阅读说明：本技术 一种从工业大麻叶子中提取大麻二酚的方法 (Method for extracting cannabidiol from industrial cannabis sativa leaves ) 是由 古景腾 谢佳勋 所跃刚 于 2021-07-29 设计创作，主要内容包括：本发明涉及大麻二酚提取技术领域,具体是一种从工业大麻叶子中提取大麻二酚的方法,为了提升浸膏得率以及大麻二酚的含量,具体包括八个步骤。本发明工艺考究,方法实用,利用预热使的大麻二酚中的羧酸衍生物完全发生脱酸反应,去除羧基,进而大幅度提升浸膏得率和大麻二酚的含量,利用蛋白酶进行水解处理,使得大麻叶植物细胞壁破碎,便于将活性物质或色素萃取处理,增加了萃取效率。(The invention relates to the technical field of cannabidiol extraction, in particular to a method for extracting cannabidiol from industrial cannabis sativa leaves, which specifically comprises eight steps in order to improve the extract yield and the content of cannabidiol. The method is exquisite in process and practical, the carboxylic acid derivatives in the cannabidiol are completely subjected to deacidification reaction by utilizing preheating, carboxyl is removed, the extract yield and the cannabidiol content are greatly improved, the cell walls of cannabis leaf plants are crushed by utilizing protease for hydrolysis treatment, active substances or pigments are conveniently extracted, and the extraction efficiency is improved.)

1. A method for extracting cannabidiol from industrial cannabis sativa leaves is characterized by comprising the following steps;

step 1: cleaning industrial hemp leaves, naturally airing, putting into a tray paved with aluminum foil paper, putting into a 110 ℃ oven for heating pretreatment for 2 hours, and cooling for later use;

step 2: placing the preheated industrial hemp leaves into a shaking table, adding a proper amount of enzyme solution, and hydrolyzing for 45min to obtain hydrolysate;

and step 3: placing the hydrolysate into a stirrer, adding 360ml of extraction solvent, stirring and mixing, and removing the extraction solvent by rotary evaporation to obtain an oily substance;

adding anhydrous methanol into the oily substance, winterizing in a refrigeration house at-37 deg.C for 1 hr, and centrifuging at-5 deg.C to obtain supernatant;

heating activated carbon corresponding to 10% of the oily matter in the supernatant for decoloring, and filtering to obtain a filtrate;

performing rotary evaporation on the obtained filtrate to obtain an extract;

and 4, step 4: precipitating the extract with water to remove impurities to obtain a water precipitation solution;

and 5: centrifuging the water precipitation solution to obtain a precipitate, and adding 10-100 v% ethanol into the precipitate to dissolve the precipitate to obtain an alcohol solution;

step 6: performing column chromatography on the obtained alcohol solution, eluting to obtain an eluent, and adding ethanol for supersaturation and dissolution to obtain a crystal;

and 7: adding purified water or ethanol into the crystal, and washing to obtain a semi-finished product;

and 8: and (4) uniformly mixing the semi-finished product with purified water, and drying to obtain the finished product of cannabidiol.

2. The method of claim 1, wherein the ratio of the industrial hemp leaf to the enzyme solution in step 2 is 1: 10, wherein the enzyme solution adopts protease.

3. The method for extracting cannabidiol from industrial cannabis sativa leaves as claimed in claim 1, wherein the extraction solvent in step 3 is n-hexane.

4. The method for extracting cannabidiol from industrial cannabis sativa leaves as claimed in claim 1, wherein the rotation speed of the stirrer in step 3 is 1000r/min, and the stirring time is 1 h.

5. The method for extracting cannabidiol from industrial cannabis sativa leaves as claimed in claim 1, wherein step 1 is further configured to: cleaning industrial hemp leaves, naturally airing, putting into a tray paved with aluminum foil paper, putting into a 100 ℃ oven for heating pretreatment for 2 hours, and cooling for later use.

6. The method for extracting cannabidiol from industrial cannabis sativa leaves as claimed in claim 1, wherein step 1 is further configured to: cleaning industrial hemp leaves, naturally airing, putting into a tray paved with aluminum foil paper, putting into a 120 ℃ oven for heating pretreatment for 2 hours, and cooling for later use.

Technical Field

The invention relates to the technical field of cannabidiol extraction, in particular to a method for extracting cannabidiol from industrial cannabis sativa leaves.

