CN111138404A - Cannabis sativa root extract and preparation method thereof - Google Patents
Cannabis sativa root extract and preparation method thereof Download PDFInfo
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- CN111138404A CN111138404A CN202010064208.5A CN202010064208A CN111138404A CN 111138404 A CN111138404 A CN 111138404A CN 202010064208 A CN202010064208 A CN 202010064208A CN 111138404 A CN111138404 A CN 111138404A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/78—Ring systems having three or more relevant rings
- C07D311/80—Dibenzopyrans; Hydrogenated dibenzopyrans
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/004—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by obtaining phenols from plant material or from animal material
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C39/00—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a six-membered aromatic ring
- C07C39/205—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a six-membered aromatic ring polycyclic, containing only six-membered aromatic rings as cyclic parts with unsaturation outside the rings
- C07C39/21—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a six-membered aromatic ring polycyclic, containing only six-membered aromatic rings as cyclic parts with unsaturation outside the rings with at least one hydroxy group on a non-condensed ring
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
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- Life Sciences & Earth Sciences (AREA)
- Botany (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to the technical field of biological medicines, and particularly relates to a cannabis root extract and a preparation method thereof, wherein the cannabis root extract is rich in cannabine, terpene alcohol, cannabinone and the like, and tetrahydrocannabinol is not detected; the obtained Cannabis sativa root extract has effects of removing blood stasis, stopping bleeding, and promoting urination. The invention provides a method for preparing a cannabis sativa root extract by a conventional method, which has the advantages of simple process and strong applicability, and is very suitable for industrial large-scale production; the prepared hemp root extract has completely retained effective components, and has obvious functions of removing blood stasis, stopping bleeding and promoting urination.
Description
Technical Field
The invention belongs to the technical field of biological medicines, and particularly relates to a cannabis sativa root extract and a preparation method thereof.
Background
Industrial hemp (Stevia rebaudiana Bertoni) is an annual plant of the genus cannabis of the family cannabinaceae, widely distributed around the world. The Cannabis plants in the world are mainly 3 species of wild Cannabis sativa (Cannabis ruderalisisch), Indian Cannabis sativa (Cannabis indica Lam) and cultivated Cannabis sativa (Cannabis sativaL), and many Cannabis varieties and subspecies are generated in the long-term biological evolution process. Cannabis sativa contains Tetrahydrocannabinol (THC), a hallucinogenic secondary metabolite, and is one of the well-known drug-source plants. For convenience of supervision and reasonable use, the varieties of cannabis with THC content of less than 0.3% in cannabis are internationally defined as industrial cannabis which does not have drug utilization value. At present, 27 countries in the world grow industrial cannabis, and 26 industrial cannabis varieties with THC content of less than 0.3% are cultivated.
The known compounds separated from the root of hemp are dozens of compounds, including cannabine (canabisacetine), anhydrocannabine (anhyrocanabisacetine), choline (choline), nervine (nervine), friedelin (friedelin), epifriedelinol (epifriedelinol), carabrone (carvone), dihydrocarvone (dihydrocarvone), β -sitosterol (β -sitosterol) [4], cannabichromene (cannabifonol), various fatty acids and 5 α -ergosta-3-one, 5 α -stigmast-3-one (5 α -stigman-3-one), campesterol (canesteol), stigmasterol (stigmasterol, 5-stigmasterol 2-0-22-one (5 α -stigman-3-one), a canoene (camoene), a-3-one, 5-7-ketonic acid, a canoenotheine (camoene), a-5-3-5-7-ketonic acid, 5-7-ketonic acid, 5-7-5-7-one, 5-7-4-5-7-one, 5-4-5-4-one, 5-4-5-4-5-one, 5-4-5-4-one, 5-4-5-4-5-4-5-one, 5-4, 5-one, 5-4-one, 5-4-5-one, 5-4.
Disclosure of Invention
In order to fully utilize bioactive components in the hemp and search the availability of the hemp root extract in the hemp, the invention provides the hemp root extract and the preparation method thereof, and the preparation method can simply and effectively obtain the hemp root extract from industrial hemp roots.
