CN109134412A - A kind of dihydromyricetin cellulose crystal and preparation method thereof - Google Patents
A kind of dihydromyricetin cellulose crystal and preparation method thereof Download PDFInfo
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- CN109134412A CN109134412A CN201811393136.8A CN201811393136A CN109134412A CN 109134412 A CN109134412 A CN 109134412A CN 201811393136 A CN201811393136 A CN 201811393136A CN 109134412 A CN109134412 A CN 109134412A
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- dihydromyricetin
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/32—2,3-Dihydro derivatives, e.g. flavanones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/40—Separation, e.g. from natural material; Purification
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Abstract
A kind of dihydromyricetin cellulose crystal and preparation method thereof, belongs to Separation of Organic Compounds field.Dihydromyricetin cellulose crystal provided by the invention is indicated with 2 θ angles and interplanar distance, shows characteristic diffraction peak at 8.80,10.24,11.93,14.62,16.63,18.98,19.95,20.72,21.73,22.59,23.41,25.33,26.02,26.87,29.61,32.87 using the alpha-emitting X-ray powder diffraction collection of Cu-K.The present invention also provides the preparation methods of above-mentioned dihydromyricetin cellulose crystal, and preparation process flow is simple, and production cost is low, and organic solvent is easily recycled, and can be used for a large amount of preparations of dihydromyricetin cellulose crystal.
Description
Technical field
The present invention relates to Separation of Organic Compounds fields, in particular to a kind of dihydromyricetin cellulose crystal and its preparation
Method.
Background technique
Vine tea is a kind of liana of Vitaceae Ampelopsis, and scientific name is ampelopsis grossdentata (Ampelopsis
Grossedentata (Hand-Mazz) W.T.Wang) be distributed mainly on China Yangtze river basin with the big portion in south, as Fujian Guangdong and Guangxi Provinces,
The ground such as Hubei And Hunan and southeastern Yunnan, young stem and leaf can be used as tea product and drink.Dihydromyricetin is that content is very high in vine tea
Flavonoids active material has the multiple efficacies such as anti-oxidant, removing free radical, antithrombotic, anti-inflammatory, antitumor, there is hypoglycemic, drop
The pharmacological actions such as blood lipid, blood pressure lowering, anti-oxidant, antithrombotic, bacteriostasis antibiosis can prevent and mitigate damage of the alcohol to liver, have
Apparent liver protection function.
Limit of the dihydromyricetin due to technology of preparing, production cost etc. of preparation is largely extracted from vine tea at present
System is difficult to reach 98% or more, does not meet the requirement of pharmaceutical developments or the product of technique in the purity for producing upper dihydromyricetin
Yield low production cost is high, it is difficult to apply in production.Therefore, the dihydromyricetin product relatively low to purity is using efficient
The crystallization technique method of low cost is further purified, the dihydromyricetin of preparation high-purity, high-quality, for improving two
Hydrogen myricetin value-added content of product and its application field of expansion are with important value and practical significance.
Summary of the invention
The purpose of the present invention is to provide a kind of new dihydromyricetin cellulose crystals.
Another object of the present invention is to provide the preparation methods of above-mentioned dihydromyricetin cellulose crystal, with process flow letter
The advantages of list, production cost is low, and organic solvent is easily recycled, the product purity and high income that produce.
The embodiment of the present invention is achieved in that
The present invention provides a kind of dihydromyricetin cellulose crystal, crystal is indicated with 2 θ angles and interplanar distance, uses Cu-
The X-ray powder diffraction collection of K α radiation 8.80,10.24,11.93,14.62,16.63,18.98,19.95,20.72,
21.73, characteristic diffraction peak is shown at 22.59,23.41,25.33,26.02,26.87,29.61,32.87.