Background

Cannabidiol is a white crystalline powder extracted from industrial hemp, and is dissolved in organic solvents such as ethanol, methanol, ether, benzene, chloroform, etc.

Through search, the Chinese patent ' a method for extracting cannabidiol from industrial cannabis sativa leaves ' (publication number: CN110041171A) ', provides a method for extracting cannabidiol from industrial cannabis sativa leaves, and belongs to the technical field of extraction of chemical drug intermediates. In order to solve the problem of large-scale waste of the existing industrial hemp leaves, the invention provides a method for extracting cannabidiol from industrial hemp leaves, which adopts the following technical scheme: (1) drying industrial hemp leaves, carrying out superfine grinding and sieving to obtain industrial hemp powder; (2) adjusting the water content of industrial hemp leaf powder to 8% -10%, and then performing microwave-assisted solvent extraction to obtain a crude extraction solution; (3) separating the crude extract with three phases to obtain solvent phase; (4) carrying out reduced pressure distillation on the solvent phase to obtain grease containing cannabidiol; (5) cannabidiol is obtained by molecular distillation, but cannabidiol exists in the form of carboxylic acid in the extraction process of the patent, so that the extract yield and the cannabidiol content are low. Accordingly, one skilled in the art provides a method for extracting cannabidiol from industrial cannabis sativa leaves, which solves the problems set forth in the background art as described above.

Disclosure of Invention

The invention aims to provide a method for extracting cannabidiol from industrial cannabis sativa leaves, so as to solve the problems in the background technology.

In order to achieve the purpose, the invention provides the following technical scheme: a method for extracting cannabidiol from industrial cannabis sativa L comprises the following steps;

step 1: cleaning industrial hemp leaves, naturally airing, putting into a tray paved with aluminum foil paper, putting into a 110 ℃ oven for heating pretreatment for 2 hours, and cooling for later use;

step 2: placing the preheated industrial hemp leaves into a shaking table, adding a proper amount of enzyme solution, and hydrolyzing for 45min to obtain hydrolysate;

and step 3: placing the hydrolysate into a stirrer, adding 360ml of extraction solvent, stirring and mixing, and removing the extraction solvent by rotary evaporation to obtain an oily substance;

adding anhydrous methanol into the oily substance, winterizing in a refrigeration house at-37 deg.C for 1 hr, and centrifuging at-5 deg.C to obtain supernatant;

heating activated carbon corresponding to 10% of the oily matter in the supernatant for decoloring, and filtering to obtain a filtrate;

performing rotary evaporation on the obtained filtrate to obtain an extract;

and 4, step 4: precipitating the extract with water to remove impurities to obtain a water precipitation solution;

and 5: centrifuging the water precipitation solution to obtain a precipitate, and adding 10-100 v% ethanol into the precipitate to dissolve the precipitate to obtain an alcohol solution;

step 6: performing column chromatography on the obtained alcohol solution, eluting to obtain an eluent, and adding ethanol for supersaturation and dissolution to obtain a crystal;

and 7: adding purified water or ethanol into the crystal, and washing to obtain a semi-finished product;

and 8: and (4) uniformly mixing the semi-finished product with purified water, and drying to obtain the finished product of cannabidiol.

As a further aspect of the invention: in the step 2, the ratio of the industrial hemp leaves to the enzyme solution is 1: 10, wherein the enzyme solution adopts protease.

As a further aspect of the invention: and (3) adopting n-hexane as an extraction solvent.

As a further aspect of the invention: in the step 3, the rotating speed of the stirrer is 1000r/min, and the stirring time is 1 h.

As a further aspect of the invention: step 1 may also be arranged as follows: cleaning industrial hemp leaves, naturally airing, putting into a tray paved with aluminum foil paper, putting into a 100 ℃ oven for heating pretreatment for 2 hours, and cooling for later use.

As a further aspect of the invention: step 1 may also be arranged as follows: cleaning industrial hemp leaves, naturally airing, putting into a tray paved with aluminum foil paper, putting into a 120 ℃ oven for heating pretreatment for 2 hours, and cooling for later use.

