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WO2022050831A1 - Processus d'extraction de composé bioactifs dérivés de matière organique d'origine végétale - Google Patents

Processus d'extraction de composé bioactifs dérivés de matière organique d'origine végétale Download PDF

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Publication number
WO2022050831A1
WO2022050831A1 PCT/MX2020/000032 MX2020000032W WO2022050831A1 WO 2022050831 A1 WO2022050831 A1 WO 2022050831A1 MX 2020000032 W MX2020000032 W MX 2020000032W WO 2022050831 A1 WO2022050831 A1 WO 2022050831A1
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extraction
solvent
molecules
stage
mixture
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Spanish (es)
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Daniel ITURBE HUITRÓN
Luis Carlos ORRANTIA CANTÚ
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/028—Flow sheets
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0211—Solvent extraction of solids in combination with an electric or magnetic field
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0288—Applications, solvents
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/10—Production of fats or fatty oils from raw materials by extracting
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0292—Treatment of the solvent
    • B01D11/0296—Condensation of solvent vapours

Definitions

  • the present invention relates to a process for the extraction of bioactive compounds, which can be obtained from organic matter of plant origin, such as plants and/or flowers and/or fruits and/or shoots and/or roots and / or tubers of plant origin, by using organic solvents and, preferably, a microwave appliance.
  • bioactive agents derived from different sources in our research specifically those obtained from biomass or organic matter from plants and/or flowers and/or fruits and/or shoots and/or roots and/or tubers of vegetable origin.
  • bioactive agents derived from biomass or organic matter from plants and/or flowers and/or fruits and/or shoots and/or roots and/or tubers of vegetable origin.
  • the dielectric properties of plant products generally decrease rapidly when the moisture content decreases to a critical moisture level, below this moisture level the reduction in loss factor decreases due to bound water from plants and /or flowers and/or fruits and/or shoots and/or roots and/or tubers of plant origin, using this structural change of the water contained inside plant products reduces the use of high temperatures, positive pressure or negative pressure , in addition to excluding the use of inorganic solvents and different phases of extraction and recirculation of the process, which has a negative impact on obtaining molecules with biological activity.
  • Document EP1439218 describes a technology for the solvent-free microwave extraction of natural compounds, which specifically refers to an apparatus for the extraction of volatile matter from biological materials, for example, vegetable oils from plants; the steam decomposes the plant cells and releases oil vapour, there is an overflow channel that transports the water condensation to the connection channel and the oil accumulates in a container to be eliminated through an extraction valve.
  • EP1618798 describes a method for extracting a volatile natural substance (I) from biological material (II) comprising: (i) providing (II) to a microwave area; (ii) create a low pressure; (iii) irradiating (II) with microwaves to release at least a portion of (I); (iv) evacuating the released (I) to a condensation area; (v) cooling the released (I); and (vi) evacuating the released (I) from the condensation area.
  • Document EP1629725 aims to extract volatile natural material (I), at least partially soluble in water, from biological material (II) (containing water), comprising providing (II) in a microwave area, illuminating (II) to release (I), evacuate to a condensation area, cool the released (I) and evacuate it from the condensation area in a hydrophobic solvent to a solution of (I) containing the receiving vessel.
  • Document W02018009514A1 describes an apparatus and method for extracting plants, where said apparatus comprises an extraction module, a separation module and a tank.
  • the method essentially includes the preparation of plant material, decarboxylation, extraction and separation of active components, by using liquid tetrafluoroethane as solvent; The process also requires the insertion of oxygen and the venting of CO2.
  • Document W02018000094A1 is a method for extracting and decarboxylating cannabinoids from cannabis plant material, the method comprising decarboxylating cannabis plant material before, during or after extraction using microwave technology. Specifically it relates to decarboxylated cannabis resins and the use of the decarboxylated resins.