The technical scheme of the invention is as follows:
a Cannabis sativa root extract is rich in cannabinoids, terpene alcohols and cannabinoids, and has no detectable content of tetrahydrocannabinol.
Preferably, the content of cannabinine, cannabigerol and cannabinoids in the cannabis root extract is greater than 60% by weight, and the content of tetrahydrocannabinol in the cannabis root extract is not detected.
The preparation method of the hemp root extract comprises the following steps:
(1) screening and dehydrating: cleaning and airing fresh industrial hemp roots, putting the aired industrial hemp roots into a shearing machine for shearing, and dehydrating and drying the sheared industrial hemp roots to prepare a crude industrial hemp root product.
(2) Crushing: pulverizing the dried industrial radix Cannabis crude product to obtain radix Cannabis granule.
(3) Leaching: pouring the prepared hemp root granules into an extraction tank, adding an extraction solvent, heating and extracting for three times.
(4) Centrifuging: and (4) performing centrifugal separation on the leaching liquor obtained in the step (3) for each time, and concentrating and recovering at 70-80 ℃ to obtain the primary leaching liquor.
(5) And (3) extraction: adding n-hexane into the primary extraction liquid obtained in the step (4) to obtain aqueous phase liquid; and adding n-butanol into the aqueous phase liquid, mixing n-butanol extract, and concentrating at 70-80 ℃ to obtain the n-butanol extract.
(6) And (3) purification: concentrating and pumping the n-butanol extract obtained in the step (5), adding a certain amount of methanol aqueous solution according to a proportion, heating for full dissolution, and filtering; separating the filtrate with macroporous resin column to obtain radix Cannabis purified solution.
(7) Concentration and drying: and (4) carrying out reduced pressure concentration on the hemp root purified liquid obtained in the step (6) at 70-80 ℃, drying and crushing to obtain a hemp root extract finished product.
The temperature of dehydration and drying in the step (1) is selected from 60-80 ℃, and the water content after drying is controlled to be below 15%.
In the step (2), the filter screen of the pulverizer is 30-50 meshes.
In the step (3), the extraction solvent is selected from C1-C4 alcohol aqueous solution, preferably methanol, ethanol or mixed aqueous solution thereof, and the concentration is 40-85%; the plastid ratio of the raw material to the extraction solvent is 1: 2-1: 6, preferably 1:3 or 1: 4; the temperature is controlled at 55-70 ℃.
The rotation speed of the centrifugal separation in the step (4) is selected from 2000-5000 rpm, preferably 2000-3500 rpm.
In the step (5), the adding proportion of n-hexane is 1: 0.5-0.8, and the adding proportion of n-butanol is 1: 2-3.
The model of the macroporous resin in the step (6) is XDA series, and the mobile phase is gradient methanol water solution.
In the step (8), the drying temperature is 40-50 ℃, and the filter screen of the pulverizer is 60-100 meshes.
The method has the advantages and the technical effects that:
after the complete large fried dough twist leaves are utilized, the industrial hemp roots are fully utilized, so that the bioactive components in the hemp are fully utilized, and guidance is provided for realizing comprehensive utilization of hemp resources and maximizing benefits. The method has the advantages of simple process, low cost of required equipment and large feeding amount, and is very suitable for industrial large-scale production.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
(1) Screening and dehydrating: cleaning 10kg of fresh industrial hemp root, airing, putting the aired industrial hemp root into a shearing machine for shearing, putting the sheared industrial hemp root into an oven, setting the drying temperature to be 80 ℃, and performing dehydration drying to prepare a crude industrial hemp root product, wherein the water content is controlled to be below 15%.
(2) Crushing: and putting the dried industrial crude cannabis sativa root into a pulverizer with a 40-mesh filter screen to prepare cannabis sativa root particles.
(3) Leaching: pouring the prepared hemp root particles into a leaching tank, adding 75% methanol water solution, heating and leaching for three times. Adding 3 times of methanol, heating to 60 deg.C, soaking and extracting for 2 hr to obtain leaching solution.
