CN110511120A - It is a kind of improve industrial hemp CBD content pre-treating method and its optimization - Google Patents
It is a kind of improve industrial hemp CBD content pre-treating method and its optimization Download PDFInfo
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- CN110511120A CN110511120A CN201910868592.1A CN201910868592A CN110511120A CN 110511120 A CN110511120 A CN 110511120A CN 201910868592 A CN201910868592 A CN 201910868592A CN 110511120 A CN110511120 A CN 110511120A
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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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- 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
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- 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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Abstract
The present invention provide it is a kind of improve industrial hemp CBD content pre-treating method and its optimization, belong to industrial hemp processing technique field, this method is converted by high temperature drying to be achieved the purpose that improve CBD content, its influence to CBD content in raw material is considered from two parameters of temperature and time, to preferably go out best pyrolytic conversion condition: 100 DEG C ~ 150 DEG C of conversion temperature of drying, drying 1 ~ 5h of transformation time, after drying conversion, industrial hemp CBD content significantly improves, average out to 1.7% ~ 3.9% improves 1 ~ 3 times.The method of the present invention is simple, and required equipment is simple, and industrialized production is easily realized, at low cost, and CBD production capacity is greatly improved.
Description
Technical field
The invention belongs to industrial hemp processing technique fields, and in particular to a kind of preceding place for improving industrial hemp CBD content
Reason method and its optimization.
Background technique
Hemp (Cannabis sativa L.subsp.sativa) is moraceae plants hemp subfamily Cannabis, annual
Herbaceous plant.Tetrahydrocannabinol (THC) content is lower than 0.3%, as industrial hemp in hemp dry product.Industrial hemp is mainly applied
In agricultural planting, weaving, clothes, papermaking, bioenergy, medicine and feed etc..Containing active in industrial hemp extract
Substance can be used for anticancer, anti-AIDS, treatment neurological disease etc.；Its natural bacteriostatic effect can be widely applied to antibacterial functions fibre
Dimension, natural antiseptic agent, germ killing drugs and spray, personal cleanliness's articles etc.；In addition, industrial hemp extract resists in uvioresistant
Significant effect on oxidation activity, can play uvioresistant in cosmetic field, remove wrinkle, nti-freckle and other effects.
The active constituent of industrial hemp floral leaf extract is abundant, including terpenes, cannboid, flavone compound and fatty acid
Deng these substances have the medical value of itself.Wherein cannboid includes tetrahydrocannabinol (THC), cannabinol (CBN), hemp
Diphenol (CBD), cannabidiolic acid (CBDA), cannabidivarin (CBDV), tetrahydro-cannabinolic acid (THCA), tetrahydrocannabinol
(THCV), cannabigerol (CBG), cannabigerolic acid (CBGA), cannabichromene (CBC) etc., wherein former three accounts for cannabinoids
90% or more of compound.Extracting active material in industrial hemp floral leaf not only has huge economic value, while adapting to current
Various demands such as environmentally protective and sustainable development, the market opportunity is huge, cannabidiol (CBD) especially in industrial hemp
It is most important active constituent in hemp floral leaf using relatively broad, is mainly used in treatment epilepsy, senile dementia, depression, pa
The neural class diseases such as golden Sen Shi disease.
The current highest industrial hemp kind of country CBD content is " cloud is No. 7 numb ", kind CBD average content 1.2% ~
1.3%, compared with foreign countries, content is relatively low, causes the industrialization production capacity of CBD lower, and enterprise competitive advantage is weaker, but breeding height contains
The kind period of amount is long, Innovation Input is larger, risk is high.
Various chemical reactions can occur under certain condition for compound, and type cannboid abundant under certain condition can phase
Mutually conversion, for example, CBD and THC are separately converted to after CBDA and THCA decarboxylation under high temperature, therefore, before raw material extraction, high temperature
Conversion can be used as the effective way of a raising industrial hemp raw material CBD content, for improve the production capacity of enterprise find one it is new
Breach.
For this purpose, the present invention dries conversion processing in industrial hemp raw material pretreatment process, through high temperature, grope not equality of temperature
Degree and influence of the drying time to raw material CBD content, preferably optimum conversion condition out, to improve CBD in industrial hemp raw material
Content.
Summary of the invention
Low for current domestic industry Hemp Varieties CBD content, the low weak tendency of production capacity is extracted in CBD industrialization, of the invention
Be designed to provide it is a kind of improve industrial hemp CBD content pre-treating method and its optimization.The present invention is from temperature and time two
A parameter considers its influence to CBD content in industrial hemp raw material, thus it is preferred that going out optimum conversion condition: drying conversion temperature
100 DEG C ~ 150 DEG C, drying 1 ~ 5h of transformation time.The method of the present invention is simple, and industrialized production is easy to accomplish, at low cost, the production of CBD
It can be greatly improved.
The specific steps of the present invention are as follows:
The screening of step 1 conversion temperature
It takes a certain amount of industrial hemp raw material to crush and mixes spare, setting different temperatures gradient: 90 DEG C, 100 DEG C, 110 DEG C, 120
DEG C, 130 DEG C, 140 DEG C, 150 DEG C, 160 DEG C, using untreated raw material as blank control (CK), each test group is weighed centainly
Sample is measured, is sampled after a certain period of time after dry, methanol ultrasonic extraction, the detection of HPLC method determines optimal conversion according to detection data
Temperature range.