  • FIGURE 1 Scheme of the process, which begins with 1) the preconditioning of the organic matter from which the bioactive agents will be extracted, which mainly consists of eliminating excess moisture to leave it at 4%, and loading a solvent in a extraction chamber, thus proceeding with the 2) solvent load, 3) solvents and other elements are injected to start the physical change of the organic matter to obtain the bioactive agents, 4) the amount is kept constant of solvent under certain conditions of temperature and pressure to ensure the extraction of the bioactives, subsequently the 5) stabilization of the molecules is carried out to preserve the properties of the molecule, so that finally a 6) tempering of the the resulting mixture, so that it can be adequately post-processed.
  • FIGURE 2 Biological material drying curve, for the standardization of objective humidity of 4%, removing exact amounts of humidity out of the biological material through a continuous flow of air at a temperature of 24 °C and the emission of microwave ranges of 0.623 Watts/g ; the moisture loss of the biological material is expressed in a time of 10 minutes under the conditions of 24°C and the emission of microwave ranges of 0.623 Watts/g, it should be noted that the traditional or conventional methods of drying eliminate the moisture of the material for periods longer than 60 minutes.
  • FIGURE 3 Biological material drying curve, for the standardization of 4% objective humidity, removing exact amounts of humidity out of the biological material by means of a continuous flow of air at a temperature of 60°C and the emission of microwave ranges of 1.245 Watts/g; The moisture loss of the biological material is expressed in a time of 5 minutes under the conditions of 60 °C and the emission of microwave ranges of 1,245 Watts/g. It should be noted that the traditional drying methods manage to eliminate the moisture from the material in periods greater than 60 minutes.
  • FIGURE 4 Biological material drying curve, for the standardization of 4% objective humidity, removing exact amounts of humidity out of the biological material by means of a continuous flow of air at a temperature of 90°C and the emission of microwave ranges of 1 .868 Watts/g ; the loss of moisture of the biological material is expressed in a time of 4 minutes under the conditions of 90 °C and the emission of microwave ranges of 1,868 Watts/g, it should be noted that the traditional drying methods manage to eliminate the moisture of the material in period greater than 60 minutes.
  • FIGURE 5 Extraction curve loaded with solvent (H2O + C6H8O7), capable of redistributing particles in a uniform movement, emitting intermittent and continuous pulses with exact microwave ranges from 0.623 Watts/g to 6.23 Watts/g in an extraction time of 15 .45 and 60 seconds, expressed in equivalent mg of gallic acid per 100g dry basis at 4% target moisture; the different powers equivalent to continuous exact microwave ranges from 0.623 Watts/g to 6.23 Watts/g are observed, distributed with an estimated time of exposure to microwaves of 15.45 and 60 seconds, expressed in mg Gallic Acid Equivalents per 100 g dry basis at 4% target moisture, so the influence of the polarity of the solvent mixture (H2O + C6H8O7) is observed, due to the polarization of the mixture to attract the compounds of interest and develop an efficient extraction, Thus, it is also observed that the maximum extraction of the compound is reached between the microwave power of 6.7 and 8 in three times proposed for the extraction, achieving a Superior extraction of 400 mg Gallic Acid Equivalents per 100
  • FIGURE 6 Extraction curve loaded with solvent (H2O), capable of redistributing particles in a uniform movement, emitting intermittent and continuous pulses with exact microwave ranges from 0.623 Watts/g to 6.23 Watts/g in an extraction time of 15.45 and 60 seconds, expressed in mg Gallic Acid Equivalents per 100 g dry basis at 4% target moisture; the different powers equivalent to continuous exact microwave ranges from 0.623 Watts/g to 6.23 Watts/g, distributed, with an estimated time of exposure to microwaves of 15.45 and 60 seconds, expressed in mg Gallic Acid Equivalents per 100 g dry basis at 4% target moisture, so the influence of the polarity of the solvent mixture (H2O) is observed, due to the polarization of the mixture to attract the compounds of interest and develop an efficient extraction, as well as It is observed that the maximum extraction of the compound is reached between the microwave power of 6,7,8 and 9 in three times proposed for the extraction, achieving a superior extraction of 200 in mg Gallic Acid Equivalents per 100 g dry base at 4 Target % moisture.
