WO2019211772A1 - Obtention d'extraits sous une forme solide - Google Patents

Obtention d'extraits sous une forme solide Download PDF

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Publication number
WO2019211772A1
WO2019211772A1 PCT/IB2019/053571 IB2019053571W WO2019211772A1 WO 2019211772 A1 WO2019211772 A1 WO 2019211772A1 IB 2019053571 W IB2019053571 W IB 2019053571W WO 2019211772 A1 WO2019211772 A1 WO 2019211772A1
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Prior art keywords
biomass
solvent
chamber
cannabis
slurry
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PCT/IB2019/053571
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English (en)
Inventor
Tomasz Popek
Steven Splinter
Anna BAKOWSKA-BARCZAK
Harmandeep KAUR
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Radient Technologies Inc.
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Publication of WO2019211772A1 publication Critical patent/WO2019211772A1/fr

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    • 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
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P25/00—Drugs for disorders of the nervous system
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01D11/0215—Solid material in other stationary receptacles
    • B01D11/0223—Moving bed of solid material
    • B01D11/0226—Moving bed of solid material with the general transport direction of the solids parallel to the rotation axis of the conveyor, e.g. worm
    • 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
    • B01D11/0215—Solid material in other stationary receptacles
    • B01D11/0253—Fluidised bed of solid materials
    • B01D11/0257—Fluidised bed of solid materials using mixing mechanisms, e.g. stirrers, jets
    • 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
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • 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
    • 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

Definitions

  • the present disclosure is generally related to a method for extracting
  • the present disclosure relates to a method of extracting and preparing a solid form of the pharmacologically active compounds.
  • Cannabis is a genus belonging to the family of cannabaceae. Three common spedes include Cannabis sativa, Cannabis indica, and Cannabis ruderalis. The genus has been indigenous to Central Asia and the Indian subcontinent. Cannabis has a long history being used for medicinal, therapeutic, and recreational purposes. The importance of cannabis in therapeutics is emphasized by the ever-increasing number of research publications related to the new indications for cannabis. For example, pharmaceutical research companies are presently developing new natural cannabinoid formulations and delivery systems to meet various regulatory requirements. Cannabis is known, for example, to be capable of relieving nausea (such as that accompanying chemotherapy), pain, vomiting, spasticity in multiple sclerosis, and increase hunger in anorexia.
  • cannabis or “cannabis biomass” encompasses the Cannabis sativa plant and also variants thereof, including subspecies sativa, indica and ruderalis, cannabis cultivars, and cannabis chemovars (varieties characterised by chemical composition), which naturally contain different amounts of the individual cannabinoids, and also plants which are the result of genetic crosses.
  • cannabis chemovars variants characterised by chemical composition
  • the term “cannabis biomass” is to be interpreted accordingly as encompassing plant material derived from one or more cannabis plants.
  • Cannabis biomass contains a unique class of terpeno-phenolic compounds known as cannabinoids or phytocannabinoids, which have been extensively studied since the discovery of the chemical structure of tetrahydrocannabinol (Delta-9-THC), commonly known as THC. Over 113 phytocannabinoids have been identified.
  • cannabinoids are generally produced by glandular trichomes that occur on most aerial surfaces of the plant.
  • the cannabinoids are biosynthesized in the plant in addic forms known as addic cannabinoids.
  • the addic cannabinoids may be slowly decarboxylated during drying of harvested plant material.
  • Decarboxylation may be hastened by heating the cannabis biomass, such as when the cannabis biomass is smoked or vaporized.
  • the prindple cannabinoids present in cannabis are the Delta-9- tetrahydrocannabinolic add (Delta-9-THCA) and cannabidiolic add (CBDA).
  • the Delta-9- THCA does not have its own psychoadive properties as is, but may be decarboxylated to Delta- 9-tetrahydrocannabinol (Delta-9-THC), which is the most potent psychoactive cannabinoid among known cannabinoids.
  • the neutral form of CBDA is cannabidiol (CBD), which is a major cannabinoid substituent in hemp cannabis. CBD is non-psychoadive and is widely known to have therapeutic potential for a variety of medical conditions.
