Method for cold extraction-emulsification of hydrophobic compounds from a raw material of natural origin by magnetic turbulence

Abstract

The invention relates to the field of methods for preparing aromatic and phytotherapeutic compositions. More particularly, the invention relates to a method for extracting-emulsifying hydrophobic molecules in an aqueous solution by applying a magnetic field and obtaining a stable emulsion. The extraction is achieved by the agitation created by the magnetic field in the form of turbulence. This extraction is carried out under cold conditions and preserves the integrity of the molecules extracted by the method.

Description

COLD EXTRACTION-EMULSIFICATION PROCESS OF HYDROPHOBIC COMPOUNDS FROM NATURAL RAW MATERIALS BY MAGNETIC TURBULENCE

[0001] The invention relates to the field of processes for preparing aromatic and phytotherapeutic compositions. More particularly, the invention concerns a process for extracting and emulsifying hydrophobic molecules in an aqueous solution by applying a magnetic field and obtaining a stable emulsion. The extraction is achieved through the agitation created by the magnetic field in the form of turbulence. This extraction is carried out at room temperature and preserves the integrity of the molecules extracted by the process. Scope of the invention

[0002] Phytocompounds have been used for centuries for their medicinal properties. Consequently, numerous methods for extracting these compounds have been developed, including maceration (soaking plants in a solvent at room temperature for several days), digestion (similar to maceration but with slight heating), infusion (immersing plants in boiling water for approximately 15 minutes), percolation (slowly passing a solvent through the plants to extract the compounds), decoction (boiling plants in water for 15 to 60 minutes), and Soxhlet extraction (using a hot solvent for continuous extraction). These methods are based on simple principles of interaction between solvents and plant material, under ambient temperature conditions or with heating.They have major limitations such as long extraction times, limited yield and high solvent consumption.

[0003] Faced with these constraints, improved extraction methods have emerged that are faster, more efficient, and more environmentally friendly. Among these advances are accelerated solvent extraction (ASE), which uses high temperature and pressure conditions to reduce extraction time; microwave-assisted extraction (MAE), which optimizes heat transfer to improve yield; ultrasonic-assisted extraction (UAE), which increases the contact surface area between the solvent and plant material; and supercritical fluid extraction (SFE), which exploits the properties of supercritical fluids such as CO₂. Other approaches, such as enzyme-assisted extraction (EAE) and pressurized hot water extraction (PHWE), also aim to meet the requirements of sustainability and efficiency.

[0004] Among modern techniques for extracting natural molecules, subcritical water extraction (SWE) stands out for its ecological nature and its ability to valorize agricultural by-products. Water, used as the sole solvent under moderate temperature and pressure conditions, exhibits adjustable dielectric properties comparable to those of traditional organic solvents, while avoiding their adverse environmental impact. However, its implementation remains costly and technically demanding, thus limiting its widespread adoption.

[0005] Extraction processes for aromatic compounds from solid raw materials rely primarily on the use of high mechanical energy coupled with stabilizing agents such as surfactants. These processes often require complex operating conditions, including high temperatures and specialized equipment such as high-pressure homogenizers, ultrasonic cleaners, or microfluidizers. While effective, these methods have significant limitations when it comes to preserving the integrity of volatile organic compounds, which are particularly sensitive to heat and intense mechanical treatment.

[0006] In recent scientific research, the application of magnetic fields has attracted increasing interest due to their effects on aqueous systems and molecular structures. Several studies have shown that magnetic fields can influence the physicochemical properties of water, notably the work of G. H. Pollack, which involved subjecting water to vibrational, light, or magnetic energy; a reorganization of the molecular order (hexagonal sheets) and a separation of charges were observed.

[0007] Magnetic fields can also play a role in fluid dynamics. By creating a controlled turbulent regime, they induce chaotic changes in pressure and flow velocity. This turbulence process, often described by the Richardson cascade model, allows energy to be transferred from large scales to smaller scales, where it is dissipated. Some experimental studies have explored the use of magnetic fields to generate small-scale turbulence in liquids. This research has demonstrated that the energy dissipation thus created is proportional to the strength of the applied magnetic field and the configuration of the moving particles in the fluid. Finally, more advanced hypotheses suggest that the application of magnetic fields could induce quantum phenomena, observed in specific liquid environments.Molecular reorganization resulting from vibrational or magnetic energy can generate a separation of charges within the medium, thus forming new structural arrangements.

