CN104523767A - Method for extracting flavones substances in cacumen biotae - Google Patents
Method for extracting flavones substances in cacumen biotae Download PDFInfo
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- CN104523767A CN104523767A CN201410785394.6A CN201410785394A CN104523767A CN 104523767 A CN104523767 A CN 104523767A CN 201410785394 A CN201410785394 A CN 201410785394A CN 104523767 A CN104523767 A CN 104523767A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/13—Coniferophyta (gymnosperms)
- A61K36/14—Cupressaceae (Cypress family), e.g. juniper or cypress
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Abstract
The invention provides a method for extracting flavones substances in cacumen biotae. The method comprises the following steps: cleaning cacumen biotae, drying and crushing the cacumen biotae to obtain cacumen biotae powder; then, adding water to uniformly mix with the cacumen biotae powder to obtain a mixed solution; freezing the mixed solution for 10-24 hours at a temperature of (-)40 DEG C to (-)20 DEG C, and putting the frozen mixed solution at the room temperature until the frozen mixed solution is molten; repeating the freezing step and room-temperature melting step for 2-3 times; adding alcohol to sufficiently mix, performing ultrasonic extraction after soaking for 1-3 hours, centrifugally separating, getting liquid supernatant, and freeze-drying, thereby obtaining a crude product; preparing the crude product into a solution with concentration of 1-3mg/mL, dropwise adding the solution into a macroporous resin column and then performing saturation adsorption, washing and removing with water after the adsorption, taking 60-80% alcohol as an eluent, recycling a solvent from the eluate, concentrating the eluate, and finally performing freeze-drying to obtain flavones substances. The method disclosed by the invention is high in extracting rate, pollution-free and low in cost.
Description
Technical field
The present invention relates to a kind of extracting method of Flavonoid substances, be specifically related to a kind of method extracting Flavonoid substances from Cacumen Platycladi.
Background technology
In recent years, due to the progress of free radical life sciences, the Flavonoid substances making to have very strong antioxidation and elimination Free Radical is subject to unprecedented attention.Its antioxidation is stronger than VE 50 times, stronger than VC 20 times, and arrives brain by blood brain barrier, the disease of control central nervous system, especially remarkable especially to the maintenance of skin, rejuvenation and blood vessel antiinflammatory action.At present, from Folium Ginkgo, Folium Perillae, cypress leaf, Flos Sophorae, Tonnae Sinensis tender leaf, flavone compound report is extracted more.But it is actually rare to extract Flavonoid substances from Cacumen Platycladi.
Cacumen Platycladi is the tender branch tip and leaf of drying of Cacumen Platycladi, containing multiple active skull cap components such as flavonoid, tannin, quintessence oils, have effect of cooling blood for hemostasis, preventing phlegm from forming and stopping coughing, wet down of dispeling the wind, growing and blacking hair, Sweeling-eliminating medicine powder poison, in Cacumen Platycladi, Flavonoid substances is one of its most important composition.Thus, in Cacumen Platycladi, the extraction of flavone compound has very important impact for the development of Food Science and medical science.
The extracting method being applied to Cacumen Platycladi Flavonoid substances at present mainly contains: organic solvent extractionprocess, enzyme extraction method, ultrasonic extraction, microwave loss mechanisms.Wherein, organic solvent extraction is the method the most widely adopted both at home and abroad, but this method cycle is long, step is many, productive rate is low, and has the residual of organic solvent in product, has impact to product quality after extraction; Enzyme extraction method must keep optimum temperature, optimal pH, higher to the condition control overflow of whole reaction; Ultrasonic wave extraction improves extraction efficiency greatly, shortens extraction time, saves solvent, and eliminates the destruction of high temperature to extract component, but during a large amount of extraction, efficiency is low; Microwave loss mechanisms, many advantages such as to have fast, solvent load is few, extraction ratio is high, cost is low and quality is good, but the composition of its finished product is not highly stable; Obviously, deficiency and the limitation which kind of extractive technique all has self, and this invention adopts freeze thawing and ultrasonic technology combined extracting, the feature of freeze-thaw technology is: cell can forming ice pellets and increase residue cytosol salinity while, occur swelling, broken, make Flavonoid substances be able to abundant release, and keep active.This technology is a kind of extracting method of efficient, environmental protection.Yet there are no the report that application freeze-thaw technology extracts Cacumen Platycladi Flavonoid substances.Experiment proves to adopt freeze thawing and ultrasonic technology combined extracting efficiently and environmental protection.
