining a liquid totum at room temperature is desired, the fatty material used is preferably an oil.

[0066] Ambient temperature means a stable but not necessarily controlled temperature, which is generally 20°C but which can be between 15°C and 27°C.

[0067] The fat preferably used in the process according to the invention is chosen not only for its effectiveness and its interest in terms of the process but also for its cost, its texturizing properties and its interest in use as a food component (energy intake for example).

[0068] The fat is preferably chosen from glycerol monolaurate, glycerol monocaprate, glycerol monomyristate, glycerol monopalmitate, glycerol monostearate, almond oil, peanut oil, argan oil, avocado oil, calophyllum oil, safflower oil, rapeseed oil, coconut oil, wheat germ oil, jojoba oil, corn oil, hazelnut oil, apricot kernel oil, virgin olive oil, palm oil, grape seed oil, castor oil, sesame oil, soybean oil, or sunflower oil, more preferably glycerol monolaurate, glycerol monocaprate, hydrogenated palm oil and hydrogenated sunflower oil, more preferably glycerol monolaurate.

[0069] Particularly advantageously, certain fatty substances used in the process according to the invention are effective solvents, that is to say they allow the transfer of molecules from the plant material into the solvent; this is the case in particular for glycerol monolaurate, glycerol monocaprate and olive oil for example, unlike for example sunflower oil or palm oil which have a lower solvent power.

[0070] Whatever their solvent power, the intrinsic properties of the fats or oils used, in particular the fats and more particularly the glycerol monolaurate, make it possible to optimize the process and the product resulting from said process. The fats or oils create an anaerobic or at least micro-anaerobic environment during the process and inhibit the survival and development of strictly aerobic microorganisms. This is intensified by the fact that the fats that can be used for the process are advantageously solid at room temperature and therefore impermeable to air and therefore restricting the colonization of microorganisms within the totum.

[0071] The Applicant was able to demonstrate that glycerol monolaurate, lauric acid monoglycerol (or 2,3-dihydroxypropyl decanoate), constitutes a particularly advantageous fatty substance according to the invention, which has multiple advantages. It is solid at room temperature and liquid from 60°C. Its use poses no risk to humans or animals. It is thermostable and retains its properties and non-toxicity during the process steps.

[0072] Due to its emulsifying properties, its use in said process makes it possible to facilitate the extraction of water from fresh plant materials from the totum, the mixing being carried out at a temperature preferably greater than or equal to 60°C and preferably with constant stirring. The use of glycerol monolaurate in the process helps to remove water from the plant cells. The emulsifying properties of glycerol monolaurate also make it possible to protect the molecules contained in the plant cells from degradation (guided by contact with water or oxygen), by optimized contact with the fat. More than heating (drying), the emulsifying properties of glycerol monolaurate also make it possible to optimize grinding by improving the plant / fat / knives contact.

[0073] Glycerol monolaurate is a natural fatty acid monoester whose composition (more polar than certain vegetable oils) particularly allows for the extraction of amphiphilic compounds such as capsaicinoids. Its use poses no risk to humans or animals.

[0074] In addition, it shows pronounced antibacterial, antifungal and anti-inflammatory activities. It can be used as an antimicrobial agent and notably inhibits the growth, in vitro but also in vivo, of Candida strains. It also acts against the growth of Gram+ but also Gram- bacteria such as Staphylococcus, Strep-tococcus, Gardnerella, Haemophilus but also Listeria monocytogenes. It also acts as a bacteriostatic, against Bacillus anthracis, that is to say it blocks its growth without killing the cells. In Staphylococcus aureus, glycerol monolaurate blocks the production of certain exo-enzymes and virulence factors such as protein A, α-hemolysin, Zeta-lactamase and toxic shock syndrome toxin 1 (TSST-1).

[0075] Its action on the inflammatory cycle has also been highlighted because a parallel and significant decrease in the quantity of pro-inflammatory cytokines (IL-8 and TNF-a) has been observed. Glycerol monolaurate can also act in synergy with other products, such as aminoglycosides, particularly in the destruction of biofilms of antibiotic-resistant strains of Staphylococcus aureus. Indeed, prior treatment with glycerol monolaurate would improve the response of biofilms to antibiotics.

[0076] Glycerol monolaurate, due to its emulsifying, solvent, physicochemical and antibacterial properties, is the fat most preferably chosen for implementing the process for preparing a totum or a filtrate according to the invention.

[0077] For reasons of implementation complexity, glycerol monolaurate has never been disclosed to replace any extraction solvent in an associated process.

[0078] Indeed, although its physicochemical properties make it an extraction solvent of choice, it is mainly for its antimicrobial (WO2016169129, WO9531966) and anti-inflammatory properties that it has been highlighted until now. Glycerol monolaurate has also been described as a constituent of a combination of essential oil molecules used as a preservative for cosmetic products (inhibition of Aspergillus niger, Candida albicans, Staphylococcus aureus, and Pseudomonas aeruginosa) (WO2019047004).

[0079] It therefore appears that the antimicrobial properties of glycerol monolaurate have been exploited in different fields of application for food decontamination, infection treatment processes (in human health), as food additives or cosmetic preservatives. Its preservative properties have been verified because the stabilization of the totum obtained by said process also involves the preservation of the latter during its storage. The use of glycerol monolaurate as the fat in the process (versus hydrogenated palm oil) has made it possible to slow down or even inhibit the proliferation of microorganisms on the product obtained.Although the antimicrobial properties of glycerol monolaurate had been previously described in the literature, its use as a solvent, in an all-in-one process of drying, grinding, eco-extraction, formulation, and stabilization of fresh plant material containing active natural metabolites of interest has never been described.

[0080] Its antimicrobial activity but also its physicochemical properties allowing the extraction of a wide range of metabolites make it a particularly preferred candidate, notably as an intelligent solvent, or solvactive, combining notable effectiveness as a solvent and providing the mixture with its antimicrobial and preservative properties described above.

