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Method for preparing cannabidiol through high-speed countercurrent chromatography separation and purification

A high-speed countercurrent chromatography and cannabidiol technology, which is applied in the field of separation and purification of cannabidiol by high-speed countercurrent chromatography, can solve the problems of low CBD purity, complex composition, CBD loss and the like, and achieves optimized process parameters, simple preparation process, The effect of reducing production costs

Active Publication Date: 2019-06-28
云南芙雅生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] 1) The components of cannabinoids in industrial hemp plants are complex. There are more than 80 known types of cannabinoids, and there are many components with similar polarities. After extraction and refining by traditional methods, the purity of CBD in the final product is not high
[0008] 2) After extraction and purification, the psychotoxic component THC can still be detected, the product safety cannot be guaranteed, and the product circulation is limited, which affects industrial production and application
[0009] 3) Repeated column chromatography separation and purification in traditional technology will inevitably lead to the loss of CBD and the decrease of yield, which will limit the production capacity

Method used

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  • Method for preparing cannabidiol through high-speed countercurrent chromatography separation and purification
  • Method for preparing cannabidiol through high-speed countercurrent chromatography separation and purification
  • Method for preparing cannabidiol through high-speed countercurrent chromatography separation and purification

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (1) Grind and dry 10kg industrial hemp, add it to 70% ethanol aqueous solution according to the ratio of material to liquid ratio of 1:5 (w / v, g / mL), mix thoroughly, and extract by ultrasonic for 120min, (control the temperature below 45°C, Protect from light), vacuum filter after the end of ultrasound, repeat the extraction of the obtained filter residue twice according to the above conditions, combine the filtrate, remove ethanol by vacuum rotary evaporation at 45 °C, concentrate to a relative density of 1.2, add 5-7 times of purified water, Under the condition of 5-8°C, sink in water for 24 hours, filter, and dry the precipitate under reduced pressure to obtain crude cannabis extract.

[0034] (2) Soak the AB-8 macroporous resin in ethanol for 24 hours, put it into a chromatographic column, and wash it with ethanol until the eluate plus an equal volume of deionized water becomes a transparent solution. Then wash with deionized water until the effluent is neutral; dis...

Embodiment 2

[0037] (1) Grind and dry 10kg of industrial hemp, add it to 80% ethanol aqueous solution according to the ratio of material to liquid ratio of 1:10 (w / v, g / mL), mix thoroughly, and extract by ultrasonic for 100min, (control the temperature below 45°C, Protect from light), vacuum filter after the end of ultrasound, repeat the extraction of the obtained filter residue twice according to the above conditions, combine the filtrate, remove ethanol by vacuum rotary evaporation at 45 °C, concentrate to a relative density of 1.2, add 5-7 times of purified water, Under the condition of 5-8°C, sink in water for 24 hours, filter, and dry the precipitate under reduced pressure to obtain crude cannabis extract.

[0038](2) Soak the D101 macroporous resin in ethanol for 24 hours, put it into a chromatographic column, and wash it with ethanol until the eluate plus an equal volume of deionized water becomes a transparent solution. Then wash with deionized water until the effluent is neutral; ...

Embodiment 3

[0041] (1) Grind and dry 10kg of industrial hemp, add it to 80% ethanol aqueous solution according to the ratio of material to liquid ratio of 1:8 (w / v, g / mL), mix thoroughly, and extract by ultrasonic for 120min, (control the temperature below 45°C, Protect from light), vacuum filter after the end of ultrasound, repeat the extraction of the obtained filter residue twice according to the above conditions, combine the filtrate, remove ethanol by vacuum rotary evaporation at 45 °C, concentrate to a relative density of 1.2, add 5-7 times of purified water, Under the condition of 5-8°C, sink in water for 24 hours, filter, and dry the precipitate under reduced pressure to obtain crude cannabis extract.

[0042] (2) Soak the AB-8 macroporous resin in ethanol for 24 hours, put it into a chromatographic column, and wash it with ethanol until the eluate plus an equal volume of deionized water becomes a transparent solution. Then wash with deionized water until the effluent is neutral; ...

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Abstract

The invention relates to a method for preparing cannabidiol through high-speed countercurrent chromatography separation and purification. The method comprises the following steps: alcohol extraction water sedimentation, macroporous resin adsorption and high-speed countercurrent chromatography separation. By combining a macroporous resin chromatographic column and a high-speed countercurrent chromatographic instrument and optimizing process parameters, high-purity cannabidiol is separated from flowers and leaves of industrial hemps, meanwhile, a psychotoxic component, namely tetrahydrocannabinol is removed, an adopted solvent is environment-friendly, is not remained, is low in cost and can be circularly utilized, so that the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of cannabidiol extraction, in particular to a method for preparing cannabidiol by separation and purification of high-speed countercurrent chromatography. Background technique [0002] Cannabis (scientific name: Cannabis sativa L.), an annual herb of the Cannabis family and the genus Cannabis. Also known as hemp, hemp, hemp, mountain silk seedlings, and jute, it has important agricultural and medicinal values. At present, more than 500 substances have been isolated from cannabis plants, including at least 86 cannabinoid compounds. Mainly including tetrahydrocannabinol (tetrahydrocannabinol, THC), cannabidiol (cannabidiol, CBD), cannabinol (cannabinol, CBN) and cannabichromene (CBC), among which the first three account for 90% of cannabinol compounds. More than %, tetrahydrocannabinol can make people hallucinogenic and addictive, and can be used as drugs. It was once banned for a long time. [0003] Due to the high ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/70C07C37/72C07C37/74C07C37/82C07C39/23
CPCC07C2601/16C07C37/004B01D15/1807B01D15/265B01D15/426B01D11/0288B01D11/0242C07C39/23C07C37/72C07C37/82
Inventor 邓秋云
Owner 云南芙雅生物科技有限公司
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