阅读说明：本技术 一种从工业***中提取***二酚(cbd)的新方法 (Novel method for extracting Cannabidiol (CBD) from industrial cannabis sativa ) 是由 姚德坤 万莉 姚德利 于 2020-06-25 设计创作，主要内容包括：本发明属于化学领域,涉及涉及一种大麻二酚(CBD)的纯化方法,特别是涉及一种从工业大麻中提取大麻二酚(CBD)的新方法。其特点是：(1)提取率高,生产步骤简单：采用生物酶解技术和超声波技术将植物细胞壁部分分解,再利用调整机械剪切力和搅拌力,迅速破坏植物细胞组织,使组织细胞内部的化学成分与溶剂充分接触,使有效万分快速溶解转移,在极短时间内达到内外溶解平衡,既大幅度提高植物中生物碱的溶出,又避免高温提取时的杂质溶出,提高生产过程中的滤过速度和纯化效果,简化后续分离纯化步骤。本发明与传统提取方法比较,无有机溶剂残留,因而对环境无污染、成本低。(2)本发明产品纯度高达到95％以上,达到药用要求,或可制备药用其衍生物。(The invention belongs to the field of chemistry, and relates to a method for purifying Cannabidiol (CBD), in particular to a novel method for extracting Cannabidiol (CBD) from industrial cannabis sativa. The method is characterized in that: (1) the extraction rate is high, and the production steps are simple: the plant cell wall is decomposed by adopting a biological enzymolysis technology and an ultrasonic technology, and then the plant cell tissue is quickly destroyed by adjusting mechanical shearing force and stirring force, so that chemical components in the tissue cell are fully contacted with a solvent, effective ten-thousandths are quickly dissolved and transferred, the internal and external dissolution balance is achieved in a very short time, the dissolution of alkaloid in the plant is greatly improved, the dissolution of impurities during high-temperature extraction is avoided, the filtration speed and the purification effect in the production process are improved, and the subsequent separation and purification steps are simplified. Compared with the traditional extraction method, the method has no organic solvent residue, thereby having no pollution to the environment and low cost. (2) The purity of the product reaches more than 95 percent, and the product meets the requirement of medicine, or the product can be used for preparing the derivatives of the medicine.)

1. A novel method for extracting Cannabidiol (CBD) from industrial cannabis sativa, comprising the steps of:

(1) crushing: crushing hemp leaves, and sieving with 40-80 mesh sieve;

(2) extraction: adding 8-12 times of water into the crushed hemp flowers and leaves, adding composite cellulase, wherein the mass percentage of the composite cellulase to the hemp flowers and leaves is 0.1-0.5%, adjusting the pH value to 5-8, performing enzymolysis for 12-36 hours at the temperature of 20-60 ℃, performing ultrasonic countercurrent extraction for 1.5-2 hours at the frequency of 40-50KHz and the temperature of 40-60 ℃, and extracting twice;

(3) and (3) filtering: filtering the completely extracted turbid solution, and combining the filtrates for 2 times to obtain filtrate;

(4) primary refining of polyamide:

mixing the obtained solution with dry polyamide powder, washing with water to remove water-soluble impurities, sequentially eluting with 20-80% ethanol, and collecting eluate to obtain extractive solution;

(5) purifying by combining polyamide and macroporous resin:

steaming the extractive solution in water bath to near dryness, adding small amount of ethanol and 1/4-1/8, mixing with polyamide powder, volatilizing solvent in water bath, placing polyamide in a percolating tube with cotton at the bottom, eluting with water to colorless, taking out, and spreading on macroporous resin 3-5 times of the medicinal materials. Filling the column by a wet method, wherein the height-diameter ratio of the resin column is 5: 1-8: 1, and the flow rate is 3-5 BV/h;

(6) ethanol elution:

eluting with ethanol solution at a flow rate of 1-3BV/h at normal temperature and pressure, wherein the elution volume is 5-7 BV;

(7) and (3) recrystallization:

adding methanol into purified Cannabidiol (CBD) according to a certain amount, heating for dissolving, performing suction filtration while the solution is hot, standing overnight, precipitating crystals, filtering, and separating the crystals; heating the residue for dissolving, recrystallizing, and repeating the above steps twice to obtain refined Cannabidiol (CBD) with purity of above 95%.

The method of the invention optimizes the technical proposal,

the composite cellulase in the step (2) comprises the following components in percentage by mass: 40-50% of cellulase, 30-40% of pectinase and 20-30% of hemicellulase.

The model number of the macroporous resin in the step (5) is one or more of AB-8, NKA-II, HPD-100 and LX-100 type resins.

2. A new process for the extraction of Cannabidiol (CBD) from industrial cannabis, as claimed in claim 1, characterized by: in the step (2), the composite cellulase comprises the following components in percentage by mass: 40-50% of cellulase, 30-40% of pectinase and 20-30% of hemicellulase.

