WO2023009442A1 - Improved process for ph-balanced cbg (# 10) - Google Patents
Improved process for ph-balanced cbg (# 10) Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 230000008569 process Effects 0.000 title claims abstract description 26
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 38
- 239000000203 mixture Substances 0.000 claims description 29
- 239000002904 solvent Substances 0.000 claims description 19
- 244000025254 Cannabis sativa Species 0.000 claims description 15
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims description 15
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims description 15
- 235000009120 camo Nutrition 0.000 claims description 15
- 235000005607 chanvre indien Nutrition 0.000 claims description 15
- 239000011487 hemp Substances 0.000 claims description 15
- 238000013019 agitation Methods 0.000 claims description 14
- 238000009472 formulation Methods 0.000 claims description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims 3
- 238000007710 freezing Methods 0.000 claims 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims 1
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 229940071648 metered dose inhaler Drugs 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 10
- 239000011521 glass Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 239000008186 active pharmaceutical agent Substances 0.000 description 3
- QHMBSVQNZZTUGM-ZWKOTPCHSA-N cannabidiol Chemical compound OC1=CC(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)=C)CCC(C)=C1 QHMBSVQNZZTUGM-ZWKOTPCHSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000001225 therapeutic effect Effects 0.000 description 3
- QHMBSVQNZZTUGM-UHFFFAOYSA-N Trans-Cannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1C1C(C(C)=C)CCC(C)=C1 QHMBSVQNZZTUGM-UHFFFAOYSA-N 0.000 description 2
- 229950011318 cannabidiol Drugs 0.000 description 2
- ZTGXAWYVTLUPDT-UHFFFAOYSA-N cannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1C1C(C(C)=C)CC=C(C)C1 ZTGXAWYVTLUPDT-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- PCXRACLQFPRCBB-ZWKOTPCHSA-N dihydrocannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)C)CCC(C)=C1 PCXRACLQFPRCBB-ZWKOTPCHSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000011514 reflex Effects 0.000 description 2
- 239000013557 residual solvent Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000009885 systemic effect Effects 0.000 description 2
- RPGGYYVWJTWVMS-ZPSVQYCPSA-N (8r,9s,10r,13s,14s,17r)-17-ethynyl-10,13-dimethyl-1,2,3,6,7,8,9,11,12,14,15,16-dodecahydrocyclopenta[a]phenanthren-17-ol;(8r,9s,13s,14s,17r)-17-ethynyl-13-methyl-7,8,9,11,12,14,15,16-octahydro-6h-cyclopenta[a]phenanthrene-3,17-diol Chemical compound OC1=CC=C2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1.C1CC[C@]2(C)[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 RPGGYYVWJTWVMS-ZPSVQYCPSA-N 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 206010043521 Throat irritation Diseases 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229930003827 cannabinoid Natural products 0.000 description 1
- 239000003557 cannabinoid Substances 0.000 description 1
- 229940065144 cannabinoids Drugs 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000002685 pulmonary effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 229940124597 therapeutic agent Drugs 0.000 description 1
- 238000010626 work up procedure Methods 0.000 description 1
Classifications
-
- 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
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/658—Medicinal preparations containing organic active ingredients o-phenolic cannabinoids, e.g. cannabidiol, cannabigerolic acid, cannabichromene or tetrahydrocannabinol
-
- 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
- A61K9/0012—Galenical forms characterised by the site of application
- A61K9/007—Pulmonary tract; Aromatherapy
- A61K9/0073—Sprays or powders for inhalation; Aerolised or nebulised preparations generated by other means than thermal energy
- A61K9/008—Sprays or powders for inhalation; Aerolised or nebulised preparations generated by other means than thermal energy comprising drug dissolved or suspended in liquid propellant for inhalation via a pressurized metered dose inhaler [MDI]
Definitions
- the background of the invention relates to metered dose, inhaler-related products, formulations, and methods of manufacturing.
- CBG is known to be a therapeutic agent, inter alia, in the realm of remediation of pain.