  • FIGURE 7 Statistical analysis of main effects of the extraction curve loaded with solvent (H2O) and (H2O + C6H8O7), capable of redistributing particles in a uniform movement, emitting intermittent and continuous pulses, exact ranges of microwaves from 0.623 Watts/g up to 6.23 Watts/g in an extraction time of 15.45 and 60 seconds, expressed in mg Gallic Acid Equivalents per 100 g dry base at 4% target moisture; the statistical analysis of main effects is observed, where the different powers equivalent to continuous exact microwave ranges from 0.623 Watts/g to 6.23 Watts/g, distributed with an estimated microwave exposure time of 15, 45 and 60 seconds, expressed in mg Equivalents of Gallic Acid per 100 g dry basis at 4% target humidity, so the influence of the polarity of the solvent mixture (H2O) and (H2O + C6H8O7) is observed, due to the polarization of the mixture to attract the compounds of interest and develop an efficient extraction, it is also observed that the maximum compound extraction is reached between the microwave power of 6, 7, 8 and 9
  • FIGURE 8 Optimized statistical analysis of main effects of the extraction curve loaded with solvent (H2O) and (H2O + C6H8O7), capable of redistributing particles in a uniform movement, emitting intermittent and continuous pulses, exact microwave ranges of 0.623 Watts/g up to 6.23 Watts/g in an extraction time of 15, 45 and 60 seconds, expressed in mg Gallic Acid Equivalents per 100 g dry basis at 4% target moisture; the statistical analysis of optimized main effects is observed where the different powers equivalent to continuous exact microwave ranges from 0.623 Watts/g to 6.23 Watts/g, distributed with an estimated microwave exposure time of 15, 45 and 60 seconds, expressed in mg Gallic Acid Equivalents per 100 g dry basis at 4% target moisture, so the influence of the polarity of the solvent mixture (H2O) and (H2O + C6H8O7) is observed, due to the polarization of the mixture to attract the compounds of interest and develop an efficient extraction, thus it is also observed that the maximum Compound extraction is achieved between microwave power 6, 7, 8 and 9 in
  • FIGURE 9 Spectrophometric analysis of the extraction loaded with solvent (H2O + C6H8O7), emitting intermittent and continuous pulses with exact microwave ranges from 0.623 Watts/g to 6.23 Watts/g in an extraction time of 15, 45 and 60 seconds, expressed in mg Gallic Acid Equivalents per 100 g dry basis at 4% target moisture; where the spectrophotometric analysis of the extraction conditions optimized in terms of time equivalent to 60 seconds, microwave power equivalent to 6,230 Watts/g and selection of solvent mixture (H2O + C6H8O7), where the amount of light absorbed is observed as a function of the wavelength used in a spectrophotometric scan from 300 to 500 nm, where the low absorbed intensity of the selected solvent mixture (H2O + C6H8O7) marked in yellow is observed, from the 400 nm range peaks of the selected solvent mixture (H2O + C6H8O7) and bioactive compounds marked in red, green and black, which indicates that the developed extraction process is capable of removing particles of biological interest from the
  • an extraction chamber in which a continuous flow of air is passed at a speed of 1 m/s, to heat the mass a microwave, which emits microwaves whose power is based on the amount of organic material loaded in the extraction chamber and the percentage of its initial humidity, which can be in the range of 85% to 65% humidity, which is It has to be reduced until reaching an approximate humidity to the stability of the material, which is from 4% to 5%, with microwave emission preferably at a power in a range of 0.623 Watts/g up to 6.23 Watts/g, this during a cycle of time from 1 to 15 minutes, preferably from 5 to 15 minutes, until reaching the indicated humidity.