  • the proportion of cannabinoids in the plant may vary from spedes to spedes, as well as vary within the same species at different times and seasons. Furthermore, the proportion of cannabinoids in a plant may further depend upon soil, dimate, and harvesting methods. Thus, based on the proportion of the cannabinoids present in a plant variety, the psychoactive and medicinal effeds obtained from different plant varieties may vary.
  • a spedfic variety of cannabis may be considered more effective or potent than others (e.g ., in providing the desired physiological effed at a desired level in an individual).
  • some spedfic combinations of pharmacologically adive compounds in a cannabis variety may be more desirable in comparison to other varieties.
  • the retention of the full mix of cannabinoids present in the original plant may be desirable for some varieties, while other varieties may be preferred in altered form due to the variances in the specific cannabinoid composition and concentrations. Such variance is further exacerbated by the presence of certain terpenoid or phenolic compounds, which may have pharmacological activity of their own and which may be desired at different concentrations in different combinations.
  • compounds may be extracted from cannabis by using conventional methods of extraction, such as maceration, decoction, or solvent extraction.
  • conventional methods may suffer from various limitations and disadvantages (e.g., extraction times may be very high so as to be impractical to scale).
  • subjecting the biomass to a prolonged extraction process may risk modification of the plant profile, negative effects on terpenes, or otherwise cause other undesirable effects that lower the quality or purity of the end product.
  • Traditional methods of extraction may therefore hamper quality and purity of the final product.
  • final concentrated or purified active compounds are often diluted or dispersed into an oil, fat or other lipid-based excipient or carrier to a desired concentration for certain uses (e.g., in a pharmaceutical, food, or cosmetic formulation).
  • SFE supercritical fluid extraction
  • Other methods such as supercritical fluid extraction (SFE) make use of supercritical fluids to selectively remove compounds from solid, semisolid, and liquid matrices in a batch process.
  • SFE is, however, dangerous and requires very high pressures to be employed (> 70 atm).
  • SFE is also inefficient and therefore not conducive to high throughputs, as well as environmentally damaging (e.g., producing large amounts of the greenhouse gas carbon dioxide as a by-product).
  • Embodiments of the present invention provide systems and methods for obtaining a solid form of a cannabis extract.
  • the processes described herein include a method for extracting bioactive compounds and formulating a solid form of a cannabis extract from a raw cannabis biomass.
  • a novel approach is provided for the extraction and formulation of a solid form of pharmaceutically active cannabinoids.
  • Exemplary methods for extracting and formulating a solid form cannabis extract from a raw cannabis biomass including preparing a raw cannabis biomass, adding a solvent to form a slurry, extracting pharmaceutically active cannabinoids via a heating process, separating the spent biomass from the extract, and producing a solid extract of pharmaceutically active cannabinoids.
  • FIG. 1 is a block diagram representation of an exemplary system for obtaining a solid form cannabis extract.
  • FIG. 2 illustrates a flow chart of a method of obtaining a solid form cannabis extract.
  • FIG. 3 is a detailed block diagram of an exemplary representation of a cannabis extraction by a continuous flow extraction chamber.
  • FIG. 4 is a detailed block diagram of an exemplary representation of a post extraction solidification process.
  • FIG. 5 is a table providing test data of target compounds concentrations of various strains of cannabis.
  • FIG. 6 illustrates a flow chart of a method of obtaining a solid form cannabis extracts.
  • Exemplary methods for extracting a solid form cannabis extract from a raw cannabis biomass including preparing a raw cannabis biomass, adding a solvent to form a slurry, extracting a pharmaceutically active cannabinoid via a heating process, separating the spent biomass from the extract, and producing a solid extract of a pharmaceutically active cannabinoid.
  • Pharmacological formulations that are stable in solid or powdered form may have additional delivery methods available to them, such as, oral capsule or tablet, suppository, inhalation, intravenous injection, etc.
  • FIG. 1 is a block diagram representation of an exemplary system 100 for obtaining a solid form cannabis extract
  • FIG. 2 is a flow chart illustrating an exemplary method for obtaining a solid form cannabis extract.
  • the term 'pharmacologically active compounds' may henceforth be used interchangeably with the term 'target components' and 'target components.'