[0081] The method according to the invention comprises a first step (a) in which the fresh plant material comprising at least 10% water by mass of water relative to its total mass (mass / mass) before or after loss on drying, taken alone or in mixture, whole or in part, is brought into contact, preferably with stirring, with the fatty substance chosen from a fat and a hydrogenated or non-hydrogenated oil, at a temperature between 50°C and 180°C, preferably between 60°C and 130°C, more preferably of the order of 100°C.

[0082] The step of bringing the fresh plant material into contact with the fatty material is preferably carried out with constant stirring of between 300 and 2500 revolutions per min (rpm), preferably with constant stirring of the order of 500 rpm.

[0083] For example, a scraper or mixer ensures constant contact of the fresh plant material, whole or in part, with the fat and also allows water to be removed during the process.

[0084] This contacting step, preferably with stirring, at a temperature between 50°C and 180°C, preferably between 60°C and 130°C, more preferably of the order of 100°C, thus consists of a mixing / heating step.

[0085] This first step of the process makes it possible to melt the fat, insofar as it is solid at room temperature, for example glycerol monolaurate or hydrogenated sunflower oil, to cook the fresh vegetable matter in contact with the fat and consequently to improve the grinding which is the following step.

[0086] This mixing / heating step is essential because it allows the evaporation, at least in part, of the water from the fresh plant material.

[0087] During this step, if the fat used is a solid fat at room temperature, it will, due to the temperature, become liquid and surround, protect the fresh vegetable matter which is subjected to an increase in temperature.

[0088] The duration of this mixing / heating step depends on the fresh plant material used and its water content.

[0089] This step must advantageously be carried out in a time necessary and sufficient for the fat, which may be solid at room temperature, to be liquefied to allow subsequent effective grinding, unlike dry grinding in fat flakes. It cannot therefore be only a few seconds, particularly for a fat which is solid at room temperature.

[0090] Advantageously, to the extent that the fatty material used has a solvent power, preferably glycerol monolaurate taken alone or in combination, it also makes it possible to extract, at least in part, that is to say transfer the metabolites of the fresh plant material into the fatty material.

[0091] The fresh plant material is preferably placed in contact with the fatty material for a period of between 5 min and 40 min, for example 10 min, 15 min, 20 min, 25 min, 30 min or 35 min, preferably between 5 min and 20 min, more preferably 10 min.

[0092] In a step (b), the vegetable matter - fat mixture obtained in (a) is then ground at a temperature of at least 50°C, preferably between 50°C and 180°C, more preferably between 60°C and 130°C, even more preferably of the order of 100°C.

[0093] The step of grinding the vegetable matter - fat mixture can last a few seconds, and is preferably carried out for a period of more than 2 minutes, preferably between 3 min and 15 min depending on the vegetable matter, more preferably between 3 min and 5 min.

[0094] The grinding is advantageously carried out in such a way that the totum obtained in fine forms a smooth paste, and that the particles of ground vegetable matter remain in suspension in the fatty matter so that, during cooling, the residue of vegetable matter does not settle below. The totum thus obtained in fine is homogeneous and contains particles invisible to the naked eye.

[0095] The grinding is advantageously carried out by toothed knives.

[0096] The grinding of the fresh vegetable matter into the fat is carried out in one times, or in several times, depending on the type of plant material and its richness, particularly in cellulose, lignin, presence of seeds, nuts or bark.

[0097] The step of grinding the vegetable matter - fatty matter mixture is preferably carried out with stirring between 500 rpm and 3500 rpm, more preferably between 1000 rpm and 2500 rpm, depending on the vegetable matter, even more preferably with constant stirring of the order of 2500 rpm thanks for example to said scraper ensuring constant contact of the ground fresh vegetable matter with the fatty matter.

[0098] The fresh plant material and / or the fatty material, advantageously the fresh material, can be provided all at once from the start of the process or alternatively in several times, for example 2 to 4 times during the process, the steps of mixing / heating (step a), grinding (step b) (and dehydration (step c)) being advantageously carried out after each addition of fresh plant material as illustrated in [fig-2].

[0099] As an illustrative example, 1 / 3 (mass / mass of the total input) of fat, preferably glycerol monolaurate, and 1 / 3 (mass / mass of the total input) of fresh plant material, preferably peppers, are added at the start of the process. They are brought into contact with stirring at 100°C for 10 min and then the mixture is ground by knives at 2500 rpm, 100°C, for 5 min; again 1 / 3 (mass / mass of the total input) of fresh plant material is added, the mixture being heated for 10 min at 100°C, and subsequently the mixture is ground for 5 min at 2500 rpm. This makes it possible to incorporate a larger proportion of fresh plant material into the fat.

[0100] According to another illustrative example, 1 / 3 (mass / mass of total input) of material fatty, preferably glycerol monolaurate, and 1 / 3 (mass / mass of the total input) of fresh plant material, preferably chili peppers, are provided from the start of the process. They are brought into contact with stirring at 100°C for 10 min, then the mixture is ground by knives at 2500 rpm, 100°C, for 5 min; again 1 / 3 (mass / mass of the total input) of another fresh plant material, advantageously an aromatic plant (for example thyme) is added, the mixture being heated for 10 min at 70°C, a lower temperature so as not to alter the volatile secondary metabolites of the aromatic plants (active), then the mixture is ground for 5 min at 2500 rpm.

[0101] The fresh plant material and the fat are advantageously used according to a final mass / mass ratio of fresh plant material to fat of 1:1 to 5:1, preferably of 1:1 to 2:1, more preferably of 1:1 to 1.5:1, the optimum being dependent on the initial water content of the fresh plant material.

