阅读说明：本技术 一种从工业***中分离纯化***酚的方法 (Method for separating and purifying cannabinol from industrial cannabis sativa ) 是由 曹建锋 李卫星 陈梦达 于 2020-04-20 设计创作，主要内容包括：本发明涉及一种从工业大麻中分离纯化大麻酚的方法,属于化学技术领域。在大麻酚粗品中加入乙醇溶液进行搅拌得到粗品乙醇溶液,将粗品乙醇溶液均匀加入到经活化完成的大孔树脂的柱中,用第一乙醇溶液对大孔树脂进行常压洗脱得到第一洗脱液和第一次洗脱大孔树脂,再用第二乙醇溶液对第一次洗脱大孔树脂进行常压洗脱得到第二洗脱液,在第二浓缩液中放入第三乙醇溶液得到浓缩乙醇溶液,将结晶物过滤并干燥即可得到含量大于等于95%的大麻酚。本发明的有益之处是：通过大麻酚在反相柱中的出峰时间与其它大麻素类物质的巨大差异性而进行分离,再经过结晶而得到高纯度的大麻酚,本发明操作简单、成本低廉适用于工业化生产,解决了大麻酚的分离纯化问题。(The invention relates to a method for separating and purifying cannabinol from industrial cannabis sativa, and belongs to the technical field of chemistry. Adding an ethanol solution into a crude cannabinol product, stirring to obtain a crude ethanol solution, uniformly adding the crude ethanol solution into a column of activated macroporous resin, carrying out normal-pressure elution on the macroporous resin by using a first ethanol solution to obtain a first eluent and a first-time elution macroporous resin, carrying out normal-pressure elution on the first-time elution macroporous resin by using a second ethanol solution to obtain a second eluent, adding a third ethanol solution into a second concentrated solution to obtain a concentrated ethanol solution, and filtering and drying a crystal to obtain the cannabinol with the content of more than or equal to 95%. The invention has the advantages that: the method is simple to operate, low in cost, suitable for industrial production and capable of solving the problem of separation and purification of the cannabinol.)

1. A method for separating and purifying cannabinol from industrial cannabis sativa, comprising the steps of:

A. preparing industrial cannabis flos (1), extracting with ethanol or supercritical method to obtain industrial cannabis extract (2), and subjecting the industrial cannabis extract (2) to water precipitation or molecular distillation to obtain cannabinol crude product (3) with content of 15% -35%;

B. adding the ethanol solution (4) into the crude cannabinol product (3) and stirring to obtain a crude ethanol solution (5);

C. uniformly adding the crude product ethanol solution (5) into a column of activated macroporous resin (6), wherein the sample loading amount is 1-3%;

D. carrying out normal pressure elution on the macroporous resin (6) by using 40-55% of first ethanol solution (7) to obtain first eluent (8) and first-time elution macroporous resin, wherein the using amount of the first ethanol solution (7) is 2-3 column volumes of the macroporous resin (6), collecting the first eluent (8) and concentrating to obtain first concentrated solution (9);

E. then, carrying out normal pressure elution on the macroporous resin subjected to the first elution by using a 60-65% second ethanol solution (10) to obtain a second eluent (11), wherein the using amount of the second ethanol solution (10) is 2-3 column volumes of the macroporous resin (6), collecting the second eluent (11) and concentrating to obtain a second concentrated solution (12);

F. adding a third ethanol solution (13) into the second concentrated solution (12) to obtain a concentrated ethanol solution (14), stirring the concentrated ethanol solution (14) until the solution is clear, adding purified water (15) into the concentrated ethanol solution (14) to form a purified ethanol solution (16), and crystallizing the purified ethanol solution (16) for 12 hours at-20 ℃ to obtain a crystal (17);

G. filtering and drying the crystal (17) to obtain the cannabinol (18) with the content of more than or equal to 95%.

2. The method for separating purified cannabinol from industrial cannabis as claimed in claim 1, characterized in that: the ratio of the crude cannabinol (3) to the ethanol solution (4) is 1 g: 5-10 ml.

3. The method for separating purified cannabinol from industrial cannabis as claimed in claim 1, characterized in that: the model of the macroporous resin (6) is D201.

4. The method for separating purified cannabinol from industrial cannabis as claimed in claim 1, characterized in that: the ratio of the second concentrated solution (12) to the third ethanol solution (13) is 1 g: 5-20 ml.

5. The method for separating purified cannabinol from industrial cannabis as claimed in claim 1, characterized in that: the volume of the purified water (15) is 10-25% of the volume of the concentrated ethanol solution (14).

The technical field is as follows:

the invention relates to a method for separating and purifying cannabinol from industrial cannabis sativa, and belongs to the technical field of chemistry.

Background art:

industrial hemp refers to a hemp which has been approved for legal cultivation and has a tetrahydrocannabinol content of less than 0.3%. China refers to industrial Cannabis as hemp (hemp), a 1-year-old herbaceous plant of the Cannabis genus (Cannabinaceae) of the family Cannabiaceae. The method has wide application, and the application comprises the fields of textile, paper making, food, medicine, health, daily chemicals, leather, automobile, building, decoration, packaging and the like, and is a classical production material.