Summary of the invention
Goal of the invention: for the weak point of the extracting method of above-mentioned Flavonoid substances, the invention provides a kind of extracting method of efficient, environmental protection.
Technical scheme: this method is carried out according to the following steps:
(1) Cacumen Platycladi cleaned, dry, pulverize, cross 40 mesh sieves, obtain Cacumen Platycladi powder, then add water, Homogeneous phase mixing; The water added and the mass ratio of Cacumen Platycladi are about 5:1.
(2) mixed liquor step (1) obtained at the temperature of-40 ~-20 DEG C freezing 10 ~ 24 hours, ambient temperatare is put until it melts; Repeat freezing-thawing step 2 ~ 3 times; So, cell can, at formation ice pellets with while increasing residue cytosol salinity, occur swelling, broken.Make Flavonoid substances be able to abundant release, and keep active.
(3) in step (2) gained mixed liquor, add ethanol fully to mix, the volume ratio of ethanol and mixed liquor is about 1:1, and after soaking 1 ~ 3h, carry out ultrasonic extraction, ultrasonic power is 60 ~ 100W; Ultrasonic temperature is 40 ~ 80 DEG C; Ultrasonic time is 20 ~ 60min; The destruction of ultrasonic cavitation cell membrane contributes to release and the stripping of flavone compound, and ultrasound wave makes extracting solution constantly shake, and contributes to solutes accumulation.Therefore, supercritical ultrasonics technology substantially reduces extraction time, improves the extraction rate of effective ingredient, the utilization rate of raw material.Carry out centrifugalize after ultrasonic end, get supernatant, lyophilizing, obtain crude product.
(4) crude product is mixed with the solution that concentration is 1 ~ 3mg/mL, be added drop-wise in macroporous resin column and carry out saturated adsorption, removing impurity is washed with water after absorption, use 60 ~ 80% ethanol as eluant again, recycling design and concentration are carried out to eluant, finally carry out lyophilizing, namely obtain Flavonoid substances.Described macroporous resin is D-101, AB-8 or DM-130.The dripping quantity of described solution is 1.5 times of column volume; The consumption of water and ethanol is 5 times of column volume.
Further, we find, if after step (2) terminates, gained mixed liquor is again freezing, melt under being then placed in ultrasound environments, ultrasonic power is 60 ~ 100W; Ultrasonic time is 60 ~ 90min, and because hyperacoustic heat effect makes water temperature increase, have water-bath effect to raw material, temperature is increased to 35 ~ 40 DEG C naturally, not only makes mixed liquor fast melt, and can promote release and the stripping of flavone compound.After melting under ultrasound environments, carrying out step (3), (4), the product extraction ratio that the method obtains improves greatly, measures Cacumen Platycladi Flavonoid substances extraction ratio and is up to 18.2%.
Beneficial effect: the present invention has following characteristics: integrated artistic simplicity of design is reasonable, creationaryly combines multiple technologies, compensate for the deficiency of monotechnics, substantially increases the extraction ratio of Flavonoid substances; Due to the particularity of Cacumen Platycladi, in leaching process of the present invention, maintain relatively low temperature, well maintain the activity of Cacumen Platycladi Flavonoid substances, make product highly stable; Solvent load of the present invention little and be easy to reclaim, cost-saving; Only used water and ethanol two kinds of solvents in leaching process, do not introduce other solvent such as chloroform, ethyl acetate, environmentally safe; These features have met the requirement of suitability for industrialized production all largely.