- An optimal mode of administration involves the use of atomizing inhalers. Integration of CBG and inhalers, utilizing currently known methods and formulations, manifest a number of significant shortcomings with respect to each of efficacious administration as well as both avoidance of adulteration and reasonable shelf life of all presently known inhaler-contained, to-be-administered CBG formulations.
- CBD cannabidiol
- inhaler-based CBG products are, by their formulations, manufacturing methodologies and post-production age by the time of their use, less efficacious that the present inventors have determined that CBG products otherwise could be, elicit unpleasant side-effects for users, and fail even to meet regulatory product adulteration standards.
- CBD cannabidiol
- the present inventors here disclose a novel and unobvious crystallization process to efficiently produce pH-balanced CBG in an oxygen-free environment that is optimally delivered in a metered-dose inhaler, without re-engineering the typical droplet size which is otherwise essential in the efficacious use of any systemic inhaler.
- the process of the present invention is a crystallization work-up that creates a more properly balance pH/CBG isolate for use into an RTSL inhaler.
- the present inventors have, through extensive research and testing, developed a CBG formulation and manufacturing process that addresses each of the above-described shortcoming of the present art.
- the next step is the addition of a high temperature Hemp distillate. a. Note: The Hemp distillate must be greater than 80% CBG by volume.
- Total % of Hemp Distillate will depend on maximum working volume of the JFR -20% working volume and 1 Kg of n- Pentane for every 1 Kg of distillate and/or the amount of available material into the main body of the JFR).
- the JFR is now ready for -40° C n-Pentane solvent rinses.
- the vacuum level should be 20 inches of mercury (inHg).
- the vacuum pump and collection vessels should be rated for 26 inHg or lower.
- d. Notes: Change the glass rated vacuum collection vessels that contain the mother liquors with clean vessels before starting step #13. None mix the mothers liquors with the rinsing solvents.
- the CBG material in the JFR is now ready for solvent rinsing. Weigh out 20% of filtered -40° C n-Pentane. (Percentage comes from the total reactor volume less 20% of reactor volume).
- the JFR is then empty of residual solvent and ready for the rinse.
- steps 13 and 14 at least 4 times or until the majority of the CBG wet- isolate is white with a little pink color.
- This material is then considered an active pharmaceutical ingredient (API).
- API active pharmaceutical ingredient
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Engineering & Computer Science (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention is a unique crystallization process that yields a more properly balanced pH/CBG Isolate for optimum use into a metered-dose inhaler.
Description
TITLE OF THE INVENTION: Improved process for pH-balanced CBG (# 10)
APPLICANT: Rapid Therapeutic Science Laboratories, LLC
INVENTORS: DRINKWINE, Duane, SCHMIDT, Donal R.
BERRIER, Sean P.
STATEMENT OR PRIORITY
[0001] This is an original, U.S. provisional patent application.
Technical Field
[0002] Generally, the background of the invention relates to metered dose, inhaler-related products, formulations, and methods of manufacturing.
Background Art
[0003] CBG is known to be a therapeutic agent, inter alia, in the realm of remediation of pain. An optimal mode of administration involves the use of atomizing inhalers. Integration of CBG and inhalers, utilizing currently known methods and formulations, manifest a number of significant shortcomings with respect to each of efficacious administration as well as both avoidance of adulteration and reasonable shelf life of all presently known inhaler-contained, to-be-administered CBG formulations.
Summary of the Invention
[0004] In the present disclosure, the inventors seek to provide, vis-a-vis prior methods, formulations and administrative devices, improved methods of formulation and associated optimal delivery means associated with the therapeutic use of cannabidiol (CBG).
[0005] The referenced challenges associated with providing means for therapeutic CBG administration are yet to be resolved in the art, in part, for failure to recognize, either the above limitations themselves, the source of the limitations, or both.
[0006] Investigations by present inventor(s) reveal that present inhaler-based CBG formulations (at least as presently generated at the manufacturing stage) are adulterated in every known instance. This, because present manufacturing methods and underlying formulations fail to prevent oxidation of certain constituents. Not only do these circumstances inherently reduce or eliminate the efficacy of the CBG formulation, but the resulting product is, or quickly after manufacturing becomes incompatible with the very operation of the selected inhaler in delivery even of otherwise optimally metered particulates. Further still, present CBG, inhaler-based products, for any or all of the foregoing issues, tend to cause throat irritation for most users, and in some users elicit a gag reflex.
