CN111978157A - Method for extracting and purifying cannabidiol from industrial cannabis sativa - Google Patents
Method for extracting and purifying cannabidiol from industrial cannabis sativa Download PDFInfo
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- QHMBSVQNZZTUGM-ZWKOTPCHSA-N cannabidiol Chemical compound OC1=CC(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)=C)CCC(C)=C1 QHMBSVQNZZTUGM-ZWKOTPCHSA-N 0.000 title claims abstract description 138
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/685—Processes comprising at least two steps in series
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/74—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/82—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by solid-liquid treatment; by chemisorption
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/84—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by crystallisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
Abstract
The invention discloses a method for extracting and purifying cannabidiol from industrial cannabis sativa, which comprises the following steps of crushing raw materials; drying; ③ leaching: adding an extracting agent into the dried flower leaf powder, wherein the content of an extract crude extract obtained by extraction is 10-15%; fourthly, dewaxing: dissolving the crude extract with 85-100% ethanol by mass, and freezing and filtering to obtain 25-40% of CBD enrichment; molecular distillation: carrying out molecular distillation on the CBD enriched material, wherein the content of the collected CBD oil is 35-70%; sixthly, column chromatography separation: performing silica gel column chromatography separation, decompression and concentration on the CBD oil to obtain crude CBD crystals with the content of more than 95%; seventhly, recovering the eluent; (iii) recrystallization of the [ CBD ]: the content of CBD finished products obtained by dissolving and filtering the CBD crude crystals by using a crystallization solvent is more than 99.5 percent. The method has the advantages of advanced, stable and feasible process, low investment, high benefit, high purity, high extraction rate and low pollution.
Description
Technical Field
The invention belongs to the technical field of extraction and separation of natural phytochemicals, and particularly relates to a method for extracting purified cannabidiol from industrial cannabis sativa.
Background
Industrial hemp refers to a hemp that has been legally planted and contains less than 0.3% Tetrahydrocannabinol (THC). At present, industrial hemp is planted in Yunnan province and Heilongjiang province in large scale, and the planting scale is enlarged year by year. The industrial HEMP (HEMP) has extremely high medicinal value and wide application, and relates to the fields of textile, paper making, food, medicine, sanitation, daily chemicals, leather, automobiles, buildings, decoration, packaging and the like. Is a classic production material and is also one of the traditional raw materials of medicinal materials and health care products in China. At present, more than 500 secondary metabolites have been isolated from cannabis plants, of which there are at least 86 cannabinol compounds. The cannabinol compounds are a specific secondary metabolite in cannabis plants, are main active ingredients in the cannabis plants, and researches on the cannabinol compounds are hot spots of cannabis researches. The main cannabinol compounds in the hemp plant include Tetrahydrocannabinol (THC), Cannabinol (CBN), Cannabidiol (CBD), Cannabigerol (CBG), cannabichromene (CBC), etc., wherein the former three compounds account for more than 90% of the cannabinol compounds.
Cannabidiol, CBD for short, is the main chemical component in medicinal plant cannabis sativa, and modern medical research shows that CBD has significant curative effect in aspects of anti-epilepsy, anti-stress, anti-inflammation and the like, and CBD is approved by the United states food and drug administration, is used for epilepsy treatment, and can also be used as a dietary supplement for improving mood and resisting anxiety. The current CBD research also finds that the compound has certain efficacy in the aspects of rheumatoid arthritis, gastroenteritis, anorexia, brain tumor and the like; in addition, the CBD oil has a strong market potential, and the CBD oil is multiplied by two years since nobody in the past few years is concerned, and products around each large CBD are continuously developed, so that the CBD becomes the most important raw material of food, medicine and cosmetics by opening industrial hemp in Europe and America. In the prior art, the processes of critical carbon dioxide extraction, chromatography and crystallization are mostly adopted in the method for extracting the CBD from the industrial hemp, but because the separation process is extensive and the cannabinoids in the industrial hemp are complex and have similar properties, particularly Tetrahydrocannabinol (THC) and Cannabidiol (CBD) are isomers, the problems of low extraction purity and extraction rate of the CBD are easily caused, most of the tetrahydrocannabinol still remains in the purified CBD, the safety of the product is not guaranteed, and the industrial production of the CBD is severely restricted. Therefore, it is objectively needed to develop a method for extracting and purifying cannabidiol from industrial cannabis sativa, which has scientific and reasonable process design and simple operation, can effectively control the extraction cost and greatly improve the product extraction purity and extraction rate.