Detailed description of the invention:
Below by way of specific embodiment, the present invention is further described:
Embodiment 1
Get fresh Cacumen Platycladi, weigh, clean, after naturally drying in the shade in baking oven 60 DEG C oven dry as raw material; Be crushed to 40 orders, obtain Cacumen Platycladi powder; Precise 20g Cacumen Platycladi powder, adds 100mL water, makes Cacumen Platycladi mixed liquor; Cacumen Platycladi mixed liquor is carried out freezing at-20 DEG C, takes out room temperature after 24h and melt, three times so repeatedly; Add dehydrated alcohol 100mL, fully mix, after soaking 2h, carry out ultrasonic extraction: ultrasonic power 60W; Ultrasonic time 20min; Ultrasonic temperature 40 DEG C; Centrifugalize, gets supernatant.Supernatant is positioned in freeze dryer and carries out frozen dried, obtain crude product; Be the solution of 1mg/mL by accurate for crude product compound concentration, be added drop-wise in AB-8 macroporous resin column and carry out saturated adsorption, maximum applied sample amount is 1.5 times of column volumes, first with the water elution removing impurity of 5 times of column volumes, use 60% ethanol elution of 5 times of column volumes again, collect eluent, concentrated, lyophilizing, obtain Cacumen Platycladi Flavonoid substances sample 2.42g.
Measure: adopt ultraviolet spectrophotometry, using rutin as standard reference material, draw rutin standard curve, measure the content of Cacumen Platycladi Flavonoid substances.
(1) drafting of standard curve
Accurately take rutin standard substance 1.0mg, be settled to 25.0mL with the ethanol that concentration is 50%.
Accurate absorption rutin standard substance (48 μ g/mL) 0.5,1.0,2.0,3.0,4.0,5.0mL is in 6 color comparison tubes, use the ethanol of 50% to 5.0mL respectively, 0.1M aluminum trichloride solution 3.0mL and 1M liquor kalii acetici 5.0mL, shakes up, is made in the same way of blank; Place 40min, question response is complete, measures absorbance in 415nm wavelength place.With rutin standard concentration (C) for abscissa, absorbance (A) is vertical coordinate drawing standard curve.
(2) mensuration of Cacumen Platycladi Flavonoid substances extraction ratio
Extraction ratio Y%=m
1/ m
2× 100%
In formula: m
1for obtaining the quality (g) of Cacumen Platycladi Flavonoid substances sample;
M
2for using the quality (g) of Cacumen Platycladi powder.
(3) mensuration of Flavonoid substances content in Cacumen Platycladi extract
Take 5mg extract and be placed in 25mL volumetric flask, by above-mentioned rutin standard curve method for drafting obtain solution, and survey its absorbance.The Flavonoid substances content in extract is calculated by standard curve.
Content P%=CVD × 10
-3/ m × 100%
In formula: C is the Flavonoid substances concentration (mg/mL) of the test solution to be measured calculated by standard curve;
V is testing sample solution cumulative volume (mL);
D is the extension rate of test solution to be measured;
M is the extract quality (mg) taken.
According to above-mentioned formula, obtaining Cacumen Platycladi Flavonoid substances extraction ratio is 12.1%, and in extract, Flavonoid substances content is 82.0%;
Adopt general extraction methods (without freezing-melt process, do not have ultrasonic assistant, other condition the same) acquired results is: Flavonoid substances extraction ratio is 3.6%, and in extract, Flavonoid substances content is 29.3%; Visible, the present invention adopts freeze thawing and ultrasonic combined technology to extract Cacumen Platycladi Flavonoid substances, can obtain that extraction ratio is high, Functionality, quality and appealing design and free of contamination product.
Embodiment 2
Precise 20g Cacumen Platycladi powder, adds 100mL water, makes Cacumen Platycladi mixed liquor; Cacumen Platycladi mixed liquor is carried out freezing at-40 DEG C, takes out room temperature after 10h and melt, three times so repeatedly; Add dehydrated alcohol 100mL, fully mix, after soaking 2h, carry out ultrasonic extraction: ultrasonic power 80W; Ultrasonic time 40min; Ultrasonic temperature 60 DEG C; Centrifugalize, gets supernatant.Supernatant is positioned in freeze dryer and carries out frozen dried, obtain crude product; Be the solution of 2mg/mL by accurate for crude product compound concentration, be added drop-wise in D-101 macroporous resin column and carry out saturated adsorption, maximum applied sample amount is 1.5 times of column volumes, first with the water elution removing impurity of 5 times of column volumes, use 70% ethanol elution of 5 times of column volumes again, collect eluent, concentrated, lyophilizing, obtain Cacumen Platycladi Flavonoid substances sample 2.74g.