[0008] Thus, recent work reports the use of a magnetic field for the preparation of a stable emulsion by magnetic turbulence from two immiscible solutions; this process is described in document WO2024 / 218090.

[0009] The state of the art also reveals a reliance on surfactants to stabilize oil-in-water emulsions. Their presence, essential in conventional formulations, poses several problems. On the one hand, these stabilizing agents, although effective, can alter the organoleptic and sensory properties of aromas, which is particularly critical in the perfume and food industries where the faithful reproduction of volatile characteristics is a priority. On the other hand, the excessive use of surfactants raises environmental and regulatory concerns, especially for applications requiring natural and ecological solutions.

[0010] Faced with these limitations, there is a need to develop innovative processes that allow for the efficient extraction of aromatic or phytotherapeutic compounds, while preserving these fragile compounds and reducing environmental impact. This need is particularly pronounced in the perfume, cosmetics, herbal medicine, and food industries, where the demand for natural and additive-free formulations continues to grow.

[0011] The inventors have developed a process for extracting valuable hydrophobic molecules from solid natural materials and stabilizing them as emulsions in water, without mechanical action or the addition of stabilizers. This approach provides access to new natural raw materials in aqueous solution for the perfume industry, as well as for various sectors of the food industry, including flavored beverages and dietary supplements.

[0012] This approach is based on the hypothesis that vibrational energy applied to the mixture would create turbulence, generating a new molecular order with charge separation that ensures strong system stability. This energy would be capable of inducing the extraction of hydrophobic compounds from a solid raw material and emulsifying these compounds, which constitute a lipid fraction, in a continuous aqueous phase. The turbulent agitation would not be physical in nature but rather akin to a quantum phenomenon. This energy would generate a rearrangement in the continuous aqueous phase and finely disperse the lipid phase of the emulsion, resulting in a new molecular arrangement and charge distribution.

[0013] This technology represents a complete break from conventional practices in the field of molecule and emulsion extraction. It enables the extraction of hydrophobic molecules contained in a solid material and their stabilization in the form of emulsions without the use of stabilizing agents or direct mechanical forces; at low temperatures and with extremely low operating energy consumption.

[0014] Beyond understanding the phenomena present and their analysis, the observed effects effectively show that the application of a magnetic field allows the extraction of hydrophobic compounds contained in a solid natural raw material and their stabilization in aqueous solution by the creation of a stable emulsion.

[0015] Thus, the present invention relates to a process for the extraction-emulsification of hydrophobic aromatic compounds from a solid natural raw material by magnetic turbulence comprising the steps of: Suspension of said solid raw material in an aqueous solution. Treatment of said solution by application of a constant and permanent magnetic field of an intensity between 300 and 2,000 mT for a duration between 30 min and 8 h.

[0016] The invention also relates to the implementation of the process as described above for the preparation of a stable oil-in-water nano-emulsion, and a process for formulating a complex aqueous composition from such a nano-emulsion. Advantages of the invention

[0017] The process according to the invention allows for the gentle extraction of hydrophobic molecules from a solid, naturally sourced raw material, at low temperatures and without any external energy input, either in static mode or with very low electrical consumption when the solution containing the solid is agitated. This extraction method is unprecedented, combining efficiency and preservation of the extracted active ingredients, without mechanical action or heating of the material.

[0018] The process allows the extraction and solubilization of hydrophobic compounds in the form of a stable and transparent / translucent or opalescent nano-emulsion without any chemical addition or surfactant.

[0019] The stable emulsified system preserves the integrity of the material, including odor characteristics, and very interestingly, even those of volatile organic compounds.

[0020] The resulting emulsion is transparent, with gradients from crystalline to translucent depending on the nature and concentration of the oil fractions. With average particle sizes ranging from 1 micron to 500 nanometers, this transparency can be explained by the formation of weak intermolecular bonds, such as Van der Waals forces.

[0021] The solubilization of the extracted compounds occurs at low temperatures while remaining efficient, as the emulsion can contain concentrations of hydrophobic molecules ranging from 1% to 30%.

[0022] Furthermore, the result of the dissipation of the applied magnetic energy in the liquid creates a natural cooling which avoids the need for external systems essential to counteract mechanical heating or that related to the extreme pressure or temperature conditions of the extraction and production processes of emulsions.