Disclosure of Invention
In order to solve the problems in the background art, the invention aims to provide the method for extracting the purified cannabidiol from the industrial cannabis sativa, which has scientific and reasonable process design and simple operation, can effectively control the extraction cost and greatly improve the product extraction purity and the extraction rate.
The invention relates to a method for extracting and purifying cannabidiol from industrial cannabis sativa, which comprises the following steps:
crushing raw materials: crushing industrial hemp flowers and leaves into flower and leaf powder with the granularity of 10-60 meshes;
drying: baking the flower and leaf powder obtained by crushing in the step I until the weight loss is more than 7%;
③ leaching: adding an extracting agent into the flower and leaf powder baked in the second step, wherein the solid-liquid ratio of the extracting agent to the flower and leaf powder is 1: 6-10, keeping the liquid level of the extracting agent at a certain height at normal temperature, soaking for 8-24 hours, adding the extracting agent again at a certain flow rate until the outflow speed of the extracting solution is the same as the adding speed of the extracting agent, recovering the extracting agent until the extracting agent is detected to be free of CBD, and evaporating and concentrating the outflow extracting solution to obtain an extract crude extract, wherein the content of the extract crude extract is 10-15%;
fourthly, dewaxing: dissolving the extract crude extract obtained in the step (III) by using ethanol with the mass concentration of 85-100%, dissolving the ethanol and the extract crude extract according to the mass-volume ratio of w/v =1: 2-10, then freezing the extract crude extract at the temperature of-40 to-5 ℃ for 4-12 h, then filtering at the temperature, wherein the filtering precision is 400-600 meshes, then collecting filtrate, recovering ethanol, wherein the collected filtrate is CBD enrichment, and the content of the CBD enrichment is 25-40%;
molecular distillation: performing molecular distillation on the CBD enrichment obtained in the step (IV), wherein the collected molecular distillation light phase is CBD oil, and the content of the CBD oil is 35-70%;
sixthly, column chromatography separation: loading the CBD oil prepared in the fifth step into a silica gel wet method with the column diameter ratio of 1: 6-10 for silica gel column chromatography separation, wherein the silica gel fineness of the silica gel chromatography column is 200-600 meshes, the loading amount of the CBD oil is 0.3-4% of the weight of the silica gel, eluting by using an eluent, then recovering the eluent, collecting a chromatographic solution, carrying out continuous sampling detection on the collected chromatographic solution by using HPLC (high performance liquid chromatography), collecting a CBD component, and concentrating the CBD component under a reduced pressure condition to obtain a CBD crude crystal, wherein the content of the CBD crude crystal is more than 95%;
recovering the eluent: evaporating and concentrating the eluent recovered in the step (c), then measuring the concentrated eluent by using a standard alcohol meter, and then blending until the reading of the fresh eluent alcohol meter is obtained, wherein the eluent can be reused;
(iii) recrystallization of the [ CBD ]: dissolving the crude CBD crystal obtained in the step (c) by using a crystallization solvent, filtering after dissolving, concentrating under reduced pressure to obtain a saturated solution, placing the saturated solution at a low temperature to separate out crystals, filtering, and drying under reduced pressure at a low temperature to obtain a finished CBD product, wherein the content of the finished CBD product is more than 99.5%.
Further, in the second step, the baking temperature of the flower and leaf powder is 100-150 ℃.
Further, in the third step, the lixiviant is one or more of ethanol, n-hexane, petroleum ether and ethyl acetate with the mass concentration of 80-100%, and during lixiviation, the temperature at normal temperature is 20-28 ℃, the liquid level height of the lixiviant is 2-5 cm, and the flow rate of the lixiviant is 180-270 mL/min.