Assay method is with embodiment 1: measuring Cacumen Platycladi Flavonoid substances extraction ratio is 13.7%, and in extract, Flavonoid substances content is 83.7%.
Adopt general extraction methods (without freezing-melt process, do not have ultrasonic assistant, other condition the same) acquired results is: Flavonoid substances extraction ratio is 3.8%, and in extract, Flavonoid substances content is 28.1%;
Embodiment 3
Precise 20g Cacumen Platycladi powder, adds 100mL water, makes Cacumen Platycladi mixed liquor; Cacumen Platycladi mixed liquor is carried out freezing at-20 DEG C, takes out room temperature after 24h and melt, three times so repeatedly; Add dehydrated alcohol 100mL, fully mix, after soaking 3h, carry out ultrasonic extraction: ultrasonic power 100W; Ultrasonic time 60min; Ultrasonic temperature 80 DEG C; Centrifugalize, gets supernatant.Supernatant is positioned in freeze dryer and carries out frozen dried, obtain crude product; Be the solution of 3mg/mL by accurate for crude product compound concentration, be added drop-wise in D-130 macroporous resin column and carry out saturated adsorption, maximum applied sample amount is 1.5 times of column volumes, first with the water elution removing impurity of 5 times of column volumes, use 80% ethanol elution of 5 times of column volumes again, collect eluent, concentrated, lyophilizing, obtain Cacumen Platycladi Flavonoid substances sample 2.88g.
Assay method is with embodiment 1: measuring Cacumen Platycladi Flavonoid substances extraction ratio is 14.4%, and in extract, Flavonoid substances content is 80.5%;
Adopt general extraction methods (without freezing-melt process, do not have ultrasonic assistant, other condition the same) acquired results is: Flavonoid substances extraction ratio is 3.9%, and in extract, Flavonoid substances content is 26.5%.
Embodiment 4
Precise 20g Cacumen Platycladi powder, adds 100mL water, makes Cacumen Platycladi mixed liquor; Cacumen Platycladi mixed liquor is carried out freezing at-20 DEG C, takes out room temperature after 24h and melt, three times so repeatedly; Add dehydrated alcohol 100mL, fully mix, after soaking 2h, carry out ultrasonic extraction: ultrasonic power 100W; Ultrasonic time 40min; Ultrasonic temperature 70 DEG C; Centrifugalize, gets supernatant.Supernatant is positioned in freeze dryer and carries out frozen dried, obtain crude product; Be the solution of 3mg/mL by accurate for crude product compound concentration, be added drop-wise in D-101 macroporous resin column and carry out saturated adsorption, maximum applied sample amount is 1.5 times of column volumes, first with the water elution removing impurity of 5 times of column volumes, use 80% ethanol elution of 5 times of column volumes again, collect eluent, concentrated, lyophilizing, obtain Cacumen Platycladi Flavonoid substances sample 2.96g.
Assay method is with embodiment 1: measuring Cacumen Platycladi Flavonoid substances extraction ratio is 14.8%, and in extract, Flavonoid substances content is 84.7%;
Adopt general extraction methods (without freezing-melt process, do not have ultrasonic assistant, other condition the same) acquired results is: Flavonoid substances extraction ratio is 4.1%, and in extract, Flavonoid substances content is 30.2%;
Flavonoid substances is compared with general extraction methods to utilize method of the present invention to extract in Cacumen Platycladi, and result of the test sees the following form:
Table 1
This invention takes as can be seen from Table 1 freezing-to melt and the technology of ultrasonic assistant extracts Flavonoid substances, in gained Cacumen Platycladi Flavonoid substances extraction ratio and extract, Flavonoid substances content is all far longer than general extraction methods.Extraction ratio about 14%, and product is stablized, in extract, Flavonoid substances content is greater than 80%.