[0023] Finally, the overall process requires electrical energy only to operate the actuators that control the distance between the permanent magnets and, if necessary, to activate a pump for circulating the solutions between the magnets. This low (or nonexistent) electrical energy requirement, along with the water savings used for cleaning the equipment, gives the process a significant environmental advantage. DETAILED DESCRIPTION OF THE INVENTION

[0024] A first object of the invention relates to a process for the extraction-emulsification of hydrophobic compounds in aqueous solution from a solid natural raw material by magnetic turbulence comprising the steps of: Suspension of said solid raw material in an aqueous solution Treatment of said solution by application of a constant and permanent magnetic field of an intensity between 300 and 2,000 mT for a duration between 30 min and 8h.

[0025] Applying a magnetic field generates turbulence within the solution. This turbulence must release sufficient energy to induce the extraction of hydrophobic compounds. This process also reduces the size of the hydrophobic droplets, resulting in a stable emulsion. In this sense, it is an extraction-emulsification process.

[0026] By "constant magnetic field" we mean a magnetic field whose intensity does not vary over time.

[0027] A "permanent magnetic field" is a field generated by a permanent magnet. Generating a permanent magnetic field requires no electrical power.

[0028] For the purposes of this invention, "magnetic turbulence" means hydrodynamic turbulence induced by one or more constant magnetic fields.

[0029] Hydrodynamic turbulence (fluid movement) is a complex and chaotic phenomenon that occurs in a fluid (liquid or gas) when it flows at sufficiently high speeds or when it is subjected to disturbing forces. It is characterized by unpredictable, disordered, and swirling movements that contrast with laminar flows, where fluid particles follow parallel and regular paths.

[0030] Hydrodynamic turbulence manifests itself as an energy spectrum, often modeled by Kolmogorov theory. This theory states that at intermediate scales, energy is transferred from large eddies to small ones without loss (energy cascade), before being dissipated by viscosity.

[0031] A magnetic field can induce turbulent flow in a conducting fluid by generating Lorentz forces, instabilities, and chaotic dynamic fluctuations in the fluid, characteristic of turbulence. The energy cascade, nonlinear interactions, and feedback between fluid motion and the magnetic field are the driving forces behind this turbulence.

[0032] In order to establish a desired magnetic turbulence, the intensity of the constant magnetic field applied to the solution must be sufficient to create a turbulent regime that causes the extraction-emulsion.

[0033] This intensity is generally between 300 mT and 2000 mT. In a preferred embodiment, this intensity is between 500 mT and 1500 mT. This intensity may vary depending on the duration of the treatment, which is generally between 30 minutes and 8 hours, preferably between 1 and 5 hours.

[0034] One particular embodiment consists of applying a magnetic intensity of between 500 mT and 1500 mT for a period of between 2h and 6h, and in a more particular embodiment of applying an intensity of between 650 mT and 950 mT for a period of between 1h and 4h.

[0035] The magnetic field applied to the solution, which creates magnetic turbulence, has an intensity of at least 300 mT measured at the surface of the magnet. This measurement can be performed using a magnetometer or gaussmeter.

[0036] The operation of a gaussmeter is based on measuring the magnetic field using magnetic sensors. The sensor is positioned near the object or electromagnetic system to be measured. The sensor detects variations in the magnetic field and converts them into a value readable on the screen. Here, the sensor is placed in contact with the surface of the magnet to obtain the local value. Preferably, the sensor is moved across the surface of the magnet, and the display shows the highest point measured.

[0037] In a particular embodiment of the invention, the sample to be treated is brought into contact with the magnetic surface through a suitable container (flexible pouch, stainless steel or ceramic container, glass tube, etc.). In this case, the intensity of the magnetic field applied to the sample corresponds to the intensity of the magnetic field measured at the surface of the magnet.

[0038] Preferably, the magnetic field used in the process according to the invention is obtained through the use of permanent magnets.

[0039] A "permanent magnet" is defined as a material or device capable of producing a persistent magnetic field without external energy input, due to the stable orientation of its internal magnetic domains. Such magnets can be composite, sintered, or made of charged polymers.

[0040] In a preferred embodiment, the permanent magnet is a neodymium magnet of grade equal to or greater than N45. In a most preferred embodiment, it is a neodymium magnet of grade N52.

[0041] The grade of a neodymium magnet indicates the magnetic energy that the material can store per unit volume. The grade corresponds to the maximum magnetic energy, called (BH)max, and is expressed in Mega Gauss-Oersted (MGOE).

