CN112645802A - Preparation method of cannabidiol broad-spectrum oil capable of effectively removing tetrahydrocannabinol - Google Patents
Preparation method of cannabidiol broad-spectrum oil capable of effectively removing tetrahydrocannabinol Download PDFInfo
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Abstract
The invention relates to a preparation method of cannabidiol broad-spectrum oil for effectively removing tetrahydrocannabinol, which comprises the following steps: pretreating raw materials; extracting cannabidiol; winterizing the crude extract; decarboxylation treatment; short-path molecular distillation; deep separation and purification. The method is favorable for reducing the content of tetrahydrocannabinol to the maximum extent during deep separation and purification of the preparative chromatography, ensures the stable quality of the finished cannabidiol broad-spectrum oil, and ensures the safety of the product; the invention reduces the overall production cost and reduces the environmental pollution. The preparation process is simple and easy to control, the THC content is obviously reduced, and the process is simplified; the whole CBD broad-spectrum oil preparation process is easier to realize automation and intellectualization, reduces the human interference, stably controls the quality and the uniformity of products, improves the production efficiency and the product yield, and reduces the consumption of raw materials and energy.
Description
Technical Field
The invention relates to the technical field of medicines, in particular to a preparation method of cannabidiol broad-spectrum oil for effectively removing tetrahydrocannabinol.
Background
Hemp (Cannabis sativa L.) originally originated from Zhongya, also called hemp, hemp and hemp, hemp and hemp thread, is an annual herbaceous plant, and the stem skin fiber of the hemp is long and tough and can be used for weaving hemp cloth, making ropes, making paper and the like; hemp has been used as a fiber, food source for over 3000 years. There are many cannabinoids in cannabis leaves, mainly cannabidiol and its carboxyl compounds.
Cannabidiol is a non-addictive component, can block adverse effects of some polyphenols on human nervous system, and has a series of physiological activity functions of treating diabetes, blocking breast cancer metastasis, resisting spasm, resisting rheumatoid arthritis, resisting insomnia, etc. In recent years, scientists also apply cannabidiol to clinical tests so as to better study the activities of the cannabidiol such as bacteriostasis, anti-inflammation, anti-cancer and the like, and provide effective guarantee for human health. In Europe and America, CBD and CBD-rich cannabis oil are widely applied to medicines, health products, cosmetics and the like, so that extraction and preparation of cannabidiol are widely regarded.
The prior relevant technology for extracting and preparing cannabidiol mainly comprises the modes of solvent extraction, steam distillation, squeezing extraction, supercritical extraction and the like, and the purification methods are column chromatography and are different only in chromatography fillers. The column chromatography method has a plurality of defects, firstly, the operation is complicated, and a plurality of steps of filling a filler into a column, loading a crude product, eluting a mobile phase, concentrating an eluent, refilling the filler and the like are required; secondly, the solvents used for chromatographic separation are considered to be health risks, and some solvents, such as methanol, chloroform and the like, may remain in the obtained product; thirdly, since the chromatographic columns are used in series from one batch to another, the product obtained by the column chromatography technique not only has frequent changes in purity, insufficient stability of product quality, but also has relatively low yield; fourth, the technique produces a large amount of solid waste, the filler. According to the relevant regulations of related national departments, the content of the tetrahydrocannabinol in the raw materials, the products or the waste materials is not higher than 0.3 percent.
With the development of the domestic Cannabidiol (CBD) preparation technology, the production and manufacturing capacity and the physicochemical regulation and control capacity must be improved in the preparation technology, and the quality stability and the safety applicability are further improved in the preparation quality so as to meet the technical and technological requirements of CBD industrial production.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation process of cannabidiol broad-spectrum oil, which has the advantages of low production cost, stable quality of CBD broad-spectrum oil, energy conservation, environmental protection and large-scale production.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a preparation method of cannabidiol broad-spectrum oil for effectively removing tetrahydrocannabinol comprises the following steps:
step (1) pretreatment of raw materials
Crushing and drying industrial hemp leaves, and storing the raw materials for later use after pretreatment;
step (2) cannabidiol extraction
Feeding the pretreated raw materials into a supercritical carbon dioxide extraction system according to a ratio for extraction to obtain a cannabidiol crude extract;
winterization treatment of the crude extract in the step (3)
Fully dissolving the crude extract in a winterization solvent, performing primary filtration, performing heat preservation winterization, and performing centrifugal separation and secondary filtration;
step (4) decarboxylation treatment
Fully dissolving the crude extract subjected to winterization treatment in a decarboxylation solvent for decarboxylation treatment, so that carboxylic acid molecules are decarboxylated to release carbon dioxide;
step (5) short path molecular distillation
Performing short-range molecular distillation and enrichment on the extractum subjected to decarboxylation treatment, and collecting light components;
step (6) deep separation and purification
Deeply separating and purifying the light components subjected to molecular distillation to remove Tetrahydrocannabinol (THC) and obtain cannabidiol broad-spectrum oil with THC content less than 0.3%.