[0102] In a step (c), the ground material obtained at the end of step (b) is heated, preferably with stirring, to a temperature of at least 50°C, preferably between 50°C and 180°C, more preferably between 60°C and 130°C, even more preferably of the order of 100°C, to dehydrate the mixture, by evaporation of the water; in the case where the fat used has solvent capacities, this step promotes the transfer of the molecules from the plant to the fat: this is called eco-extraction.

[0103] The duration of this heating step is dependent on the initial water content of the plant material used in the process. The higher the water content, the longer the heating / mixing time (step c) and water evaporation time must be.

[0104] This additional heating step is preferably carried out with constant stirring.

[0105] The heating of the ground material is preferably carried out with constant stirring with a scraper at 500 rpm for 5 to 40 min, for example 10 min, 15 min, 20 min, 25 min, 30 min, 35 min, preferably 5 min to 20 min, more preferably 10 min, at a temperature of 100°C in order to continue and optimize the eco-extraction of the metabolites of plant material in the fat.

[0106] This step is particularly advantageous because it makes the active plant metabolites more bioavailable by removing them from the plant cells, while nevertheless being protected from potential degradation by their immediate contact with the fat.

[0107] Also and particularly advantageously, to the extent that the fat used has a solvent power, it allows the extraction of the metabolites of the plant material in the fat or oil to continue. This is more particularly the case when glycerol monolaurate is used as a fat, taken alone or in combination, or even olive oil.

[0108] According to a particularly preferred embodiment of the method according to the invention, the steps of mixing / heating (step a), grinding (step b), and heating / mixing the ground material (step c), are preferably carried out in the dark.

[0109] Darkness means the total absence of light, visible or invisible, natural or artificial.

[0110] Carrying out the method according to the invention in the dark advantageously makes it possible to protect the molecules from degradation due to light (UV) and thus to avoid any loss of molecules of interest by oxidation.

[0111] Furthermore, carrying out the steps of heating / mixing and grinding the fresh plant material directly in the fat, and in the dark, makes it possible to reduce the risk of oxidation and loss of active compounds.

[0112] As an example of a device allowing the implementation of the method according to the invention, mention may be made of the ROBOQBO 8L® or the HYDROGRIND® equipped with toothed knives with a rotation speed of between 500 and 3000 rpm, an integrated heating system allowing the products to be heated to 180°C, and also a 900 mbar vacuum system and a cleaning system. The water evacuated in the form of steam throughout the process is eliminated through an outlet placed on the upper part of the machine.

[0113] Such a device therefore makes it possible in particular to control the conditions relating to both the atmosphere (O2 / CO2, ventilation), the humidity, the temperature and the agitation of the fresh plant material used in the method according to the invention. These are important conditions to control when working on fresh plants.

[0114] The method according to the invention thus makes it possible to dry fresh plant materials and to preserve all their metabolic richness in the hot fat at a temperature between 50°C and 180°C, in order to avoid any degradation by oxidation of the fragile molecules.

[0115] The grinding of the plants is also carried out in hot fatty matter, preferably at a temperature between 50°C and 180°C, which facilitates grinding and limits the contact of the cellular contents of the plant matter with the oxygen in the air.

[0116] A temperature of at least 50°C, preferably between 50°C and 180°C, more preferably between 60°C and 130°C, even more preferably of the order of 100°C, is therefore applied throughout the process.

[0117] The mixture of fat / fresh plant is stirred throughout the process by a scraper rotating at a speed of between 300 rpm and 600 rpm, advantageously constantly at 500 rpm,

[0118] Advantageously, the method according to the invention is carried out for a total duration of between 13 min and 60 min to minimize energy costs, for example 15 min, 18 min, 20 min, 23 min or even 25 minutes.

[0119] During the process, the water is removed in the form of steam. Water vapor is released throughout the process. Heating / mixing at a temperature preferably between 60°C and 130°C, more preferably of the order of 100°C, grinding the plant material in the fat, then heating / mixing again preferably between 60°C and 130°C, more preferably of the order of 100°C and constant stirring during the process will allow the water to be removed from the plant cells, and ultimately to obtain a totum or a filtrate depleted in water. The phenomena of hydrolysis of plant molecules, entrainment in steam and oxidation are limited by the fact that the plant material is introduced and cooked in the fat and that the release of metabolites takes place, during grinding and mixing at preferred temperatures of 100°C, in the liquid fat.In addition, the plant cells are completely surrounded by the liquid fat during the process.

[0120] The water content of a sample of the dehydrated ground material obtained at the end of step (c) is measured, for example, by infrared balance.

[0121] At the end of step (c), a solid or liquid totum at room temperature with a water content less than or equal to 4% by mass of the total mass of the totum, preferably less than 2.5% (mass / mass), more preferably less than or equal to 1% (mass / mass), is finally recovered in a final step (d).

[0122] For example, using this process, the plants are dehydrated (or dried) after 13 minutes of heating and grinding in fat or oil, advantageously at 100°C, and this up to 99%.

[0123] According to another embodiment of the invention, the method can integrate, at the same time or in an additional step, the application of microwaves and / or ultrasound so as to accelerate the speed of evaporation of water from the plant material and the extraction of plant metabolites in the fatty material having a solvent power.

[0124] According to a preferred embodiment of the method according to the invention, an additional step of filtration of the vegetable matter - fatty matter mixture thus obtained is carried out at the end of step (b) or (c). This filtration makes it possible to eliminate the vegetable matter residues having a particle size greater than 200 μm or preferably 100 μm, before being recovered to obtain a solid or liquid filtrate at room temperature.

[0125] For example, the separation of the filtrate and the residue of plant material is carried out by hot filtration (for example 90°C) under vacuum or by centrifugation (for example 3000g) at hot temperature (for example 90°C).