[0042] For identical dimensions and geometry, a higher-grade magnet material will exert a force approximately proportional to its (BH)max. The grade is derived from the intrinsic magnetic properties of the magnet alloy: remanence, coercivity, and intrinsic coercivity. These values ​​depend on the exact composition of the alloy, its microstructure (grain size, crystallographic texture, homogeneity, obtained through sintering or injection molding), the heat treatment, and the magnetization process.

[0043] For neodymium magnets, the grade number corresponds to the (BH)max. Thus, a grade N45 magnet has a (BH)max of approximately 45 MGOe and a grade N52 magnet has a (BH)max of approximately 52 MGOe.

[0044] However, the grade is not the only descriptive parameter of a magnet. For the same grade, the actual attractive force depends strongly on the geometry (thickness, magnet length, L / D ratio), the magnetic circuit configuration (pole pieces, air gap) and the distance to the steel part.

[0045] Thus, within the framework of the present invention, the magnet used preferably has a minimum surface area of ​​25 cm² 2 (for example a 5x5 cm square). This minimum surface area per magnet is increased when 2 or more pairs are used, particularly when a magnet system is implemented.

[0046] Thus, in a preferred embodiment of the invention, the neodymium magnets used produce a (BH)max equal to or greater than 45 MGOe, or even equal to or greater than 48 MGOe, or even equal to or greater than 50 MGOe and preferably equal to or greater than 52 MGOe.

[0047] To create a magnetic field suitable for the needs of the process described in the invention, an array of fixed magnets can be used. These magnets can be arranged in various configurations, such as a magnet cage or other specific assemblies, to form particular structures. In these systems, the magnets are positioned and fixed in such a way as to force poles of the same sign to remain opposite each other. The magnets are arranged by placing at least two magnetic poles of identical polarity in opposition, by assembling permanent magnets in rows of identical North / North, South / South, or alternating North / South polarities. The magnets are placed close together to obtain the desired magnetic intensity; the distance between the magnets depends, in particular, on the volume of the solution to be treated, and the intensity can be adjusted according to the duration of the treatment.

[0048] In a preferred embodiment of the invention, the magnetic field is generated by placing at least one pair of magnets of identical polarity and strength in opposition. In a particular embodiment, the magnetic field is generated by placing two magnets (a pair) of identical polarity and strength in opposition.

[0049] In particular embodiments of the invention, the magnetic field is generated by at least two pairs of magnets of identical polarity arranged in north / north, south / south or alternating north / south rows. The magnets may in particular form a magnetic system.

[0050] For the purposes of this invention, a "magnetic system" is defined as a fixed structure comprising several magnets (at least two pairs) whose properties and behaviors emerge from the complex interaction between several components or degrees of freedom. Each magnet influences the overall field according to its orientation, intensity, and relative position. This interaction can lead to areas of reinforcement (if the fields add together) or partial cancellation (if the fields oppose each other). Furthermore, the magnets themselves can influence each other: their magnetic moments can adjust or reorient themselves slightly under the effect of the magnetic forces they exert on one another, thus modifying the overall field. This dynamic makes the behavior of magnetic fields in a multi-magnet system both rich and disordered, but not random.

[0051] In a particular embodiment of the invention, the magnetic field is generated by a magnetic system. In a magnetic system, each pair of magnets consists of magnets of the same strength.

[0052] It is understood that in a magnet system according to the invention, the magnets are fixed and generate a constant magnetic field. No electric current is applied to the system; the magnetic field is generated solely by the opposing forces between the magnets, preferably permanent magnets. In particular, no oscillating current is applied, and the magnetic system generates no heat.

[0053] The "gradient" of a magnetic field represents the spatial variation of the intensity or direction of the magnetic field in a certain region of space.

[0054] The superposition of magnetic fields can lead to complex gradients within the magnetic field. The main factors influencing the gradients in such a configuration are the strength and orientation of the magnets, the distance between the magnets, and the geometric configuration.

[0055] Magnetic field gradients, combined with fluid motion, can create hydromagnetic instabilities. Instabilities such as those observed in magnetic convection or Tayler instabilities can occur if the magnetic fields are sufficiently strong. These instabilities amplify the initial disturbances, creating vortices or chaotic structures within the fluid.