  • the biological material modifies the microstructural composition of the cells that make up the different parts of plants and/or flowers and/or fruits and/or shoots and/or roots and/or tubers. of plant origin, which favors the extraction of bioactive molecules linked to the free water content of the biological material, these conditions of low relative humidity, in a range of 4% to 5%, generate the appropriate conditions for the extraction of bioactive molecules in a second stage of the process.
  • having a humidity of 4% makes it easier to achieve structural damage to the cells that make up the biological material in the solvent, which can be water and/or ethanol and/or acetic acid, which have properties of high dipole moment and facilitates the formation of hydrogen bonds, that is, a molecule or ion is soluble in water and/or ethanol and/or acetic acid, for which it can interact with its molecules through hydrogen bonds or interactions of the ion-dipole type.
  • the solubility of ions in water and/or ethanol and/or acetic acid, with anions that have oxygen atoms, can form hydrogen bonds, since oxygen acts as an acceptor of these.
  • said organic material is in ideal conditions to carry out the loading of a solvent in the extraction chamber, where said solvent is preferably organic, polar or protic polar, and can be water and/or ethanol and/or acetic acid, and where the proportion of the solvent to come into contact with the biological material is from 50 to 100 mL per 100 g of biomass on a dry basis, with a humidity of 4%.
  • the microwave emission is maintained with the same characteristics used in stage 1.
  • water or ethanol or acetic acid is used as the sole solvent at 100%.
  • a mixture of solvents with a concentration of 10% to 70% is used, using any of the three solvents that are water and/or ethanol and/or acetic acid.
  • mixtures resulting from the design are used by means of statistical calculation tools, such as the design of complex mixtures of said solvents, obtaining the quantitative proportion to measure the concentration in percentage, molarity, normality, and parts per million.
  • bioactive compounds are sensitive to drastic changes in temperature, pressure and water activity, in addition to being scarce in proportion to the cellular structure that compose them in their entirety from plants and/or flowers and/or fruits and /or sprouts and/or roots and/or tubers of vegetable origin, therefore, in order to determine the operating parameters at each stage, and be able to extract said bioactive molecules, compounds of biological interest or with therapeutic potential, the difference in electronegativity of bonds as geometry, to determine whether or not the dipole moments cancel by the geometric arrangement of the bonds (for example, in water, which is angular, the dipole moments will not cancel and the molecule will be polar , but in ethanol, which is trigonal, they will cancel out due to said geometry and will be globally apolar).
  • the difference in electronegativity will be another of the parameters that can be used to determine which of these compounds is the one with the greatest ionic character or the greatest covalent character depending on the polarity of the bioactive molecules of interest, considering the solvent. that can remove these bioactive molecules and preserve their therapeutic properties, in addition to being an organic solvent that allows concentrating the highest content of said molecules to be preserved and evaluated for their biological activity in therapies or protocols in vitro, in vivo and medical protocols.
  • Nanoparticles for example, Icosahedron, Liposome, Nanocluster, Gold Nip, Dendrimers, Quantum Dot, Polymeric, Nanotriangle and Nanocube.
  • Nanofibers such as Nano textile fiber, carbon, cellulose, mainly Carbon 60 fullerenes, although not limited to them.
  • Polar molecules eg water, ethanol and/or acetic acid
  • Molecules with Z potential such as phospholipids, fatty acids, albumin, dextrone, chitosan, cellulose derivatives, poly-acrylates, poly-acrylamides and/or poly-esters.
  • the injection of the solvent mixture is regulated according to the volume of biological material to be processed and the dielectric properties of the biological material loaded in the extraction chamber.