Further, we have studied hyperacoustic application in freezing-melting process.Specific embodiment is as follows:
Embodiment 5
Precise 20g Cacumen Platycladi powder, adds 100mL water, makes Cacumen Platycladi mixed liquor; Cacumen Platycladi mixed liquor is carried out freezing at-20 DEG C, takes out room temperature after 24h and melt, three times so repeatedly; Water liquid is positioned in freeze dryer and carries out frozen dried, obtains crude product; Be the solution of 3mg/mL by accurate for crude product compound concentration, be added drop-wise in D-101 macroporous resin column and carry out saturated adsorption, maximum applied sample amount is 1.5 times of column volumes, first with the water elution removing impurity of 5 times of column volumes, use 80% ethanol elution of 5 times of column volumes again, collect eluent, concentrated, lyophilizing, obtain Cacumen Platycladi Flavonoid substances sample 1.16g.
Assay method is with embodiment 1: Cacumen Platycladi Flavonoid substances extraction ratio 5.8%, and in extract, Flavonoid substances content is 83.9%;
Embodiment 5-1
Precise 20g Cacumen Platycladi powder, adds 100mL water, makes Cacumen Platycladi mixed liquor; Cacumen Platycladi mixed liquor is carried out freezing at-20 DEG C, takes out room temperature after 24h and melt, secondary so repeatedly; And then carrying out freezing at-20 DEG C, take out after 24h and melt under ultrasound environments, due to ultrasonic heat effect, temperature is increased to 35 DEG C naturally, and after about 80min melts, water liquid is positioned in freeze dryer and carries out frozen dried, obtains crude product; Be the solution of 3mg/mL by accurate for crude product compound concentration, be added drop-wise in D-101 macroporous resin column and carry out saturated adsorption, maximum applied sample amount is 1.5 times of column volumes, first with the water elution removing impurity of 5 times of column volumes, use 80% ethanol elution of 5 times of column volumes again, collect eluent, concentrated, lyophilizing, obtain Cacumen Platycladi Flavonoid substances sample 2.38g.
Assay method is with embodiment 1: Cacumen Platycladi Flavonoid substances extraction ratio 11.9%, and in extract, Flavonoid substances content is 84.1%;
Embodiment 4-1
Precise 20g Cacumen Platycladi powder, adds 100mL water, makes Cacumen Platycladi mixed liquor; Cacumen Platycladi mixed liquor is carried out freezing at-20 DEG C, takes out room temperature after 24h and melt, secondary so repeatedly; And then carry out freezing at-20 DEG C, take out after 24h and melt under ultrasound environments, due to ultrasonic heat effect, temperature is increased to 36 DEG C naturally, and about 80min adds dehydrated alcohol 100mL after melting, abundant mixing, after soaking 2h, carries out ultrasonic extraction: ultrasonic power 100W; Ultrasonic time 40min; Ultrasonic temperature 70 DEG C; Centrifugalize, gets supernatant.Residue is carried out process 1 time as stated above, merges supernatant; Supernatant is positioned in freeze dryer and carries out frozen dried, obtain crude product; Be the solution of 3mg/mL by accurate for crude product compound concentration, be added drop-wise in D-101 macroporous resin column and carry out saturated adsorption, maximum applied sample amount is 1.5 times of column volumes, first with the water elution removing impurity of 5 times of column volumes, use 80% ethanol elution of 5 times of column volumes again, collect eluent, concentrated, lyophilizing, obtain Cacumen Platycladi Flavonoid substances sample 3.64g.
Assay method is with embodiment 1: measuring Cacumen Platycladi Flavonoid substances extraction ratio is 18.2%, and in extract, Flavonoid substances content is 84.3%.
Result of the test sees the following form:
Table 2
As seen from Table 2 in freezing-melting process, melt under ultrasound environments, effectively can improve the extraction ratio of Cacumen Platycladi Flavonoid substances.This is because melt under ultrasonic environment, because hyperacoustic heat effect makes water temperature substantially maintain 35 ~ 40 DEG C, make mixed liquor fast melt, its cavitation can promote release and the stripping of flavone compound simultaneously, improves the extraction ratio of Cacumen Platycladi Flavonoid substances.