[0056] When magnets create areas of strong repulsion or magnetic pressure gradients in the fluid, shear flows can form. These flows are known to become turbulent if their amplitude exceeds a certain threshold (critical Reynolds number).

[0057] Within the scope of the present invention, magnetic turbulence can be obtained using a magnetic system. In a magnetic system according to the invention, the magnetic field is generated by placing at least two fixed magnets of the same polarity and strength in opposition, the intensity of the magnetic field thus generated being greater than or equal to -300 mT. The magnetic intensity can therefore be generated by any number of pairs of magnets meeting this definition. Thus, it is possible to combine 2 pairs of magnets, 3 pairs of magnets, 4 pairs of magnets, at least 5 pairs of magnets, between 2 and 10 pairs of magnets, and any other combination.

[0058] The magnets used to create the magnetic field are arranged to create a space for the aqueous solution containing the solid material from which hydrophobic compounds are to be extracted. The solution can be contained in a bag, for example, a polypropylene bag. Preferably, the solution is positioned between the magnets so that the mixture is subjected to the magnetic field.

[0059] Alternatively, the solution can be subjected to a magnetic field created by a single magnet if the intensity of the field generated is sufficient to create the required magnetic turbulence. The mixture can be placed in a static position or set in motion during the treatment.

[0060] The application of an aqueous solution containing solids to a constant and permanent magnetic field allows the extraction of lipid components contained in the solid matter, the reduction in size of particles immiscible in water, and the stabilization of the emulsion which then presents a transparent or translucent appearance.

[0061] For the purposes of this invention, "aqueous solution" means pure or demineralized water; this water may be enriched, for example, with vitamins and / or amino acids.

[0062] The solid raw material is of natural origin, the objective being to extract hydrophobic compounds of interest and emulsify them finely in an aqueous solution. The efficiency of the process allows for a good extraction yield and the preparation of a stable composition with a concentration of extracted compounds that can reach up to 30%.

[0063] For the purposes of this invention, "solid raw material of natural origin" means a material of plant or animal origin.

[0064] When of plant origin, it can be chosen from whole fresh or dried plants, flowers, seeds, roots, flowering tops, plant by-products, or any other part of the plant likely to contain hydrophobic molecules. The term "raw material of plant origin" encompasses all plant organisms, including parts of trees or shrubs, flowers, succulents, mosses, etc.This can be organic matter of plant origin such as dead wood, possibly decomposing or fermented plant matter… We can mention, without being exhaustive, the following plants whose aromas are sought after both for their aromas used in cooking, and for the olfactory notes used in perfumery: vanilla, clove, ginger… but also all medicinal plants from which phytocompounds can be extracted for use in cosmetics, phytotherapy or in food supplements.

[0065] In a particular embodiment of the invention, the plant-based raw material is chosen from vanilla, cloves, and ginger.

[0066] When it is of animal origin, it can be chosen from, for example, ambergris produced by sperm whales or castoreum.

[0067] The solid raw material is suspended in an aqueous solution in which the hydrophobic compounds are found after extraction. This aqueous solution can be defined as a solution whose solvent is water and whose conductivity is between 0.05 and 800 microSiemens / cm, preferably between 0.05 and 30 microSiemens / cm.

[0068] Suspension is achieved through physical action. This is preferably a "gentle" mechanical agitation, such as manual stirring, the use of a propeller shaker, a homogenizer, or a pump connected to a recirculation loop. This suspension must not affect the raw material in order to preserve the naturalness of the hydrophobic molecules. Therefore, in the context of this invention, suspension does not rely on techniques such as sonication or the addition of surfactants or other agents designed to improve dispersion.

[0069] Thus, the invention relates to the use of a magnetic field with an intensity between 300 and 2,000 mT for a duration between 30 min and 8h to extract hydrophobic compounds of interest from a solid plant or animal raw material.

[0070] A second object of the invention relates to the implementation of the process as described above for the preparation of a stable aromatic or phytotherapeutic oil-in-water nano-emulsion.

[0071] The extraction process described above allows the hydrophobic compounds extracted through the application of a magnetic field to be emulsified. The resulting emulsion is oil-in-water. It is stable over time and resistant to temperature changes. The stability of the emulsion ensures the stability of the aromatic and phytocompounds, and their preservation over time.

