CN110317126A - A kind of method and system for extracting cannabidiol in industrial hemp with microwave-assisted Subcritical Water Extraction technology - Google Patents
A kind of method and system for extracting cannabidiol in industrial hemp with microwave-assisted Subcritical Water Extraction technology Download PDFInfo
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- CN110317126A CN110317126A CN201910590733.8A CN201910590733A CN110317126A CN 110317126 A CN110317126 A CN 110317126A CN 201910590733 A CN201910590733 A CN 201910590733A CN 110317126 A CN110317126 A CN 110317126A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
- B01D11/0265—Applying ultrasound
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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
- C07C37/004—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by obtaining phenols from plant material or from animal material
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- 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 kind of methods that microwave-assisted Subcritical Water Extraction technology extracts cannabidiol, belong to industrial hemp field, steps are as follows: step 1: directly crushing after fresh hemp plant is freezed；Step 2: water is passed through smashed hemp plant and carries out microwave-assisted Subcritical Water Extraction, when the microwave abstracting, control microwave frequency is 300-3000MHz, power 200-1200w, and control coolant-temperature gage is 100 DEG C~374 DEG C, extracting pressure is 10~22MPa, recycle-water all is evaporated from gained liquid phase every time after extraction in extraction 10~60 minutes every time, after repeating extraction three times, cannabidiol concentrate is obtained；Step 3: cannabidiol concentrate is diluted, and is carried out gradient elution to the cannabidiol concentrate after dilution by chromatographic column, is collected target eluent；Target eluent is concentrated, crystallization obtains cannabidiol product；The invention also discloses a kind of system, it is used to carry out above-mentioned extraction process.
Description
Technical field
The present invention relates to industrial hemp fields.
Background technique
Hemp (Cannabis sativa L.subsp.sativa) is a kind of annual grass with important medical value
This plant belongs to moraceae plants hemp subfamily Cannabis.There are three types of (cannabidiols for hemp plant extract main active
CBD, cannabinol CBN, tetrahydro hemp THC), wherein THC is a kind of ingredient being addicting.Hemp plant is to people's hallucinogenic action
Mainly for THC concentration come what is depended on, the kind of THC < 0.3% does not have psychotropic activity.Therefore EU Committee has formulated unified mark
Standard can plant THC content in hemp dry product and be known as " industrial hemp " not above 0.3%.
The cannboid isolated from hemp at present is more than 80 kinds existing, mainly include cannabidiol CBD, tetrahydro hemp THC,
Cannabinol CBN and cannabigerol CBC etc., research finds that CBD can hinder THC to influence nerve system of human body, and has important
Pharmacological activity.In addition to this, Recent study is found, CBD has tranquilizing soporific, treatment epilepsy, neuroprotection, multiple sclerosis
A series of physiological functions such as disease, rheumatic arthritis, oncotherapy are a kind of in the natural of the great application prospect of medicine and other fields
Active constituent.
Since CBD has a large amount of bioactivity and its medical value, extracting CBD from hemp floral leaf has extensively
Wealthy market prospects.There is the report of some extracting methods about cannabidiol CBD in public information at present.For example,
CN201410052776 discloses one kind and extracts dihydro cannabinol (CBD) technique from industrial hemp, just using solvent extraction method
Hexane extracts, and is enriched with macroreticular resin and silica gel, and CBD product is obtained.CN201811468947 discloses a kind of from work
The method of separation and Extraction cannabidiol in sparetime university's hemp plant, use solvent extraction method (95%) ethyl alcohol, petroleum ether extraction, and
It is purified using silica gel column chromatography and C18 column chromatography joint technology, has finally obtained cannabidiol product.
CN201710631532 discloses a kind of method using supercritical carbon dioxide extracting cannabidiol and its cannabidiol product,
It using CO_2 supercritical technology, is extracted using different entrainers, the subsequent operations such as is filtered, separated, having finally obtained hemp
Two phenolic products.It is wherein that CN201610087327 discloses one kind rich in cannabidiol with the closest prior art of the present invention
The numb medicinal extract of fire and preparation method thereof, which uses subcritical butane abstraction technique, and have passed through at low temperature winterization
Reason, centrifugation, filtering and decoloration and etc. obtain the numb medicinal extract of fire rich in cannabidiol and CN201810948441 is disclosed
A kind of Subcritical Water Extraction technology extract cannabidiol method, this method use Subcritical Water Extraction technology, by extraction,
Column chromatography, crystallization and etc. obtained the product of cannabidiol.