  • the organic matter since the organic matter is already in the extraction chamber at 4% humidity, with the solvent or the mixture of solvents, as well as with the emission of microwaves, the physical change in the biological material begins. ; where the organic solvent, for example water and/or ethanol and/or acetic acid, removes from the interior of the cells the molecules with biological activity which are polarly attached to the organic solvent phase, leaving the original structure that contained them in the form of plants and/or flowers and/or fruits and/or shoots and/or roots and/or tubers of plant origin, this migration is only possible if the solvent is capable of reaching the internal cellular microstructures that make up the biological material, that the dielectric constant 8' and the loss factor 8" of free water increase with increasing temperature.
  • the organic solvent for example water and/or ethanol and/or acetic acid
  • the loss factor 8 decreases with the increase in frequency and is less at 2450 Mhz than at 915 Mhz, being a permanent condition in any biological material that contains water in its exterior and interior composition.
  • the microwave device emit microwaves in the form of intermittent pulses, increasing power gradually and continuously, in power ranges from 0.623 Watts/g to 6.23 Watts/g during extraction times of 15, 30, 45 and 60 seconds, considering the number of cycles Hertz per second, repeating these conditions during the extraction cycle of molecules with biological activity, depending on the time and watts required to emit the microwave frequency considering the changes in the material for each fraction of time equivalent to this cycle of 15, 30, 45 and 60 seconds, for a total time between 1 and 15 min, preferably 5 to 15 min, since there is a relationship of temperature increase between the transmission of microwaves through a substance and the concentration of the substance, as well as between the transmission and the length of the body that the microwaves cross, due to the rotation of the dipole in the solvent organic (water, ethanol and/or acetic acid).
  • the organic solvent phase water, ethanol and acetic acid
  • the organic solvent phase charged with the necessary polarity to join the molecules of biological interest, expands the cell walls contracted by the drying process and cutting said cell structure, thus In this way, the bioactive molecules can transit the cellular microstructures towards their exterior, forming a solvent mixture with bioactive molecules polarly bound to said organic solvent.
  • each biological material has unique properties, therefore, to consider the exact times of microwave transmission, an experimental test with response variables is performed, standardizing the procedure through the analysis of main effects considering a statistically representative sample.
  • bioactive molecules can transit the cellular microstructures to the outside of these, forming a solvent mixture and bioactive molecules polarly bound to the organic solvent used for extraction.
  • the evaporation of solvents is derived from the conditions of microwave emission, where the organic solvent absorbs and distributes microwave energy in the biological material, said material and the mixture of organic solvent, with polar molecules, continuously modify the dielectric constant of the mixture of the solvent and the bioactive molecules, for which the capacity of the material to absorb these microwaves is related to the dielectric properties with respect to temperature depending on the frequency, the relationship in the bonds of water, free water, the ionic conductivity and the composition of the material, therefore the concentration of the solvent must be constant to avoid drastic changes in the physical properties of the mixtures, avoiding the evaporation of the solvent.
  • the bioactive molecules contained in the organic solvent due to changes in pH, thermolability, UV light, changes in atmospheric pressure, presence of oxygen, nitrogen and other gases typical of the atmosphere, it is injected into the extraction chamber pH stabilizing solutions, mixtures of ions, for example, Na, P, Mg, preferably, where each increases or decreases polarity depending on the concentration of the mixture of bioactive molecules and gas mixtures at atmospheric pressures stable, considering that the properties of the solvent can vary depending on the density and atmospheric pressure, which allows the reduction of damage by UV radiation, in this way we obtain bioactive molecules with therapeutic potential for various diseases, and that the mixture of solvents retain position properties of functional groups with therapeutic potential that allow the extraction process to continue on.