[0072] The term "nano-emulsion" refers to an emulsion composed of two immiscible liquid phases, one of which is dispersed within the other as droplets with an average size of 500 nm, and overall sizes ranging from 1.5 microns to 250 nm. In this case, it is an oil-in-water nano-emulsion, meaning it contains oil droplets dispersed in an aqueous solution. The nano-emulsion has a translucent or opalescent appearance. Specifically, this nano-emulsion is obtained without the addition of a surfactant.

[0073] For the purposes of this invention, "aromatic compound" means any hydrophobic compound to which a taste or odor is associated for applications in cooking, particularly in the food industry, and in perfumery (body perfumes, home fragrances, and cosmetics). These may include volatile organic compounds (VOCs).

[0074] For the purposes of this invention, "phytocompound" means any hydrophobic chemical compound derived from plant material. This includes, in particular, compounds described as active ingredients and used in herbal medicine and food supplements.

[0075] Remarkably, the emulsion is obtained cold and can contain concentrations ranging from 1% to 15% of hydrophobic compounds: it is stable and obtained without any stabilizing agent. For example, the emulsion's stability can be achieved by treating a mixture of pure water and an aromatic oil fraction to be dispersed, specifically the hydrophobic fraction containing molecules extracted from the naturally occurring solid raw material.

[0076] In a particular embodiment of the invention, the aromatic nano-emulsion is a concentrate of at least one essential oil. This is an aqueous formulation of essential oils. The essential oil concentration can reach up to 30%, which is quite remarkable. This new formulation addresses market needs where the use of essential oils is limited by their immiscibility in water. It makes it possible to offer easy-to-use aqueous solutions of essential oils. The concentration can be adapted to specific requirements and helps manage the risk of overdose.

[0077] A third object of the invention relates to a method for formulating a complex aqueous aromatic or phytotherapeutic composition comprising: The preparation of a nano-emulsion according to the method defined above; The mixing of this nano-emulsion with at least one other aqueous composition.

[0078] The "at least one other aqueous composition" can be an aromatic or non-aromatic composition and / or phytotherapeutic or non-phytotherapeutic.

[0079] This process allows the preparation of various aromatic or phytotherapeutic compositions such as an aqueous perfume, a cosmetic composition, a flavored drink, a flavored food, an aqueous composition of essential oils, an aqueous extract for use as a food supplement.

[0080] The present invention will be better understood by reading the following examples, which are provided by way of illustration and should in no way be considered as limiting the scope of the present invention. DESCRIPTION OF THE FIGURES

[0081] Gas chromatographic analysis of clove extract. Top: Control corresponding to the profile of a clove extract not treated by the process according to the invention (identical preparation conditions). Middle: Clove extract obtained by the process according to the invention. Bottom: Peak of eugenol, the main component of clove. Reference profile of the molecule CAS 97-53-0 at 500 ppm.

[0082] Gas chromatographic analysis of vanilla extract: Top: Control vanilla corresponding to the profile of an untreated vanilla extract (preparation conditions identical). Middle: Vanilla extract obtained by the process according to the invention. Bottom: Vanilla extract: reference profile of the molecule CAS No. 121-33-5 at 500 ppm. EXAMPLES

[0083] EXAMPLE 1: Extraction-emulsification process carried out using citrus peels

[0084] Prior art: To extract aromatic substances from citrus fruits cold, without resorting to the hydrodistillation process, a method of treatment by expression is commonly practiced.

[0085] This process is reserved for the fresh pericarp of citrus fruits. It consists of bursting, through various mechanical methods such as abrasion, compression, incision, or perforation, the pockets located on the surface of the peel (epicarp) of these fruits, which contain the essential oil. The released oil is then collected by a stream of water. As the two substances are immiscible, they are separated by decantation.

[0086] Method according to the invention: It allows, in the same sequence by contact with a stream of water at room temperature, the extraction and emulsification of citrus essential oil in a single operation.

[0087] In this example, 18 grams of fresh zest are removed from a Bergamot lemon by peeling the peel. The zest is cut into strips approximately 2 cm long and then placed in a 50-micron thick, low-density polypropylene bag with 162 g of demineralized water. The zest represents 10% of the total preparation.

[0088] The material used to create the magnetic field is an assembly of permanent magnets generating an intensity of 450 mT, and steel forming a pattern capable of delivering the magnetic energy required to achieve the desired emulsion extraction result.