Further, in the step (1), in the industrial hemp flower and leaf raw material pretreatment process, the crushed raw material is 5-20 meshes, the drying temperature is 100-200 ℃, and the water content is less than 8% after drying.
Further, in the step (2), in the supercritical carbon dioxide extraction process, the extraction temperature is 35-80 ℃, the extraction time is 1.5-3 h, and the extraction pressure is 20-40 MPa.
Further, in the step (3), the solid-to-liquid ratio of the crude extract to the winterization solvent is 1: 5-1: 20, the winterization temperature is-100 to-20 ℃, and the heat preservation time is 10 to 24 hours.
Further, in the step (4), the decarboxylation temperature is 65 ℃ to-105 ℃.
Further, in the step (5), the short-path molecular distillation is divided into three stages, wherein a thin film evaporator is adopted in the first stage, and short-path evaporators are adopted in the second stage and the third stage; the temperature of the short-path molecular distillation is 120-200 ℃, and the vacuum degree is 0.001-0.1 mbar.
The crude extract is subjected to decarboxylation after winterization, which is beneficial to the later-stage preparation of the chromatogram, so that the THC content in the CBD broad-spectrum oil can be effectively reduced, and the stable quality of the CBD broad-spectrum oil is ensured.
The preparative chromatographic system is provided with a high-pressure protection system, the highest safe working pressure is adjustable, and the system is automatically stopped when the pressure of the system exceeds the highest working pressure safety value so as to protect the chromatographic system.
Compared with the prior art, the invention has the following advantages:
1) in the production process, the CBD crude extract is subjected to winterization, centrifugal separation, filtration and the like, particularly after decarboxylation, carboxyl in 11-nor-9-carboxyl-delta 9-THC which is one of main components in industrial hemp is directly removed, so that the content of tetrahydrocannabinol is reduced to the maximum extent during deep separation and purification of the prepared chromatogram, the stable quality of finished Cannabidiol (CBD) broad-spectrum oil is ensured, and the safety of the product is ensured.
2) The winterization solvent, the elution solvent and other reagents used in the whole production process are ethanol and water, and can be recycled, so that the overall production cost is reduced, and the environmental pollution is reduced.
3) The short-range molecular distillation system and the preparative chromatography system are matched with each other, so that the CBD crude extract has more advantages in the aspects of purifying, removing a solvent in the extract, decoloring, removing harmful metals and chemical residues and the like, and the preparation process is simple and easy to control, the THC content is obviously reduced, and the process is simplified; the whole CBD broad-spectrum oil preparation process is easier to realize automation and intellectualization, reduces the human interference, stably controls the quality and the uniformity of products, improves the production efficiency and the product yield, reduces the consumption of raw materials and energy sources, and meets the technical and technological requirements of CBD broad-spectrum oil in the aspects of production and manufacturing capability, quality stability, safe applicability, energy conservation, consumption reduction and the like during large-scale industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention. In the following description, for the purpose of clearly illustrating the structure and operation of the present invention, reference will be made to the accompanying drawings by way of directional terms, but terms such as "front", "rear", "left", "right", "up", "down", etc. should be construed as words of convenience and should not be construed as limiting terms.
Example 1
As shown in fig. 1, the method for preparing cannabidiol broad-spectrum oil for effectively removing tetrahydrocannabinol of this example comprises the following steps:
step (1) pretreatment of raw materials
Crushing and drying industrial hemp leaves, and storing the raw materials for later use after pretreatment; the industrial hemp flower and leaf raw material is crushed to 5 meshes in the pretreatment process, the drying temperature is 100 ℃, and the water content is 7.2% after drying.