Subcritical fluid extraction is using the fluid of subcritical state or the mixed solution of subcritical fluids as solvent, with solute
Target components are extracted from natural products by processes such as extraction, evaporation precipitation, compression, condensing recoveries in succession in system
A kind of new technology.In the presence of LPG, propane, butane, R600a, DME, R134a and sulfur hexafluoride etc. are with subcritical fluids state,
The diffusion of molecule enhances, and mass transfer velocity is accelerated, permeability to low pole in natural products and apolar substance and molten
Solution ability significantly improves.It is extracted under subcritical environment, it is complete not destroy heat-sensitive ingredients, purpose object, is considered as environmentally protective, preceding
A wide change property technology of scape.Extracted object is not directed to middle polarity and strong pole mainly for low pole, liposoluble constituent
The target components of property.
Microwave abstracting is certain organic components and the matrix made in solid or semisolid substance using the effect of electromagnetic field
It efficiently separates, and is able to maintain a kind of separation method of the script compound state of analysis object.Microwave refers to frequency 300,000,000
The conspicuous electromagnetic wave to 300 gigahertzs.Microwave has fluctuation, high frequency, thermal characteristics and non-thermal characteristics four characteristics, makes to extract
Rate improves several times, and can reduce extraction temperature, guarantees the quality of extract to the maximum extent, and in microwave abstracting, inhales
The difference for receiving microwave ability can be such that certain components in some regions or extraction system of base matter are selectively heated, thus
It separates extracted substance from matrix or system, enters relatively poor with smaller dielectric constant, microwave absorption capacity
In extractant.
Application publication number is that the patent document of CN 108929201A discloses a kind of Subcritical Water Extraction technology extraction hemp
The method of diphenol, in the patent document, this method be by the means of Subcritical Water Extraction to drying, grind after it is big
Numb plant carries out Subcritical Water Extraction, will dilute after extract liquor concentrating and impurity removing, then by chromatographic column row gradient elution, washes to target
Cannabidiol product is obtained after de- liquid concentration, crystallization.The method and tradition of above-mentioned offer cannabidiol extract cannabidiol
Method requires that raw material is first carried out high temperature drying, converts CBDA decarboxylation to while reducing moisture during being somebody's turn to do
CBD.Therefore extracting cycle is long, and technique is responsible for, and equipment investment is big.
Application publication number is that 103073649 A of CN discloses a kind of microwave radiation Subcritical water chromotagraphy biomass (rice
Grass) active ingredients method, by microwave radiation-Subcritical water chromotagraphy novel process, to biomass (Value of Spartina Anglica) activity
Effective component extracts.But when microwave radiation Subcritical water chromotagraphy different substance, to microwave and subcritical
Each parameter selection of water is most important, under some parameters, can not effectively extract effective ingredient, for need to extract
Composition, selecting suitable technological parameter is a technical problem, is also not present microwave radiation subcritical water in the prior art
It extracts in cannabidiol.
The existing mode for extracting CBD, including required during Subcritical Water Extraction CBD first that sample is high in an oven
Temperature is dry, converts CBD for CBDA decarboxylation while reducing moisture during being somebody's turn to do.Dry one side equipment investment in baking oven
Big complex process, another aspect energy consumption are also relatively high.
Since CBD is not dissolved in water, although the property of subcritical water changes, the solubility of CBD in water can be made to increase,
But CBD can not be made from preferably dissolving out into water in cell, affect effect of extracting.
Summary of the invention
It is an object of the invention to: in view of the above problems, disclose a kind of microwave-assisted Subcritical Water Extraction skill
The method that art extracts cannabidiol, this method is the means by microwave-assisted Subcritical Water Extraction directly to undried industry
Hemp plant extracts, and will dilute after extract liquor concentrating and impurity removing, then carries out gradient elution by column chromatography separation method, to mesh
Cannabidiol product is obtained after the concentration of mark eluent, crystallization.With microwave-assisted Subcritical Water Extraction, when extraction is not by raw material
Water content influence, do not need to dry in advance, and Extracting temperature is high, convert CBD for CBDA while extraction.