[0007] In short: present, inhaler-based CBG products are, by their formulations, manufacturing methodologies and post-production age by the time of their use, less efficacious that the present inventors have determined that CBG products otherwise could be, elicit unpleasant side-effects for users, and fail even to meet regulatory product adulteration standards.
[0008] In view of the foregoing, it would be advantageous to have a product that eliminates reactivity and irritation in the human airway that causes the cough reflex so that cannabidiol (CBG) may be inhaled as a systemic treatment through the pulmonary route of administration.
[0009] In view of the foregoing, it would be further advantageous to create a more stabilized, unadulterated, properly balanced pH CBG Isolate.
[0010] In view of the foregoing, it would be further advantageous to utilize a process that balances CBG pH and creates an oxygen-free environment that is stable throughout long-term storage.
[0011] The present inventors here disclose a novel and unobvious crystallization process to efficiently produce pH-balanced CBG in an oxygen-free environment that is optimally delivered in a metered-dose inhaler, without re-engineering the typical droplet size which is otherwise essential in the efficacious use of any systemic inhaler. [0012] The process of the present invention is a crystallization work-up that
creates a more properly balance pH/CBG isolate for use into an RTSL inhaler.
DESCRIPTION OF EMBODIMENTS
[0013] The present inventors have, through extensive research and testing, developed a CBG formulation and manufacturing process that addresses each of the above-described shortcoming of the present art.
[0014] The optimal steps in the here disclosed CBG product formulation methodology include:
1. Filter -40° C n-Pentane (solvent) through a 2 micron filter paper and APICAL Buchner filter funnel. a. Note. The amount will depend on the size of the Jacketed Filter Reactor (JFR). Example: When using a 5L APICAL filter reactor, use 200mL of
-40° C solvent for each purification step.
2. Add ~5% of 80% of the total working volume of the JFR of filtered -40° C n- Pentane into the main body of the JFR.
3. Prior to adding Hemp distillate to the JFR, heat the distillate to 60° C. Once the distillate is at 60° C, proceed to the next step.
4. The next step is the addition of a high temperature Hemp distillate. a. Note: The Hemp distillate must be greater than 80% CBG by volume.
5. Charge the Hemp distillate (Total % of Hemp Distillate will depend on maximum working volume of the JFR -20% working volume and 1 Kg of n- Pentane for every 1 Kg of distillate and/or the amount of available material into the main body of the JFR).
6. Then add 1 Kg of filtered -40° C n-Pentane (solvent) to every 1 Kg of greater than 80% CBG distillate to the main body of the JFR.
7. Agitate the n-Pentane and distillate, which will create an aqueous solution. Turn on the overhead motor and propeller assembly of the JFR and set the motor to -125 RPM to create a homogenous solution. a. Note: The agitation must form a slight vortex - if no vortex is present, then increase the RPM in 15 RPM increments until a noticeable vortex is achieved.
