CN110251987B - Extraction method for improving cannabidiol content - Google Patents
Extraction method for improving cannabidiol content Download PDFInfo
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- CN110251987B CN110251987B CN201910536255.2A CN201910536255A CN110251987B CN 110251987 B CN110251987 B CN 110251987B CN 201910536255 A CN201910536255 A CN 201910536255A CN 110251987 B CN110251987 B CN 110251987B
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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)
- A61K36/60—Moraceae (Mulberry family), e.g. breadfruit or fig
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/16—Evaporating by spraying
- B01D1/18—Evaporating by spraying to obtain dry solids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- 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
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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- 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
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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Abstract
The invention relates to the technical field of plant extraction, and discloses an extraction method for improving cannabidiol content. The extraction method of the invention extracts industrial hemp, and the obtained industrial hemp extract is concentrated, evaporated and enriched to obtain paste, and then is baked at the temperature of 85-95 ℃. The extraction method selects the specific node to bake the extracted industrial hemp extract, can obviously improve the content of CBD in the extract at a proper temperature, keeps the low-level THC content which is lower than the standard of 0.3 percent, and provides a simple, convenient and effective extraction process for the development and utilization of industrial hemp.
Description
Technical Field
The invention relates to the technical field of plant extraction, in particular to an extraction method for improving cannabidiol content.
Background
The main chemical substances in cannabis are cannabinoids, and the main components of cannabinoids are cannabidiolic acid (CBDA), Cannabidiol (CBD), Tetrahydrocannabinol (THC) and cannabinol, and exist in the form of cannabidiolic acid in plant bodies. According to the literature report, cannabidiol is a cannabis extract with the widest application prospect in cannabis, is a light yellow resin or crystal, and has obvious curative effects on various diseases such as epilepsy, cancer, multiple sclerosis and the like in medicine. Tetrahydrocannabinol is a psychoactive ingredient, and the content of tetrahydrocannabinol in industrial cannabis can not exceed 0.3%. Therefore, the method has important significance for increasing the cannabidiol extraction amount and reducing the tetrahydrocannabinol extraction amount in industrial cannabis.
Disclosure of Invention
In view of the above, the present invention aims to provide an extraction method capable of significantly increasing the content of cannabidiol;
another object of the present invention is to provide an extraction method that increases cannabidiol content while reducing its tetrahydrocannabinol content;
in order to achieve the above purpose, the invention provides the following technical scheme:
an extraction method for increasing cannabidiol content comprises extracting industrial hemp, concentrating the obtained industrial hemp extract, evaporating to dryness to enrich paste, and baking at 85-95 deg.C.
Aiming at the problem of low cannabidiol extraction amount of the current industrial cannabis sativa, the invention improves the cannabidiol content in the extract by baking the industrial cannabis sativa extract at a specific temperature after extraction, and simultaneously maintains the tetrahydrocannabinol content at a lower level, which is lower than 0.3%.
Preferably, the extraction of the industrial hemp is carried out by subjecting the industrial hemp to a thermal reflux extraction using an extraction solvent. Wherein the mass-volume ratio of the industrial hemp to the extraction solvent in the thermal reflux extraction is preferably 1g:20 mL; the extraction solvent is preferably methanol; the hot reflux extraction time is 1h, and the times are two.
Preferably, the temperature is 85 ℃, 86 ℃, 87 ℃, 88 ℃, 89 ℃, 90 ℃, 91 ℃, 92 ℃, 93 ℃, 94 ℃ or 95 ℃; in addition, the baking can be carried out at the temperature of 85-95 ℃ with variable temperature.
Preferably, the baking time is 30min to 180min, more preferably 180 min.
According to the invention, the contents of two groups of CBDA and CBD which are extracted and concentrated into the baked enriched paste and not baked are compared, and an HPLC spectrogram shows that the content of CBD of the baked enriched paste is obviously increased, and the content of CBDA is reduced; whereas the unbaked treatment group showed the opposite result. Meanwhile, different baking times are set, the content changes of CBDA, CBD and THC are detected, and the result shows that the content of CBD is gradually increased and the content of CBDA is gradually decreased along with the extension of baking time at 85 ℃ and 95 ℃, and the content of THC is stabilized at an extremely low level; when the baking is carried out at the temperature lower than 85 ℃ or higher than 95 ℃, the CBD content is not obviously improved or the CBD content is reduced along with the baking time;
in addition, the invention also sets processing groups of different baking nodes for comparison, and HPLC results show that a comparison group 1 which does not perform any baking processing and a comparison group 2 which performs baking on the industrial hemp raw material before extraction only have certain difference in the content of CBDA, but the content of CBD is not obviously different; whereas comparative group 3 and example 1, which were subjected to post-extraction baking, both exhibited a higher content of CBD, except that the two differed in the content of CBDA.
According to the technical scheme, the specific node is selected for baking the extracted industrial hemp extract, the content of CBD in the extract can be obviously improved at a proper temperature, the low-level THC content is kept and is lower than the standard of 0.3%, and a simple, convenient and effective extraction process is provided for development and utilization of industrial hemp.
Drawings
FIG. 1 shows HPLC spectra of the enriched paste after the baked and unbaked treatments;
FIG. 2 shows the effect of different baking times at 65 ℃ on the CBD content;
FIG. 3 shows the effect of different baking times at 85 ℃ on the CBD content;
FIG. 4 shows the effect of different baking times at 95 ℃ on the CBD content;
FIG. 5 shows the effect of different baking times at 105 ℃ on the CBD content;
FIG. 6 shows the effect of different baking times at 115 ℃ on the CBD content;
FIG. 7 shows HPLC profiles of extracts from different extraction methods.
