CN111978158A - Method for extracting purified hypocannabidiol from industrial cannabis sativa - Google Patents
Method for extracting purified hypocannabidiol from industrial cannabis sativa Download PDFInfo
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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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for extracting purified sub-cannabidiol from industrial cannabis sativa, which comprises the following steps of crushing raw materials; secondly, baking; ③ leaching: leaching the roasted flower and leaf powder by adding a leaching agent, recovering the leaching agent, and evaporating and concentrating the effluent extracting solution to obtain an extract crude extract; fourthly, dewaxing: dissolving the extract with ethanol, freezing, and filtering to obtain filtrate as CBDV enriched substance; molecular distillation: carrying out desolventizing and molecular distillation on the CBDV enriched substance to obtain CBDV fatty oil; sixthly, resin column chromatography separation: dissolving CBDV fatty oil by using 50-60% ethanol by mass concentration, and then loading the sample into a resin column by a wet method for chromatographic separation to obtain a crude CBDV product; seventhly, recovering the eluent; (iii) recrystallization of CBDV: dissolving the crude CBDV product with ethanol, filtering, concentrating under reduced pressure, recrystallizing, and filtering to obtain CBDV crystal. The method has the advantages of simple process, environmental protection, low cost and high efficiency, and the purity of the prepared product is more than 99 percent.
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 hypocannabidiol 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, researches find that the cannabinoid components in industrial cannabis are more than 140, wherein the most important part of the research and development is Cannabidiol (CBD), however, along with the deep research, the secondary Cannabidiol (CBDV) is more and more emphasized, and the large-scale purification of CBDV has important significance for the development of industrial cannabis. CBDV and CBD are very similar, CBDV not only having the medicinal role of CBD, for example: anti-epilepsia, anti-inflammation, anti-depression, etc., and CBDV also has anti-nausea and neuroprotective effects. Foreign pharmaceutical companies enter into research on CBDV in many ways, the prospect of CBDV will be better and better in the future, CBDV has a meaning of replacing CBD, however, compared with CBD, extraction and purification of CBDV have higher process difficulty, high-purity CBDV crystals are difficult to obtain, and if the problem of extraction and purification of CBDV cannot be solved, industries cannot be developed better, and the CBDV cannot serve human health. Therefore, it is objectively needed to develop a method for extracting purified hypocannabidiol from industrial cannabis with reasonable, efficient, concise and environment-friendly process and high product extraction purity.
Disclosure of Invention
In order to solve the problems in the background art, the invention aims to provide a method for extracting purified hypocannabidiol from industrial hemp, which has the advantages of reasonable, efficient, simple and environment-friendly process and high product extraction purity.
The invention relates to a method for extracting purified hypocannabidiol from industrial cannabis sativa, which comprises the following steps:
crushing raw materials: crushing industrial hemp flowers and leaves into flower and leaf powder;
baking: baking the flower and leaf powder prepared 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, then keeping the liquid level height of the extracting agent at 2-5 cm under the temperature condition of 25-28 ℃, soaking for 8-24 h, adding the extracting agent again at the speed of 180-270 mL/min, ensuring that the outflow speed of an extracting solution is the same as the adding speed of the extracting agent, extracting until the extracting agent does not have CBDV after detection, recovering the extracting agent, and evaporating and concentrating the outflow extracting solution to obtain an extract crude extract;
fourthly, dewaxing: dissolving the crude extract of the extract obtained in the third step by using ethanol with the mass concentration of 85-100%, dissolving the ethanol and the crude extract of the extract according to the mass-volume ratio of w/v =1: 2-10, then freezing the crude extract of the 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, and collecting the filtrate as CBDV enrichment;
molecular distillation: desolventizing and molecular distilling the CBDV enriched material prepared in the step (iv), wherein during molecular distillation, feeding is carried out at the temperature of 60-120 ℃, distillation is carried out at the temperature of 120-220 ℃, the vacuum degree is kept at 1-20 Pa, the condensation temperature is 50-130 ℃, and the molecular distillation light phase collected by distillation is CBDV fatty oil;
sixthly, resin column chromatography separation: dissolving the CBDV fatty oil prepared in the fifth step by using 50-60% ethanol by mass concentration, loading the dissolved CBDV fatty oil into a resin column by a wet method for chromatographic separation, then performing gradient elution by using 50-60%, 60-62% and 62-65% ethanol eluent, collecting CBDV components, performing continuous sampling detection by using HPLC (high performance liquid chromatography), flushing the resin column by using 95% ethanol by mass concentration when no CBDV exists in the eluent, then performing resin column balance by using 50-60% methanol solution by mass concentration for next use, and finally performing reduced pressure concentration on the CBDV components to obtain a crude CBDV product;
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 CBDV: dissolving the crude CBDV prepared in the step (c) by using 75-90% ethanol by mass concentration, filtering after dissolving, concentrating under reduced pressure to obtain a saturated solution, standing the saturated solution at the temperature of 0-minus 30 ℃ to separate out crystals, filtering, and drying under reduced pressure at low temperature to obtain CBDV crystals with the content of the CBDV crystals being more than 99%.