  • System 100 illustrated in FIG. 1 can include a raw biomass holding chamber 102 into which a raw biomass may be provided in step 202 of FIG. 2.
  • a raw biomass may be present in form of dried, ground, non-decarboxylated flowers (such as buds) of a cannabis plant.
  • the raw biomass can be any part of the cannabis plant which may contain cannabinoids including, but not limited to, leaves, stems, rooms, and the like.
  • Said raw cannabis biomass can be provided to the raw biomass holding chamber 102 of system 100.
  • the average particle size of the raw biomass may lie between approximately 0.5 mm and approximately 10 mm.
  • the raw biomass may contain target compounds that need to be extracted.
  • the raw biomass may be heated to approximately 125°C for approximately 45 minutes to decarboxylate the cannabinoid carboxylic adds into their neutral cannabinoid forms.
  • the mass of decarboxylated cannabis following such treatment may be reduced from the originally provided mass (for example, 11.7% weight loss).
  • the raw biomass may be a dried, non-decarboxylated cannabis biomass.
  • the raw biomass may be a fresh, non-dried, non-decarboxylated cannabis biomass.
  • the raw biomass may be sampled and analyzed in a sampling chamber 120.
  • the raw biomass may be sampled and analyzed using several methods.
  • the raw biomass may be analyzed to determine cannabinoid content and create a cannabinoid profile (providing the specific cannabinoids present in the sample and concentrations thereof) of the sampled raw biomass.
  • a cannabinoid profile providing the specific cannabinoids present in the sample and concentrations thereof
  • Such analysis may be performed using an Ultra High Performance Liquid Chromatography coupled with Mass Spectrometry (UPLC-MS) detection technique.
  • UPLC-MS Ultra High Performance Liquid Chromatography coupled with Mass Spectrometry
  • a terpene profile of the raw biomass may be created using a Gas Chromatography-Mass Spectrometry (GC-MS) detection technique.
  • GC-MS Gas Chromatography-Mass Spectrometry
  • the cannabinoid profile can include the total cannibinoids content (wt%), concentration of individual cannabinoids (wt%), TCHA+THC (wt%), CBD+CBDA (wt%), total THC equivalents (determined using the formula THC+THCA x0.877 (wt%)), and total CBD equivalents (determined using the formula CBD+CBDAxO.877 (wt%)).
  • the cannabinoid profile created can be used to determine the amount of acidic and neutral cannabinoids which may be extracted.
  • the raw biomass may be ground into small particles in biomass preparation chamber 104 to obtain a prepared biomass.
  • the size of the particles of the ground biomass may range from between about 0.5 mm to about 10 mm.
  • the biomass preparation process may be performed utilizing one or more of a grinding machine, a shredding machine, a biomass pulverizing machine, and the like.
  • the prepared biomass may then be provided from biomass preparation chamber 104 to a prepared biomass holding chamber 106.
  • the prepared biomass may be used in the formation of a slurry in step 208.
  • the slurry may be formed in slurry formation chamber 108, where one or more solvents from a solvent holding chamber 110 and the prepared biomass from the prepared biomass chamber 106 are combined.
  • the solvent added to the prepared biomass may be selected with different dielectric and solvent parameter properties.
  • the solvent may be, for example, an edible or food-grade solvent or emulsifier used to standardize active compounds in pharmaceutical, nutraceutical, functional, food, or cosmetic formulations.
  • the solvent may be water, an alcohol group, an alkene group, a ketone group, a polyunsaturated fatty acid (PUFA), corn oil, safflower oil, borage oil, flax oil, canola oil, cottonseed oil, soybean oil, olive oil, sunflower oil, coconut oil, palm oil, monoglycerides, diglycerides, triglycerides, medium chain triglycerides (MCT), long chain tryglycerides, ledthin, limonene, essential oils of spices, herbs, or other plants, fish oil, glycerol, glycols, or mixtures thereof.
  • ethanol may be used as the solvent.
  • the solvent-to-raw biomass ratio may be maintained at approximately 5 liters per kg to approximately 10 1/kg to ease the pumping operation of the slurry. In an embodiment, the solvent-to-biomass ratio may be maintained as low as possible.