  • mixtures of ions for example, Na, P, Mg, preferably, where each increases or decreases polarity depending on the concentration of the mixture of bioactive molecules and gas mixtures at atmospheric pressures stable, considering that the properties of the solvent can vary depending on the density and atmospheric pressure, which allows the reduction of damage by UV radiation, in this way we obtain bioactive molecules
  • the phase II operating temperature depends on the thermodynamic stability characteristics that occur when a system is in its lowest energy state or chemical equilibrium with its surroundings. This may be a dynamic equilibrium, where individual molecules or atoms change shape, but their total number in a particular form or state is conserved from the bioactive molecules of the cells that make up the different parts of plants and/or flowers and/or fruits and/or shoots and/or roots and/or tubers of plant origin, to be processed or preserved without losing properties.
  • bioactive molecules of interest concentrated in the solvent, or a combination of them, they present high temperatures derived from the process, so that said mixture must be tempered to reduce the temperature to a range of 20°C to 4°C, a temperature at which the organic matter can be properly handled for processing; In addition, this will achieve the preservation of the properties of the bioactive material.
  • the extraction chamber has a continuous air flow system that injects cold air at refrigeration temperature to reduce the temperature gradient of the mixture of solvent and molecules with biological activity.
  • Said continuous air flow system displaces cold air, performs a gradual decrease in the temperature of the extraction chamber at a speed of 2 m/s at temperatures below 0°C, reducing the effective diffusion coefficient of 20 m 2 /s. that allows the preservation or inactivation of chemical or biological processes typical of the mixture of solvent (water and/or ethanol and acetic acid) and molecules with biological activity.
  • the separation of the organic matter resulting from the process can be carried out, that is, the mixture of solvent and molecules with biological activity, this can be done with the help of a rotary flow pump, by gravity and centrifugation, where the by-product obtained are structural cells of plants and/or flowers and/or fruits and/or shoots and/or roots and/or tubers of plant origin, which can be reprocessed or integrated into compost mixtures to be reused as an organic product, since they are free of inorganic compounds or inorganic solvents. Since these inorganic compounds are made up of different elements, but in which their main component is not always carbon, water being the most abundant. In inorganic compounds, it could be said that almost all known elements participate.
  • a sampling of the mixture of solvent and resulting molecules can be carried out, this with the objective of evaluating the quantity and presence of the molecules of interest with biological activity through spectrophotometric analysis, determining In this way the efficiency of the process and collect the necessary data of the mixture, its performance depends on each species and variety of biological material, in addition to other variables such as whether the plant is fresh or dry; or if they are leaves, stems or inflorescences.
  • the recovery of the solvent(s) and the bioactive molecules is carried out.
  • the mixture of solvent and molecules with biological activity has as a by-product structural cells or micro residues of plants and/or flowers and/or fruits and/or shoots and/or roots and/or tubers of vegetable origin that contain starches, sugars, cells, protein and other compounds typical of the structure of the material, which can be processed for the formation of new products or materials of biological interest
  • said cellular structure can be separated from the solvent mixture, for example, by centrifugation at 2500 RPM , for 30 min and a temperature of 4 °C, to eliminate the supernatant of the mixture and reserve the solvent with the mixture of molecules of interest with biological activity, precipitating the extraction product for every 100 g dry base is 2.6 g dry base of bioactive compounds equivalent to 2.6 % of the volume of the biological material.
  • the mixture of solvent and molecules with biological activity can be concentrated by Rotavapor to evaporate 33% of the solvent content under conditions of: 240 RPM, 70°C and vacuum pressure of 800 mbar, for 2 hours, to later be centrifuged at 2500 RPM, for 30 min and a temperature of 4 °C, to eliminate the supernatant of the mixture and reserve the solvent with the mixture of molecules of interest with biological activity.
  • the bioactive molecules of the previous stage can be preconditioned by measuring the Z potential and the inclusion of phospholipids, fatty acids, albumin, dextrone, chitosan, cellulose derivatives, poly-acrylates, poly-acrylamides and poly- ester to be processed into by-products by means of lyophilization, spray-drying, microencapsulation, nanoencapsulation, nanomilling, electrospinning or electrospinning, nanoscaffolding, and functionalized by means of simple or complex matrices, to be microdosed, encapsulated, or functionalized for controlled release.