Furthermore, in the step I, the particle size of the mosaic powder is 10-40 meshes.
Further, in the second step, the baking temperature of the flower and leaf powder is 100-130 ℃.
Further, in the third step, the extracting agent is ethanol with the mass concentration of 80-100%.
Further, in the step (sixthly), the resin fineness of the resin column is 200-600 meshes, and the sample loading amount of the CBDV grease is 0.5-3% of the volume of the resin.
Further, in the step (sixthly), the amount of ethanol with a mass concentration of 50-60% is 1-4 column volumes, the amount of ethanol with a mass concentration of 60-62% is 2-6 column volumes, the amount of ethanol with a mass concentration of 62-65% is 2-3 column volumes, and the amount of ethanol with a mass concentration of 95% is 2-3 column volumes.
In the present invention, CBD and CBDV are explained as follows:
cannabidiol, CBD, is a natural component extracted from the cannabis plant and has the molecular formula C21H30O 2. The character is represented by white to light yellow resin or crystal, the melting point is 66-67 ℃, the crystal is almost insoluble in water, and the crystal is dissolved in organic solvents such as ethanol, methanol, ether, benzene, chloroform and the like.
CBDV, can be used for treating nervous diseases, and can be obtained by extracting industrial cannabis with alcohol to obtain extract containing cannabidiol with molecular formula of C19H26O 2.
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 CBDV can be rapidly separated out, the cost of subsequent separation and purification and the use amount of a solvent can be reduced, and the dipped extract is subjected to reasonable dewaxing technology, resin column chromatography and recrystallization separation technology, and the extraction rate of CBDV can be higher and the product purity is higher by reasonably controlling the parameters of dewaxing, chromatography and recrystallization. Meanwhile, the invention is extracted simultaneously with other cannabinoids extracts such as CBD in the actual production, the extraction and purification of CBDV can be realized on the premise of not increasing equipment, the investment of equipment cost can be effectively controlled, and the whole production process does not use other organic solvents, only uses ethanol in the whole process, is a pure natural and pollution-free extraction process, avoids the introduction of toxic and harmful substances, and is relatively friendly to the environment. The extraction process used by the invention has the advantages of environmental protection, simple operation, high extraction rate and high content of the obtained CBDV crystal, provides another thought for researching CBDV and cannabinoids, and has great significance.
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, and THC is tetrahydrocannabinol.