Further, in the fifth step, the process conditions of the molecular distillation are as follows: feeding at the temperature of 60-120 ℃, distilling at the temperature of 120-220 ℃, keeping the vacuum degree at 1-20 Pa, and keeping the condensation temperature at 50-130 ℃;
further, in the step (sixthly), the eluent is a solvent mixed by two or more of ethyl acetate, chloroform, dichloromethane, normal hexane and petroleum ether according to the volume ratio. Preferably, the eluent is ethyl acetate and n-hexane, and the volume ratio of the ethyl acetate to the n-hexane is 98-95: 2-5; the eluent is dichloromethane and n-hexane, and the volume ratio of the dichloromethane to the n-hexane is 1: 1.5-5; the eluent is chloroform and petroleum ether, and the volume ratio of the chloroform to the petroleum ether is 1: 8-15).
Further, in step viii, the crystallization solvent is n-heptane; after dissolving the CBD crude crystals, concentrating under reduced pressure until the volume of the saturated solution is one third of that of the dissolved solution, and stopping concentrating; the temperature for crystallization is 0 to minus 30 ℃ under the condition of low temperature, and the crystallization time is 4 to 24 hours.
Compared with the prior art, the method has the advantages that the crushed flower and leaf powder is subjected to dipping treatment by using the leaching agent, the cell wall permeability of the crushed flower and leaf powder is strong, the leaching agent easily penetrates through the cell wall to enter cells, the effective component CBD can be rapidly separated out, the cost of subsequent separation and purification and the use amount of a solvent can be reduced, and the THC component in the extract can be effectively removed by reasonably controlling the parameters of dewaxing, chromatography and recrystallization through reasonable dewaxing technology, column silica gel chromatography and recrystallization separation technology of the dipped extract, so that the extraction rate of CBD is higher, and the product purity is higher. The invention adopts a continuous dipping method for extraction, combines the extraction mode of precious and fine medicinal materials and the characteristics of CBD, selects the best extraction solvent and simple equipment, improves the extraction rate of CBD, reduces the production cost, has both yield and cost in large-scale production, adopts the method for extracting CBD, has the advantages of less investment, high benefit and little pollution, and has high content of CBD crystals prepared by a simple and reasonable production process, and the purity can reach more than 99.5 percent.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to be limiting in any way, and any modifications or alterations based on the teachings of the present invention are intended to fall within the scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains, as the following abbreviations and their corresponding materials appear in the present invention: CBDV is cannabidivarin, CBD is cannabidiol, CBG is cannabigerol, THCV is tetrahydrocannabivarin, and THC is tetrahydrocannabinol.
Example 1:
the method for extracting and purifying cannabidiol from industrial cannabis sativa as described in example 1, comprises the following steps:
crushing raw materials: 10kg of industrial hemp flower and leaf are crushed into flower and leaf powder with the granularity of 10 meshes;
drying: baking the flower and leaf powder obtained by crushing in the step I, wherein the baking temperature of the flower and leaf powder is 100 ℃, and baking until the weight loss is more than 7%;
③ leaching: adding an extracting agent into the flower and leaf powder baked in the second step, wherein the extracting agent is ethanol with the mass concentration of 80-100%, the solid-to-liquid ratio of the extracting agent to the flower and leaf powder is 1:6, keeping the liquid level of the extracting agent at a certain height at the temperature of 20 ℃, the liquid level of the extracting agent at 2cm, soaking for 8 hours, adding the extracting agent again at a certain flow rate, enabling the outflow speed of the extracting solution to be the same as the adding speed of the extracting agent, enabling the flow rate of the extracting agent to be 180mL/min, recovering the extracting agent after extraction is finished when the extracting agent does not have CBD after detection, evaporating and concentrating the outflow extracting solution to obtain 540g of an extract crude extract, wherein the content of the extract crude extract is 10%;