[0126] To this end, another object of the invention relates to a process for preparing a solid or liquid filtrate, characterized in that it comprises the following steps according to which: - a fresh plant material comprising at least 10% water by mass of its total mass before or after loss on drying, taken alone or in a mixture, whole or in part, is brought into contact, preferably with stirring, with a fatty material chosen from a hydrogenated or non-hydrogenated fat or oil, at a temperature between 50°C and 180°C; - the mixture of vegetable matter and fat thus obtained is then ground at a temperature between 50°C and 180°C; - the ground material thus obtained is heated, preferably with stirring, to a temperature between 50°C and 180°C, preferably between 60°C and 130°C, more preferably of the order of 100°C, to dehydrate the mixture; - an additional step of mixing the ground material obtained at the end of step (b) at a temperature between 50°C and 180°C, preferably between 60°C and 130°C, more preferably of the order of 100°C is carried out; - the dehydrated ground material thus obtained is filtered hot or cold depending on the fat used; and - a solid or liquid filtrate at room temperature comprising a water content of less than or equal to 4% by mass of the total mass of the filtrate, preferably less than 2.5% (mass / mass), more preferably less than or equal to 1% (mass / mass) is recovered, the plant material residues having a particle size greater than 200 pm or preferably 100 pm having been eliminated.

[0127] The water content of the total or solid or liquid filtrate at room temperature thus recovered is advantageously measured at the end of the process, as is the water activity, and will be correlated with the lifespan of the product (microbial contamination-degradation of active ingredients).

[0128] If the fat has antimicrobial properties, such as advantageously glycerol monolaurate, and the water in the fresh plant material is eliminated in its entirety, the final totum or filtrate will be optimally stabilized for storage and preservation. If the fat becomes solid again at room temperature, the totum is a product advantageously formulated as is.

[0129] To this end, another object concerns a solid or liquid totum or filtrate at room temperature capable of being obtained by the process according to the invention.

[0130] At the end of the process according to the invention, the totum or filtrate thus obtained is a smooth paste stabilized by its low humidity level and / or by its antimicrobial properties, which can be poured immediately into a suitable container.

[0131] In the case of the use of oils or fats which are liquid at room temperature, the totum thus obtained is liquid with substantially fine dried vegetable particles. resulting from grinding in suspension in oil or fat. The liquid totum can be filtered to remove residues of plant matter having a particle size greater than 200 or preferably 100 μm and the filtrate used as is or in a mixture with other compounds.

[0132] This totum or filtrate, the dried plant particles of which are fine, preferably less than 100 μm, is preferably preserved in solid form if the fat used is a fat whose melting point is higher than room temperature. The totum or filtrate, which is solid at room temperature, can then be remelted in order to be incorporated into a mixture or ground in order to be used in an additional process of encapsulation or addition of another material, plant-based or not.

[0133] The totum produced during said process is defined as the mixture of dried-dehydrated, ground, possibly eco-extracted, formulated and stabilized plant matter in fat.

[0134] In the case where the fat used has no solvent power and no extraction is done, the totum is a mixture of finely ground plant particles, surrounded and protected by the fat. Using two fats in combination, such as glycerol monolaurate and sunflower oil, allows both extraction with glycerol monolaurate and protection with glycerol monolaurate and sunflower oil.

[0135] The filtrate obtained by the process according to the invention is free of particles and essentially comprises the metabolites extracted from the starting fresh plant material.

[0136] The fact that the fats used can be solid at room temperature reinforces the protection of the plant molecules in the totum or filtrate, and therefore the preservation of the totum or filtrate over time. Indeed, the surface area of ​​the cooled and solid totum or filtrate in contact with air and light is very limited and therefore the proportion of active metabolites that can be directly subjected to degradation by oxygen, temperature, humidity and light is very limited because the fat is impermeable to air. The totum or filtrate that is solid at room temperature is therefore a stabilized state of the fresh plant material used in the process.

[0137] The totum or filtrate obtained according to the invention is depleted in water, with a content of less than or equal to 4% water by mass of the total mass of the filtrate, preferably less than 2.5% (mass / mass), more preferably less than or equal to 1% (mass / mass), the water from the plant material having been eliminated during said process.

[0138] The totum, or filtrate in the case where the fatty matter has the capacity, even limited, to extract, produced by the process according to the invention comprises active compounds extracted from the fresh plant matter.

[0139] Among the active compounds of interest and targeted, that is to say preferred, during the application of said process, we can cite a family of alkaloids: capsaicinoids (capsaicin, dihydrocapsaicin, nordihydrocapsaicin).

[0140] By the process according to the invention, it is also possible to extract carotenoid type pigments (capsanthin, lutein, capsorubin, zeaxanthin, zeto-carotene, beta-cryptoxanthin, zeto-cryptoxanthin, antheraxanthin) and chlorophylls.

[0141] The temperature of the process may be adapted in order to extract and not to deteriorate molecules of aromatic and volatile types such as p-cymene, y-terpinene, a -pinene, 1,8-cineole, œ-sabinene hydrate, linalool, camphor, borneol, terpinen-4-ol, trans-p-mentha-l(7),8-dien-2-ol, verbenone, bomylacetate, a-terpineol, carvone, thymol, carvacrol, piperitenone, eugenol, a-ylangene, carvacrol acetate, methyl-eugenol, caryophyllene, a-humulene, czs-calamenene, a-calacorene, caryophyllene oxide, 14-hydroxy-(Z) caryophyllene, abetatriene, 14-hydroxy-9-epi-(E) caryophyllene but also certain pigments, vitamins, amino acids or any other heat-sensitive molecule.

