Method for preparing cannabidiol

A cannabidiol and chromatography technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of time-consuming and labor-intensive processing, large consumption of organic solvents, unsatisfactory comprehensive yield, etc. The effect of large sample volume and short separation cycle

Active Publication Date: 2020-11-24
YUNNAN HEMPMON PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, most of the existing CBD purification processes need to consume a large amount of organic solvents, and the follow-up treatment is time-consuming and labor-intensive, and the comprehensive yield is not ideal

Method used

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  • Method for preparing cannabidiol
  • Method for preparing cannabidiol
  • Method for preparing cannabidiol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] In this embodiment, cannabis flowers and leaves are prepared by supercritical fluid chromatography to prepare cannabidiol, and the operation method is as follows:

[0050] Weigh 50g of dried cannabis flower leaves, extract twice with 500mL n-hexane at 25°C, combine the extracts, concentrate to an anhydrous thick paste (weight 4.17g, converted cannabidiol is 0.92g), and use n-heptane Dissolve at 30°C, pass through a short column of silica gel packed with 1.1 g of silica gel, rinse with 5 mL of n-heptane, combine, inject into a supercritical fluid chromatography injection valve, and perform continuous gradient separation. Equipment parameters are: equipment model: CS-SFC50, chromatographic column: high-purity silica gel (Hedera Si) 9μm 15×250mm, column temperature: 30°C, back pressure: 12MPA, detection wavelength: 220nm. The mobile phase elution procedure is:

[0051] time (min) Flow rate (mL / min) A: CO 2

B: Dichloromethane C: Methanol 0 2 95％...

Embodiment 2

[0062] In this embodiment, cannabis flowers and leaves are prepared by supercritical fluid chromatography. The difference between the operation method and Example 1 is only the mobile phase elution procedure, which is:

[0063] time (min) Flow rate (mL / min) A: CO 2

B: Dichloromethane 0 2 95％ 5％ 5 2 65％ 30％ 52 2 45％ 55％ 60 2 95％ 5％

[0064] Collect the target peak product at 18.5-21.4min, and recover the solvent; collect 0-4min, recover the solvent and then destroy it; collect the other peaks and recover the solvent to make an oily thick paste for later use.

[0065] The target peak product is concentrated under reduced pressure and vacuum dried, and crushed to a size below 100 mesh to obtain the high-purity cannabidiol product. Use high performance liquid chromatography to carry out the detection of its purity, and specific content is consistent with embodiment 1, and its liquid chromatogram is as follows Figure 4 As shown,...

Embodiment 3

[0068] In this example, a large amount of cannabis flowers and leaves are prepared by supercritical fluid chromatography to prepare cannabidiol, and the operation method is as follows:

[0069] Weigh 5Kg of dried cannabis flower leaves, extract twice with 50L 95% ethanol at 25°C, combine the extracts, concentrate to an anhydrous thick paste (weight 514g, converted cannabidiol is 93.22g), and use n-heptane : Ethyl acetate (V / V=8:1) was dissolved at 30°C, passed through a short column of silica gel packed with 260g of silica gel, rinsed with 100mL of n-heptane, merged, injected into the supercritical fluid chromatography injection valve, and carried out continuous Isocratic elution. The equipment parameters are: equipment model: CS-SFC100, chromatographic column: phenylene ether group bonded silica gel 25 μm 80×400 mm, column temperature: 40°C, back pressure: 15MPA, detection wavelength: 220nm. The mobile phase elution procedure is:

[0070] time (min) Flow rate (m...

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Abstract

The invention relates to a method for preparing cannabidiol. The method comprises the following steps: separating a sample solution containing cannabidiol by adopting supercritical fluid chromatography to obtain high-purity cannabidiol, wherein a mobile phase in the supercritical fluid chromatography is supercritical carbon dioxide added with a modifier. According to the method, the high-purity cannabidiol can be efficiently and simply separated, the content of a main impurity, namely, cannabidiol, can be remarkably reduced, the purity of the cannabidiol is up to 97.59% to 99.89%, the sample loading amount is large, the separation period is short, the comprehensive yield is remarkably increased, and the organic solvent residue is low; and meanwhile, the method is suitable for separation and purification of various samples containing cannabidiol, is also suitable for industrial large-scale production and has a very wide application range.

Description

technical field [0001] The invention belongs to the technical field of industrial extraction, in particular to a method for preparing cannabidiol, in particular to a method for preparing high-purity cannabidiol by supercritical fluid chromatography. Background technique [0002] Cannabinoids are a class of active substances contained in cannabis plants, mainly including tetrahydrocannabinol (THC), tetrahydrocannabinoid (THCV), cannabidiol (CBD), cannabigerol (CBG), and cannabidiol (CBG). Cannabis phenol (CBDV) and other components, these five account for more than 90% of cannabinoids. Cannabidiol (CBD) is one of the most important non-addictive components in the plant. It has pharmacological activities such as anti-spasmodic, anti-rheumatic arthritis, and anti-anxiety, and can hinder the effects of tetrahydrocannabinol (THC) on the human nervous system. The adverse effects have become a hot spot in drug development. However, the properties of these cannabinols are very sim...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/68C07C37/72C07C37/82C07C39/23
CPCC07C37/004C07C37/685C07C37/72C07C37/82C07C2601/16C07C39/23Y02P20/54
Inventor 于朝晖高伟博柳旭常坦然赵丽梅
Owner YUNNAN HEMPMON PHARMA CO LTD
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