fourthly, dewaxing: dissolving the crude extract of the extract obtained in the third step by using ethanol with the mass concentration of 85%, dissolving the ethanol and the crude extract of the extract according to the mass-volume ratio of w/v =1:2, then freezing the crude extract at the temperature of-40 ℃ for 4h, then filtering the crude extract at the temperature, wherein the filtering precision is 400 meshes, then collecting filtrate, recovering the ethanol, wherein the collected filtrate is CBD enrichment, and the content of the CBD enrichment is 25%;
molecular distillation: and (4) carrying out molecular distillation on the CBD enrichment prepared in the step (IV), wherein the process conditions of the molecular distillation are as follows: feeding at 60 ℃, distilling at 120 ℃, keeping the vacuum degree at 1Pa, keeping the condensation temperature at 50 ℃, and collecting 104g of molecular distillation light phase CBD oil with the CBD oil content of 35%;
sixthly, column chromatography separation: loading the CBD oil prepared in the fifth step into a silica gel wet method with the column diameter ratio of 1:6 for silica gel column chromatography separation, wherein the silica gel fineness of the silica gel chromatography column is 200 meshes, the loading amount of the CBD oil is 0.3 percent of the weight of the silica gel, eluting by using an eluent, and then recovering the eluent, wherein the eluent is ethyl acetate and n-hexane, the volume ratio of the ethyl acetate to the n-hexane is 98-95: 2-5, collecting the chromatographic solution, continuously sampling and detecting the collected chromatographic solution by using HPLC, collecting the CBD component, concentrating the CBD component under the reduced pressure condition to obtain a CBD crude crystal, the content of the CBD crude crystal is more than 95 percent, the HPLC is short for high performance liquid chromatography, the high performance liquid chromatography detection takes liquid as a mobile phase, pumping the mobile phases such as single solvents with different polarities or mixed solvents with different proportions, buffer solutions and the like into a chromatographic column filled with a stationary phase by using a high pressure transfusion system, after the components in the column are separated, the components enter a detector for detection, so that the analysis of a sample is realized;
recovering the eluent: evaporating and concentrating the eluent recovered in the step (c), then measuring the concentrated eluent by using a standard alcohol meter, and then blending until the reading of the fresh eluent alcohol meter is obtained, wherein the eluent can be reused;
(iii) recrystallization of the [ CBD ]: dissolving the crude CBD crystal prepared in the step (c) by using a crystallization solvent, wherein the crystallization solvent is n-heptane, filtering after dissolving, concentrating under reduced pressure to obtain a saturated solution, stopping concentrating when the volume of the saturated solution is one third of that of the dissolved solution, placing the saturated solution at a low temperature to separate out crystals, placing the crystals at the low temperature of 0 ℃ for 4 hours, filtering, and drying under reduced pressure at the low temperature to obtain 65g of a finished CBD product, wherein the content of the finished CBD product is more than 99.5%.
In this example 1, a process route for extracting CBD from industrial hemp through crushing, drying, leaching, dewaxing, chromatographic separation and recrystallization is established, the process is advanced, stable and feasible, has the advantages of low investment, high benefit, high purity, high extraction rate and low pollution, and is suitable for large-scale industrial production, the purity of CBD prepared in this example 1 reaches 99.6%, and the extraction rate reaches 65%.
Example 2:
the method for extracting and purifying cannabidiol from industrial cannabis sativa as described in example 2, comprises the following steps:
crushing raw materials: 10kg of industrial hemp flower and leaf are crushed into flower and leaf powder with the granularity of 40 meshes;
drying: baking the flower and leaf powder obtained by crushing in the step I, wherein the baking temperature of the flower and leaf powder is 125 ℃, and baking until the weight loss is more than 7%;