[0142] Indeed, volatile or thermolabile molecules from plants can volatilize or be degraded even from ambient temperatures (Ormeno et al., Extracting and trapping biogenic volatile organic compounds stored in plant species. TrAC Trends in Analytical Chemistry, 30(7), 978-989, 2011; Flores et al., Nanostructured Systems containing an essential oil: protection against volatilization. Quimica Nova, 34(6), 968-972, 2011; Schweiggert et al., Effects of processing and storage on the stability of free and esterified carotenoids of red peppers (Capsicum annuum L.) and hot chili peppers (Capsicum frutescens L.). European Food Research and Technology, 225(2), 261-270, 2007; Radünz et al., Study of essential oil from guaco leaves submitted to different drying air temperature. Engenharia na Agricultura, 18(3), 241-247, 2010).However, in the case of the said process, taking into account the protection by the fat, if the conservation in the totum of volatile or thermolabile plant molecules must be favored, the temperature of the process must be adapted and not exceed 80°C.

[0143] Advantageously, the temperature should be between 50°C and 80°C, more advantageously between 50°C and 60°C, preferably with a vacuum application.

[0144] According to a particular embodiment of the invention, in the case where thermolabile compounds are of particular interest, a lower temperature can be applied throughout the process (60°C instead of 100°C) with the application of vacuum. Putting the mixture under tension makes it possible to reduce the melting and evaporation temperature of the water. In fact, water boils at 100°C under an atmospheric pressure of 1013.25 hPa. Under a pressure of 700 hPa, water boils between 90°C and 91°C. Under a pressure of 300 hPa, water boils between 73°C and 75°C. Thus, reducing the pressure makes it possible in certain cases to treat fragile molecules that cannot withstand high temperatures, to apply a lower temperature and still eliminate the water by evaporation.

[0145] Conversely, higher temperatures are sometimes necessary in order to eco-extract molecules that are more difficult to extract (due to matrix effects or other) and these higher temperatures also make it possible to increase the extraction, grinding and water removal yield and to make the fat less viscous and therefore easier to handle.

[0146] The process is adaptable in terms of temperature, duration of contact between plant material and fat, and volume. This makes it possible to extract a certain range of active plant compounds from a wide variety of plant species. Heat-sensitive compounds such as terpene-type aromatic compounds can thus be extracted and integrated into the filtrate or totum.

[0147] Furthermore, all of the extracted compounds can act in synergy with each other and with the solvactive (intelligent solvent, i.e. with solvent properties capable of carrying out the eco-extraction of the active ingredients but also possessing biological properties of interest (antimicrobial) and formulation matrix) which is preferentially glycerol monolaurate, depending on their properties (antioxidant, antimicrobial, anti-inflammatory, etc.).

[0148] Given the physicochemical properties of glycerol monolaurate, a wide range of molecules (polar, apolar, amphiphilic) can theoretically be extracted into the solvent and contribute to the biological activity of the totum or filtrate (increase in the bioavailability of these molecules extracted from the plant matrix). By way of non-limiting example, we can cite among other compounds, alkaloids, carotenoids, polyphenols, fatty acids, vitamins, oses or even amino acids.

[0149] The totum or filtrate preferentially obtained has, due to the presence of glycerol monolaurate, but also of the various pigments extracted during the process, a smooth, colored and shiny appearance.

[0150] In the case where the extracted plant material comes from an aromatic plant (rosemary or oregano to name but two), the totum has the characteristic odor of these plants.

[0151] The invention also relates to the use of a totum or a filtrate according to the invention, for the preparation of a food composition, preferably for animal nutrition, or cosmetics.

[0152] Thus, the totum or the filtrate loaded with compounds of interest can then be formulated according to the needs and the targeted animals and proposed for example for their different properties as feed additives for livestock. As non-limiting examples, the filtrate or the totum are preferably formulated under powder, granule, pebble, ointment, paste, capsule, microcapsule or tablet form.

[0153] Finally, the invention has as its last object a composition comprising a totum or a filtrate according to the invention, for its pharmaceutical, nutraceutical or animal health use.

[0154] The preservation during storage and the shelf life of the product are optimized by the fact that it can contain glycerol monolaurate, an antimicrobial agent and solid at room temperature, thus protecting, in its center, the active molecules from oxidation and light.

[0155] By nutraceutical product is meant a totum or filtrate obtained by the process from foods, formulated for example in the form of powder, granule, pebble, ointment, paste, capsule, microcapsule or tablet, having a beneficial physiological effect or ensuring protection in particular against chronic diseases. Examples

[0156] The present invention will now be illustrated by means of the following examples:

[0157] Example 1: Process according to the invention for preparing a totum or a filtrate

[0158] [fig.l] illustrates the sequence of the different stages inherent in the process of the invention and the products resulting therefrom.

[0159] Either a first step of bringing into contact the fresh plant raw material(s) which may be whole plants, parts of plants (fruits, leaves, etc.), industrial co-products, fresh (with a water content greater than 10%), preferably fruits of the genus Capsicum and the fatty material(s), preferably glycerol monolaurate, and mixing them at a temperature of 100°C advantageously (or between 50 and 180°C).

[0160] This is followed by a step of grinding the vegetable matter into the fat, still at high temperature (100°C).

[0161] Then a step of mixing and dehydration of the ground material by evaporation of the water contained in the latter (ideally at 100°C or more). The mixing time and therefore dehydration of the totum will be all the longer as the water content of the starting fresh plant was high. The duration of the process must be adapted by taking into account the water content of the fresh plant material(s) to be dehydrated and stabilized by said process.

[0162] Following these steps, a totum is obtained with a water content less than or equal to 4% by mass of the total mass of the totum. The water content of the totum is measured with an infrared balance.

[0163] Example 2: Particular embodiment of the process according to the invention for preparing a totum or a filtrate, in which the addition of fresh plant material is done in two stages

[0164] [Fig.2] illustrates an example of a two-stage supply of fresh plant material. Each supply is followed by the steps of mixing, grinding, dehydration, i.e. a cycle.