The screening of step 2 transformation time
Under the conditions of optimal conversion temperature range, different time gradient: 0.5h, 1h, 2h, 3h, 4h, 5h, 6h, 7h is set, with not
For the raw material of processing as blank control (CK), each test group weighs a certain amount of sample, a certain amount of sample is taken after dry, methanol is super
Sound extracts, the detection of HPLC method, determines best drying transformation time according to detection data.
The optimization of step 3 conversion condition is verified
After optimal conversion temperature and time has been determined, with optimal conditions, setting centainly repeats collimation test, with verifying
The reliability and stability of Optimal Parameters.A certain amount of sample, methanol ultrasonic extraction, the detection of HPLC method are taken after drying.
Beneficial effects of the present invention:
1, the present invention reaches the content for improving industrial hemp CBD by pyrolytic conversion, and compared with breed breeding, the period is short, research and development
At low cost, enterprise's investment is small, and risk is low.
2, the optimum conversion condition that the present invention preferably goes out: 100 DEG C ~ 150 DEG C of conversion temperature of drying, drying transformation time 1 ~
5h, under this optimal conditions, industrial hemp CBD content can be improved 2 ~ 3 times, average content 2.6% ~ 3.9%.
3, this pre-treating method is simple, and required equipment is simple, and Yi Shixian in commercial process, operating cost is low, CBD
Production capacity be greatly improved.
4, the moisture content of the raw material after drying conversion is low, convenient for storage, and is conducive to subsequent means of supercritical extraction.
Specific embodiment
With reference to embodiments, the present invention will be described in further detail.
Embodiment 1
Industrial hemp floral leaf is crushed to 40 mesh, respectively at different temperatures: 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C, 130 DEG C, 140
DEG C, 150 DEG C, 160 DEG C, using untreated raw material as blank control (CK), each processing weighs 300g sample, after dry 2h,
10g sample is accurately weighed, adds methanol ultrasonic extraction 3 times of 10 times of volumes, each 30min is collected by filtration filtrate, after concentrated by rotary evaporation
Methanol constant volume to 100ml, the detection of HPLC method the results are shown in Table 1.
After drying conversion processings using 90 DEG C ~ 160 DEG C high temperature, in industrial hemp floral leaf raw material CBD content it is average 1.7% ~
3.9%, it improves that 1 ~ 3 times, 90 DEG C and 160 DEG C of changing effect is slightly worse, is 1 times of control, preferably 100 DEG C ~ 150 DEG C are best
Dry conversion temperature range.
Influence of the different conversion temperatures of table 1 to CBD content in floral leaf raw material
Embodiment 2
Industrial hemp floral leaf is crushed to 40 mesh, in 130 DEG C of freeze-day with constant temperature different times: 0.5h, 1h, 2h, 3h, 4h, 5h, 6h,
7h, using untreated raw material as blank control (CK), each processing weighs 300g sample, accurately weighs 10g sample, adds 10 times
The methanol ultrasonic extraction of volume 3 times, each 30min, filtrate is collected by filtration, methanol constant volume is to 100ml, HPLC method after concentrated by rotary evaporation
Detection, the results are shown in Table 2.
From table 2 it can be seen that CBD content is significantly improved in raw material after 130 DEG C of high temperature drying conversions, average 1.7% ~
3.9%, compared with the control, averagely improve 1 ~ 3 times.The changing effect of 0.5h, 6h, 7h are slightly worse, improve 1 times, preferably 1h ~ 5h
Most preferably to dry transformation time range.
Influence of the 2 pyrolytic conversion time of table to CBD content in industrial hemp raw material
Embodiment 3
Industrial hemp floral leaf is crushed to 40 mesh, 100 DEG C of freeze-day with constant temperature 5h optimize verifying, and under equal conditions, 3 groups of weights are arranged
Multiple, using untreated raw material as blank control (CK), each processing weighs 500g sample, accurately weighs 20g sample, adds 10 times
The methanol ultrasonic extraction of volume 3 times, each 30min, filtrate is collected by filtration, methanol constant volume is to 100ml, HPLC method after concentrated by rotary evaporation
Detection, the results are shown in Table 3.
Embodiment 4
Industrial hemp floral leaf is crushed to 40 mesh, 150 DEG C of freeze-day with constant temperature 1h optimize verifying, and under equal conditions, 3 groups of weights are arranged
Multiple, using untreated raw material as blank control (CK), each processing weighs 500g sample, accurately weighs 20g sample, adds 10 times
The methanol ultrasonic extraction of volume 3 times, each 30min, filtrate is collected by filtration, methanol constant volume is to 100ml, HPLC method after concentrated by rotary evaporation
Detection, the results are shown in Table 3.