Compared with the prior art, the invention has the beneficial effects that: the method is exquisite in process and practical, the carboxylic acid derivatives in the cannabidiol are completely subjected to deacidification reaction by utilizing preheating, carboxyl is removed, the extract yield and the cannabidiol content are greatly improved, the cell walls of cannabis leaf plants are crushed by utilizing protease for hydrolysis treatment, active substances or pigments are conveniently extracted, and the extraction efficiency is improved.

Drawings

FIG. 1 is a data plot of a test example of cannabidiol extracted from industrial cannabis sativa leaves.

Detailed Description

Example 1

In the embodiment of the invention, the method for extracting cannabidiol from industrial cannabis sativa leaves is characterized by comprising the following steps;

step 1: cleaning industrial hemp leaves, naturally airing, putting into a tray paved with aluminum foil paper, putting into a 110 ℃ oven for heating pretreatment for 2 hours, and cooling for later use;

step 2: placing the preheated industrial hemp leaves into a shaking table, adding a proper amount of enzyme solution, and hydrolyzing for 45min to obtain hydrolysate;

and step 3: placing the hydrolysate into a stirrer, adding 360ml of extraction solvent, stirring and mixing, and removing the extraction solvent by rotary evaporation to obtain an oily substance;

adding anhydrous methanol into the oily substance, winterizing in a refrigeration house at-37 deg.C for 1 hr, and centrifuging at-5 deg.C to obtain supernatant;

heating activated carbon corresponding to 10% of the oily matter in the supernatant for decoloring, and filtering to obtain a filtrate;

performing rotary evaporation on the obtained filtrate to obtain an extract;

and 4, step 4: precipitating the extract with water to remove impurities to obtain a water precipitation solution;

and 5: centrifuging the water precipitation solution to obtain a precipitate, and adding 10-100 v% ethanol into the precipitate to dissolve the precipitate to obtain an alcohol solution;

step 6: performing column chromatography on the obtained alcohol solution, eluting to obtain an eluent, and adding ethanol for supersaturation and dissolution to obtain a crystal;

and 7: adding purified water or ethanol into the crystal, and washing to obtain a semi-finished product;

and 8: and (4) uniformly mixing the semi-finished product with purified water, and drying to obtain the finished product of cannabidiol.

Further, in the step 2, the ratio of the industrial hemp leaves to the enzyme solution is 1: 10, wherein the enzyme solution adopts protease.

Further, n-hexane is used as an extraction solvent in the step 3.

Further, the rotating speed of the stirrer in the step 3 is 1000r/min, and the stirring time is 1 h.

Example 2

Carried out exactly as in example 1, in contrast to example 1: step 1: cleaning industrial hemp leaves, naturally airing, putting into a tray paved with aluminum foil paper, putting into a 100 ℃ oven for heating pretreatment for 2 hours, and cooling for later use.

Example 3

The process is carried out exactly as in example 1, and differs from examples 1 and 2 in that: step 1: cleaning industrial hemp leaves, naturally airing, putting into a tray paved with aluminum foil paper, putting into a 120 ℃ oven for heating pretreatment for 2 hours, and cooling for later use.

Test example:

and (3) testing groups: examples 1, 2, 3 and the reference example (extractum prepared by a conventional method (without preheating treatment));

the test contents are as follows: the content of cannabidiol in the extracts prepared in the reference examples in example 1, example 2 and example 3 was respectively tested;

and (3) testing results: refer to the description and the attached figure 1.

From the above data it can be derived: the carboxylic acid derivative in industrial hemp leaves is decarboxylated through preheating treatment, so that the extract yield and the content of cannabidiol are increased, and then, according to the attached figure 1 of the specification, the data of the embodiment 1, the embodiment 2 and the embodiment 3 are better than those of the reference example, meanwhile, the extract yield and the content of cannabidiol of the embodiment 1 are stabilized at the highest values, and the embodiment 3 and the embodiment 2 are in the lower peak section of the embodiment 1 along with the change of the preheating temperature.

In summary, the following steps: the method is exquisite in process and practical, the carboxylic acid derivatives in the cannabidiol are completely subjected to deacidification reaction by utilizing preheating, carboxyl is removed, the extract yield and the cannabidiol content are greatly improved, the cell walls of cannabis leaf plants are crushed by utilizing protease for hydrolysis treatment, active substances or pigments are conveniently extracted, and the extraction efficiency is improved.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention are equivalent to or changed within the technical scope of the present invention.