3. A new process for the extraction of Cannabidiol (CBD) from industrial cannabis, as claimed in claim 1, characterized by: in the step (5), the model of the macroporous resin is one or more of AB-8, NKA-II, HPD-100 and LX-100 type resins.

The technical field is as follows:

the invention belongs to the field of chemistry, and relates to a method for purifying Cannabidiol (CBD), in particular to a novel method for extracting Cannabidiol (CBD) from industrial cannabis sativa.

Background art:

cannabidiol (CBD) is the major chemical component of the medicinal plant cannabis sativa, extracted from the female cannabis plant, one of the most common compounds in the trichome of female cannabis plants, CBD is an inactive component, a non-addictive component of cannabis sativa, that is CBD does not let hi, but THC. Also because of the fantasy effects of cannabis caused by THC, which has taken up the historical stage, CBD was ignored for decades until 2013, the american limited television news web first presented charlotte's story. Cannabidiol returns to the sight of people. Cannabidiol (CBD) has pharmacological effects of resisting spasm, resisting anxiety, and resisting inflammation. CBD not only can be used for treating various difficult and complicated diseases, but also can effectively eliminate the hallucinogenic effect of Tetrahydrocannabinol (THC) on human bodies, and is called as an anti-drug compound (anti-marijuana compound).

The application of CBD in the medical field is mainly based on its protective effect on the nervous system. The CBD analogue has stable heredity and good pharmacokinetic property, and scientists synthesize a series of CBD analogues through continuously modifying the CBD structure, and the analogues have different pharmacological activities and can act on different diseases.

The invention content is as follows:

the invention aims to overcome the defects of relatively low extraction rate, low extraction purity and the like of the conventional technology and provide a novel method for extracting Cannabidiol (CBD) from industrial cannabis sativa. The method comprises the following steps:

(1) crushing: crushing hemp leaves, and sieving with 40-80 mesh sieve;

(2) extraction: adding 8-12 times of water into the crushed hemp flowers and leaves, adding composite cellulase, wherein the mass percentage of the composite cellulase to the hemp flowers and leaves is 0.1-0.5%, adjusting the pH value to 5-8, performing enzymolysis for 12-36 hours at the temperature of 20-60 ℃, performing ultrasonic countercurrent extraction for 1.5-2 hours at the frequency of 40-50KHz and the temperature of 40-60 ℃, and extracting twice;

(3) and (3) filtering: filtering the completely extracted turbid solution, and combining the filtrates for 2 times to obtain filtrate;

(4) primarily refining polyamide;

mixing the obtained solution with dry polyamide powder, washing with water to remove water-soluble impurities, sequentially eluting with 20-80% ethanol, and collecting eluate to obtain extractive solution;

(5) purifying by combining polyamide and macroporous resin:

steaming the extractive solution in water bath to near dryness, adding small amount of ethanol and 1/4-1/8, mixing with polyamide powder, volatilizing solvent in water bath, placing polyamide in a percolating tube with cotton at the bottom, eluting with water to colorless, taking out, and spreading on macroporous resin 3-5 times of the medicinal materials. Filling the column by a wet method, wherein the height-diameter ratio of the resin column is 5: 1-8: 1, and the flow rate is 3-5 BV/h;

(6) ethanol elution:

eluting with ethanol solution at a flow rate of 1-3BV/h at normal temperature and pressure, wherein the elution volume is 5-7 BV;

(7) and (3) recrystallization:

adding methanol into purified Cannabidiol (CBD) according to a certain amount, heating for dissolving, performing suction filtration while the solution is hot, standing overnight, precipitating crystals, filtering, and separating the crystals; heating the residue for dissolving, recrystallizing, and repeating the above steps twice to obtain refined Cannabidiol (CBD) with purity of above 95%.

The method of the invention optimizes the technical proposal,

the composite cellulase in the step (2) comprises the following components in percentage by mass: 40-50% of cellulase, 30-40% of pectinase and 20-30% of hemicellulase.

The model number of the macroporous resin in the step (4) is one or more of AB-8, NKA-II, HPD-100 and LX-100 type resins.

The method of the invention has the following technical effects:

(1) the extraction rate is high, and the production steps are simple: the plant cell wall is decomposed by adopting a biological enzymolysis technology and an ultrasonic technology, and then the plant cell tissue is quickly destroyed by adjusting mechanical shearing force and stirring force, so that chemical components in the tissue cell are fully contacted with a solvent, effective ten-thousandths are quickly dissolved and transferred, the internal and external dissolution balance is achieved in a very short time, the dissolution of alkaloid in the plant is greatly improved, the dissolution of impurities during high-temperature extraction is avoided, the filtration speed and the purification effect in the production process are improved, and the subsequent separation and purification steps are simplified. Compared with the traditional extraction method, the method has no organic solvent residue, thereby having no pollution to the environment and low cost.

(2) The purity of the product reaches more than 95 percent, and the product meets the requirement of medicine, or the product can be used for preparing the derivatives of the medicine.

Detailed Description

The examples which follow are given by way of illustration only for the further detailed description of the process of the invention and are not intended to limit the invention in any way.