Embodiment 5
Industrial hemp floral leaf is crushed to 40 mesh, 130 DEG C of freeze-day with constant temperature 2h optimize verifying, and under equal conditions, 3 groups of weights are arranged
Multiple, using untreated raw material as blank control (CK), each processing weighs 500g sample, accurately weighs 20g sample, adds 10 times
The methanol ultrasonic extraction of volume 3 times, each 30min, filtrate is collected by filtration, methanol constant volume is to 100ml, HPLC method after concentrated by rotary evaporation
Detection, the results are shown in Table 3.
Embodiment 6
Industrial hemp floral leaf is crushed to 40 mesh, 120 DEG C of freeze-day with constant temperature 3h optimize verifying, and under equal conditions, 3 groups of weights are arranged
Multiple, using untreated raw material as blank control (CK), each processing weighs 500g sample, accurately weighs 20g sample, adds 10 times
The methanol ultrasonic extraction of volume 3 times, each 30min, filtrate is collected by filtration, methanol constant volume is to 100ml, HPLC method after concentrated by rotary evaporation
Detection, the results are shown in Table 3.
Influence of the pyrolytic conversion to raw material CBD content under 3 optimal conditions of table
From table 3 it can be seen that under the conditions of Optimal Parameters, convert CBD content in postindustrial cannabis leaf raw material it is average 2.6% ~
3.9%, hence it is evident that be higher than blank control, can be improved 2 ~ 3 times.
Above embodiments are only the explanations that makes an explanation to the present invention, do not carry out any limit to protection scope of the present invention
System.To those skilled in the art, all to exist without departing from same embodiment or change made by the technology of the present invention spirit
Within protection scope of the present invention.
Claims (6)
1. a kind of pre-treating method for improving industrial hemp CBD content and its optimization, which comprises the steps of:
The screening of step 1 conversion temperature
It takes a certain amount of industrial hemp raw material to crush and mixes spare, setting different temperatures gradient and blank control (CK), each
Test group weighs a certain amount of sample, and dry to take a certain amount of sample, methanol ultrasonic extraction after a certain period of time, HPLC method detects, according to
Detection data determines optimal conversion temperature range；
The screening of step 2 transformation time
Under the conditions of optimal conversion temperature range, sets different time gradient and blank control (CK), each test group weigh
A certain amount of sample, takes a certain amount of sample, methanol ultrasonic extraction after dry, the detection of HPLC method determines best dry according to detection data
Dry transformation time；
The optimization of step 3 conversion condition is verified
After optimal conversion temperature and time has been determined, with optimal conditions, setting repeats collimation test, to verify optimization
The reliability and stability of parameter；A certain amount of sample, methanol ultrasonic extraction are taken after drying, the detection of HPLC method determines best drying
The technological parameter of conversion.
2. a kind of pre-treating method for improving industrial hemp CBD content according to claim 1 and its optimization, feature exist
In the industrial hemp raw material includes: the combination of one or more of flower, leaf, stalk core, root, seed shell arbitrary proportion, excellent
Select floral leaf raw material.
3. a kind of pre-treating method for improving industrial hemp CBD content according to claim 1 and its optimization, feature exist
In,
(1) in the step 1, raw material is crushed to 10 ~ 40 mesh；
(2) in the step 1, test set temperature range is 90 DEG C ~ 160 DEG C, and gradient is 10 DEG C；
(3) in the step 1, the blank control is the sample without drying and processing；
(4) in the step 1, the drying time is 2 ~ 3h；
(5) in the step 1, the sample size of every group of test process is not less than 200g, and detection is not less than 10g with sample size；
(6) in the step 1, methanol usage is 10-20 times of sample size when extraction；
(7) in the step 1, ultrasound number at least 3 times when extraction, 10-30min/ times, ultrasonic power 3000-5000W, temperature
25-50℃。
4. a kind of pre-treating method for improving industrial hemp CBD content according to claim 1 and its optimization, feature exist
In,
(1) in the step 2, the sample and step 1 are sample after crushing with a batch；
(2) in the step 2, the optimum temperature range is 100 DEG C ~ 150 DEG C；
(3) in the step 2, the time gradient is 0.5h, 1h, 2h, 3h, 4h, 5h, 6h, 7h；
(4) in the step 2, the optimal conversion time range is 1h ~ 5h.
5. a kind of pre-treating method for improving industrial hemp CBD content according to claim 1 and its optimization, feature exist
In,
(1) in the step 3, the sample and above-mentioned steps are same batch sample；
(2) in the step 3, the optimal conversion technological parameter are as follows: 100 DEG C ~ 150 DEG C of temperature, time 1h ~ 5h；
(3) in the step 3, the repeat number is no less than 3 groups.
6. a kind of pre-treating method for improving industrial hemp CBD content according to claim 1 and its optimization, feature exist
In after pyrolytic conversion, CBD content can be improved 1 ~ 3 times in industrial hemp raw material, and average content is up to 1.7 ~ 3.9%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113332285A (en) * | 2021-07-26 | 2021-09-03 | 大理大学 | Application of BMS470539 in preparation of medicine for treating Alzheimer's disease |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113332285A (en) * | 2021-07-26 | 2021-09-03 | 大理大学 | Application of BMS470539 in preparation of medicine for treating Alzheimer's disease |
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Application publication date: 20191129 |