Extraction process of the present invention uses microwave-assisted Subcritical Water Extraction technology, when shortening extraction compared with traditional handicraft
Between 50%-90%, compare with traditional handicraft, yield improves 0.4%, while the purity of the extract of obtained CBD is up to
99.8%, and chemical organic reagent is not used, it is environmentally protective, rapidly and efficiently, it is more conducive to industrialization.
The method and step that microwave-assisted Subcritical Water Extraction technology disclosed by the invention extracts cannabidiol is as follows:
Step 1: it is directly crushed after fresh hemp plant is freezed；
Step 2: water is passed through smashed hemp plant and carries out microwave-assisted Subcritical Water Extraction, the microwave abstracting
When, control microwave frequency is 300-3000MHz, power 200-1200w, and control coolant-temperature gage is 100 DEG C~374 DEG C, extraction pressure
Power is 10~22MPa, is extracted 10~60 minutes every time, and every time after extraction, recycle-water is all evaporated from gained liquid phase, is repeated
After extraction three times, cannabidiol concentrate is obtained；
Step 3: cannabidiol concentrate is diluted, and carries out ladder to the cannabidiol concentrate after dilution by chromatographic column
Degree elution, collects target eluent；Target eluent is concentrated, crystallization obtains cannabidiol product.
In a preferred embodiment, the fresh plant after freezing is crushed to 10~20 mesh in step 1.
In a preferred embodiment, in step 2, smashed material is placed in extractor, with the speed of 1m3/h
It spends and is passed through pure water into extractor.
In a preferred embodiment, in step 3, pure water dilution is added in cannabidiol concentrate, passes through chromatographic column
Gradient elution is carried out to the cannabidiol concentrate after dilution, collects target eluent；The target eluent of gradient elution is closed
And be concentrated under reduced pressure at 50 DEG C~70 DEG C, solid content is removed, cannabidiol secondary concentration liquid, cannabidiol secondary concentration are obtained
95% ethyl alcohol supersaturation dissolution is added, up to cannabidiol product after being dried after acquisition crystal with pure water in liquid.
In a preferred embodiment, chromatographic column chromatograph the step of use: first by cannabidiol concentrate be added 4-
10 pure water are diluted, and make the solid content 1%-2% of dilution, are carried out gradient elution using macroporous absorbent resin, i.e., are first used
The ethyl alcohol of 10%~30%v/v cleans, then with the ethanol elution of 75%~90%v/v.
In a preferred embodiment, column chromatography filler be macroreticular resin, selected from HPD600, HPD450,
HPD5000, HPD826, HPD722, D101, AB-8, NKA-9, X-5, ADS-17's is one or more.
The invention also discloses a kind of system that microwave-assisted Subcritical Water Extraction technology extracts cannabidiol, the system packets
It includes:
Extraction cells extract industrial hemp raw material by microwave-assisted subcritical water, so that cannabidiol is molten
Solution is in subcritical water；
Evaporation element, evaporation element are connected by pipeline with extraction cells, and the water of cannabidiol is dissolved in extraction cells
Solution enters evaporation element, and evaporation element is evaporated recycle-water to the water dissolution dissolved with cannabidiol, obtains cannabidiol
Concentrate；
Storage element, for storing cannabidiol concentrate to be treated；
Solvent storage element, is connected to evaporation element, recycles the evaporation recycle-water of evaporation element, and mentions to extraction cells
For aqueous solvent.
In a preferred embodiment, the extraction cells include extractor, and extraction cells further include being located at extraction
Take the microwave generator in tank.
In a preferred embodiment, the solvent storage element includes condenser and solvent tank, solvent
Storage tank is connected to by pipeline with evaporation element, and the condenser is located on the pipeline, and solvent tank is passed through water by pipeline
It is sent into extractor after booster pump, solvent flow control valve.
In a preferred embodiment, the evaporation element includes evaporator.
Cannabidiol in microwave-assisted Subcritical water chromotagraphy industrial hemp disclosed by the invention does not need drying former material
Material, while the yield of CBD is also improved, using the technological parameter in method disclosed by the invention, especially this method, can make
Obtain the CBD product that purity is up to 99.7%.In the present invention, it is not used any organic reagent, i.e. safety and environmental protection, economic and practical,
The method that cannabidiol is extracted from hemp floral leaf that can guarantee efficient recovery rate again, solves the prior art and extracts cannabidiol
When poor solvent residual contamination, at high cost, the period is long, is difficult to realize the problems such as industrial amplification production.