③ leaching: adding an extracting agent into the flower and leaf powder baked in the second step, wherein the extracting agent is a mixture of normal hexane and petroleum ether, the solid-to-liquid ratio of the extracting agent to the flower and leaf powder is 1:8, keeping the liquid level of the extracting agent at a certain height at 25 ℃, keeping the liquid level of the extracting agent at 4cm, soaking for 18h, adding the extracting agent again at a certain flow rate, ensuring that the outflow speed of an extracting solution is the same as the adding speed of the extracting agent, the flow rate of the extracting agent is 220mL/min, recovering the extracting agent after extraction is finished when the extracting agent is detected to be free of CBD, evaporating and concentrating the outflow extracting solution to obtain 600g of crude extract, wherein the content of the crude extract is 12.5%;
fourthly, dewaxing: dissolving the crude extract of the extract obtained in the third step by using 92% ethanol with mass concentration, dissolving the ethanol and the crude extract of the extract according to the mass-volume ratio of w/v =1:7, then freezing the crude extract at the temperature of-25 ℃ for 8 hours, then filtering the crude extract at the temperature, wherein the filtering precision is 500 meshes, then collecting filtrate, recovering the ethanol, wherein the collected filtrate is CBD enrichment, and the content of the CBD enrichment is 32%;
molecular distillation: and (4) carrying out molecular distillation on the CBD enrichment prepared in the step (IV), wherein the process conditions of the molecular distillation are as follows: feeding at 95 ℃, distilling at 170 ℃, keeping the vacuum degree at 12Pa, and the condensation temperature at 95 ℃, wherein the collected molecular distillation light phase is 120g of CBD oil, and the content of the CBD oil is 60%;
sixthly, column chromatography separation: loading the CBD oil prepared in the fifth step into a silica gel wet method with the column diameter ratio of 1:8 for silica gel column chromatography separation, wherein the silica gel fineness of the silica gel chromatographic column is 400 meshes, the loading amount of the CBD oil is 3% of the weight of the silica gel, eluting by using an eluent, then recovering the eluent, the eluent is dichloromethane and n-hexane, the volume ratio of the dichloromethane to the n-hexane is 1:3.5, collecting the chromatographic solution, carrying out continuous sampling detection on the collected chromatographic solution by using HPLC, collecting the CBD component, concentrating the CBD component under the reduced pressure condition to obtain a CBD crude crystal, the content of the CBD crude crystal is more than 95%, the HPLC is the abbreviation of high performance liquid chromatography, the detection of the high performance liquid chromatography uses liquid as a mobile phase, and a high-pressure transfusion system is adopted to pump the mobile phases such as single solvents with different polarities or mixed solvents with different proportions, buffer solutions and the like into the chromatographic column filled with a, after the components in the column are separated, the components enter a detector for detection, so that the analysis of a sample is realized;
recovering the eluent: evaporating and concentrating the eluent recovered in the step (c), then measuring the concentrated eluent by using a standard alcohol meter, and then blending until the reading of the fresh eluent alcohol meter is obtained, wherein the eluent can be reused;
(iii) recrystallization of the [ CBD ]: dissolving the crude CBD crystal prepared in the step (c) by using a crystallization solvent, wherein the crystallization solvent is n-heptane, filtering after dissolving, concentrating under reduced pressure to obtain a saturated solution, stopping concentrating when the volume of the saturated solution is one third of that of the dissolved solution, placing the saturated solution at a low temperature to separate out crystals, placing the crystals at the low temperature of-20 ℃ for 18 hours, filtering, and drying under reduced pressure at the low temperature to obtain 70g of a finished CBD product, wherein the content of the finished CBD product is more than 99.5%.
In the embodiment 2, a process route for extracting the CBD from the industrial hemp through crushing, drying, leaching, dewaxing, chromatographic separation and recrystallization is established, the process is advanced, stable and feasible, has the advantages of low investment, high benefit, high purity, high extraction rate and low pollution, and is suitable for large-scale industrial production, the purity of the CBD prepared in the embodiment 2 reaches 99.8%, and the extraction rate reaches 70%.