Step (2) cannabidiol extraction
Feeding the measured raw materials into a supercritical carbon dioxide extraction system according to a ratio for extraction to obtain a cannabidiol crude extract; in the supercritical carbon dioxide extraction process, the extraction temperature is 35 ℃, the extraction time is 1.5h, and the extraction pressure is 20 MPa.
Winterization treatment of the crude extract in the step (3)
Fully dissolving the crude extract in a winterization solvent, performing primary filtration, performing heat preservation winterization, and performing centrifugal separation and secondary filtration; the solid-liquid ratio of the crude extract to the winterization solvent is 1: and 5, winterization temperature is-100 ℃, and heat preservation time is 10 hours.
Step (4) decarboxylation treatment
Fully dissolving the crude extract subjected to winterization treatment in a decarboxylation solvent for decarboxylation treatment, and removing carboxyl from carboxylic acid molecules to release carbon dioxide, wherein the decarboxylation temperature is 65 ℃.
Step (5) short path molecular distillation
Performing short-range molecular distillation enrichment on the extractum subjected to decarboxylation treatment, and collecting light components; the short-path molecular distillation is divided into three stages, wherein the first stage adopts a thin film evaporator, and the second stage and the third stage adopt short-path evaporators. The short-path molecular distillation temperature is 120 ℃, and the vacuum degree is 0.001.
Step (6) deep separation and purification
And (3) deeply separating and purifying the light components subjected to molecular distillation in a preparative chromatograph to remove THC, so as to obtain Cannabidiol (CBD) broad-spectrum oil with THC content less than 0.3%.
The crude extract is subjected to decarboxylation after winterization, which is beneficial to the later-stage preparation of the chromatogram, so that the THC content in the CBD broad-spectrum oil can be effectively reduced, and the stable quality of the CBD broad-spectrum oil is ensured.
The preparation chromatographic system runs automatically, original high-performance polymer chromatographic packing is adopted, and the operating pressure of a chromatographic column is 2.0 MPa.
The preparative chromatographic system is provided with a high-pressure protection system, the highest safe working pressure is adjustable, and the preparative chromatographic system is automatically stopped when the system pressure exceeds the highest working pressure safety value so as to protect the chromatographic system.
Example 2
The preparation method of the cannabidiol broad-spectrum oil for effectively removing tetrahydrocannabinol of the embodiment comprises the following steps:
step (1) pretreatment of raw materials
Crushing and drying industrial hemp leaves, and storing the raw materials for later use after pretreatment; the industrial hemp flower and leaf raw material is crushed to 20 meshes in the pretreatment process, the drying temperature is 200 ℃, and the water content is 8% after drying.
Step (2) cannabidiol extraction
Feeding the measured raw materials into a supercritical carbon dioxide extraction system according to a ratio for extraction to obtain a cannabidiol crude extract; in the supercritical carbon dioxide extraction process, the extraction temperature is 80 deg.C, the extraction time is 1.5h, and the extraction pressure is 40 MPa.
Winterization treatment of the crude extract in the step (3)
Fully dissolving the crude extract in a winterization solvent, performing primary filtration, performing heat preservation winterization, and performing centrifugal separation and secondary filtration; the solid-liquid ratio of the crude extract to the winterization solvent is 1: 20, winterization temperature is-20 ℃, and heat preservation time is 24 h.
Step (4) decarboxylation treatment
Fully dissolving the crude extract subjected to winterization treatment in a decarboxylation solvent for decarboxylation treatment, and removing carboxyl from carboxylic acid molecules to release carbon dioxide, wherein the decarboxylation temperature is 105 ℃.
Step (5) short path molecular distillation
Performing short-range molecular distillation enrichment on the extractum subjected to decarboxylation treatment, and collecting light components; the short-path molecular distillation is divided into three stages, wherein the first stage adopts a thin film evaporator, and the second stage and the third stage adopt short-path evaporators. The short path molecular distillation temperature was 200 ℃ and the vacuum was 0.1 mbar.
Step (6) deep separation and purification
And (3) deeply separating and purifying the light components subjected to molecular distillation in a preparative chromatograph to remove THC, so as to obtain Cannabidiol (CBD) broad-spectrum oil with THC content less than 0.3%.