Using extraction equipment and process conditions of the invention, according to water vapour without the characteristics such as bad residual, reaction time be short,
It is extracted under closed, anaerobic subcritical environment, cannabidiol can not only be discharged to greatest extent, and can effectively avoided each
The oxidative deformation and poor solvent residual contamination of kind active constituent.In addition, can be saved using pure water as solvent because of organic reagent wave
Take bring cost, is more conducive to the large-scale production and a wide range of popularization of industrial hemp.Experiment discovery, using subcritical water
Abstraction technique changes the property of water, significantly increases the solubility of cannabidiol in water, improve yield of extract and
CBD yield.
Extraction process of the invention is a process that is totally enclosed, can control circulation, is eliminated compared with the existing technology
After extract liquor is taken out, then the process being concentrated, CBD concentrate (medicinal extract) can be directly obtained, therefore, extraction process of the invention is more
What is added is simple, avoids unnecessary step and loss.
The present invention use microwave-assisted Subcritical water chromotagraphy when, with water as solvent, under the action of microwave field, hydrone by
High-speed rotation state is changed into excitation state, this is a kind of unstable state of high-energy.Hydrone or vaporization are at this time to reinforce
The driving force of extracted component, and microwave energy is a kind of nonionic for rotating and causing molecular motion by Ion transfer and dipole
Change radiation energy, hydrone has certain polarity, and instantaneous polarization can be generated under the action of microwave field, make reversal campaign,
To generate vibration, tearing and the interparticle friction and collision of key, and it is quickly generated a large amount of thermal energy, promotes cell rupture,
So that CBD is overflowed and is diffused into water, enters in the relatively poor water of smaller dielectric constant, microwave absorption capacity.Microwave
Extraction can also change the polarity of hydrone, and exacerbate polar movement, dissolve out CBD preferably in water.
Detailed description of the invention
Fig. 1 is an extracting system schematic diagram of the invention；
Marked in the figure: 1- extractor, 2- evaporator, 3- condenser, 4- solvent tank, 5- sample holding vessel, 6- booster pump,
7- microwave generator, the first regulating valve of 8-, the second regulating valve of 9-, 10- solvent flow control valve, 11- inlet valve.
Specific embodiment
With reference to the accompanying drawing, the present invention is described in detail.
Embodiment 1: being first crushed to 10 mesh for the fresh plant after freezing, and smashed material is placed in extractor, with
1m3The speed of/h is passed through pure water into extractor, is 300MHz, power 200w in microwave frequency, 250 DEG C of temperature, extraction is pressed
Subcritical Water Extraction is carried out under the subcritical state of power 12MPa, is extracted 60 minutes, recycle-water is evaporated, and after repeating extraction three times, is obtained
To the concentrate of cannabidiol；
Secondly it is that 4-10 times of pure water of its weight is diluted by the addition of cannabidiol concentrate, makes the solid content of dilution
1% -2%, gradient elution is carried out using macroporous absorbent resin, i.e., is first cleaned with the ethyl alcohol of 10%v/v, then with the second of 75%v/v
Alcohol elution, collects target eluent；The target eluent of gradient elution is merged, is concentrated under reduced pressure at 60 DEG C, solid content is removed,
Obtain cannabidiol secondary concentration liquid；
Finally, cannabidiol secondary concentration liquid to be added 95% ethyl alcohol supersaturation dissolution, use pure water after obtaining crystal
Up to cannabidiol product after washing is dry.
Embodiment 2: being first crushed to 20 mesh for the fresh plant after freezing, and smashed material is placed in extractor, with
1m3The speed of/h is passed through pure water into extractor, is 3000MHz, power 1200w in microwave frequency, 374 DEG C of temperature, extracts
Subcritical Water Extraction is carried out under the subcritical state of pressure 22MPa, is extracted 60 minutes, and recycle-water is evaporated, after repeating extraction three times,
Obtain the concentrate of cannabidiol；
Secondly it is that 4-10 times of pure water of its weight is diluted by the addition of cannabidiol concentrate, makes the solid content of dilution
1% -2%, gradient elution is carried out using macroporous absorbent resin, i.e., is first cleaned with the ethyl alcohol of 30%v/v, then with the second of 75%v/v
Alcohol elution, collects target eluent；The target eluent of gradient elution is merged, is concentrated under reduced pressure at 70 DEG C, solid content is removed,
Obtain cannabidiol secondary concentration liquid；
Finally, cannabidiol secondary concentration liquid to be added 95% ethyl alcohol supersaturation dissolution, use pure water after obtaining crystal
Up to cannabidiol product after washing is dry.