Example 1:
the method for extracting purified cannabidiol from industrial cannabis sativa according to example 1 comprises the following steps:
crushing raw materials: crushing industrial hemp flowers and leaves into flower and leaf powder, wherein the granularity of the flower and leaf powder is 10 meshes;
baking: baking the flower and leaf powder prepared in the step I until the weight loss is more than 7%, wherein the baking temperature of the flower and leaf powder is 100 ℃;
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 height of the extracting agent at 2cm under the temperature condition of 25 ℃, soaking for 8h, extracting by using ethanol, completely dissolving CBDV (cubic boron vehicle Virus) components in the flower and leaf powder in the ethanol, adding the extracting agent again at the speed of 180mL/min, enabling the outflow speed of the extracting solution to be the same as the addition speed of the extracting agent, finishing extraction when the extracting agent is detected to be free of CBDV, recovering the extracting agent, and evaporating and concentrating the outflow extracting solution to obtain an extract crude extract;
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 of the extract at the temperature of-40 ℃ for 4 hours, then filtering the crude extract of the extract at the temperature, wherein the filtering precision is 400 meshes, then collecting filtrate, recovering the ethanol, and collecting the filtrate which is CBDV enrichment;
molecular distillation: desolventizing and molecular distilling the CBDV enriched material prepared in the step (iv), wherein during molecular distillation, feeding is carried out at 60 ℃, distillation and distillation are carried out at 120 ℃, the vacuum degree is kept at 1Pa, the condensation temperature is 50 ℃, and the molecular distillation light phase collected by distillation is CBDV fatty oil;
sixthly, resin column chromatography separation: dissolving the CBDV grease oil prepared in the fifth step by using 50% ethanol by mass concentration, then loading the dissolved CBDV grease oil into a resin column by a wet method for chromatographic separation, wherein the resin fineness of the resin column is 200 meshes, the loading amount of the CBDV grease oil is 0.5% of the volume of the resin, then performing gradient elution by using 50%, 60% and 62% ethanol eluents, collecting CBDV components, wherein the 50% ethanol dosage is 1 column volume, the 60% ethanol dosage is 2 column volumes, the 62% ethanol dosage is 2 column volumes, the 95% ethanol dosage is 2 column volumes, performing continuous sampling detection by using HPLC (high performance liquid chromatography) eluent, flushing the resin column by using 95% ethanol when no CBDV exists, then performing resin column balance by using 50% methanol solution for next use, finally performing reduced pressure concentration on the CBDV components to obtain a crude CBDV product, HPLC is high performance liquid chromatography, which is an important branch of chromatography, liquid is used as a mobile phase, a high pressure transfusion system is adopted, the mobile phases such as single solvents with different polarities or mixed solvents with different proportions, buffer solutions and the like are pumped into a chromatographic column filled with a stationary phase, and after 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 CBDV: dissolving the crude CBDV prepared in the step (c) by using 75% ethanol by mass concentration, filtering after dissolving, concentrating under reduced pressure to obtain a saturated solution, placing the saturated solution at the temperature of 0 ℃ to separate out crystals, filtering, and drying under reduced pressure at low temperature to obtain CBDV crystals with the content of the CBDV crystals being more than 99%.
In this example 1, the method for preparing hypocannabidiol does not contain cannabidiol in separation and purification, and the whole process only uses ethanol and has no residue of undesirable organic solvents. The method has the advantages of simple process, environmental protection, low cost and high efficiency, and the detection proves that the purity of the CBDV crystal prepared in the embodiment 1 is 99.3% and the yield is improved to 89.6% from the original 60%.
Example 2:
the method for extracting purified cannabidiol from industrial cannabis sativa according to example 2 comprises the following steps:
crushing raw materials: crushing industrial hemp flowers and leaves into flower and leaf powder, wherein the granularity of the flower and leaf powder is 25 meshes;
baking: baking the flower and leaf powder prepared in the step I until the weight loss is more than 7%, wherein the baking temperature of the flower and leaf powder is 120 ℃;
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 1:8, then keeping the liquid level height of the extracting agent at 4cm under the temperature condition of 26.5 ℃, soaking for 18h, extracting by using ethanol, completely dissolving CBDV components in the flower and leaf powder in the ethanol, adding the extracting agent again at the speed of 220mL/min, enabling the outflow speed of the extracting solution to be the same as the adding speed of the extracting agent, finishing extraction when the extracting agent is detected to be free of CBDV, recovering the extracting agent, and evaporating and concentrating the outflow extracting solution to obtain an extract crude extract;
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 =1:6, then freezing the crude extract of the extract at the temperature of-25 ℃ for 8 hours, then filtering the crude extract of the extract at the temperature, wherein the filtering precision is 500 meshes, then collecting filtrate, recovering the ethanol, and collecting the filtrate which is CBDV enrichment;
molecular distillation: desolventizing and molecular distilling the CBDV enriched material prepared in the step (iv), wherein during molecular distillation, feeding is carried out at 90 ℃, distillation and distillation are carried out at 180 ℃, the vacuum degree is kept at 13Pa, the condensation temperature is 90 ℃, and the molecular distillation light phase collected by distillation is CBDV fatty oil;
sixthly, resin column chromatography separation: dissolving the CBDV grease oil prepared in the fifth step by using 55% ethanol by mass concentration, then loading the dissolved CBDV grease oil into a resin column by a wet method for chromatographic separation, wherein the resin fineness of the resin column is 400 meshes, the loading amount of the CBDV grease oil is 2% of the volume of the resin, then performing gradient elution by using ethanol eluents with the mass concentrations of 55%, 61% and 63%, collecting CBDV components, wherein the mass concentration of 55% ethanol is 3 column volumes, the mass concentration of 61% ethanol is 4 column volumes, the mass concentration of 62% ethanol is 2.5 column volumes, the mass concentration of 95% ethanol is 2.5 column volumes, performing continuous sampling detection by using HPLC, flushing the resin column by using 95% ethanol when no CBDV exists in the eluent, then performing resin column balance by using 55% methanol solution for next use, finally performing reduced pressure concentration on the CBDV components to obtain a crude CBDV product, HPLC is high performance liquid chromatography, which is an important branch of chromatography, liquid is used as a mobile phase, a high pressure transfusion system is adopted, the mobile phases such as single solvents with different polarities or mixed solvents with different proportions, buffer solutions and the like are pumped into a chromatographic column filled with a stationary phase, and after 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 CBDV: dissolving the crude CBDV prepared in the step (c) by using ethanol with the mass concentration of 82%, filtering after dissolving, concentrating under reduced pressure to obtain a saturated solution, placing the saturated solution at the temperature of minus 20 ℃ to separate out crystals, filtering, and drying under reduced pressure at low temperature to obtain CBDV crystals with the content of the CBDV crystals being more than 99%.