The present invention also provides the preparation methods of above-mentioned dihydromyricetin cellulose crystal comprising following steps:
Dihydromyricetin crude product is dissolved in ethanol solution and is dissolved by heating, filtrate is obtained by filtration；
It concentrates filtrate to after ethyl alcohol mass percent is 5-10% using macroporous resin adsorption, macroreticular resin is cold
But to successively being washed using the ethanol solution that water and mass percent are 30-40% after 25-30 DEG C, then it is with mass percent
The ethanol solution washing macroreticular resin of 80-95% obtains eluent；
Eluent is concentrated, is crystallized, crystal is obtained by filtration, it is dry after washing.
In preferred embodiments of the present invention, the mass percentage of dihydromyricetin exists in above-mentioned dihydromyricetin crude product
70% or more.
In preferred embodiments of the present invention, when above-mentioned use macroreticular resin adsorbs filtrate, macroreticular resin is used
1-2h is adsorbed at 40-50 DEG C.
In preferred embodiments of the present invention, it is above-mentioned using water washing macroreticular resin when, use 2-3 times of macroreticular resin volume
Water washing 1-2 times.
In preferred embodiments of the present invention, after above-mentioned use water washing macroreticular resin, with 2-3 times of macroreticular resin volume
The ethanol solution that mass percent is 30-40% washs 1-2 times.
In preferred embodiments of the present invention, after above-mentioned use water and ethanol solution washing macroreticular resin, macroreticular resin is used
The ethanol solution that 2-3 times of volume of mass percent is 80-95% elutes 2-3 times.
In preferred embodiments of the present invention, the above-mentioned quality hundred that eluent is concentrated under reduced pressure into ethyl alcohol at 50-70 DEG C
Divide than being 10-20%, obtains concentrate, then naturally cool to concentrate and water after mixing by the volume ratio of 1:2-3
25-30 DEG C, it is cooled to 5-10 DEG C with the cooling rate of 10 DEG C/h, crystal is obtained by filtration after standing still for crystals 8-12h.
In preferred embodiments of the present invention, above-mentioned washing is will be dry after water washing 2-3 times of 20-30 DEG C of crystal.
In preferred embodiments of the present invention, above-mentioned drying is carried out under the conditions of 60-90 DEG C and vacuum decompression.
The beneficial effect of the embodiment of the present invention is: dihydromyricetin cellulose crystal provided in an embodiment of the present invention is with 2 θ angles and crystalline substance
What interplanar distance indicated, using the alpha-emitting X-ray powder diffraction collection of Cu-K 8.80,10.24,11.93,14.62,16.63,
18.98, show that feature is spread out at 19.95,20.72,21.73,22.59,23.41,25.33,26.02,26.87,29.61,32.87
Penetrate peak.The embodiment of the invention also provides the preparation methods of above-mentioned dihydromyricetin, including dihydromyricetin crude product is dissolved in second
Alcoholic solution simultaneously dissolves by heating, and filtrate is obtained by filtration；It concentrates filtrate to after ethanol content is 5-10% and uses macroreticular resin
Absorption is successively washed using the ethanol solution that water and mass percent are 30-40% after macroreticular resin is cooled to 25-30 DEG C,
Macroreticular resin, which is washed, with the ethanol solution that mass percent is 80-95% again obtains eluent；By eluent concentration, crystallization, mistake
Filter obtains crystal, dry after washing.The preparation method of the dihydromyricetin has process flow simple, and production cost is low, ethyl alcohol
Solvent is easily recycled.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Photo when Fig. 1 is dihydromyricetin crystallization in the absorb-elute concentrate of the preparation of the embodiment of the present invention 1；
Fig. 2 is the microscopic morphology photo of dihydromyricetin cellulose crystal prepared by the embodiment of the present invention 1；
Fig. 3 is the HPLC map of dihydromyricetin cellulose crystal prepared by the embodiment of the present invention 1；
Fig. 4 is the HPLC map of dihydromyricetin reference substance；
Fig. 5 is the X-ray diffracting spectrum of dihydromyricetin crystal powder.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
The preparation method of dihydromyricetin cellulose crystal provided in an embodiment of the present invention is specifically described below.