[0165] This specific case is applied when it is desired to significantly load the totum with plant matter. The plant supply must nevertheless preferably be treated in at least two stages, given that the proportion of plant, before evaporation of the water, must be close to that of the fat so that there is contact from the start of the process and the fat can surround all the plant cells during the initial mixing.

[0166] During the second addition, the water from the fresh plant material added at the start of the process will have been eliminated, at least in part, and the volume of plant thus reduced in order to make room for a new addition.

[0167] The application of vacuum or the increase in the process time can be carried out in order to accelerate the evaporation of water during said process to obtain a totum with a content of less than or equal to 4% water by mass of the total mass of the totum.

[0168] Example 3: Dehydration of different fresh plant materials via said process and comparison with the process on dry plant powder

[0169] Fresh plant materials comprising a water content of 69% to 94% (Table 1) followed the drying / grinding process in 2 separate fats at proportions of plant material varying from 70 to 50% (Table 2). The process was carried out in a ROBOQBO® mixer / grinder, equipped with toothed knives with a rotation speed of 500 to 3000 rpm, an integrated heating system allowing the products to be heated up to 120°C and a 900 mbar vacuum system.

[0170] The plant materials and the fats / oils were respectively brought into contact according to the defined proportions (Table 2) and heated to a temperature of 100°C for 10 minutes with stirring between 500 rpm and 3000 rpm.

[0171] Grinding was then carried out for 5 or 10 min (depending on the plants) minutes always at 100°C.

[0172] Following grinding, the ground plant material / melted fat was stirred with a mixer for 20 or 25 min at 2500 rpm, thus allowing for prolonged heating of the ground material, evaporation of the water, and in the case where the fat has solvent properties, the transfer of the plant metabolites to the fat.

[0173] Water vapor was evacuated throughout the process through an air outlet on the upper face of the machine.

[0174] At the end of the process, the smooth paste thus obtained is poured immediately, before setting at room temperature, into aluminum trays. The humidity measurement was carried out with an infrared balance (and validated by drying the plant materials and products in an oven).

[0175] The method was also carried out with dry chili powder having a water content of 5.11% and glycerol monolaurate (50:50) as a control.

[0176] Table 1: Measurement of the water content of the plant materials used Fresh Fruits Water Content Red Pepper 87% Green Chili 92% Habanero Chili 91% Ai! 69% Ginger 94% Grape 80% Thyme 79%

[0177] Table 2: Little obtained after 40 min at 100°C Water content of the totem Pir "te R fresh + GML 50:50 fresh v. chili + GML 50.50 Habanero (V. and RJ fresh * GML 50:50 Fresh V. chili + hydrogenated palm oil 50:50 Fresh R. chili + hydrogenated palm oil 50:50 Fresh V. chili + GML 70:30 Fresh ginger + GML 50:50 Fresh Aii + GML 50:50 Fresh thyme + GML 50:50 2.40% 1% 2.12% 0.63% 0.79% 0.71% 0.77% 0.78% 0.60% Dry chili powder f GML 50:56 0.23%

[0178] The product from the process with dry plant powder has a water content of 0.23% (Table 2).

[0179] As illustrated by the results in Table 2, the products obtained by the process according to the invention from fresh plant materials and glycerol monolaurate have water contents of 0.6% to 2.4%. The products obtained by the process according to the invention from fresh plants and hydrogenated palm oil have water contents of 0.63% to 0.79%.

[0180] Thus, the totum obtained from fresh material or dry material is stable because it has a water content of less than 4%. The method according to the invention therefore makes it possible to replace the drying and grinding upstream of the plant material, a step costly in terms of energy and chemical loss, by grinding and dehydration all-in-one with the ultimate obtaining of a stabilized totum.

[0181] Example 4: Example of parameters of the process according to the invention using a fresh Habanero pepper (water content 91%) and glycerol monolaurate (GML or MGL)

[0182] The different stages of the method according to the invention are implemented according to the conditions defined in Table 3 below.

[0183] Table 3: ROBOQBO TEST PROTOCOL Grindercooker PROTOCOL Formula: GML 50% = 1000 g Fresh plant material Whole Habanero chili pepper 50% = 1000 g Device settings: Product temperature requested 100°C obtained 98°C Grinding mixer speed 3000 rpm Grinding time 5 min Cooking speed 2500 rpm Cooking time before grinding 10 min Cooking and mixing time after grinding 20 min Raw material temperature at inlet 19 X Use of vacuum 700 mbar NO Product characteristic: Product appearance Smooth without seed particles Organoleptic analysis: sensation of spiciness, scale from 1 to 10 Ambient 2, in mouth 6 Humidity moisture meter 1 2.12%

[0184] The totum thus obtained comprises a water content of the order of 2% and has the appearance of a smooth and homogeneous paste as illustrated by [fig.3] and having a strong sensation of spiciness.

[0185] Example 5: Measurement of the impact of the process on the metabolites of interest extracted from peppers

[0186] The process described below was carried out using Habanero peppers, the water content of which is indicated in Table 1 above. The results of chemical analyses of the carotenoids extracted from the totum thus obtained are highlighted below.

[0187] Method implemented: - Glycerol monolaurate (GML or MGL) (1 kg) and whole Habanero pepper fruits (1 kg) were introduced into the ROBOQBO® and heated (cooked) at 100°C for 10 min. - This was followed by a grinding stage lasting 5 min at 100°C (knives throughout the grinding stage at 3000 rpm). - Following the grinding step, heating (cooking) was extended for 20 min at 100°C with mixing by the scrapers at 2500 rpm in order to allow the evaporation of the remaining water and also the transfer of the chili metabolites to the MGL (role of solvent). - The process therefore has a total duration of 35 min.

[0188] The totum obtained was hot-poured into a mold, and observed in section then ground in order to observe its physical behavior during grinding (viscosity, granulometry, color, odor and pungency).