(4) Centrifuging: and (4) performing centrifugal separation on the leaching liquor obtained in the step (3) at the rotating speed of 3500r/min, and recovering and concentrating to obtain the primary leaching liquor.
(5) And (3) extraction: adding 0.5 time of n-hexane into the primary extract obtained in the step (4), fully shaking up and standing, and taking aqueous phase liquid; and adding 2.5 times of n-butanol into the aqueous phase liquid, fully shaking, standing, extracting for 3 times, combining the extracts, and concentrating at 70-80 ℃ to obtain an n-butanol extract.
(6) And (3) purification: concentrating and pumping the n-butanol extract obtained in the step (5) at 70-80 ℃, adding 20% methanol aqueous solution according to 5 times of the amount of the concentrate, heating to fully dissolve the concentrate, and filtering; separating the filtrate with XDA series macroporous resin column, and eluting with gradient methanol water solution to obtain radix Cannabis purified solution.
(7) Concentration and drying: and (4) concentrating and pumping the cannabis sativa root purified liquid obtained in the step (6) at 70-80 ℃, putting the obtained concentrate into an oven, setting the drying temperature at 45 ℃, performing vacuum pumping, drying, and crushing by using a 100-mesh filter screen to obtain 360g of a cannabis sativa root extract finished product.
Example 2
(1) Screening and dehydrating: cleaning 10kg of fresh industrial hemp root, airing, putting the aired industrial hemp root into a shearing machine for shearing, putting the sheared industrial hemp root into an oven, setting the drying temperature to be 80 ℃, and performing dehydration drying to prepare a crude industrial hemp root product, wherein the water content is controlled to be below 15%.
(2) Crushing: and putting the dried industrial crude cannabis sativa root into a pulverizer with a 40-mesh filter screen to prepare cannabis sativa root particles.
(3) Leaching: pouring the prepared hemp root particles into a leaching tank, adding 80% methanol water solution, and heating and leaching for three times. Adding 3 times of methanol, heating to 60 deg.C, soaking and extracting for 2 hr to obtain leaching solution.
(4) Centrifuging: and (4) performing centrifugal separation on the leaching liquor obtained in the step (3) at the rotating speed of 3500r/min, and recovering and concentrating to obtain the primary leaching liquor.
(5) And (3) extraction: adding 0.5 time of n-hexane into the primary extract obtained in the step (4), fully shaking up and standing, and taking aqueous phase liquid; and adding 2.5 times of n-butanol into the aqueous phase liquid, fully shaking, standing, extracting for 3 times, combining the extracts, and concentrating at 70-80 ℃ to obtain an n-butanol extract.
(6) And (3) purification: concentrating and pumping the n-butanol extract obtained in the step (5) at 70-80 ℃, adding 20% methanol aqueous solution according to 5 times of the amount of the concentrate, heating to fully dissolve the concentrate, and filtering; separating the filtrate with XDA series macroporous resin column, and eluting with gradient methanol water solution to obtain radix Cannabis purified solution.
(7) Concentration and drying: and (3) concentrating and draining the hemp root purified liquid obtained in the step (6) at 70-80 ℃, putting the obtained concentrate into an oven, setting the drying temperature at 45 ℃, performing vacuum drying, and crushing by using a 100-mesh filter screen to obtain 356g of hemp root extract finished product.
Example 3
(1) Screening and dehydrating: cleaning 10kg of fresh industrial hemp root, airing, putting the aired industrial hemp root into a shearing machine for shearing, putting the sheared industrial hemp root into an oven, setting the drying temperature to be 80 ℃, and performing dehydration drying to prepare a crude industrial hemp root product, wherein the water content is controlled to be below 15%.
(2) Crushing: and putting the dried industrial crude cannabis sativa root into a pulverizer with a 40-mesh filter screen to prepare cannabis sativa root particles.