Claims (9)
1. extract a method for Flavonoid substances in Cacumen Platycladi, it is characterized in that carrying out according to the following steps:
(1) cleaned by Cacumen Platycladi, dry rear pulverizing, obtain Cacumen Platycladi powder, then add water, Homogeneous phase mixing obtains mixed liquor;
(2) by mixed liquor at the temperature of-40 ~-20 DEG C freezing 10 ~ 24 hours, ambient temperatare is put until it melts; Repeat freezing-room temperature thawing step 2 ~ 3 times;
(3) in step (2) gained mixed liquor, add ethanol fully to mix, after soaking 1 ~ 3h, carry out ultrasonic extraction, centrifugalize, get supernatant, lyophilizing, obtain crude product;
(4) crude product is mixed with the solution that concentration is 1 ~ 3mg/mL, be added drop-wise in macroporous resin column and carry out saturated adsorption, removing impurity is washed with water after absorption, use 60 ~ 80% ethanol as eluant again, recycling design and concentration are carried out to eluant, finally carry out lyophilizing, namely obtain Flavonoid substances.
2. the method for claim 1, is characterized in that the mass ratio of water and Cacumen Platycladi is 5:1.
3. the method for claim 1, is characterized in that the volume ratio 1:1 of ethanol and mixed liquor.
4. the method for claim 1, is characterized in that being the mixed liquor of gained in step (2) after freezing 10 ~ 24 hours, to be placed in ultrasound wave and to melt, then carry out step (3) at the temperature of-40 ~-20 DEG C.
5. the method for claim 1, is characterized in that in supersound extraction process, and ultrasonic power is 60 ~ 100W; Ultrasonic time is 20 ~ 60min; Ultrasonic temperature is 40 ~ 80 DEG C.
6. method as claimed in claim 4, it is characterized in that in supersound extraction process, ultrasonic power is 60 ~ 100W; Ultrasonic time is 69 ~ 90min.
7. the method for claim 1, is characterized in that described macroporous resin is D-101, AB-8 or DM-130.
8. the method for claim 1, is characterized in that the dripping quantity of described solution is 1.5 times of column volume; The consumption of water and ethanol is 5 times of column volume.
9. extract a method for Flavonoid substances in Cacumen Platycladi, it is characterized in that carrying out according to the following steps:
Cleaned by Cacumen Platycladi, dry rear pulverizing, obtain Cacumen Platycladi powder, then add water, Homogeneous phase mixing obtains mixed liquor; By mixed liquor at the temperature of-40 ~-20 DEG C freezing 10 ~ 24 hours, ambient temperatare was put until it melts; Repeat freezing-room temperature thawing step secondary; Again freezing, be placed in ultrasound wave and melt, after thawing, lyophilizing, obtains crude product; Crude product is mixed with the solution that concentration is 1 ~ 3mg/mL, is added drop-wise in macroporous resin column and carries out saturated adsorption, after absorption, wash removing impurity with water, use 60 ~ 80% ethanol as eluant again, recycling design and concentration are carried out to eluant, finally carries out lyophilizing, namely obtain Flavonoid substances.
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| CN105055463B (en) * | 2015-07-28 | 2019-04-09 | 华南理工大学 | One kind having active cacumen biotae polyphenol of anti-trioxypurine and its preparation method and application |
| CN105267299A (en) * | 2015-09-22 | 2016-01-27 | 盐城工学院 | Perilla flavone and perilla flavone derivative extraction method |
| CN105581943A (en) * | 2016-01-05 | 2016-05-18 | 南京科技职业学院 | Application of Chinese Arborvitae twig extract in shampoo |
| CN105640827A (en) * | 2016-01-05 | 2016-06-08 | 南京科技职业学院 | Method for preparing shampoo by adopting simple physical means |
| CN107595900A (en) * | 2017-08-18 | 2018-01-19 | 合肥丰洁生物科技有限公司 | A kind of extracting method of Thuja extract |
| CN110680776A (en) * | 2018-07-05 | 2020-01-14 | 伽蓝（集团）股份有限公司 | Application of arborvitae |
| CN114470012A (en) * | 2022-02-08 | 2022-05-13 | 上海章华保健化妆品有限公司 | Extraction method and application of cacumen biotae extract |
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