[0189] Due to its capacity to be a solvent, glycerol monolaurate makes it possible to obtain a much more colorful totum because the metabolites of the fresh chili pepper, here more specifically the carotenoids, have been eco-extracted and transferred from the fresh plant material to the fat (GML).

[0190] The totum with glycerol monolaurate therefore has a more attractive character for humans or animals.

[0191] The dosage of carotenoids (comparison of fresh fruit, fruit dried at 100°C, and product from said process) was thus carried out.

[0192] Methanolic extractions were thus carried out from: 1) fresh Habanero pepper fruit; 2) whole fruits oven-dried at 100°C of Habanero pepper; and 3) of the totum resulting from the process, from Habanero pepper, as described above.

[0193] Following these extractions, the extracts were analyzed by UHPLC-DAD-MS / MS. The carotenoids were identified by their representative DAD spectrum. Some carotenoids could be quantified by parallel analysis of a standard range of the analytical standard. Each dosage was normalized in order to be placed in equivalent of the dry mass of the pepper and to be able to establish a comparison as to the potential loss of metabolites following drying.

[0194] The comparative quantification of the carotenoids identified in the samples of fresh Habanero peppers, oven-dried at 100°C and dehydrated according to the method according to the invention, is illustrated by [fig.4] representing the sum of the areas of the following metabolites (UHPLC-MSMS, MRM identification mode): beta-carotene; beta-cryptoxanthin; zeaxanthin; U_3.44; capsanthin; capsorubin; U_5.75; U_10.51; putative capsanthin myristate; putative capsanthin palmitate; putative capsorubin laurate myristate; putative violaxanthin dimyristate; U_111.19; putative capsanthin myristate palmitate; lutein.

[0195] According to the results thus obtained, the sum of the identified carotenoids is much higher, as expected, in the fresh fruit (Habanero pepper).

[0196] On the other hand, advantageously and not obviously, the sum of the identified carotenoids is in greater quantity in the totum resulting from the process according to the invention (54% of the fresh fruit) than in the pepper dried in the oven at 100°C (47% of the fresh fruit).

[0197] Thus, dehydration by the process according to the invention generally protects this class of molecules from degradation by heat or at least does not cause more degradation than during dehydration in an oven, for a lower energy cost provided by the all-in-one nature of the process.

[0198] More particularly, the absolute quantification (pg / g dry matter of chili pepper) of different carotenoids of interest in nutrition / animal health, classified in order of interest (A) lutein; B) Zeto-carotene; C) zeaxanthin) identified in the samples of fresh Habanero peppers, oven-dried at 100°C and dehydrated according to the process according to the invention, is illustrated by [fig.5].

[0199] According to the results thus obtained, lutein and zeto-carotene, like most of the carotenoids studied in the products based on green, red and Habanero peppers, are in higher concentration in the fresh fruit. On the other hand, advantageously and not obviously, the quantity of these carotenoids of interest is higher in the totum resulting from the process according to the invention than in the oven-dried pepper.

[0200] In a more isolated manner and without real explanation except perhaps bonds with the fatty matter (matrix effect due to their polarity, bonds with the glycerol monolaurate and trapping by the matrix) which could prevent their total extraction, certain metabolites (zeaxanthin) are present in greater quantity (in the fresh fruit and) the dried fruit in comparison with the total resulting from the process.

[0201] The dosage of capsaicin, the main alkaloid giving the chili pepper its spicy character and of interest in animal nutrition / health, in particular for its anti-inflammatory potential, was also carried out (comparison of fresh fruit, fruit dried at 100°C, and product from said process).

[0202] Methanolic extractions were thus carried out from: 1) fresh Habanero pepper fruits on one hand and red pepper on the other; 2) whole fruits oven-dried at 100°C of Habanero chili pepper on the one hand and red chili pepper on the other; and 3) of the total resulting from the process, from Habanero pepper on the one hand and red pepper on the other hand, as described above.

[0203] The extracts were also analyzed by UHPLC-DAD-MS / MS as described in the carotenoid analysis section. Each dosage was normalized to be equivalent to the dry mass of the pepper and to be able to establish a comparison regarding the potential loss of metabolites following drying.

[0204] The absolute quantification of capsaicin in samples of fresh Habanero peppers and red peppers, oven-dried at 100°C and dehydrated according to the method according to the invention, is illustrated by [fig.6] (A- case of Habanero pepper and B- case of red pepper) representing the quantity of capsaicin in mg / g (UHPLC-MSMS, MRM identification mode).

[0205] Habanero pepper contains a significant level of capsaicin (10.9 mg / g DM) compared to red pepper (0.67 mg / g DM).

[0206] In the case of the Habanero pepper as in that of the red pepper, the same trend was observed. The capsaicin concentration of the pepper dried in the oven at 100°C is significantly lower than that of the fresh pepper (43% and 81%, in dry mass equivalent of the fresh pepper, respectively for the Habanero pepper and the red pepper).

[0207] Interestingly and very advantageously, the capsaicin content of the totum resulting from said process (in equivalent dry mass of chili contained in the totum) is almost equivalent to the content of fresh chili, i.e. 95% for Habanero chili and 99% for red chili.

[0208] To summarize, according to the results thus obtained, the capsaicin studied in Habanero and red peppers is in higher concentration in fresh fruits but in a quasi-equivalent manner in the totum resulting from said process. A very low loss is therefore observed during the dehydration of the pepper fruits by said process in total opposition to the drying of the fruits in the oven which induces a loss of between 19% and 57% of the capsaicin initially contained in the fresh fruit depending on the genetics of the pepper treated.

[0209] Example 6: Microbiological study on the conservation of totum

[0210] The method described in Example 1 was implemented.

[0211] The results of the microbial development observed from the suspensions of totum obtained from: 1) 50% palm oil / 50% fresh Habanero pepper; and 2) 50% glycerol monolaurate (GML or MGL) / 50% fresh Habanero pepper; are compiled in Table 4 below.