Set the temperature control system (TCS) heating/cooling circulator to a jacket temperature of -35° C while maintaining a slight vortex for -1.5 hours. a. The Huber Ministat 230 TCS is used for a 5L APICAL Filter reactor. Then set the TCS to 30° C to cool the jacket of the JFR. After 30° C is achieved, let agitate for -15 minutes. Next, mix 1 gram of potassium carbonate (K2CO3) with 2 grams of filter distilled water (D/H2O) by weight in a separate beaker until all the potassium is dissolved. Add the mixture into the main body of the JFR. a. Note: Never add D/H2O or K2CO3 directly to the aqueous mixture without dissolving the K2CO3 in D/H2O. Agitate the homogenous solution for 15 to 20 minutes. Check for a pH value of 6 to 7. Repeat step #6, if necessary, until the proper pH level is achieved. a. Note: pH of raw distillate varies from batch to batch. Lower the TCS to a jacket temperature of 25° C. After the jacket temperature reaches 25° C, agitate for -5 minutes. Continue to lower the jacket temperature by 5° C increments, remembering to let agitate for -5 minutes for every temperature change until the JFR reaches a temperature of 10° C. After 10° C is achieved in the JFR, let agitate for -5 minutes at -10° C. Then add 0.001% of CBG seeds. After adding the seeds to the main body of the JFR, agitate for -15 minutes. a. Note (%) will come from total volume weight of distillate and solvent combined. Lower the jacket filter reactor temperature to 5° C. After jacket temperature reaches 5° C, leave for -5 minutes, then set temperature to 0° C. After jacket temperature reaches 0° C, agitate for -5 minutes. Continue changing the jacket temperature in 5° increments until -20° C is reached or until the material will not agitate. (Turn off the agitation motor). a. Note: The material in the JFR is now in a wet-powder state. Then remove the residual solvent (Mother Liquors) in the JFR, which contains left over, unwanted cannabinoids, some CBG and the impurities that were in the distillate. a. Note. Utilizing a vacuum pump control system and vacuum rated glass collection vessels, start pulling out the residual
material (Mother Liquors) through the bottom valve until there is no more solvent/material exiting the JFR. Once the vacuum control lines that are connected to the bottom valve and the lines going into the vacuum rated glass collection vessels are empty, the JFR is now ready for -40° C n-Pentane solvent rinses. b. Note. The vacuum level should be 20 inches of mercury (inHg). c. Note: The vacuum pump and collection vessels should be rated for 26 inHg or lower. d. Notes: Change the glass rated vacuum collection vessels that contain the mother liquors with clean vessels before starting step #13. Never mix the mothers liquors with the rinsing solvents. The CBG material in the JFR is now ready for solvent rinsing. Weigh out 20% of filtered -40° C n-Pentane. (Percentage comes from the total reactor volume less 20% of reactor volume). Example: a 20L Jacketed Filter Reactor will have a solvent rinse of 800mL of -40° C n-Pentane, (20L x 20% -20% = 800mL). Charge the main body of the JFR with 20% of -40° C n-Pentane that contains the wet-powder (isolate). This is the first rinse. After adding the rinsing solvent, keep it in the JFR for ~5 minutes. Remove the -40° C n-Pentane rinsing solvent. a. Note. Removal is accomplished by utilizing vacuum pump control and vacuum rated glass collection vessels. Start pulling out the rinsing solvent by vacuum through the vacuum rated glass vessel and bottom valve until there is no more solvents exiting the JFR. Once the vacuum control lines in the vacuum rated glass collection vessels and lines connected to the bottom valve are empty, the JFR is then empty of residual solvent and ready for the rinse. Repeat steps 13 and 14 at least 4 times or until the majority of the CBG wet- isolate is white with a little pink color. Next, take a sample of the isolate and send it to the analytical lab for HPLC testing. The sample must have a purification of 99+% purity. If not, more solvent rinses are necessary. Once the purity level is reached, move to next step. Offloading and Purification proceeds immediately after proper purity level is achieved. Remove the isolate from the JFR with SS or PTFE spoons and place the material in a 2 micron filter paper and APICAL Buchner filter funnel.
24. After removing the isolate and placing it into the 2 micron filter paper and APICAL Buchner filter funnel, level and smooth the isolate until a flat or level cake is achieved. Then add filtered -40° C n-Pentane to the top of the isolate (Cake) until it covers all of the isolate, making sure that there are no holes or cracks in the cake. If there are holes or cracks, then smooth the cake with an SS or PTFE spoon, as this will ensure a uniform wash. Wait ~3-minutes, then pull the vacuum until no more solvent is seen being pulled through the purification system. Repeat this step 4-times.
25. Next, add D/hhO to the top of the cake until it covers all of the isolate, again, making sure that there are no cracks or holes in the cake. Wait ~3 minutes, then pull the vacuum until there is no more solvent seen being pulled through the 2 micron filter paper and APICAL Buchner filter funnel. Repeat this step 4 times. a. Note: If more rinses are needed, then repeat steps 18 and 19.