Example 3:
the method for extracting and purifying cannabidiol from industrial cannabis sativa as described in example 3, comprises the following steps:
crushing raw materials: 10kg of industrial hemp flowers and leaves are crushed into flower and leaf powder with the granularity of 60 meshes;
drying: baking the flower and leaf powder obtained by crushing in the step I, wherein the baking temperature of the flower and leaf powder is 150 ℃, and baking until the weight loss is more than 7%;
③ leaching: adding an extracting agent into the flower and leaf powder baked in the second step, wherein the extracting agent is a mixture of 100% ethanol, n-hexane, petroleum ether and ethyl acetate, the solid-to-liquid ratio of the extracting agent to the flower and leaf powder is 1:10, keeping the liquid level of the extracting agent at a certain height at 28 ℃, the liquid level of the extracting agent is 5cm, soaking for 24 hours, adding the extracting agent again at a certain flow rate, the outflow speed of the extracting solution is the same as the addition speed of the extracting agent, the flow rate of the extracting agent is 270mL/min, extracting until the extracting agent is detected to have no CBD, recovering the extracting agent, evaporating and concentrating the outflow extracting solution to obtain 460g of crude extract, and the content of the crude extract is 15%;
fourthly, dewaxing: dissolving the crude extract of the extract obtained in the third step by using 100% ethanol with mass concentration, dissolving the ethanol and the crude extract of the extract according to the mass-volume ratio of w/v =1:10, then freezing the crude extract at the temperature of-5 ℃ for 12 hours, then filtering the crude extract at the temperature, wherein the filtering precision is 600 meshes, then collecting filtrate, recovering ethanol, wherein the collected filtrate is CBD enrichment, and the content of the CBD enrichment is 40%;
molecular distillation: and (4) carrying out molecular distillation on the CBD enrichment prepared in the step (IV), wherein the process conditions of the molecular distillation are as follows: feeding at 120 ℃, distilling at 220 ℃, keeping the vacuum degree at 20Pa, keeping the condensation temperature at 130 ℃, and collecting 120g of molecular distillation light phase CBD oil with the CBD oil content of 55%;
sixthly, column chromatography separation: loading the CBD oil prepared in the fifth step into a silica gel wet method with the column diameter ratio of 1:10 for silica gel column chromatography separation, wherein the silica gel fineness of the silica gel column is 600 meshes, the loading amount of the CBD oil is 4 percent of the weight of the silica gel, eluting by using an eluent, then recovering the eluent, the eluent is chloroform and petroleum ether, the volume ratio of the chloroform to the petroleum ether is 1:15, collecting the chromatographic solution, performing continuous sampling detection on the collected chromatographic solution by using HPLC, collecting the CBD component, concentrating the CBD component under the reduced pressure condition to obtain a CBD crude crystal, the content of the CBD crude crystal is more than 95 percent, the HPLC is short for high performance liquid chromatography, the detection of the high performance liquid chromatography adopts liquid as a mobile phase, adopting a high pressure transfusion system, pumping the single solvent with different polarities or the mixed solvent with different proportions, the buffer solution and other mobile phases into the chromatographic column filled with a stationary phase, and after the components in the column are separated, the sample enters a detector for detection, so that the analysis of the sample is realized;
recovering the eluent: evaporating and concentrating the eluent recovered in the step (c), then measuring the concentrated eluent by using a standard alcohol meter, and then blending until the reading of the fresh eluent alcohol meter is obtained, wherein the eluent can be reused;
(iii) recrystallization of the [ CBD ]: dissolving the crude CBD crystal prepared in the step (c) by using a crystallization solvent, wherein the crystallization solvent is n-heptane, filtering after dissolving, concentrating under reduced pressure to obtain a saturated solution, stopping concentrating when the volume of the saturated solution is one third of that of the dissolved solution, placing the saturated solution at a low temperature to separate out crystals, placing the crystals at the low temperature of-30 ℃ for 24 hours, filtering, and drying under reduced pressure at the low temperature to obtain 60g of a finished CBD product, wherein the content of the finished CBD product is more than 99.5%.
In this embodiment 3, a process route for extracting CBD from industrial hemp through crushing, drying, leaching, dewaxing, chromatographic separation and recrystallization is established, the process is advanced, stable and feasible, has the advantages of low investment, high benefit, high purity, high extraction rate and low pollution, and is suitable for large-scale industrial production, the purity of CBD prepared in this embodiment 3 reaches 99.9%, and the extraction rate reaches 60%.