The embodiment of the invention provides a kind of dihydromyricetin, crystal is indicated with 2 θ angles and interplanar distance, is used
The alpha-emitting X-ray powder diffraction collection of Cu-K 8.80,10.24,11.93,14.62,16.63,18.98,19.95,
20.72, characteristic diffraction peak is shown at 21.73,22.59,23.41,25.33,26.02,26.87,29.61,32.87.
The embodiment of the invention also provides a kind of preparation methods of above-mentioned dihydromyricetin comprising following steps: by two
Hydrogen myricetin crude product is dissolved in ethanol solution and dissolves by heating, and filtrate is obtained by filtration；Concentrating filtrate to ethanol content is 5-
Macroporous resin adsorption is used after 10%, successively uses water after macroreticular resin is cooled to 25-30 DEG C and mass percent is 30-
40% ethanol solution washing, then wash macroreticular resin with the ethanol solution that mass percent is 80-95% and obtain eluent；It will
Eluent is concentrated, crystallizes, crystal is obtained by filtration, dry after washing.Wherein, in dihydromyricetin crude product dihydromyricetin quality
The mass percent of percentage composition dihydromyricetin in 70% or more, preferred dihydromyricetin crude product is 70-95%.
The preparation method of dihydromyricetin provided in an embodiment of the present invention is that dihydromyricetin crude product is dissolved in ethanol solution
And dissolve by heating, filtrate is obtained by filtration tentatively to remove the insoluble impurity in part, then concentrates filtrate to ethanol solution matter
Amount percentage is handled when being 5-10% using macroporous resin adsorption, is adsorbed onto the dihydromyricetin in filtrate on macroreticular resin,
And macroreticular resin removal impurity successively is washed with the ethanol solution that water and mass percent are 30-40%, finally use quality percentage
Macroreticular resin is washed than the ethanol solution for 80-95% and collects washing solution, is obtained the eluent of dihydromyricetin, will be eluted
Liquid is concentrated under reduced pressure, crystallizes, crystal is obtained by filtration, and washing and drying obtains dihydromyricetin finished product.
The preparation of dihydromyricetin cellulose crystal provided in an embodiment of the present invention is using the purifying of macroporous resin adsorption wash crystallization
Method, the method for more current aqueous solution repeated recrystallize can save mostly subcrystalline operation, and the solution single knot after removal of impurities
The dihydromyricetin of the available high-purity of crystalline substance, greatly simplifies process flow, while yield also with higher.The technique is not
Using toxic chemical reagent and basic agent, the molecular structure of dihydromyricetin, Environmental compatibility lover, alcoholic solvent are not destroyed
Recyclable to be recycled, less energy consumption, production cost is low, and process flow is simple, is suitble to the requirement of serialization large-scale production.
Wherein, it is preferable to use macroreticular resin adsorbs 1- at 40-50 DEG C when being adsorbed using macroreticular resin to filtrate
2h, is then cooled to 25-30 DEG C, this method can dihydromyricetin sufficiently in absorption filtrate, and use macroporous resin adsorption
The lower temperature of Shi Caiyong and change without violent pH, operating condition is mild, is conducive to point for keeping dihydromyricetin natural
Minor structure and bioactivity keep the quality of dihydromyricetin finished product.
In addition, first using the water washing macroreticular resin of 2-3 times of macroreticular resin volume, then with macropore tree when washing macroreticular resin
The alcoholic solution that the mass percent of 2-3 times of rouge volume is 30-40% washs 1-2 times, finally uses the matter of 2-3 times of macroreticular resin volume
The ethanol solution that amount percentage is 80-95% elutes dihydromyricetin from macroreticular resin, can will be in dihydromyricetin crude product
Other do not adsorb or impurity that adsorption capacity is weak efficiently separates, to greatly improve the purity of dihydromyricetin cellulose crystal.
