Preparation method of cannabidivarin crystal

A technology of cannabidiol and cannabidiol oil, which is applied in the field of industrial preparation of cannabinoid crystals, can solve the unfavorable transportation, storage and use of cannabidiol products, which are difficult to meet safety supervision departments, and are not suitable for large-scale production Application and other issues, to achieve the effect of low cost, low consumption and high recycling rate

Active Publication Date: 2021-11-23
云南翰谷生物科技有限公司
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Problems solved by technology

However, these schemes are complicated to operate, use a large amount of solvent, and have high production costs, making them unsuitable for large-scale production applications.
[0005] In addition, the existing methods are difficult to effectively and stably control the THC content <0.3%, which is difficult to meet the requirements of the safety supervision department, and is not conducive to the transportation, storage and use of cannabidiol products

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  • Preparation method of cannabidivarin crystal
  • Preparation method of cannabidivarin crystal
  • Preparation method of cannabidivarin crystal

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preparation example Construction

[0023] Specifically, the present invention provides a method for preparing cannabidiol crystals, characterized in that the method comprises the following steps:

[0024] (1) Extracting the industrial hemp powder with a first solvent, concentrating the extract containing cannabidiol obtained after extraction, to obtain a concentrated extract;

[0025] (2) dissolving the concentrated extract with an aqueous alkaline solution for saponification;

[0026] (3) adding a second solvent to the mixture of step (2) for the first extraction, adding a third solvent to the lower aqueous phase for the second extraction, concentrating the upper extract obtained from the second extraction to obtain a refined product;

[0027] (4) dissolving the refined product with a fourth solvent, performing chromatographic purification, and concentrating the eluent containing cannabidiol to obtain cannabidiol oil;

[0028] (5) Mixing the cannabidiol oil with a crystallization solvent for crystallization t...

Embodiment 1

[0067] Weigh 200 g of industrial hemp flower leaf powder with a particle size of 40 mesh, use 6 times the amount of acetone to carry out stirring extraction at 25° C. (normal temperature) for 2 hours, and extract 3 times. The acetone extract was concentrated to obtain 6.51 g of concentrated extract extract. The analysis results showed that the CBDV content was 6.67%, and the extraction rate was 98.69%.

[0068] The obtained cannabidiol extract extract (6.51 g) was dissolved in 65 mL of 1% aqueous sodium hydroxide solution, and kept at a constant temperature of 80° C. for 3 hours. Add 65mL of n-hexane:petroleum ether=1:2 mixture for extraction, concentrate the extract to recover the organic solvent, and remove the upper organic phase containing some other cannabinoids and impurities. 65 mL of ethyl acetate was added to the water layer for extraction, and the upper layer extract was concentrated to obtain 2.5 g of subcannabinoid refined product. Analysis of crystallization sho...

Embodiment 2

[0073] Weigh 2000 g of industrial hemp flower leaf powder with a particle size of 40 mesh, use 6 times the amount of acetone to carry out stirring extraction at 25° C. (normal temperature) for 2 hours, and extract 3 times. The acetone extract was concentrated to obtain 66.32 g of concentrated extract extract. The analysis results showed that the CBDV content was 6.51%, and the extraction rate was 98.12%.

[0074] The obtained cannabidiol extract extract (66.32g) was dissolved in 663mL of 1% aqueous sodium hydroxide solution, and kept at a constant temperature of 80°C for 3h. Add 663 mL of n-hexane:petroleum ether=1:2 mixture for extraction, concentrate the extract to recover the organic solvent, and remove the upper organic phase containing some other cannabinoids and impurities. 663 mL of ethyl acetate was added to the water layer for extraction, and the upper layer extract was concentrated to obtain 24.6 g of subcannabinoid refined product. Analysis of the crystals showed ...

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Abstract

The invention relates to a preparation method of a cannabidivarin crystal. The method comprises the steps of: (1) extracting industrial cannabis sativa powder with a first solvent, and concentrating a leaching solution containing cannabidivarin obtained after extraction to obtain a concentrated extract; (2) dissolving the concentrated extract in an alkaline aqueous solution, and carrying out saponifying; (3) adding a second solvent into the mixture in the step (2) for first extraction, adding a third solvent into the lower-layer water phase for second extraction, and concentrating an upper-layer extract obtained from the second extraction to obtain a refined substance; (4) dissolving the refined substance in a fourth solvent, performing chromatographic purification, and concentrating the eluent to obtain a cannabidivarin oily substance; and (5) mixing the oily substance with a crystallization solvent, and crystallizing. According to the method, a high-purity cannabidivarin crystal can be obtained at a high total extraction rate, the energy consumption is low, the consumption of the organic solvent is low, the method is more energy-saving and environment-friendly, the method is particularly suitable for industrial application, and the crystal product does not contain addictive components.

Description

technical field [0001] The invention relates to the field of industrial preparation of cannabinoid crystals, in particular to a preparation method of high-purity cannabidiol crystals. Background technique [0002] Cannabis (Cannabis sativa L.) is an annual herb with important economic value and medicinal value, also known as hemp, hemp, hemp, mountain silk hemp, jute and industrial hemp. The content of tetrahydrocannabinol (THC), the addictive component in industrial hemp, is less than 0.3%, which can be legally carried out in large-scale cultivation and industrial development and utilization. [0003] At present, there are more than 60 cannabinoid compounds isolated from cannabis, including tetrahydrocannabinol (THC), cannabinol (CBN), cannabidiol (CBD), cannabidiol (CBDV) and their carboxyl compounds etc., wherein the first three account for more than 90% of cannabinoids. Among many cannabinoid compounds, CBDV is a non-addictive component with good anti-epileptic activit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/23C07C37/68C07C37/84C07C37/82C07C37/86C07C37/72
CPCC07C37/685C07C37/84C07C37/82C07C37/86C07C37/72C07C2601/16C07B2200/07C07C39/23
Inventor 肖丰坤陈黎飞李琳婧陈曼程涛姚国凯张秀雨
Owner 云南翰谷生物科技有限公司
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