The crude extract is subjected to decarboxylation after winterization, which is beneficial to the later-stage preparation of the chromatogram, so that the THC content in the CBD broad-spectrum oil can be effectively reduced, and the stable quality of the CBD broad-spectrum oil is ensured.
The preparative chromatographic system is operated in full automation, original high-performance polymer chromatographic packing is adopted, and the operating pressure of a chromatographic column is 2.0 MPa.
Example 3
The preparation method of the cannabidiol broad-spectrum oil for effectively removing tetrahydrocannabinol of the embodiment comprises the following steps:
step (1) pretreatment of raw materials
Crushing and drying industrial hemp leaves, and storing the raw materials for later use after pretreatment; the industrial hemp flower and leaf raw material is crushed to 10 meshes in the pretreatment process, the drying temperature is 170 ℃, and the water content is 7.6% after drying.
Step (2) cannabidiol extraction
Feeding the measured raw materials into a supercritical carbon dioxide extraction system according to a ratio for extraction to obtain a cannabidiol crude extract; in the supercritical carbon dioxide extraction process, the extraction temperature is 50 ℃, the extraction time is 2.5h, and the extraction pressure is 30 MPa.
Winterization treatment of the crude extract in the step (3)
Fully dissolving the crude extract in a winterization solvent, performing primary filtration, performing heat preservation winterization, and performing centrifugal separation and secondary filtration; the solid-liquid ratio of the crude extract to the winterization solvent is 1: 10, winterization temperature is-40 ℃, and the heat preservation time is 20 h.
Step (4) decarboxylation treatment
Fully dissolving the crude extract subjected to winterization treatment in a decarboxylation solvent for decarboxylation treatment, and removing carboxyl from carboxylic acid molecules to release carbon dioxide, wherein the decarboxylation temperature is 85 ℃.
Step (5) short path molecular distillation
Performing short-range molecular distillation enrichment on the extractum subjected to decarboxylation treatment, and collecting light components; the short-path molecular distillation is divided into three stages, wherein the first stage adopts a thin film evaporator, and the second stage and the third stage adopt short-path evaporators. The short path molecular distillation temperature was 160 ℃ and the vacuum was 0.06 mbar.
Step (6) deep separation and purification
And (3) deeply separating and purifying the light components subjected to molecular distillation in a preparative chromatograph to remove THC, so as to obtain Cannabidiol (CBD) broad-spectrum oil with THC content less than 0.3%.
The crude extract is subjected to decarboxylation after winterization, which is beneficial to the later-stage preparation of the chromatogram, so that the THC content in the CBD broad-spectrum oil can be effectively reduced, and the stable quality of the CBD broad-spectrum oil is ensured.
The preparative chromatographic system is operated in full automation, original high-performance polymer chromatographic packing is adopted, and the operating pressure of a chromatographic column is 2.0 MPa.
In the embodiment 1, compared with the traditional compound extraction method, the supercritical carbon dioxide extraction process has remarkable advantages, ensures the extraction rate, and simultaneously does not involve chemical reagents, thereby fundamentally avoiding the problem of reagent residue in the product and avoiding the pollution of the chemical reagents to the environment; the method has mild operation conditions, and plays a positive role in protecting heat-sensitive and easily-oxidized compounds; the operation is simple and convenient, and the manpower consumption is greatly reduced; it can efficiently and rapidly complete extraction and separation, and reduce time consumption.
During the production process, the CBD crude extract is subjected to winterization, centrifugal separation, filtration and the like, particularly after decarboxylation, carboxyl in 11-nor-9-carboxyl-delta 9-tetrahydrocannabinol which is one of main components in industrial hemp is directly removed, so that the content of the tetrahydrocannabinol is reduced to the maximum extent during deep separation and purification of the preparation chromatogram, the stable quality of finished product Cannabidiol (CBD) broad-spectrum oil is ensured, and the safety of the product is ensured.
The molecular distillation process is not operated under the condition of being far away from the boiling point, so that the energy consumption can be greatly saved; the heating time is short, the heat damage of the heat-sensitive substances is reduced, and the decomposition or polymerization of the substances is avoided; while the relative volatility of molecular distillation is greater than that of conventional distillation. Therefore, separation of substances is more easily achieved.