In this example 2, the method for preparing hypocannabidiol does not contain cannabidiol in separation and purification, and the whole process only uses ethanol, and has no residue of undesirable organic solvents. The method has the advantages of simple process, environmental protection, low cost and high efficiency, and the detection proves that the purity of the CBDV crystal prepared in the embodiment 2 is 99.7% and the yield is improved to 90.2% from the original 60%.
Example 3:
the method for extracting purified cannabidiol from industrial cannabis sativa according to embodiment 3, comprises the following steps:
crushing raw materials: crushing industrial hemp flowers and leaves into flower and leaf powder, wherein the granularity of the flower and leaf powder is 40 meshes;
baking: baking the flower and leaf powder prepared in the step I until the weight loss is more than 7%, wherein the baking temperature of the flower and leaf powder is 130 ℃;
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 1:10, keeping the liquid level height of the extracting agent at 5cm under the temperature condition of 28 ℃, soaking for 24h, extracting by using ethanol to completely dissolve CBDV components in the flower and leaf powder in the ethanol, adding the extracting agent again at the speed of 270mL/min to ensure that the outflow speed of the extracting solution is the same as the addition speed of the extracting agent, finishing extraction when the extracting agent is detected to be free of CBDV, recovering the extracting agent, and evaporating and concentrating the outflow extracting solution to obtain an extract crude extract;
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 of the extract at the temperature of-5 ℃ for 12 hours, then filtering the crude extract of the extract at the temperature, wherein the filtering precision is 600 meshes, then collecting filtrate, recovering the ethanol, and collecting the filtrate which is CBDV enrichment;
molecular distillation: desolventizing and molecular distilling the CBDV enriched material prepared in the step (iv), wherein during molecular distillation, feeding is carried out at 120 ℃, distillation and distillation are carried out at 220 ℃, the vacuum degree is kept at 20Pa, the condensation temperature is 130 ℃, and the molecular distillation light phase collected by distillation is CBDV fatty oil;
sixthly, resin column chromatography separation: dissolving the CBDV grease oil prepared in the fifth step by using 60% ethanol by mass concentration, then loading the dissolved CBDV grease oil into a resin column by a wet method for chromatographic separation, wherein the resin fineness of the resin column is 600 meshes, the loading amount of the CBDV grease oil is 3% of the volume of the resin, then performing gradient elution by using ethanol eluents with the mass concentrations of 60%, 62% and 65%, collecting CBDV components, wherein the usage amount of 60% ethanol is 4 column volumes, the usage amount of 62% ethanol is 6 column volumes, the usage amount of 65% ethanol is 3 column volumes, the usage amount of 95% ethanol is 3 column volumes, performing continuous sampling detection by using HPLC, flushing the resin column by using 95% ethanol when no CBDV comes out from the eluent, then performing resin column balance by using 60% methanol solution for next use, finally performing reduced pressure concentration on the CBDV components to obtain a crude CBDV product, HPLC is high performance liquid chromatography, which is an important branch of chromatography, liquid is used as a mobile phase, a high pressure transfusion system is adopted, the mobile phases such as single solvents with different polarities or mixed solvents with different proportions, buffer solutions and the like are pumped into a chromatographic column filled with a stationary phase, and after 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 CBDV: dissolving the crude CBDV prepared in the step (c) by using 90% ethanol by mass concentration, filtering after dissolving, concentrating under reduced pressure to obtain a saturated solution, placing the saturated solution at the temperature of minus 30 ℃ to separate out crystals, filtering, and drying under reduced pressure at low temperature to obtain CBDV crystals with the content of the CBDV crystals being more than 99%.