[0212] Table 4: Product MGL / fresh Habanero pepper qno? 'rfy? 5 bacterial colonies (CFU) Fungal colony not observed No bacterial or fungal colonies Product pqlme oil / fresh Habanero pepper OU / jy ..A j / a 66 bacterial colonies (CFU> 7 fungal colonies Bacterial colonies 340 .Fungal colonies about 80 (difficult to count due to "spreading of colors;

[0213] Thus, due to its solvent properties (extraction of plant metabolites and antimicrobial properties, glycerol monolaurate is a preferred fat for the stabilization of fresh plants and preservation of the totum (storage). The totum obtained with palm oil may require the use of preservative(s).

[0214] Example 7: Process carried out from fresh Habanero pepper in glycerol monolaurate with addition of the plant material in two stages

[0215] The different stages of the process (with the addition of the plant material in two stages, i.e. the completion of two cycles as illustrated by [fig.2]) according to the invention are implemented according to the conditions more particularly defined in Table 5 below.

[0216] Table 5: ROBOQBO TEST PROTOCOL Grinder cooker PROTOCOL Formula: GML SOOg Fresh plant material Whole Habanero chili 1000g (500g cycle 1 + 500g cycle 2) Device settings: Product temperature HO'C Cooking time before grinding cycle 1 10min Cooking speed cycle 1 500 rpm Grinding time cycle 1 10 min Grinding mixer speed cycle 1 3000 rpm Cooking and mixing time after grinding cycle 1 10min Cooking time before grinding cycle 2 10min Cooking speed cycle 2 500 rpm Grinding time cycle 2 10 min Grinding mixer speed cycle 2 3000 rpm Cooking and mixing time after grinding cycle 2 10min Raw material temperature at inlet 17 'C Use of vacuum 700 stay NO Product characteristic: Product appearance Color red dark - color and odor more pronounced than for the 50% GML / 50% Hananero fresh product Humidity humidim be 1 4.00%

[0217] The totum thus obtained comprises a water content of the order of 2% and has the appearance of a smooth and homogeneous paste, dark red in color, with a more pronounced color and odor than for the totum obtained according to example 4 (with the addition of the chili pepper at one time and carrying out a single cycle).

Claims

Claims

1. A process for preparing a totum which is a mixture of a vegetable matter with a fat which is solid at room temperature, characterized in that it comprises the following steps according to which: (a) the vegetable matter is fresh and comprises at least 10% water by mass of water relative to its total mass (mass / mass) before or after loss on drying, taken alone or as a mixture, whole or in part, is brought into contact, preferably with stirring, with the fat chosen from a fat and a hydrogenated oil, at a temperature between 50°C and 180°C; (b) the vegetable matter - fat mixture thus obtained is then ground at a temperature between 50°C and 180°C; (c) the ground material obtained at the end of step (b) is heated, preferably with stirring, at a temperature between 50°C and 180°C to dehydrate the mixture;and (d) a solid totum at room temperature comprising a water content of less than or equal to 4% by mass of the total mass of the totum is recovered.;

2. Method according to claim 1, characterized in that an additional step of filtration of the dehydrated ground material obtained at the end of step (c) is carried out, to recover a solid filtrate at room temperature.

3. Method according to one of claims 1 or 2, characterized in that steps (a), (b) and (c) are carried out in the dark.

4. Method according to one of the preceding claims, characterized in that the fresh plant material, taken alone or in a mixture, is chosen from fruits, whole plants, aerial parts of plants, roots, bulbs, tubers, seeds, skins, pulps, macerates, cakes, or any other by-product of plant material.

5. Method according to claim 4, characterized in that the fresh plant material is chosen in whole or in part from wormwood, yarrow, garlic, wild garlic, artemisia, artichoke, pink berry, goji berry, burdock, basil, coffee, chamomile, cinnamon, blackcurrant, lemon, lemongrass, hemp, coriander, turmeric, cypress, eucalyptus, fenugreek, ash, juniper, clove, ginseng, ginger, pomegranate, hibiscus, hops, bay leaf, lavender, lemon grass, alfalfa, flax, mint, peppermint, mallow, lemon balm, mustard, white mustard, walnut, hazelnut, orange, oregano, nettle, onion, paprika, pansy, pepper, chili, pine, dandelion, pepper, rosemary, grape, savory, sage, wild thyme, marigold, tansy, tea, thyme, clover, goldenrod, preferably peppers and chilies of the genus Capsicum annuum, frutescens, chilies of the genus Capsicum chinense, garlic, ginger, grape, thyme, paprika, more preferably chilies of the genus Capsicum annuum, frutescens, and chilies of the genus Capsicum chinense.

6. Method according to one of the preceding claims, characterized in that the hydrogenated fat or oil, taken alone or as a mixture, is chosen from glycerol monolaurate, glycerol monocaprate, glycerol monomyristate, glycerol monopalmitate, glycerol mono-stearate, almond oil, peanut oil, argan oil, avocado oil, calophyllum oil, safflower oil, rapeseed oil, coconut oil, wheat germ oil, jojoba oil, corn oil, hazelnut oil, apricot kernel oil, virgin olive oil, palm oil, grape seed oil, castor oil, sesame oil, soybean oil, or sunflower oil, preferably glycerol monolaurate, glycerol monocaprate, hydrogenated palm oil and hydrogenated sunflower oil, more preferably glycerol monolaurate.

7. Solid totum or filtrate at room temperature capable of being obtained by the process according to one of claims 1 to 6.

8. Use of a totum or filtrate according to claim 7, for the preparation of a food or cosmetic composition.

9. Composition comprising a totum or filtrate according to claim 7, for its pharmaceutical, nutraceutical or animal health use.