Embodiment 3: being first crushed to 15 mesh for the fresh plant after freezing, and smashed material is placed in extractor, with
1m3The speed of/h is passed through pure water into extractor, is 3000MHz, power 1200w in microwave frequency, 200 DEG C of temperature, extracts
Subcritical Water Extraction is carried out under the subcritical state of pressure 22MPa, is extracted 60 minutes, and recycle-water is evaporated, after repeating extraction three times,
Obtain the concentrate of cannabidiol；
Secondly it is that 4-10 times of pure water of its weight is diluted by the addition of cannabidiol concentrate, makes the solid content of dilution
1% -2%, gradient elution is carried out using macroporous absorbent resin, i.e., is first cleaned with the ethyl alcohol of 25%v/v, then with the second of 80%v/v
Alcohol elution, collects target eluent；The target eluent of gradient elution is merged, is concentrated under reduced pressure at 65 DEG C, solid content is removed,
Obtain cannabidiol secondary concentration liquid；
Finally, cannabidiol secondary concentration liquid to be added 95% ethyl alcohol supersaturation dissolution, use pure water after obtaining crystal
Up to cannabidiol product after washing is dry.
Embodiment 4: as shown in Figure 1, present embodiment discloses hemps in a kind of microwave-assisted sub-critical extraction industrial hemp
The system of diphenol, including pass through the sequentially connected extractor 1 of pipeline, evaporator 2, condenser 3, solvent tank 4 and sample storage
Deposit tank 5.Microwave generator 7 built in extractor 1 improves the yield and efficiency of extraction, and microwave abstracting carries out in extractor 1, extraction
Take tank 1 with solvent inlet and material input port.
The outside of extractor 1 is equipped with temperature controller and pressure controller, maintains extractor in the temperature and pressure of setting
In range, the efficiency of extraction is improved.Solvent tank 4 has solvent outlet, solvent storage for storing extractant, solvent tank 4
The solvent outlet of tank 4 is connected with the solvent inlet of extractor 1.Pipeline between solvent tank 4 and extractor 1 is equipped with booster pump
6, the solvent in solvent tank 4 is pumped in extractor by booster pump 6, and the pipeline between booster pump 6 and solvent tank 4 is equipped with
Solvent flow control valve 10, what solvent flow control valve 10 can control solvent is passed through speed.
Evaporator 2 is used to evaporate solvent and recycle, and has temperature controller outside evaporator 2, the bottom of evaporator 2 passes through pipeline
It is connected with sample bomb 5, the pipeline between sample bomb 5 and evaporator 2 is equipped with inlet valve 11.Condenser 3 will evaporate
Solvent condensation out, the pipeline between extractor 1 and evaporator 2 is equipped with the first regulating valve 8, between evaporator 2 and condenser 3
Pipeline is equipped with the second regulating valve 9, adjusts the pressure of the first regulating valve 8 and the second regulating valve 9 control extractor.
When microwave-assisted Subcritical Water Extraction technology extracts cannabidiol CBD, comminution of material is put by material input port
In extractor 1, water is uniformly passed through in extractor 1 by water in solvent tank 4 by booster pump 6, adjust pressure controller and
Temperature controller controls extractor pressure and temperature, while microwave generator 7 is actuated for microwave abstracting, the liquid in extractor 1
Phase (being dissolved with the subcritical water of CBD) enters evaporator 2, and the water in evaporator 2, which is recycled in solvent tank 4, to be recycled,
Solvent utilization rate is improved, the remaining liquid of evaporator 1 is the CBD solution of concentration, opens inlet valve for CBD concentrate and is stored in sample
It is spare in product holding vessel 5.After pure water dilution is added in above-mentioned CBD concentrate, the elution of column chromatographic grade is carried out, target is collected and washes
De- liquid, is concentrated, and crystallization obtains CBD product.
