Method for separating and purifying cannabidiol

A cannabidiol, separation and purification technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve the problems of separation and purification of cannabidiol, and achieves easy recovery and reuse, high separation efficiency, and simple system Effect

Active Publication Date: 2020-06-09
NANJING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Invention idea: The technical idea of ​​the present invention is mainly based on the principle of reverse high performance liquid chromatography, the purpose is to solve the practical problem of separation and purification of cannabidiol in cannabis plant extract or cannabis oil

Method used

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  • Method for separating and purifying cannabidiol
  • Method for separating and purifying cannabidiol
  • Method for separating and purifying cannabidiol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1. Take PS10-100 adsorption material (particle size is 10-20μm, specific surface area is 800-900m 2 / g, pore diameter 400-600A, pore volume 0.7-0.9cm 3 / g) is the stationary phase column, the column volume is (column: 7.8*300mm column volume about 14.32mL); control the sample loading flow rate to 0.3BV / min, and complete the sample loading. During the sample loading process, the column pressure is 1.5Mpa; Wherein, the sample loaded is cannabis leaf extract (chromatogram as shown in figure 1 Shown), wherein, the massfraction of cannabidiol is 0.3%, and impurity is pigment, THC, grease matter.

[0042] 2. Use the mixed solution of methanol and water as the mobile phase, methanol / water=70 / 30 isocratic elution, the flow rate is 0.3

[0043] BV / min, collect 16-23min fractions; among them, during the elution process, the column pressure is 1.3-1.5MPa, during the elution process, the chromatogram of the fractions is as follows image 3 shown.

[0044] 3. The fraction in step...

Embodiment 2

[0048] 1. Take PS10-100 adsorption material (particle size is 10-20μm, specific surface area is 800-900m 2 / g, pore diameter 400-600A, pore volume 0.7-0.9cm 3 / g) is the stationary phase column, the column volume is (column: 7.8*300mm column volume about 14.32mL); control the sample loading flow rate to 0.3BV / min, and complete the sample loading. During the sample loading process, the column pressure is 1.5Mpa; Wherein, the sample loaded is cannabis leaf extract, wherein the mass fraction of cannabidiol is 0.3%, and the impurities are pigment, THC, and oil.

[0049] 2. Use the mixed solution of methanol and water as the mobile phase, methanol / water=80 / 20 isocratic elution, the flow rate is 0.3BV / min, and the fraction is collected for 12-20min; wherein, during the elution process, the column pressure is 1.3- 1.5Mpa.

[0050] 3. The fraction in step (2) is evaporated and crystallized to obtain the cannabidiol product with a purity of 99.2% and an extraction rate of 92%.

Embodiment 3

[0052] 1. Take PS10-100 adsorption material (particle size is 20-50μm, specific surface area is 800-1000m 2 / g, pore diameter 400-800A, pore volume 0.7-1cm 3 / g) is the stationary phase column, the column volume is (column: 7.8*300mm column volume about 14.32mL); control the sample loading flow rate to 0.3BV / min, and complete the sample loading. During the sample loading process, the column pressure is 1.5Mpa; Wherein, the sample loaded is cannabis leaf extract, wherein the mass fraction of cannabidiol is 0.3%, and the impurities are pigment, THC, and oil.

[0053] 2. Use the mixed solution of methanol and water as the mobile phase, methanol / water=70 / 30 isocratic elution, the flow rate is 0.3BV / min, and the fraction is collected for 16-23min; wherein, during the elution process, the column pressure is 1.2- 1.4Mpa.

[0054] 3. The fraction in step (2) is evaporated and crystallized to obtain the cannabidiol product with a purity of 98.9% and an extraction rate of 93.2%.

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Abstract

The invention discloses a method for separating and purifying cannabidiol, which comprises the following steps: loading a cannabidiol-containing mother solution into a chromatographic separation column containing a solid adsorption material, eluting with an eluent, collecting the eluent, and carrying out evaporative crystallization on the eluent to obtain the cannabidiol. The solid adsorption material has a particle size of 5-50 [mu] m, a specific surface area of 400-1000 m<2> / g, a pore size of 80-1000 A and a pore volume of 0.6-1.2 cm<3> / g. The method has the advantages that (1) the requirement on equipment is low and is controlled within 3Mpa, and the possibility is provided for industrialization; the separation efficiency is high, and the purity of cannabidiol is higher than 99.5%; (2)one-step purification is adopted, activated carbon and macroporous adsorption resin are not needed for impurity removal, and more convenience and quickness are achieved; (3) a high polymer material isadopted, so that acid resistance and alkali resistance are better; and (4) the use amount of the eluent is less, and when the flow rate of the eluent is 0.3 BV / min, the cannabidiol can be completelyeluted by six column volumes.

Description

technical field [0001] The invention relates to a method for separating and purifying cannabidiol, which belongs to the technical field of separation and purification of bio-based raw materials. Background technique [0002] Cannabis is an annual herb belonging to the Cannabis family Cannabis genus, widely distributed (cultivated or wild) all over the world. my country has a long history of cannabis cultivation. At present, my country's cannabis cultivation is mainly concentrated in Yunnan and Northeast China, which are rich in resources. [0003] Current research shows that cannabis stem material and cannabis leaves contain more than 70 chemical substances known as cannabinoids, among which cannabidiol (CBD) and tetrahydrocannabinol (THC) have the highest content. Tetrahydrocannabinol (THC) is the hallucinogenic active ingredient that makes marijuana the leading drug. However, cannabidiol (CBD) is a non-toxic and non-addictive active ingredient, and it can also block the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/82C07C37/68C07C39/23
CPCC07C37/004C07C2601/16C07C39/23
Inventor 江伟魏士明任连兵李俊孙平
Owner NANJING UNIV
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