In eluent condensing crystallizing, the mass percent that eluent is first concentrated under reduced pressure into ethyl alcohol at 50-70 DEG C is
5-10% obtains concentrate, and concentrate and water are then naturally cooled to 25-30 by the volume ratio of 1:0.5-1 after mixing
DEG C, it is cooled to 5-10 DEG C with the cooling rate of 10 DEG C/h, crystal is obtained by filtration after standing still for crystals 8-12h.Eluent condensing crystallizing
When, it is concentrated under reduced pressure recycles ethyl alcohol therein first, then adding water to stand at low temperature is precipitated dihydromyricetin crystallization, by subtracting
Pressure is concentrated and adds water low temperature crystallization technology, the concentration of dihydromyricetin and satiety concentration in adjustable concentrated mother liquor, to adjust
The crystallization rate for controlling dihydromyricetin realizes the regulation of crystallization process and crystal habit in range to a certain degree, obtains high-purity
The dihydromyricetin of degree crystallizes.
In preferred embodiments of the present invention, it will be separated by filtration after 20-30 DEG C of crystal water washing 2-3 times at 60-90 DEG C
It is dried under vacuum decompression environment, which is conducive to be dehydrated crystal sufficiently, is conducive to keep dihydromyricetin
Bioactivity and finished product quality.
Macroreticular resin of the present invention is using macroreticular resins such as existing conventional D-101, AB-8；Ethanol solution is equal
Refer to the aqueous solution of ethyl alcohol；Vacuum decompression, that is, negative pressure of vacuum.
Feature and performance of the invention are described in further detail below in conjunction with specific embodiment.
Embodiment 1
A kind of dihydromyricetin cellulose crystal is present embodiments provided, is prepared using preparation method below, specific work
Skill is as follows:
S11, by 30g mass percentage be 70% dihydromyricetin crude product and 1000ml mass percent concentration be
60% ethanol solution mixing, is heated to 60 DEG C of stirring and dissolvings, filtrate is then obtained by filtration while hot.
S12, filtered fluid is concentrated under reduced pressure at 60 DEG C when ethyl alcohol mass percent is 5% using D-101 macroreticular resin
It is adsorbed, macroreticular resin is cooled to 25 DEG C after heat preservation absorption 1.5h at 45 DEG C.
S13, with water washing macroreticular resin 1 time of 3 times of macroreticular resin volume, then with 2 times of macroreticular resin volume of quality hundred
Point than for 30% ethanol solution wash macroreticular resin 2 times, finally using 2 times of macroreticular resin mass percent be 95% second
Alcoholic solution washs macroreticular resin 2 times, collects washing solution and obtains eluent.
S14, eluent is concentrated under reduced pressure into the mass percentage content of ethyl alcohol at 60 DEG C is about 20%, is concentrated
Liquid, is added after the water of 3 times of its volume to mix slowly into concentrate and naturally cools to 25 DEG C, is cooled to 5 with the speed of 10 DEG C/h
DEG C, standing overnight is precipitated dihydromyricetin crystallization, as shown in Figure 1, crystal settling is collected by filtration.
S15, by crystal settling with 25 DEG C water washing 3 times, it is dry in 90 DEG C of reduced vacuums after filter paper filtering, obtain dihydro poplar
Syphilis, yield 80%.
Micro- sem observation is used to the dihydromyricetin that above-described embodiment 1 is prepared, as shown in Fig. 2, with dihydromyricetin
Plain standard items (mark purity >=98%, HPLC method) are control, are detected using HPLC, purity >=99%, HPLC map
As shown in Figure 3, Figure 4, in addition, the X-ray diffracting spectrum for the dihydromyricetin that embodiment 1 is prepared is as shown in Figure 5.
The wherein measurement chromatographic condition of HPLC: (Wuhan Sai Erfu science and technology is limited for LC-300 analytic type high performance liquid chromatograph
Company)；Chromatographic column: Thermo C18(4.6 × 250mm, 5 μm)；Column temperature: 28 DEG C；Mobile phase: -1% acetic acid of methanol (25:75)；
Flow velocity: 1mL/min；Detection wavelength: 294nm；Sample volume: 20 μ L.