This will depend on the quality of the initial Hemp distillate. b. Note: Before offloading the cake (isolate) from the 2 micron filter paper and APICAL Buchner filter funnel, test a small sample with ethanol. Mix the isolate with ethanol into a sample vial and shake it for ~30 seconds. The color should appear slightly purple. If the color is yellowish, then the material has too many contaminants and re-crystallization must be redone.
26. Offload the isolate by using an SS or PTFE spoon into glass trays. Break up the isolate into small pieces for faster drying. Place non-shredding towels over the glass drying trays.
27. Place the isolate that is in the glass drying trays in the vacuum oven. Set the temperature to 30° C and start pulling vacuum. Once the vacuum level is below atmosphere, slowly add nitrogen (N2) through a control valve and let dry overnight, removing all unwanted solvent and oxygen from the isolate.
This material is then considered an active pharmaceutical ingredient (API). a. Warning: Always keep the nitrogen (N2) level below atmospheric conditions to avoid building up pressure. b. Note: Never set the oven temperature above 35° C.
28. Offload the isolate (API) into two non-static bags: the first will contain the material, the second will provide secondary containment. Then zip tie both bags and place them in a non-transparent container with a lock out tag. The bags are then purged of O2 and vacuumed and/or filled with N2.
[0015] The CBG product resulting from the above process represents a substantial improvement over any known CBG product in every respect in relation to product efficacy, shelf life, and user tolerance.
[0016] Although the invention has been described with reference to specific embodiments, this description is not meant to be construed in a limited sense. Various modifications of the disclosed embodiments, as well as alternative embodiments of the inventions will become apparent to persons skilled in the art upon the reference to the description of the invention. It is, therefore, contemplated that the appended claims will cover such modifications that fall within the scope of the invention.
Claims
Claims
We claim:
1. A process for producing an improved CBG formulation comprising the steps of: introduce a first measure of n-Pentane at below freezing temperature to a vessel having a working volume; in a hemp charging step, introduce a first measure of hemp distillate, heated to above freezing level to said vessel to produce a first mixture of said first measure of n-Pentane and said first measure of said hemp distillate; perform an agitation step by agitating said first mixture within said vessel; during said agitation step add to said first mixture a measure of aqueous potassium carbonate solution to produce a second mixture; during said agitation step, reduce the temperature of said first mixture until said first mixture achieves a substantially non-fluidic state at a terminal agitation step temperature; remove mother liquors from said second mixture through application of a vacuum to said second mixture to produce an first isolate; perform a first solvent rinsing step of said first isolate through application of a second measure of n-Pentane cooled to below freezing temperature, after which said n-Pentane is substantially removed by application of vacuum to said first isolate; perform an first aqueous rinsing step to said first isolate after said first solvent rinsing step, after which water used in said first aqueous rinsing step is substantially removed by application of vacuum to said first isolate; and perform a storage step by placing said first isolate within a substantially inert gaseous atmosphere substantially devoid of oxygen.
2. The process of claim 1 wherein said first measure of n-Pentane is cooled to at least -205 C before introduction into said vessel.
3. The process of claim 1 wherein said first measure of said Hemp distillate is heated to at least 405 C before introduction into said vessel.
4. The process of claim 1 wherein: said first measure of n-Pentane is cooled to at least -205 C before introduction into said vessel; and said first measure of said Hemp distillate is heated to at least 405 C before introduction into said vessel.
5. The process of Claim 1 wherein said first aqueous rinsing step comprises the use substantially of a solution of D/H20 and K2CO3.
6. The process of claim 1 wherein said first measure of n-Pentane is cooled to between approximately -205 C and approximately -405 C before introduction into said vessel.
7. The process of claim 1 wherein said first measure of said Hemp distillate is heated to between approximately 405 C and approximately 605 C before introduction into said vessel.
8. The process of claim 1 wherein: said first measure of n-Pentane is cooled to between approximately -205 C and approximately -405 C before introduction into said vessel; and
said first measure of said Hemp distillate is heated to between approximately 405 C and approximately 605 C before introduction into said vessel.