In the embodiment, preparative chromatography is a novel high-efficiency and energy-saving separation technology which is suitable for the development of science and technology and production needs. The sample loading amount of the prepared chromatographic polymer filler is 5 times that of silica gel, the filler consumption is greatly reduced, the equipment specification is smaller, the service life is 5 times that of the silica gel, meanwhile, the solvent consumption is greatly reduced, the production efficiency is greatly improved, the production process is more environment-friendly, and the product purification cost is obviously reduced. In the cannabidiol production process, preparative chromatography is an effective tool for meeting the challenges of product cost, quality standards and production efficiency.
According to the embodiment, by controlling the process parameters such as sample loading amount, mobile phase and fluid distribution, CBD products with different qualities can be obtained, and a refined CBD product with the yield of more than 90% and the purity of more than 99% is also obtained, and no THC (tetrahydrocannabinol) is detected in the product by adopting the process disclosed by the invention. The whole CBD broad-spectrum oil preparation process is easier to realize automation and intellectualization, reduces the human interference, stably controls the quality and the uniformity of products, improves the production efficiency and the product yield, reduces the consumption of raw materials and energy sources, and meets the technical and technological requirements of CBD broad-spectrum oil in the aspects of production and manufacturing capability, quality stability, safe applicability, energy conservation, consumption reduction and the like during large-scale industrial production.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the present invention. It will be understood by those skilled in the art that any modification, equivalent replacement, or improvement made on the technical solutions or parts of the technical features described in the above embodiments can be included in the scope of protection of the present invention within the spirit and principle of the present invention.
Claims (6)
1. A preparation method of cannabidiol broad-spectrum oil for effectively removing tetrahydrocannabinol is characterized in that: the method comprises the following steps:
step (1) pretreatment of raw materials
Crushing and drying industrial hemp leaves, and storing the raw materials for later use after pretreatment;
step (2) cannabidiol extraction
Feeding the pretreated raw materials into a supercritical carbon dioxide extraction system according to a ratio for extraction to obtain a cannabidiol crude extract;
winterization treatment of the crude extract in the step (3)
Fully dissolving the crude extract in a winterization solvent, performing primary filtration, performing heat preservation winterization, and performing centrifugal separation and secondary filtration;
step (4) decarboxylation treatment
Fully dissolving the crude extract subjected to winterization treatment in a decarboxylation solvent for decarboxylation treatment, so that carboxylic acid molecules are decarboxylated to release carbon dioxide;
step (5) short path molecular distillation
Performing short-range molecular distillation and enrichment on the extractum subjected to decarboxylation treatment, and collecting light components;
step (6) deep separation and purification
Deeply separating and purifying the light components subjected to molecular distillation to remove Tetrahydrocannabinol (THC) and obtain cannabidiol broad-spectrum oil with THC content less than 0.3%.
2. The method of claim 1, wherein: in the step (1), in the industrial hemp flower and leaf raw material pretreatment process, the crushed raw material reaches 5-20 meshes, the drying temperature is 100-200 ℃, and the water content after drying is less than 8%.
3. The method of claim 1, wherein: in the step (2), in the supercritical carbon dioxide extraction process, the extraction temperature is 35-80 ℃, the extraction time is 1.5-3 h, and the extraction pressure is 20-40 MPa.
4. The method of claim 1, wherein: in the step (3), the solid-to-liquid ratio of the crude extract to the winterization solvent is 1: 5-1: 20, the winterization temperature is-100 to-20 ℃, and the heat preservation time is 10 to 24 hours.
5. The method of claim 1, wherein: in the step (4), the decarboxylation temperature is 65 ℃ to-105 ℃.
6. The method of claim 1, wherein: in the step (5), the short-path molecular distillation is divided into three stages, wherein a thin film evaporator is adopted in the first stage, and short-path evaporators are adopted in the second stage and the third stage; the temperature of the short-path molecular distillation is 120-200 ℃, and the vacuum degree is 0.001-0.1 mbar.
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| WO2024088290A1 (en) * | 2022-10-27 | 2024-05-02 | 云南麻叶生物科技有限公司 | Preparation method for zero-thc industrial cannabinoid oil |
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