In this example 3, the method for preparing hypocannabidiol does not contain cannabidiol in separation and purification, and the whole process only uses ethanol, and has no residue of undesirable organic solvents. The method has the advantages of simple process, environmental protection, low cost and high efficiency, and the detection proves that the purity of the CBDV crystal prepared in the embodiment 3 is 99.7% and the yield is improved to 88.5% from the original 60%.
Claims (6)
1. A method for extracting purified sub-cannabidiol from industrial cannabis sativa is characterized by comprising the following steps:
crushing raw materials: crushing industrial hemp flowers and leaves into flower and leaf powder;
baking: baking the flower and leaf powder prepared 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, then keeping the liquid level height of the extracting agent at 2-5 cm under the temperature condition of 25-28 ℃, soaking for 8-24 h, adding the extracting agent again at the speed of 180-270 mL/min, ensuring that the outflow speed of an extracting solution is the same as the adding speed of the extracting agent, extracting until the extracting agent does not have CBDV after detection, recovering the extracting agent, and evaporating and concentrating the outflow extracting solution to obtain an extract crude extract;
fourthly, dewaxing: dissolving the crude extract of the extract obtained in the third step by using ethanol with the mass concentration of 85-100%, dissolving the ethanol and the crude extract of the extract according to the mass-volume ratio of w/v =1: 2-10, then freezing the crude extract of the 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, and collecting the filtrate as CBDV enrichment;
molecular distillation: desolventizing and molecular distilling the CBDV enriched material prepared in the step (iv), wherein during molecular distillation, feeding is carried out at the temperature of 60-120 ℃, distillation is carried out at the temperature of 120-220 ℃, the vacuum degree is kept at 1-20 Pa, the condensation temperature is 50-130 ℃, and the molecular distillation light phase collected by distillation is CBDV fatty oil;
sixthly, resin column chromatography separation: dissolving the CBDV fatty oil prepared in the fifth step by using 50-60% ethanol by mass concentration, loading the dissolved CBDV fatty oil into a resin column by a wet method for chromatographic separation, then performing gradient elution by using 50-60%, 60-62% and 62-65% ethanol eluent, collecting CBDV components, performing continuous sampling detection by using HPLC (high performance liquid chromatography), flushing the resin column by using 95% ethanol by mass concentration when no CBDV exists in the eluent, then performing resin column balance by using 50-60% methanol solution by mass concentration for next use, and finally performing reduced pressure concentration on the CBDV components to obtain a crude CBDV product;
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 CBDV: dissolving the crude CBDV prepared in the step (c) by using 75-90% ethanol by mass concentration, filtering after dissolving, concentrating under reduced pressure to obtain a saturated solution, standing the saturated solution at the temperature of 0-minus 30 ℃ to separate out crystals, filtering, and drying under reduced pressure at low temperature to obtain CBDV crystals with the content of the CBDV crystals being more than 99%.
2. The method for extracting purified cannabidiol from industrial cannabis sativa as claimed in claim 1, wherein in step (i), the particle size of the floral leaf powder is 10-40 mesh.
3. 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 100-130 ℃.
4. The method of claim 1, wherein the extractant is ethanol with a mass concentration of 80-100%.
5. The method for extracting and purifying cannabidiol from industrial cannabis sativa as claimed in claim 1, characterized in that in step (sixty), the resin fineness of the resin column is 200-600 mesh, and the sample loading amount of CBDV lipid oil is 0.5-3% of the resin volume.
6. The method for extracting and purifying cannabidiol from industrial cannabis sativa as claimed in claim 1, characterized in that in step (c), 50-60% by mass of ethanol is used in an amount of 1-4 column volumes, 60-62% by mass of ethanol is used in an amount of 2-6 column volumes, 62-65% by mass of ethanol is used in an amount of 2-3 column volumes, and 95% by mass of ethanol is used in an amount of 2-3 column volumes.
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