Embodiment 2
A kind of dihydromyricetin is present embodiments provided, is the method system that dihydromyricetin is extracted using vine tea below
It is standby to obtain, the specific process is as follows:
S21, the dihydromyricetin crude product and 1000ml mass percentage that are 70% by 35g dihydromyricetin mass percentage
The ethanol solution that specific concentration is 70% mixes, and is heated to 70 DEG C of stirring and dissolvings, filtrate is then obtained by filtration while hot.
S22, filtered fluid is concentrated under reduced pressure at 70 DEG C when ethyl alcohol mass percent is 10% using D-101 macroreticular resin
It is adsorbed, macroreticular resin is cooled to 25 DEG C after heat preservation absorption 1h at 50 DEG C.
S23, with water washing macroreticular resin 1 time of 3 times of macroreticular resin volume, then with 2 times of macroreticular resin volume of quality hundred
Point than for 40% ethanol solution wash macroreticular resin 3 times, finally using 2 times of macroreticular resin mass percent be 90% second
Alcoholic solution washs macroreticular resin 2 times, collects washing solution and obtains eluent.
S24, eluent is concentrated under reduced pressure into the mass percentage content of ethyl alcohol at 70 DEG C is about 15%, into concentrate
It is added after the water of 2.5 times of its volume to mix slowly and naturally cools to 25 DEG C, be cooled to 5 DEG C with the speed of 10 DEG C/h, stand overnight
Dihydromyricetin crystallization is precipitated, crystal settling is collected by filtration.
S25, crystal settling is washed with water 2 times, it is dry in 85 DEG C of reduced vacuums after filter paper filtering, obtain dihydromyricetin
Element, yield 82%；
The dihydromyricetin that above-described embodiment 2 is prepared is detected using HPLC method, purity >=99%.
Embodiment 3
A kind of dihydromyricetin is present embodiments provided, is the method system that dihydromyricetin is extracted using vine tea below
It is standby to obtain, the specific process is as follows:
S31, the dihydromyricetin crude product and 1000ml mass percentage that are 70% by 40g dihydromyricetin mass percentage
The ethanol solution that specific concentration is 80% mixes, and is heated to 80 DEG C of stirring and dissolvings, filtrate is then obtained by filtration while hot.
S32, filtrate is concentrated under reduced pressure at 70 DEG C ethyl alcohol mass percent be 10% when using D-101 macroreticular resin into
Macroreticular resin is cooled to 25 DEG C after heat preservation absorption 1h at 50 DEG C by row absorption.
S33, with water washing macroreticular resin 2 times of 2 times of macroreticular resin volume, then with 2 times of macroreticular resin volume of quality hundred
Point than for 40% ethanol solution wash macroreticular resin 2 times, finally using 3 times of macroreticular resin mass percent be 80% second
Alcoholic solution washs macroreticular resin 3 times, collects washing solution and obtains eluent.
S34, by 65 DEG C of mass percentage contents for being concentrated under reduced pressure into ethyl alcohol of eluent it is about 10%, is added into concentrate
It is mixed slowly after the water of 2 times of its volume and naturally cools to 25 DEG C, be cooled to 5 DEG C with the cooling rate of 10 DEG C/h, standing overnight makes
Dihydromyricetin crystallization is precipitated, and then crystal settling is collected in screening.
S35, by crystal settling with appropriate water washing 3 times, it is dry in 80 DEG C of reduced vacuums after filter paper filtering, obtain dihydro poplar
Syphilis, yield 85%；
The dihydromyricetin that above-described embodiment 3 is prepared is detected using HPLC method, purity >=98%.
In conclusion the present invention provides a kind of preparation method of dihydromyricetin cellulose crystal, which can be effective
Removal dihydromyricetin crude product in impurity, significantly improve the purity of dihydromyricetin, its purity can be made to reach 98% or more,
The yield of dihydromyricetin is up to 80% or more simultaneously.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of dihydromyricetin cellulose crystal, which is characterized in that the dihydromyricetin cellulose crystal is indicated with 2 θ angles and interplanar distance
, using the alpha-emitting X-ray powder diffraction collection of Cu-K 8.80,10.24,11.93,14.62,16.63,18.98,
19.95, characteristic diffraction peak is shown at 20.72,21.73,22.59,23.41,25.33,26.02,26.87,29.61,32.87.