[0089] First, a mild steel plate measuring 27 cm long, 12 cm wide, and 1.5 cm thick is prepared. It is enclosed on all four sides by a band 1 cm wide and 2 cm high. Three neodymium permanent magnets, each measuring 10 cm x 10 cm x 2 cm, are then placed on the plate. It is important to alternate their polarity, in this case, north / south / north.

[0090] A second shelf, exactly identical to the first, is placed above the first, in direct opposition. The height between the shelves is variable and adjustable.

[0091] The bag containing the lemon preparation is placed on the bottom tray, 7 cm from the top tray for 70 minutes then 4 cm for 80 minutes.

[0092] The result is a stable, dark yellow emulsion with a strong lemon odor and no oily traces or residue.

[0093] The final pH of the resulting emulsion is 3.96. It is maintained with 0.4% potassium sorbate.

[0094] The emulsion is stable in an oven at 50°, at room temperature and at 4° for two months.

[0095] EXAMPLE 2: Qualitative and quantitative analysis of aromatic extracts obtained by the process according to the invention by chromatography

[0096] Two reference plant-based raw materials with low water solubility were used to demonstrate the efficiency of the process: cloves and vanilla. The analysis focused on the extraction of the following:

[0097] - eugenol contained in cloves, which is soluble at 2.463g / 100ml

[0098] - vanillin contained in vanilla, which is soluble at 1g / 100 ml.

[0099] The procedure used is as follows:

[0100] A so-called "Control" sample was prepared by mixing 1g of whole cloves with 15g of demineralized water at 21°C.

[0101] A so-called "Treated" sample was prepared in the same way but it was subjected to a magnetic field for 110 min.

[0102] The same protocol was applied to 1g of vanilla bean mixed with 15g of demineralized water at 21°C.

[0103] Gas chromatographic analyses were carried out in a university laboratory to evaluate the concentrations of targeted molecules and to compare the treated and control samples. Results obtained from cloves

[0104] The results are presented at.

[0105] The representative peak of eugenol present in clove essential oil appears at a retention time of 10.353 minutes. For a standard with a concentration of 500 ppm, the peak area is 644433.

[0106] In the analysis of the control sample, the eugenol peak appears at a retention time of 10.416 minutes and an area of ​​83721.

[0107] On the analysis of the treated sample, we find the peak of eugenol at 10.421 minutes with an area of ​​1628551.

[0108] We can see that the eugenol peak is not saturated, so we need to calculate the concentration of eugenol present in the samples.

[0109] NamesConcentration in ppmStandard Area500644433Treated Sample12631628551Control Sample64.983721

[0110] Table 1: Eugenol concentrations in the samples

[0111] We can see that there is 19.5 times more eugenol in the treated sample than in the control sample. This result demonstrates that the application of a magnetic field allows for the very efficient extraction of eugenol molecules present in cloves.

[0112] The calculations were performed as follows:

[0113]

[0114]

[0115] Results obtained from vanilla

[0116] The results are presented at.

[0117] Vanillin present in the vanilla pod is released after a retention time of 7.017 minutes. For a reference molecule concentration of 500 ppm, the peak area is 344557.

[0118] In the analysis of the control sample, the representative peak of vanillin appears at a retention time of 6.882 minutes and an area of ​​1085839.

[0119] In the analysis of the treated sample, the vanillin peak appears at 6.865 minutes with an area of ​​28892960. We observe that the vanillin peak is saturated, which indicates that its concentration in the sample is too high.

[0120] We can therefore perform a calculation to estimate the concentration of vanillin present in the samples, however for the Treated sample the concentration obtained will be a minimum concentration of vanillin present in it due to the phenomenon of saturation.

[0121] NamesConcentration in ppmStandard Area500344557Treated Sample4192728892960Control Sample15751085839

[0122] Table 2: Vanillin concentration in the samples

[0123] The results in Table 2 show that there is 26 times more (at least) vanillin in the Treated sample than in the Control sample.

[0124] The calculations were performed as follows:

[0125]

[0126]

[0127]

[0128] EXAMPLE 3: Extraction-emulsification of the products of ginger distillation

[0129] Ginger is mainly cultivated for its large rhizomes which, being storage organs, are mainly made up of starch, proteins and lipids but also contain 1 to 4% essential oil as well as certain phenolic compounds responsible for its spicy note: gingerols (with an ''s'' because the side chain of the molecule can be more or less long) as well as their derivatives gingerdiols and deoxygingerols (paradols).