  • the cannabinoid profile created using the raw biomass material can be used in determining the desired solvent-to-biomass ratio of the slurry.
  • the slurry may be transferred from the slurry formation chamber 108 to an extraction chamber 112 where such slurry is subjected to heat at step 210.
  • the slurry may be transported to the extraction chamber 112 using a set of mechanical conveyors (e.g ., a slurry pump, a screw conveyor, or a worm gear).
  • the slurry may be subjected to a thermal process, such as that provided by a microwave generator 114.
  • the slurry may be transported into an extraction chamber 112 through a tube. At least one portion of the extraction chamber 112, or the entire extraction chamber 112, can be microwave transparent.
  • This microwave transparent portion of the evacuation chamber 112 may allow microwaves (e.g., microwaves generated using a magnetron of microwave generator 114) to pass through the extraction chamber 112 and heat the slurry inside.
  • the slurry may be heated within the extraction chamber 112 to a certain temperature by exposing the slurry to the microwave for a predefined time, with a predefined, controlled, microwave energy density range.
  • the slurry may be heated to a temperature range of approximately 20°C to approximately 75°C with a contact time of approximately 1 minute to approximately 30 minutes, and a microwave energy density range of approximately 0.1 kW per 1kg of biomass (0.1 kW/kg) to approximately 10 kW/kg.
  • the procedure (e.g., time, temperature, or energy range) used in the extraction process can be adjusted based on the cannabinoid profile of the raw biomass in order to achieve a desired extraction efficiency.
  • the methods described herein can be conducted on an industrial scale. In at least one example, the methods can be performed on samples of over 1,000 kg to over 10,000 kg of biomass per extraction.
  • the microwave energy, contact time and temperature range can be selected specifically to avoid decarboxylation of the cannabinoids.
  • the heating process described herein can, in at least some examples, facilitate the extraction of various (pharmacologically active) compounds from the prepared biomass into the solvent.
  • the extraction chamber 112 may be filled completely with solvent prior to the extraction process in order to remove air and other gases from the extraction chamber 112.
  • the extraction chamber 112 may be purged with an inert gas such as nitrogen prior to the extraction process in order to remove air and other oxidizing gases from the extraction chamber 112.
  • the extraction chamber 112 can produce a partially-concentrated ethanolic extract.
  • the slurry and compounds extracted from the biomass may be transferred to a separation chamber 116, where the slurry is subject to filtration and separation at step 212.
  • Such separation can be performed within a separation chamber 116 and may result in the isolation of the slurry components from each other: the spent biomass and the solvent(s) containing the extracted compounds.
  • the separation process may be performed using filtration, centrifuge, and other similar processes. In other embodiments, the spent biomass and the solvent can be separated by centrifugation.
  • the spent biomass and the solvent(s) containing the extracted compounds may be transferred into a spent biomass holding chamber 118 and solvent recovery chamber 122, respectively.
  • the spent biomass from spent biomass holding chamber 118 may be sampled and analyzed at step 214.
  • the sampling of the spent biomass may be performed in a sampling chamber 120.
  • the spent biomass may be sampled and analyzed to detect the remaining cannabinoid content of the spent biomass and create a cannabinoid profile of the sample.
  • the spent biomass may be sampled and analyzed using several methods. For example, the analyses may be performed using an Ultra High Performance Liquid Chromatography coupled with Mass Spectrometry (UPLC-MS) detection techniques.
  • UPLC-MS Ultra High Performance Liquid Chromatography coupled with Mass Spectrometry
  • a terpene profile of the biomass may be determined using a Gas Chromatography-Mass Spectrometry (GC-MS) detection techniques.
  • GC-MS Gas Chromatography-Mass Spectrometry
  • the spent biomass may then be incinerated or mixed with a deactivating agent in disposal system 128.
  • a deactivating agent in disposal system 128.
  • clay may be used as the deactivating agent.
  • the solvent recovered from the separation chamber 116 can be transferred to solvent recovery chamber 122 for reuse in in another extraction process.
  • the solvent may be recovered from the extract/solvent mixture using a distillation, an evaporation process, or any other suitable solvent removal or recovery process, providing the solvent and a desolventized extract.