In a specific embodiment, using the system extraction process hemp of the extraction cannabidiol in embodiment 4
Cannabidiol in floral leaf, specific extracting method are as follows:
1) the industrial hemp floral leaf 10kg before taking away the florescence crushed 10-20 mesh after freezing 10h at a temperature of -20 DEG C；
2) crushed material of step 1) is put into extractor, by the water in solvent tank uniformly across the extraction that raw material are housed
Take tank；
3) start microwave generator built in extractor, control water flow is 1m3/ h, microwave frequency 2000MHz, power are
800w, extraction temperature are 374 DEG C, extracting pressure 22Mpa；
4) subcritical water dissolved with CBD in extractor is put into evaporator, every time circulation 40 minutes, by 3
After secondary circulation is extracted, stops water circulation, by the water in evaporator at 58 DEG C, solvent tank is recycled under the conditions of 0.2Mpa.It releases
CBD condensed liquid.0.5kg medicinal extract is obtained, CBD content is up to 50% in medicinal extract.
5) CBD concentrate is carried out gradient to CBD concentrate using chromatographic column and washed after 5 times of volume pure water dilutions are added
It is de-, collect target eluent；Above-mentioned target eluent is merged, is concentrated under reduced pressure at 58 DEG C, obtains CBD secondary concentration liquid；By CBD
95% ethyl alcohol supersaturation dissolution is added in secondary concentration liquid, obtain after crystal with pure water it is dry after up to white or light
Yellow CBD crystallizes 0.16kg.
It takes a small amount of CBD to crystallize, carries out efficient liquid phase chromatographic analysis, normalization method, the purity for calculating CBD are according to area
99.6%.The yield of cannabidiol is 1.6%.
Embodiment 5,
Using the extracting method of embodiment 4, difference is only that, changes microwave frequency, using the different microwave frequencies in table 1
It extracts 4 times, calculates yield of extract, CBD content and CBD yield, the results are shown in Table 1:
| Microwave frequency MHz | Yield of extract % | CBD content % | CBD yield % | |
| 1 | 300 | 1.4 | 25.8 | 0.22 |
| 2 | 500 | 2.4 | 26.2 | 0.35 |
| 3 | 1000 | 3.4 | 30.5 | 0.7 |
| 4 | 2000 | 4.2 | 50 | 1.7 |
Table 1
Find out in table 1, when extraction as the raising of microwave frequency, CBD yield of extract improve, CBD content can also be improved,
CBD yield can also improve.
Using the extracting method of embodiment 4, difference is only that, changes microwave power, using the different microwave in table 2
It extracts 4 times, calculates yield of extract, CBD content and CBD yield, the results are shown in Table 2:
| Microwave power w | Yield of extract % | CBD content % | CBD yield % | |
| 1 | 200 | 2.0 | 23.9 | 0.27 |
| 2 | 400 | 2.8 | 24.7 | 0.40 |
| 3 | 600 | 3.6 | 29.4 | 0.8 |
| 4 | 800 | 4.7 | 50 | 2.0 |
Table
Find out in table 2, when extraction as the raising of microwave power, CBD yield of extract improve, CBD content can also be improved,
CBD yield can also improve.
Using the extracting method of embodiment 4, difference is only that, changes extraction temperature, using the different extraction temperatures in table 3
It extracts 4 times, calculates yield of extract, CBD content and CBD yield, the results are shown in Table 3:
| Temperature DEG C | Yield of extract % | CBD content % | CBD yield % | |
| 1 | 100 | 1.8 | 24.1 | 0.22 |
| 2 | 200 | 2.3 | 26.3 | 0.37 |
| 3 | 300 | 3.7 | 30 | 0.8 |
| 4 | 374 | 5.3 | 50 | 1.9 |
Table 3
Find out in table 3, when extraction as the raising of extraction temperature, CBD yield of extract improve, CBD content can also be improved,
CBD yield can also improve.