Claims (7)
1. A method for extracting purified cannabidiol from industrial cannabis sativa, comprising the steps of:
crushing raw materials: crushing industrial hemp flowers and leaves into flower and leaf powder with the granularity of 10-60 meshes;
drying: baking the flower and leaf powder obtained by crushing in the step I until the weight loss is more than 7%;
③ leaching: adding an extracting agent into the flower and leaf powder baked in the second step, wherein the solid-liquid ratio of the extracting agent to the flower and leaf powder is 1: 6-10, keeping the liquid level of the extracting agent at a certain height at normal temperature, soaking for 8-24 hours, adding the extracting agent again at a certain flow rate until the outflow speed of the extracting solution is the same as the adding speed of the extracting agent, recovering the extracting agent until the extracting agent is detected to be free of CBD, and evaporating and concentrating the outflow extracting solution to obtain an extract crude extract, wherein the content of the extract crude extract is 10-15%;
fourthly, dewaxing: dissolving the extract crude extract obtained in the step (III) by using ethanol with the mass concentration of 85-100%, dissolving the ethanol and the extract crude extract according to the mass-volume ratio of w/v =1: 2-10, then freezing the extract crude extract at the temperature of-40 to-5 ℃ for 4-12 h, then filtering at the temperature, wherein the filtering precision is 400-600 meshes, then collecting filtrate, recovering ethanol, wherein the collected filtrate is CBD enrichment, and the content of the CBD enrichment is 25-40%;
molecular distillation: performing molecular distillation on the CBD enrichment obtained in the step (IV), wherein the collected molecular distillation light phase is CBD oil, and the content of the CBD oil is 35-70%;
sixthly, column chromatography separation: loading the CBD oil prepared in the fifth step into a silica gel wet method with the column diameter ratio of 1: 6-10 for silica gel column chromatography separation, wherein the silica gel fineness of the silica gel chromatography column is 200-600 meshes, the loading amount of the CBD oil is 0.3-4% of the weight of the silica gel, eluting by using an eluent, then recovering the eluent, collecting a chromatographic solution, carrying out continuous sampling detection on the collected chromatographic solution by using HPLC (high performance liquid chromatography), collecting a CBD component, and concentrating the CBD component under a reduced pressure condition to obtain a CBD crude crystal, wherein the content of the CBD crude crystal is more than 95%;
recovering the eluent: evaporating and concentrating the eluent recovered in the step (c), then measuring the concentrated eluent by using a standard alcohol meter, and then blending until the reading of the fresh eluent alcohol meter is obtained, wherein the eluent can be reused;
(iii) recrystallization of the [ CBD ]: dissolving the crude CBD crystal obtained in the step (c) by using a crystallization solvent, filtering after dissolving, concentrating under reduced pressure to obtain a saturated solution, placing the saturated solution at a low temperature to separate out crystals, filtering, and drying under reduced pressure at a low temperature to obtain a finished CBD product, wherein the content of the finished CBD product is more than 99.5%.
2. The method for extracting cannabidiol from industrial hemp according to claim 1, wherein the baking temperature of the flower and leaf powder in the step (II) is 100-150 ℃.
3. The method for extracting and purifying cannabidiol from industrial cannabis sativa according to claim 1, wherein in step (iii), the leaching agent is one or more of ethanol, n-hexane, petroleum ether and ethyl acetate with a mass concentration of 80-100%, and the temperature at normal temperature is 20-28 ℃, the liquid level of the leaching agent is 2-5 cm, and the flow rate of the leaching agent is 180-270 mL/min.
4. The method for extracting and purifying cannabidiol from industrial cannabis sativa as claimed in claim 1, wherein in the fifth step, the process conditions of molecular distillation are as follows: feeding at the temperature of 60-120 ℃, distilling at the temperature of 120-220 ℃, keeping the vacuum degree at 1-20 Pa, and keeping the condensation temperature at 50-130 ℃.
5. The method for extracting and purifying cannabidiol from industrial cannabis according to claim 1, wherein in step (sixty), the eluent is a mixture of two or more solvents selected from ethyl acetate, chloroform, dichloromethane, n-hexane and petroleum ether.
6. The method for extracting and purifying cannabidiol from industrial cannabis sativa as claimed in claim 5, wherein the eluent is ethyl acetate and n-hexane, and the volume ratio of ethyl acetate to n-hexane is 98-95: 2-5; the eluent is dichloromethane and n-hexane, and the volume ratio of the dichloromethane to the n-hexane is 1: 1.5-5; the eluent is chloroform and petroleum ether, and the volume ratio of the chloroform to the petroleum ether is 1: 8-15.
7. The method for extracting cannabidiol from industrial cannabis according to claim 1, wherein in step (b), the crystallization solvent is n-heptane; after dissolving the CBD crude crystals, concentrating under reduced pressure until the volume of the saturated solution is one third of that of the dissolved solution, and stopping concentrating; the temperature for crystallization is 0 to minus 30 ℃ under the condition of low temperature, and the crystallization time is 4 to 24 hours.
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