  • the cellular structure of plants and/or flowers and/or fruits and/or shoots and/or roots and/or tubers of plant origin can be processed to be dehydrated, frozen or preserved for later processes, such as generation of compost, syngas, compost pellets, biopolymers, biofilms, mainly, so that said cellular structure can be used in any process of reuse of organic products.
  • the Humulus lupulus variety was placed in the extraction cylinder of the aforementioned extraction equipment, this with the aim of removing exact amounts of moisture out of the biological material through a continuous flow of air at a speed of 2.0 m/s at a temperature of 90 °C and the emission of exact ranges of microwave power (1,868W/g) with a final drying time of 10 min in a volume of 100 g of material at an initial percentage of 65%, taking a sample from the material at 2.5 minutes and qualifying the humidity by means of the aqualab equipment to continue the process for another 2.5 min and confirm the stability of the material at 4%. Reducing the weight and volume to a weight of 35 g.
  • a mixture of organic solvents such as water and/or ethanol and/or acetic acid is injected into the extraction chamber.
  • this mixture of solvents and organic molecules with defined polar charges are injected into the extraction chamber in a controlled extraction sequence based on the material's exposure time to microwave sources.
  • the polarity of the solvent mixture is selected with deionized water in a volume of 500 mL, at a pH of 4.5 and a charge of CeHsO? at 0.1% g/v, these conditions of stability of the molecules with biological activity, allow the exposure of the organic matter to heat in a time of 5 to 10 seconds, thus allowing to stop the evaporation of the organic solvents that are emitted , this in the form of intermittent and continuous pulses, in exact microwave ranges from 0.623 Watts/g to 6.23 Watts/g in an extraction time of 15, 30, 45 and 60 seconds, considering the number of Hertz cycles per second, replicating this information during the extraction cycle of the molecules with biological activity, depending on the time and watts required to emit the microwave frequency considering the changes in the material for each fraction of time equivalent to this cycle of 15, 30, 45 and 60 seconds, for a total time not exceeding 10 min.
  • the charged solvent phase with the necessary polarity to bind to the molecules of biological interest expands the cell walls contracted by the drying process, cutting and modifying said cellular structure, the bioactive molecules can transit from the cellular microstructures to the outside these, forming a solvent mixture with bioactive molecules polarly bound to said organic solvent used for extraction.
  • a second injection of the solvent mixture with deionized water was performed to recover the equivalent volume of 500 mL, at a pH of 4.5 and a charge of CeHaO? at 0.1% g/v, once the physical change in the properties of the biological material has been generated, the organic solvent removes the molecules with biological activity from the interior of the cells by joining polarly to the organic solvent phase, abandoning the structure that contained them in the material of biological origin of the Cannabaceae family, of the plantae kingdom, using the variety Humulus lupulus, the losses due to evaporation of the condensing solvent and the vapors generated during the extraction processes, are condensed by means of a refrigerated reflux at 12 °C reestablishing the balance of the mixture without modifying the concentration and therefore, the physical and chemical properties of the same, the mixture of solvent and molecules with biological activity, has as a by-product structural cells of Humulus lupulus, which can be separated of the solvent mixture, extracting the mixture with a rotary flow pump,
  • the mixture of solvent and molecules of Humulus lupulus, with biological activity can be concentrated by Rotavapor to evaporate 33% of the solvent content under conditions of: 240 RPM, 70°C and vacuum pressure of 800 mbar, for 2 hours, to later be centrifuged at 2500 RPM, for 30 min and a temperature of 4 °C, to eliminate the supernatant of the mixture and reserve the solvent with the mixture of molecules of interest with biological activity.
  • the molecules of Humulus lupulus, with biological activity are preserved in refrigeration at 12°C for their subsequent processing or transformation into by-products of therapeutic interest, the yield of the extraction per 100 g dry base is 2.6 g dry base of bioactive compounds with biological activity, exceeding 3 to 4 times the traditional yields for the extraction of products derived from the Cannabaceae family, of the plantae kingdom, for which similar results could be obtained in the varieties of the genus Cannabis Sativa.