  • the solvent may be recovered from the extracted components by a vacuum distillation or vacuum evaporation process, and the recovered solvent can be stored in the solvent recovery chamber 122.
  • ethanol solvent used to form the slurry with the raw biomass may be recovered from the desolventized extract using a vacuum distillation or evaporation process.
  • the extracted compounds may be dispersed via homogenization to produce a dispersion.
  • an exdpient may be added to improve physical properties of the extracted compounds.
  • the exdpient may be utilized to streamline processing operations, and may therefore be added before, during, or after the solvent recovery step 216.
  • the exdpient may be dextrins (induding, but not limited to, malrodextrins, alpha-cydodextrins, beta-cydodextrins, gamma- cydodextrins, starches, and celluloses), emulsifiers (induding, but not limited to, gums, polysorbates, colloids, polysaccharides, and the like), inert minerals or salts.
  • calcium carbonate or a similar desiccant may be used.
  • silicon dioxide or other free flowing agent may be used.
  • polymers e.g. cellulosic polymers
  • the desolventized extrad may then be solidified through a solidification process, at step 218, performed in a solidification chamber 124.
  • the desolventized extrad can be solidified by performing a drying process.
  • Step 218 may continue and the solidified extract may be further processed using a solid processing chamber 126.
  • the processes which may be performed for solidification of the extract may indude, but are not limited to, temperature and pressure adjustments, spray drying, lyophilization (e.g., freeze drying), or any other suitable solidification process.
  • the solidification of the extract may be achieved using multiple processes.
  • the solidification of the extrad may be achieved through a drying process, which may indude, but is not limited to, spray drying, tumble drying, fluidized bed drying, or a combination of multiple such drying processes.
  • the solid extrad may be further processed to into a powder form by mechanical operations, such as milling, grinding, pulverizing, sieving, or combinations thereof.
  • the powder can be used to produce a capsule.
  • an exdpient e.g ., an inactive substance
  • the excipient may be utilized to streamline processing operations, as described above. Both the excipient and the solidification technique may be selected in order to obtain specific, desired properties in the final extract. Additionally, the solid extract may be blended with other solid or liquid components, granulated, pressed or extruded into a desired shape, or processed using a combination of these techniques.
  • the final formulation may be a solid form of cannabinoid extract and can be provided to a product holding chamber 128.
  • sampling and analysis of the solidified extract may be performed, at step 220.
  • the sampling and analysis of the formulated extract may be performed in the sampling chamber 120.
  • the formulated extract may be sampled and analyzed using several techniques.
  • sampling and analysis of the formulated extract may be performed to determine cannabinoid content and create a cannabinoid profile of the solidified cannabinoid extract (e.g., THCA, THC, CBDA, CBD, and total cannabinoids).
  • the sampling and analysis may be performed using an Ultra High Performance Liquid Chromatography coupled with Mass Spectrometry (UPLC-MS) detection technique.
  • UPLC-MS Ultra High Performance Liquid Chromatography coupled with Mass Spectrometry
  • a terpene profile of the solidified cannabinoid may be determined using a Gas Chromatography-Mass Spectrometry (GC-MS) detection technique.
  • GC-MS Gas Chromatography-Mass Spectrometry
  • FIG. 3 is a detailed block diagram of a system for the production of a solid form cannabis extract using a continuous flow extraction apparatus.
  • a slurry may be formed by combining the prepared biomass with a solvent, as described above, in the slurry formation chamber 302. This slurry can then be transferred to an extraction chamber 304.
  • the extraction chamber 304 may contain a continuous flow chamber 306 therein, such as an agitator, an auger, or a worm gear.
  • the extraction chamber 304 can be used to transport the slurry through the chamber (e.g., a tube or a pipe), wherein at least one portion of the chamber is microwave transparent.
  • the microwave transparent portion of the chamber allows microwaves from a microwave generator 308 (e.g., microwaves generated using a magnetron) to pass through and heat the slurry inside the chamber.
  • the slurry can be heated to a predetermined temperature by exposing the slurry to the microwaves, for a predefined period of time, with a predefined microwave energy density range.
  • the power, or energy density range, of the microwaves can be varied in order to achieve a maximum extraction efficiency.