[0130] The main gingerol is [6]-gingerol. It degrades mainly into [6]-shogaol (pungent) during dehydration and into zingerone during cooking / distillation.

[0131] The steam distillation of ginger from its rhizome yields the following products: Ginger essential oil:

[0132] It is composed of volatile aromatic compounds. The main active compounds include zingiberene, citral, camphene, and other terpenes responsible for the characteristic aroma of ginger. Ginger hydrosol:

[0133] This is the aromatic water that remains after distillation. It contains traces of water-soluble compounds and is used in cosmetics or as a culinary ingredient for its mild and aromatic properties.

[0134] These products have applications in the food, cosmetic, pharmaceutical, and aromatherapy industries for their stimulating, anti-inflammatory, and digestive properties.

[0135] In this example, the process according to the invention is applied to different products from the distillation of fresh ginger, namely: essential oil, hydrosol and exhausted rhizomes, cut into horizontal slices 1.5 cm thick.

[0136] 30 g of rhizomes are taken and mixed with 90 g of room-temperature hydrosol in a polypropylene bag. The mixture is then placed on the magnetic tray, with the top of the tray positioned 4.5 cm above the bag. The treatment is applied for 150 minutes.

[0137] The result is a slightly cloudy water with a pronounced pungent taste. This characteristic is evidence of the presence of shogaol, a phenolic compound responsible for ginger's spiciness. Shogaol is not extracted in the essential oil and is not present in the hydrosol because it remains primarily stored in the solid matter of the rhizome, including the residue after distillation. The presence of shogaol in the aqueous fraction confirms the extraction of this molecule under the influence of the applied magnetic field.

[0138] To obtain the full range of aromas characteristic of fresh ginger (unheated, undistilled), 1g of ginger essential oil can be added to the previously obtained enriched aqueous extract. The bag is then placed back on the magnetic tray, with the top part positioned 2 cm from the bag, for 20 minutes. Another 1g of ginger essential oil is then incorporated three times under strictly identical conditions, for a total of 4g dissolved in the preparation.

[0139] This example illustrates the possibilities offered by the process according to the invention, namely the preparation of an aqueous ginger extract comprising the various aromatic fractions of the rhizome, in particular that which is not extracted by distillation but is obtained by this process. It is possible to add the aqueous extract (hydrosol) and the oily extract (essential oil) and to emulsify the mixture using the applied magnetic field.

Claims

Extraction-emulsification process of hydrophobic compounds in aqueous solution from a solid natural raw material by magnetic turbulence comprising the steps of: Suspension of said solid raw material in an aqueous solution Treatment of said solution by application of a constant and permanent magnetic field of an intensity between 300 and 2000 mT for a duration between 30 min and 8h. The method according to claim 1 characterized in that the magnetic field is generated by placing at least one pair of magnets of identical polarity and of the same strength in opposition. The method according to claim 2 characterized in that the magnetic field is generated by at least two pairs of magnets of identical polarity arranged in north / north, south / south or alternating north / south rows. A method according to any one of claims 2 or 3 wherein said magnets are permanent magnets. A method according to any one of the preceding claims, wherein said permanent magnet is a neodymium magnet producing a maximum magnetic energy equal to or greater than 45 MGOe. A method according to any one of the preceding claims, wherein the magnetic field is generated by a magnetic system. A process according to any one of the preceding claims, wherein said aqueous solution is pure or demineralized water, optionally enriched with vitamins and / or amino acids. A process according to any one of the preceding claims, wherein said raw material of natural origin is chosen from a material of vegetable origin or a material of animal origin. A process according to claim 8 wherein said vegetable raw material is selected from vanilla, cloves, ginger. A process according to any one of claims 1 to 9 for the preparation of a stable aromatic or phytotherapeutic oil-in-water nano-emulsion. A process according to claim 10 characterized in that said nano-emulsion is a concentrate of at least one essential oil. Method for formulating a complex aqueous aromatic or phytotherapeutic composition comprising: The preparation of a nano-emulsion according to the process defined in claim 7 or 8. The mixing of this nano-emulsion with at least one other aqueous composition. A process according to claim 12 characterized in that said aromatic or phytotherapeutic composition is an aqueous perfume, a cosmetic composition, an aromatic beverage, an aqueous composition of essential oils, an aqueous extract for use as a food supplement.

Images