(3) Leaching: pouring the prepared hemp root particles into a leaching tank, adding 60% methanol water solution, and heating and leaching for three times. Adding 3 times of methanol, heating to 60 deg.C, soaking and extracting for 2 hr to obtain leaching solution.
(4) Centrifuging: and (4) performing centrifugal separation on the leaching liquor obtained in the step (3) at the rotating speed of 3500r/min, and recovering and concentrating to obtain the primary leaching liquor.
(5) And (3) extraction: adding 0.5 time of n-hexane into the primary extract obtained in the step (4), fully shaking up and standing, and taking aqueous phase liquid; and adding 2.5 times of n-butanol into the aqueous phase liquid, fully shaking, standing, extracting for 3 times, combining the extracts, and concentrating at 70-80 ℃ to obtain an n-butanol extract.
(6) And (3) purification: concentrating and pumping the n-butanol extract obtained in the step (5) at 70-80 ℃, adding 20% methanol aqueous solution according to 5 times of the amount of the concentrate, heating to fully dissolve the concentrate, and filtering; separating the filtrate with XDA series macroporous resin column, and eluting with gradient methanol water solution to obtain radix Cannabis purified solution.
(7) Concentration and drying: and (4) concentrating and draining the hemp root purified liquid obtained in the step (6) at 70-80 ℃, putting the obtained concentrate into an oven, setting the drying temperature at 45 ℃, performing vacuum drying, and crushing by using a 100-mesh filter screen to obtain 380g of a hemp root extract finished product.
Example 4
(1) Screening and dehydrating: cleaning 10kg of fresh industrial hemp root, airing, putting the aired industrial hemp root into a shearing machine for shearing, putting the sheared industrial hemp root into an oven, setting the drying temperature to be 80 ℃, and performing dehydration drying to prepare a crude industrial hemp root product, wherein the water content is controlled to be below 15%.
(2) Crushing: and putting the dried industrial crude cannabis sativa root into a pulverizer with a 40-mesh filter screen to prepare cannabis sativa root particles.
(3) Leaching: pouring the prepared hemp root particles into a leaching tank, adding 75% methanol water solution, heating and leaching for three times. Adding methanol 4 times of the hemp root particles, heating to 60 deg.C, soaking and extracting for 2h to obtain leaching solution.
(4) Centrifuging: and (4) performing centrifugal separation on the leaching liquor obtained in the step (3) at the rotating speed of 3500r/min, and recovering and concentrating to obtain the primary leaching liquor.
(5) And (3) extraction: adding 0.5 time of n-hexane into the primary extract obtained in the step (4), fully shaking up and standing, and taking aqueous phase liquid; and adding 2.5 times of n-butanol into the aqueous phase liquid, fully shaking, standing, extracting for 3 times, combining the extracts, and concentrating at 70-80 ℃ to obtain an n-butanol extract.
(6) And (3) purification: concentrating and pumping the n-butanol extract obtained in the step (5) at 70-80 ℃, adding 20% methanol aqueous solution according to 5 times of the amount of the concentrate, heating to fully dissolve the concentrate, and filtering; separating the filtrate with XDA series macroporous resin column, and eluting with gradient methanol water solution to obtain radix Cannabis purified solution.
(7) Concentration and drying: and (3) concentrating and pumping the cannabis sativa root purified liquid obtained in the step (6) at 70-80 ℃, putting the obtained concentrate into an oven, setting the drying temperature to be 45 ℃, performing vacuum pumping, drying, and crushing by using a 100-mesh filter screen to obtain 408g of a cannabis sativa root extract finished product.
The results show that the preparation method provided by the invention has the characteristics of simple process, low cost of required equipment, large feeding amount and the like, and is very suitable for industrial large-scale production. The refined cannabis sativa root extract has better effects of removing blood stasis, stopping bleeding, promoting urination and the like, and has more remarkable medicinal value.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A Cannabis sativa root extract is rich in cannabinoids, terpene alcohols and cannabinoids, and has no detectable content of tetrahydrocannabinol.