Claims (10)
1. a kind of method that microwave-assisted Subcritical Water Extraction technology extracts cannabidiol, which is characterized in that steps are as follows:
Step 1: it is directly crushed after fresh hemp plant is freezed；
Step 2: being passed through smashed hemp plant for water and carry out microwave-assisted Subcritical Water Extraction, when the microwave abstracting, control
Microwave frequency processed is 300-3000MHz, power 200-1200w, and control coolant-temperature gage is 100 DEG C~374 DEG C, extracting pressure 10
~22MPa is extracted 10~60 minutes every time, and every time after extraction, recycle-water is all evaporated from gained liquid phase, repeats extraction three
After secondary, cannabidiol concentrate is obtained；
Step 3: cannabidiol concentrate is diluted, and is carried out gradient to the cannabidiol concentrate after dilution by chromatographic column and is washed
It is de-, target eluent is collected, target eluent is concentrated, crystallization obtains cannabidiol product.
2. the method that microwave-assisted Subcritical Water Extraction technology according to claim 1 extracts cannabidiol, feature exist
In the fresh plant after freezing is crushed to 10~20 mesh in step 1.
3. the method that microwave-assisted Subcritical Water Extraction technology according to claim 2 extracts cannabidiol, feature exist
In in step 2, smashed material is placed in extractor, with 1m3The speed of/h is passed through pure water into extractor.
4. the method that microwave-assisted Subcritical Water Extraction technology according to claim 3 extracts cannabidiol, feature exist
In in step 3, pure water dilution is added in cannabidiol concentrate, is carried out by chromatographic column to the cannabidiol concentrate after dilution
Gradient elution collects target eluent, and the target eluent of gradient elution is merged, is concentrated under reduced pressure, goes at 50 DEG C~70 DEG C
Except solid content, cannabidiol secondary concentration liquid is obtained, 95% ethyl alcohol supersaturation dissolution is added in cannabidiol secondary concentration liquid,
Up to cannabidiol product after being dried after acquisition crystal with pure water.
5. the method that microwave-assisted Subcritical Water Extraction technology according to claim 4 extracts cannabidiol, chromatographic column layer
The step of analysis, uses: being first that 4-10 times of pure water of its quality is diluted by the addition of cannabidiol concentrate, contains consolidating for dilution
Amount is 1%-2%, carries out gradient elution using macroporous absorbent resin, i.e., is first cleaned with the ethyl alcohol of 10%~30%v/v, then use
The ethanol elution of 75%~90%v/v.
6. the method that microwave-assisted Subcritical Water Extraction technology according to claim 5 extracts cannabidiol, column chromatography
Filler is macroreticular resin, selected from HPD600, HPD450, HPD5000, HPD826, HPD722, D101, AB-8, NKA-9, X-5,
ADS-17's is one or more.
7. the system that a kind of microwave-assisted Subcritical Water Extraction technology extracts cannabidiol, which is characterized in that the system includes:
Extraction cells extract industrial hemp raw material by microwave-assisted subcritical water, so that cannabidiol is dissolved in
In subcritical water；
Evaporation element, evaporation element are connected by pipeline with extraction cells, and the aqueous solution of cannabidiol is dissolved in extraction cells
Into evaporation element, evaporation element is evaporated recycle-water to the water dissolution dissolved with cannabidiol, obtains cannabidiol concentration
Liquid；
Storage element, for storing cannabidiol concentrate to be treated；
Solvent storage element, is connected to evaporation element, recycles the evaporation recycle-water of evaporation element, and provide water to extraction cells
Solvent.
8. the system that microwave-assisted Subcritical Water Extraction technology according to claim 7 extracts cannabidiol, feature exist
In the extraction cells include extractor (1), and extraction cells further include the microwave generator in extractor.
9. the system that microwave-assisted Subcritical Water Extraction technology according to claim 8 extracts cannabidiol, feature exist
In the solvent storage element includes condenser (3) and solvent tank (4), and solvent tank passes through pipeline and evaporation element
Connection, the condenser are located on the pipeline, and solvent tank is controlled water by booster pump (6), solvent flux by pipeline
Valve (10) is sent into extractor afterwards.
10. the system that microwave-assisted Subcritical Water Extraction technology according to claim 9 extracts cannabidiol, feature exist
In the evaporation element includes evaporator (2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910590733.8A CN110317126A (en) | 2019-07-02 | 2019-07-02 | A kind of method and system for extracting cannabidiol in industrial hemp with microwave-assisted Subcritical Water Extraction technology |
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