  • the heating process can transfer the target components to the solvent phase, and the heated slurry can then exit the extraction chamber and enter a separation chamber 310.
  • the slurry may then be separated to obtain a spent biomass and a solvent comprising the extracted components, which can be transferred to a spent biomass holding chamber 312 and a solvent recovery chamber 314, respectively.
  • FIG. 4 is a detailed block diagram of a solid form cannabis extraction system.
  • the solvent and extracted components can enter a solvent recovery chamber 404.
  • the materials in the solvent recovery chamber 404 can then be processed through an additional separation chamber 406.
  • the separation chamber 406 can use any separation process including, but not limited to, filtration, centrifugation, or any other suitable separation process known in the art.
  • separation may be by vacuum evaporation or distillation.
  • separation may be by thin film vacuum evaporation, e.g., wiped film evaporation.
  • extracted components 408 and a solvent 410 may be obtained.
  • the extracted components 408 may then be transported to the solidification chamber 412.
  • the extracted components 408 may be solidified in solidification chamber 412.
  • the solidification chamber 412 may involve a drying process, which can include, but is not limited to, spray drying, tumble drying, fluidized bed drying, or a combination of multiple such processes.
  • the solvent 410 may be recycled for use in a later extraction.
  • FIG. 5 is a table providing data collected regarding the concentrations of target compounds present in raw biomass samples from different cultivars or strains of cannabis.
  • concentrations of each of the target compounds can be measured using a variety of analytic testing devices including, but not limited to, gas chromatographs, high performance liquid chromatographs, or mass spectrometers.
  • the raw cannabis biomass may be harvested from various strains of cannabis, at multiple locations, and under different conditions.
  • the biomass may be sampled and inspected using chemical, mechanical, or optical methods prior to performing an extraction process.
  • FIG. 5 is a table providing test data related to various cannabis biomass samples collected from different cannabis cultivars (strains), locations and, on different dates.
  • five cultivars (A, B, C, D, and E) obtained from location 1 were analyzed by UHPLC and found to have wide variability in cannabinoid profiles (e.g ., THCA, THC,
  • cultivars (F, G, and H) from different locations also were found to have variability in cannabinoid profile.
  • cultivar G from location 3 was determined to have very low concentrations of cannabinoids.
  • identical cultivar samples (I) were obtained from location 4 on different days (e.g., date X and date Y) were analyzed by UHPLC and found to have variability in cannabinoid profile just based on the different date of harvest.
  • the conditions used during the extraction of the pharmacologically active components from the raw cannabis biomass as described herein may be adjusted and controlled based on the results of the raw biomass sampling and analysis, as described above, so as to increase purity and yield of cannabis extract.
  • a method 600 for obtaining a solid form cannabis extract is provided in FIG. 6.
  • the method 600 can begin at step 602, where a prepared cannabis biomass can be provided.
  • the prepared cannabis biomass may comprise target compounds for extraction.
  • the raw cannabis biomass may be present in form of dried, ground, and non- decarboxylated flowers (such as buds) of a cannabis plant.
  • the reaw biomass may include either fresh or frozen non-decarboxylated cannabis plants.
  • the method 600 can continue to step 604, wherein a slurry may be formed by adding a solvent to the prepared cannabis biomass material.
  • the solvent added to the prepared cannabis biomass material may be selected based on specific dielectric and solvent parameter properties.
  • the solvent may be selected from the group including, but not limited to, an alcohol group, an alkane group, a ketone group, and mixtures of various solvents, including water.
  • the slurry may be transferred to an extraction chamber at step 606 for the extraction of target cannabinoid components from the slurry.
  • the slurry may be transported to the extraction chamber using a set of mechanical conveyors.
  • the slurry may be heated to a predetermined temperature by exposing the slurry to heat (such as microwave heat), for a predefined period of time, within a predefined energy range.
  • the extraction process can produce of step 606 can produce a spent biomass and a solvent/extract mixture.
  • the spent biomass can be separated from the
  • the solvent may be recovered from the mixture by a distillation process.
  • the solvent may be recovered from the mixture by a distillation process.
  • downstream process may comprise concentration, separation, isolation, and formulation.