Detailed Description
The invention discloses an extraction method for improving the content of cannabidiol, and a person skilled in the art can appropriately improve process parameters by referring to the content in the text. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the extraction methods of the present invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications of the extraction methods described herein, as well as appropriate variations and combinations of the methods described herein, may be made to implement and use the techniques of the present invention without departing from the spirit and scope of the invention.
In the specific embodiment, except for the due technical differences in the comparative test, the test environments of the other used raw materials, reagents and the like are kept consistent;
the extraction method for increasing the content of cannabidiol provided by the invention is further explained below.
Example 1: the extraction method of the invention
Methanol is used as an extraction solvent, and the ratio of material to liquid is 1g: the industrial hemp is extracted by hot reflux in a water bath at 85 ℃ for 1 hour for 2 times in a proportion of 20 mL. Concentrating and evaporating the extractive solution of Cannabis sativa L to dryness to obtain enriched paste, baking at 85 deg.C, 86 deg.C, 87 deg.C, 88 deg.C, 89 deg.C, 90 deg.C, 91 deg.C, 92 deg.C, 93 deg.C, 94 deg.C or 95 deg.C for 30-180min, preferably 100-180 min;
example 2: effect of baking on CBD content
Two groups of industrial hemp with the same source and quality are extracted according to the extraction method of example 1, except that one group is completely referred to the method of example 1, and the other group is not roasted; the baking temperature is 90 ℃, and the baking time is 3h (180 min); the two groups of enrichment pastes are sampled with the same quality of samples, methanol is used for fixing the volume to 100mL, 1mL is absorbed and put into an injector to be injected after passing through an organic filter membrane, and then HPLC detection is carried out on the obtained extract substances of each group, and the result is shown in figure 1.
As is apparent from fig. 1, the CBDA content in the unbaked enriched paste is significantly higher than that of CBD, and after baking, the CBD content is significantly increased, and the corresponding CBDA content is significantly decreased, and it is presumed that the CBDA in the enriched paste is converted into CBD by the baking operation.
Example 3: effect of different baking times and temperatures on CBD content
The extraction was carried out according to example 1 with setting of five baking temperatures of 65 deg.C, 85 deg.C, 95 deg.C, 105 deg.C and 115 deg.C, respectively, with the baking time starting from 0, sampling every 30min, and plotting into content line graphs, and the results are shown in FIGS. 2-6.
As can be seen from fig. 2 to 6, the content of CBD gradually increased and the content of CBDA gradually decreased with the baking time at 85 ℃ and 95 ℃, and the THC content stabilized at an extremely low level; while when the baking is carried out at a temperature lower than 85 ℃ or higher than 95 ℃, the CBD content is not obviously increased or the CBD content is reduced along with the baking time.
Example 4: comparative testing of different extraction protocols
On the basis of the scheme of the embodiment 1 of the invention, the following comparison groups are respectively set up:
comparative group 1: reference is made to the extraction process of example 1, except that no baking is carried out;
comparative group 2: referring to the extraction method of example 1, except that the industrial hemp was roasted before extraction;
comparative group 3: reference is made to the extraction process of example 1, except that no concentration is carried out;
comparing example 1 with the above 3 groups of methods, the baking temperature and time are kept the same, the concentration operation is kept the same, samples with the same quality are sampled from each group, dissolved by methanol and added to 100mL, 1mL is absorbed and put into a syringe, and then sample injection is carried out after passing through an organic filter membrane, and then HPLC detection is carried out on the obtained extract substances of each group, and the result is shown in figure 7.
As can be seen from fig. 7, the comparative group 1 in which no roasting treatment was performed and the comparative group 2 in which the industrial hemp raw material was roasted before extraction were only slightly different in the CBDA content, but the CBD content was not significantly different; whereas comparative group 3 and example 1, which were subjected to post-extraction baking, both exhibited a higher content of CBD, a significant decrease in CBDA content occurred, and comparative group 3 and example 1 were distinguished by a difference in CBDA content.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (1)
1. An extraction method for improving cannabidiol content is characterized in that industrial cannabis is subjected to hot reflux extraction by using methanol, the mass volume ratio of the industrial cannabis to an extraction solvent is 1g:20mL, the obtained industrial cannabis extract is concentrated, evaporated and evaporated to dryness to enrich paste, and then the paste is baked at the temperature of 95 ℃ for 100-180 min.
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| CN109646992A (en) * | 2019-01-28 | 2019-04-19 | 周继铭 | The method of cannabidiol enriched substance is extracted from industrial hemp |
| CN109803643A (en) * | 2016-07-15 | 2019-05-24 | S.S.斯坦纳公司 | The decarboxylation of cannabidiolic acid in hemp biological matter and Cannador |
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| CN109700789A (en) * | 2019-02-28 | 2019-05-03 | 西藏育宁生物科技有限责任公司 | A kind of purposes of cannabidiol extract |
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| CN109803643A (en) * | 2016-07-15 | 2019-05-24 | S.S.斯坦纳公司 | The decarboxylation of cannabidiolic acid in hemp biological matter and Cannador |
| CN109646992A (en) * | 2019-01-28 | 2019-04-19 | 周继铭 | The method of cannabidiol enriched substance is extracted from industrial hemp |
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