2. a kind of preparation method of dihydromyricetin cellulose crystal as described in claim 1, which is characterized in that it includes following step
It is rapid:
Dihydromyricetin crude product is dissolved in ethanol solution and is dissolved by heating, filtrate is obtained by filtration；
The filtrate decompression is concentrated into after ethyl alcohol mass percent is 5-10% using macroporous resin adsorption, by the macropore tree
Rouge is successively washed using the ethanol solution that water and mass percent are 30-40% after being cooled to 25-30 DEG C, then uses mass percent
Eluent is obtained for the ethanol solution washing macroreticular resin of 80-95%；
The eluent is concentrated, is crystallized, crystal is obtained by filtration, it is dry after washing.
3. the preparation method of dihydromyricetin cellulose crystal according to claim 2, which is characterized in that the dihydromyricetin is thick
The mass percentage of dihydromyricetin is 70% or more in product.
4. the preparation method of dihydromyricetin cellulose crystal according to claim 2, which is characterized in that using macroreticular resin to institute
When stating filtrate and being adsorbed, 1-2h is adsorbed at 40-50 DEG C using macroreticular resin.
5. the preparation method of dihydromyricetin cellulose crystal according to claim 2, which is characterized in that using big described in water washing
When the resin of hole, water washing 1-2 times of 2-3 times of macroreticular resin volume is used.
6. the preparation method of dihydromyricetin cellulose crystal according to claim 2, which is characterized in that using big described in water washing
After the resin of hole, washed 1-2 times with the ethanol solution that 2-3 times of mass percent of macroreticular resin volume is 30-40%.
7. the preparation method of dihydromyricetin cellulose crystal according to claim 2, which is characterized in that use water and ethanol solution
After washing the macroreticular resin, 2-3 is eluted with the ethanol solution that 2-3 times of mass percent of macroreticular resin volume is 80-95%
It is secondary.
8. the preparation method of dihydromyricetin cellulose crystal according to claim 2, which is characterized in that the eluent exists
The mass percent that ethyl alcohol is concentrated under reduced pressure at 50-70 DEG C is 10-20%, obtains concentrate, and concentrate and water are then pressed 1:
The volume ratio of 2-3 naturally cools to 25-30 DEG C after mixing, is cooled to 5-10 DEG C with the cooling rate of 10 DEG C/h, stands knot
Crystal is obtained by filtration after brilliant 8-12h.
9. the preparation method of dihydromyricetin cellulose crystal according to claim 2, which is characterized in that the washing is will be described
Crystal is dried afterwards with water washing 2-3 times of 20-30 DEG C.
10. the preparation method of dihydromyricetin cellulose crystal according to claim 2, which is characterized in that the drying is in 60-
It is carried out under the conditions of 90 DEG C and vacuum decompression.
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| CN110054606A (en) * | 2019-06-05 | 2019-07-26 | 闽江学院 | A kind of dihydromyricetin-Halomine pharmaceutical co-crystals and preparation method |
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| CN101007797A (en) * | 2007-01-12 | 2007-08-01 | 广东药学院 | Method for extracting dihydromyricetin from Japanese raisin tree seed |
| CN104876903A (en) * | 2014-02-27 | 2015-09-02 | 天津药物研究院有限公司 | Crystallization form of dihydromyricetin, preparation method thereof and pharmaceutical composition containing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110054606A (en) * | 2019-06-05 | 2019-07-26 | 闽江学院 | A kind of dihydromyricetin-Halomine pharmaceutical co-crystals and preparation method |
| CN110054606B (en) * | 2019-06-05 | 2021-04-27 | 闽江学院 | Dihydromyricetin-berberine hydrochloride pharmaceutical co-crystal and preparation method thereof |
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Application publication date: 20190104 |