2. The cannabis sativa root extract and the preparation method thereof as claimed in claim 1, wherein the combined percentage of cannabinoids, cannabigerol and cannabinoids in the cannabis sativa root extract is greater than 60%, and the weight percentage of tetrahydrocannabinol is not detected.
3. The cannabis sativa root extract and the preparation method thereof as claimed in claim 1 or 2, wherein: the preparation method of the hemp root extract comprises the following steps:
(1) screening and dehydrating: cleaning and airing fresh industrial hemp roots, putting the aired industrial hemp roots into a shearing machine for shearing, and dehydrating and drying the sheared industrial hemp roots to prepare a crude industrial hemp root product;
(2) crushing: pulverizing the dried industrial crude radix Cannabis product to obtain radix Cannabis granule;
(3) leaching: pouring the prepared hemp root particles into a leaching tank, adding a leaching solvent, heating and leaching for three times;
(4) centrifuging: performing centrifugal separation on the leaching liquor obtained in the step (3) for each time, and concentrating and recovering at 70-80 ℃ to obtain primary leaching liquor;
(5) and (3) extraction: adding n-hexane into the primary extraction liquid obtained in the step (4) to obtain aqueous phase liquid; adding n-butanol into the aqueous phase liquid, mixing n-butanol extract, and concentrating at 70-80 deg.C to obtain n-butanol extract;
(6) and (3) purification: concentrating and pumping the n-butanol extract obtained in the step (5), adding a certain amount of methanol aqueous solution according to a proportion, heating for full dissolution, and filtering; separating the filtrate with macroporous resin column to obtain radix Cannabis purified solution;
(7) concentration and drying: and (4) carrying out reduced pressure concentration on the hemp root purified liquid obtained in the step (6) at 70-80 ℃, drying and crushing to obtain a hemp root extract finished product.
4. The cannabis sativa root extract and the preparation method thereof as claimed in claim 3, wherein the temperature of the dehydration and drying in the step (1) is selected from 60 to 80 ℃, and the water content after drying is controlled to be below 15%.
5. The cannabis sativa root extract and the preparation method thereof as claimed in claim 3, wherein the pulverizer mesh size in step (2) is 30-50 mesh.
6. A cannabis root extract and a preparation method thereof as claimed in claim 3, wherein the extraction solvent in step (3) is selected from C1-C4 alcohol aqueous solution, preferably methanol, ethanol or a mixed aqueous solution thereof, with a concentration of 40-85%; the plastid ratio of the raw material to the extraction solvent is 1: 2-1: 6, preferably 1:3 or 1: 4; the temperature is controlled at 55-70 ℃.
7. A cannabis sativa root extract and a method for the production thereof as claimed in claim 3, wherein the centrifugation in step (4) is performed at a speed of 2000-5000 rpm, preferably 2000-3500 rpm.
8. A cannabis sativa root extract and a preparation method thereof as claimed in claim 3, characterized in that in the step (5), the adding ratio of n-hexane is 1: 0.5-0.8, and the adding ratio of n-butanol is 1: 2-3.
9. A cannabis root extract and a method for the production thereof as claimed in claim 3 wherein the macroporous resin type in step (6) is XDA series and the mobile phase is gradient methanol in water.
10. The cannabis sativa root extract and the preparation method thereof as claimed in claim 3, wherein the drying temperature in the step (8) is 40-50 ℃, and the mesh of the pulverizer is 60-100 mesh.
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| CN202010064208.5A CN111138404A (en) | 2020-01-20 | 2020-01-20 | Cannabis sativa root extract and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111773271A (en) * | 2020-07-23 | 2020-10-16 | 云南绿新生物药业有限公司 | An ointment containing radix Cannabis extract for stopping bleeding and removing blood stasis, and its preparation method |
-
2020
- 2020-01-20 CN CN202010064208.5A patent/CN111138404A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111773271A (en) * | 2020-07-23 | 2020-10-16 | 云南绿新生物药业有限公司 | An ointment containing radix Cannabis extract for stopping bleeding and removing blood stasis, and its preparation method |
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