9. The process of Claim 1 wherein said first aqueous rinsing step comprises the use substantially a solution of D/H20 and K2CO3.
10. The process of Claim 1 wherein for every volumetric part of hemp distillate introduced into said vessel during said hemp charging step, approximately 1/3 of said volume of n-Pentane is introduced into said vessel.
11. The process of Claim 1 wherein said substantially inert gaseous atmosphere of said storage step consists essentially of nitrogen gas.
12. The process of Claim 1 further comprising the step of adding a first measure of CBG seeds during said agitation step.
14. The process of Claim 1 wherein said agitation step comprises reducing the temperature of said first mixture in a plurality of increments, at each said increment allowing the temperature of said first mixture to a desired incremental temperature before proceeding to a next said increment, or to said terminal agitation step temperature.
15. The process of Claim 8 wherein said agitation step comprises reducing the temperature of said first mixture in a plurality of increments, at each said increment allowing the temperature of said first mixture to a desired incremental temperature before proceeding to a next said increment, or to said terminal agitation step temperature.
16. The process of Claim 1 wherein said terminal agitation step temperature is between -05 C and approximately -205 C.
17. The process of Claim 14 wherein said terminal agitation step temperature is between -05 C and approximately -205 C.
18. The process of Claim 15 wherein said terminal agitation step temperature is between -05 C and approximately -205 C.
19. The process of Claim 1 wherein said vessel is a jacketed filter reactor.
20. The process of Claim 14 wherein said vessel is a jacketed filter reactor.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US202163259575P | 2021-07-26 | 2021-07-26 | |
| US63/259,575 | 2021-07-26 |
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| WO2023009442A1 true WO2023009442A1 (en) | 2023-02-02 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030017216A1 (en) * | 2001-07-23 | 2003-01-23 | Schmidt Robert Gustav | Isolation of herbal and cannabinoid medicinal extracts |
| US7321027B2 (en) * | 2000-04-28 | 2008-01-22 | President And Fellows Of Harvard College | Small technetium-99m and rhenium labeled agents and methods for imaging tumors |
| US20130079531A1 (en) * | 2011-09-27 | 2013-03-28 | Rm3 Labs LLC | Process for the Rapid Extraction of Active Ingredients from Herbal Materials |
| WO2016153347A1 (en) * | 2015-03-23 | 2016-09-29 | Echo Pharmaceuticals B.V. | Cannabidiol isolate from industrial-hemp and use thereof in pharmaceutical and/or cosmetic preparations |
| US20170189463A1 (en) * | 2015-02-24 | 2017-07-06 | Ers Holdings, Llc | Method for Conducing Concentrated Cannabis Oil to Be Stable, Emulsifiable and Flavorless for Use in Hot Beverages and Resulting Powderized Cannabis Oil |
-
2022
- 2022-07-25 WO PCT/US2022/038197 patent/WO2023009442A1/en unknown
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7321027B2 (en) * | 2000-04-28 | 2008-01-22 | President And Fellows Of Harvard College | Small technetium-99m and rhenium labeled agents and methods for imaging tumors |
| US20030017216A1 (en) * | 2001-07-23 | 2003-01-23 | Schmidt Robert Gustav | Isolation of herbal and cannabinoid medicinal extracts |
| US20130079531A1 (en) * | 2011-09-27 | 2013-03-28 | Rm3 Labs LLC | Process for the Rapid Extraction of Active Ingredients from Herbal Materials |
| US20170189463A1 (en) * | 2015-02-24 | 2017-07-06 | Ers Holdings, Llc | Method for Conducing Concentrated Cannabis Oil to Be Stable, Emulsifiable and Flavorless for Use in Hot Beverages and Resulting Powderized Cannabis Oil |
| WO2016153347A1 (en) * | 2015-03-23 | 2016-09-29 | Echo Pharmaceuticals B.V. | Cannabidiol isolate from industrial-hemp and use thereof in pharmaceutical and/or cosmetic preparations |
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