The folium Cannabis contains more than 15 kinds of cannabinol derivatives, and more important ones include cannabinol, cannabidiol, tetrahydrocannabinol, cannabinolic acid, cannabidiolic acid, and tetrahydrocannabinolic acid.

Cannabinol is called CBN for short, has a molecular formula of C21H26O2, has a melting point of 77 ℃, has the activities of relieving cough, relieving spasm, relieving pain, calming, improving sleep and the like, and has high medical research value.

The existing preparation method of cannabinol is complex, the extraction efficiency is low, the extraction purity is low, and aiming at the problems, a novel method for separating and purifying cannabinol from industrial cannabis is needed in the industry so as to solve the problems in the industry.

The invention content is as follows:

the technical problem to be solved by the invention is as follows: provides a method for separating and purifying cannabinol from industrial cannabis so as to solve the problems in the industry.

In order to solve the technical problems, the invention is realized by the following technical scheme: a method for separating and purifying cannabinol from industrial cannabis sativa comprises the following steps:

A. preparing industrial cannabis sativa, extracting by an alcohol method or a supercritical method to obtain an industrial cannabis sativa extract, and performing water precipitation or molecular distillation on the industrial cannabis sativa extract to obtain a cannabinol crude product with the content of 15% -35%;

B. adding an ethanol solution into the crude cannabinol product, and stirring to obtain a crude ethanol solution;

C. uniformly adding the crude ethanol solution into a column of activated macroporous resin, wherein the sample loading amount is 1-3%;

D. carrying out normal pressure elution on the macroporous resin by using 40-55% of first ethanol solution to obtain first eluent and first-time elution macroporous resin, wherein the using amount of the first ethanol solution is 2-3 column volumes of the macroporous resin, collecting the first eluent and concentrating to obtain first concentrated solution;

E. then carrying out normal pressure elution on the macroporous resin subjected to the first elution by using 60% -65% of second ethanol solution to obtain second eluent, wherein the using amount of the second ethanol solution is 2-3 column volumes of the macroporous resin, collecting the second eluent and concentrating to obtain second concentrated solution;

F. adding a third ethanol solution into the second concentrated solution to obtain a concentrated ethanol solution, stirring the concentrated ethanol solution until the concentrated ethanol solution is clear, then adding purified water into the concentrated ethanol solution to form a purified ethanol solution, and crystallizing the purified ethanol solution at-20 ℃ for 12 hours to obtain a crystal;

G. filtering and drying the crystal to obtain the cannabinol with the content of more than or equal to 95 percent.

Preferably, the ratio of the crude cannabinol product to the ethanol solution is 1 g: 5-10 ml.

Preferably, the model of the macroporous resin is D201.

Preferably, the ratio of the second concentrated solution to the third ethanol solution is 1 g: 5-20 ml.

Preferably, the volume of the purified water is 10% to 25% of the volume of the concentrated ethanol solution.

Compared with the prior art, the invention has the advantages that: the method is simple to operate, low in cost, suitable for industrial production and capable of solving the problem of separation and purification of the cannabinol.

Description of the drawings:

the invention is further described below with reference to the accompanying drawings.

FIG. 1 is a flow chart of the present invention.

In the figure: 1 part of industrial cannabis sativa; 2, industrial hemp extract; a crude cannabinol product 3; ethanol solution 4; crude ethanol solution 5; macroporous resin 6; a first ethanol solution 7; a first eluent 8; a first concentrated solution 9; a second ethanol solution 10; a second eluent 11; a second concentrated solution 12; a third ethanol solution 13; concentrating the ethanol solution 14; purified water 15; purifying the ethanol solution 16; crystalline material 17; cannabinol 18.

The specific implementation mode is as follows:

the invention is described in detail below with reference to the following figures and embodiments:

before proceeding, the following terms are explained:

the supercritical extraction method is a method of extracting and separating effective components from liquid or solid by using fluid in a supercritical state as an extractant. CO2 is the most common Supercritical Fluid (SF) for supercritical fluid extraction because of its non-toxic, non-corrosive and moderate critical conditions (7.488 MPa, 304.15K).

The alcohol extraction method is also called ethanol extraction method, and refers to a method of separating and purifying a substance using ethanol as a solvent by utilizing the solubility of ethanol. The method is widely applied to chemical experiments, chemical purification, chemical pharmacy, preparation of traditional Chinese medicines and the like.

Molecular distillation is a distillation process operated under high vacuum where the mean free path of the vapor molecules is greater than the distance between the evaporation and condensation surfaces, thereby allowing the separation of liquid mixtures by differences in the evaporation rates of the components of the feed solution.

The water extraction and alcohol precipitation method, called water-alcohol method for short, is a method for refining water extract after adding alcohol into the water extract concentrated solution of traditional Chinese medicine to make it reach different alcohol contents, reducing the solubility of some medicinal components in the alcohol solution to reduce copy and precipitate, and making solid-liquid separation.

FIG. 1 is a flow diagram of the present invention, and the flow of FIG. 1 is illustrated by various embodiments.