  • the solvent may be separated from target components.
  • the solvent is separated from the target components via an evaporation process.
  • the evaporation process may be carried out by heating or via vacuum distillation, or in any of the methods described above.
  • the target components can be solidified using a downstream process, as described in detail above.
  • the downstream solidification process may comprise concentration, separation, isolation, and formulation, to obtain a final solidified extract.
  • the method 600 can being with a prepared cannabis biomass provided at step 602.
  • the prepared biomass can be in the form of dried
  • decarboxylated cannabis flowers ground to a particle size of approximately 8 mm.
  • a slurry can then be formed at step 604 using a ratio of 10 liters of ethanol for each kilogram of prepared biomass.
  • the slurry can then be transferred to an extractor at step 606 for a pre-defined time at a pre-defined temperature, and the spent biomass can be separated from the slurry at step 608.
  • the cannabis extract/ethanol mixture is concentrated under vacuum until the mixture is reduced to approximately one fifth (1/5) of its initial volume.
  • This concentrated extract can then be transferred to a solidification chamber, such as an homogenizer, at step 612 to create an emulsion using carrageenan gum, maltodextrin and silica as the carrier.
  • the relative amount of exdpient was optimized in order to obtain a standardized solid formulation of cannabis containing approximately 20% w/w THC.
  • the emulsion was solidified by spray drying at a temperature of approximately 120°C in the solid processing chamber, such as that described with respect to FIG. 1.
  • the emulsion is solidified until the extract becomes a dried powder.
  • the dried powder was sampled using a sampling chamber as described with respect to FIG. 1 and analyzed to determine the THC content by UHPLC.
  • the resulting standardized THC powder was used to formulate capsules containing approximately 20 mg THC per capsule, mixing the powder with dextrin and lactose fillers and colloidal silicon dioxide as a free flowing agent.
  • a prepared cannabis biomass is provided at step 602 in the form of dried, decarboxylated cannabis flowers ground to a particle size of approximately 8 mm.
  • a slurry was then formed at step 604 using ethanol to create a ratio of 10 liters of ethanol per kilogram of prepared biomass, the slurry was transferred to an extraction chamber at step 606 for a pre-defined period of time at a pre-defined temperature.
  • the spent biomass was separated from the slurry at step 608.
  • the cannabis extract/ethanol mixture was concentrated under vacuum to produce a concentrated cannabis extract containing approximately 45% THC.
  • This concentrated extract was then mixed with a 40% solution of hy d I oxy pro py I - (: > -cy cl od e x t ri n in ethanol during homogenization.
  • the prepared emulsion was then spray dried at a temperature of approximately 120°C in the solid processing chamber, such as that described with respect to FIG. 1 in order to produce a solid form of a cannabis extract ( e.g ., a dried powder).
  • the dried powder was then sampled in a sampling chamber, such as that described with respect to FIG. 1, and analyzed for THC content by UHPLC.
  • the resulting standardized THC powder was determined to contain approximately 4% THC.

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Abstract

La présente invention concerne un système et un procédé d'obtention d'extraits de cannabis sous forme solide. Le procédé comprend la fourniture d'une matière première de biomasse contenant une quantité de composés cibles pour l'extraction. La matière première de biomasse peut être décarboxylée, broyée ou pulvérisée pour obtenir une biomasse de cannabis préparée. Une suspension peut être préparée en ajoutant un solvant à la biomasse de cannabis préparée. Les constituants cibles peuvent être extraits de la suspension par traitement dans un extracteur à écoulement continu. Le solvant peut être séparé d'une biomasse épuisée ; en outre, le solvant peut être séparé des constituants cibles par chauffage et évaporation du solvant. Successivement, les constituants cibles peuvent être solidifiés par un procédé en aval, tel qu'une concentration, séparation, un isolement, et une formulation. Dans un mode de réalisation préféré, l'extrait peut être entièrement ou partiellement débarrassé d'un solvant et mélangé avec un excipient avant un procédé de séchage par pulvérisation.
PCT/IB2019/053571 2018-05-03 2019-05-02 Obtention d'extraits sous une forme solide WO2019211772A1 (fr)

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