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  • Wood Science & Technology (AREA)
  • Animal Behavior & Ethology (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

La présente invention se rapporte à un processus qui permet l'extraction de composés bioactifs à partir de matière biologique, avec des rendements ou des concentrations de 1 à 3 fois supérieurs à ceux des processus classiques; une réduction du temps d'exposition des molécules à hautes températures, ainsi que la quantités de diluants employés pour effectuer l'extraction de molécules ayant une activité biologique présentant un intérêt. Au moyen de ce processus, on obtient des molécules bioactives à partir de matière organique d'origine végétale, comme le sont les plantes et/ou les fruits et/ou les pousses et/ou les tubercules qui contiennent des composés bioactifs ayant un intérêt thérapeutique, lesquels peuvent être extraits pour être concentrés et traités en vue d'être administrés et présenter des effets thérapeutiques.
PCT/MX2020/000032 2020-09-04 2020-10-15 Processus d'extraction de composé bioactifs dérivés de matière organique d'origine végétale Ceased WO2022050831A1 (fr)

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MXMX/A/2020/009245 2020-09-04
MX2020009245A MX2020009245A (es) 2020-09-04 2020-09-04 Proceso de extracción de compuestos bioactivos derivados de materia orgánica de orígen vegetal.

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WO2022050831A1 true WO2022050831A1 (fr) 2022-03-10

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116059691A (zh) * 2023-03-07 2023-05-05 美尚(广州)化妆品股份有限公司 一种通过高β-折叠含量蚕丝蛋白纳米纤维萃取活性物质的方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1618798A1 (fr) * 2004-07-20 2006-01-25 Milestone S.r.l. Extraction par microondes de composés naturels volatils
FR2925898A1 (fr) * 2007-12-28 2009-07-03 Jean Pierre Lablanchy Procede et systeme d'extraction d'huile essentielle a forte teneur en thymoquinone a partir de la plante de nigella sativa
CN104327951A (zh) * 2014-10-23 2015-02-04 郑州工业应用技术学院 一种热空气精油提取装置
WO2019211795A1 (fr) * 2018-05-03 2019-11-07 Radient Technologies Inc. Extraction assistée par micro-ondes à écoulement continu de biomasse de cannabis
WO2019211794A1 (fr) * 2018-05-03 2019-11-07 Radient Technologies Inc. Extraction à l'aide d'un extracteur assisté par micro-ondes

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1618798A1 (fr) * 2004-07-20 2006-01-25 Milestone S.r.l. Extraction par microondes de composés naturels volatils
FR2925898A1 (fr) * 2007-12-28 2009-07-03 Jean Pierre Lablanchy Procede et systeme d'extraction d'huile essentielle a forte teneur en thymoquinone a partir de la plante de nigella sativa
CN104327951A (zh) * 2014-10-23 2015-02-04 郑州工业应用技术学院 一种热空气精油提取装置
WO2019211795A1 (fr) * 2018-05-03 2019-11-07 Radient Technologies Inc. Extraction assistée par micro-ondes à écoulement continu de biomasse de cannabis
WO2019211794A1 (fr) * 2018-05-03 2019-11-07 Radient Technologies Inc. Extraction à l'aide d'un extracteur assisté par micro-ondes

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116059691A (zh) * 2023-03-07 2023-05-05 美尚(广州)化妆品股份有限公司 一种通过高β-折叠含量蚕丝蛋白纳米纤维萃取活性物质的方法
CN116059691B (zh) * 2023-03-07 2023-08-15 美尚(广州)化妆品股份有限公司 一种通过高β-折叠含量蚕丝蛋白纳米纤维萃取活性物质的方法

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