CN105646515A - Preparation method of parthenolide - Google Patents
Preparation method of parthenolide Download PDFInfo
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- CN105646515A CN105646515A CN201510998196.2A CN201510998196A CN105646515A CN 105646515 A CN105646515 A CN 105646515A CN 201510998196 A CN201510998196 A CN 201510998196A CN 105646515 A CN105646515 A CN 105646515A
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- feverfew
- medicinal extract
- ethyl acetate
- organic solvent
- methylene dichloride
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/04—Ortho-condensed systems
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- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
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Abstract
The invention provides a preparation method of parthenolide. The method comprises the following steps: adding water to crushed feverfew to wet the crushed feverfew, and extracting the wetted feverfew with an organic solvent to obtain an extract liquid; concentrating the obtained extract liquid, and disposing the obtained concentrate to obtain an extract paste; dissolving the obtained extract paste in ethanol, and filtering the obtained solution; and adding an adsorbent to the obtained filtrate, decolorizing the filtrate, filtering the obtained solution, dissolving the filtered filter cake in an organic solvent, concentrating the dissolved filter cake, and drying the obtained concentrate to obtain parthenolide. The method has the advantages of simplicity, low production cost, easy industrial production, and high content reaching 50%.
Description
Technical field
The invention belongs to feverfew extraction and isolation field, it relates to the preparation method of a kind of feverfew lactone, it is specifically related to a kind of method extracting feverfew lactone from feverfew.
Background technology
Feverfew lactone is extraction and isolation Sesquiterpene compound out from feverfew raw material, it can extensively be sent out and be used for the treatment of multiple inflammatory diseases, comprise heating, migraine and sacroiliitis etc., its action temperature and, untoward reaction is little, also find that feverfew lactone also has antitumor, atherosclerosis, the multiple pharmacologically active such as antiviral in recent years, become one of focus of natural product in the world.
Namely application number 201010168478.7, by raw material of southern magnolia root skin after solvent extraction extracts, through column chromatography for separation, after collecting required composition, then obtain feverfew lactone with appropriate solvent crystallization.
Application number 201310400236.X, is specifically related to take Costunolide as raw material, obtains feverfew lactone through synthesis.
Application number 201310441944.8, first dries naturally by the plant material leaf collected, and pulverizing, screening obtain leaf powder, carbon dioxide upercritical fluid extraction, and silica gel separation obtains the feverfew internal ester monomer of more than 99%.
Application number 201110187388.7, gets mountain yulan or purple yulan, Flos micheliae Albae dry root skin, pulverizes into powder, 95% extraction using alcohol, medicinal extract with 20% dissolve with ethanol, then the color being extracted with ethyl acetate to extraction liquid becomes light, merges organic solvent, silicagel column separation.
Application number 200710099763.6 is taking yulan leaf or spends as raw material, pulverizes, and through solvent extraction, non-polar organic solvent obtains yulan total lactones after extracting, and yulan total lactones through column chromatography shunting, namely obtains extract of the present invention after composition needed for collecting again.
Application number 200710117745.6, yulan leaf or flower, after water soaking, adopt extraction using alcohol, and the extraction of low polar organic solvent can obtain thick lactone, and thick lactone can obtain extract of the present invention again after silica gel column chromatography is separated.
The separation of feverfew lactone mainly being obtained by extraction, extraction, silicagel column separation at present, its operational path is complicated, cost height.
Summary of the invention
Problem to be solved by this invention is to provide the preparation method of the feverfew lactone that a kind of operational path is simple and content is high.
The technical scheme solved the problem: the preparation method of the feverfew lactone provided, comprises the following steps:
Step 1 is extracted
In the European feverfew after pulverizing, add water soak, adopt organic solvent extraction, obtain extracting solution;
Described organic solvent is any one or multiple mixing in methyl alcohol, ethanol, acetone, ethyl acetate, methylene dichloride, sherwood oil;
Step 2 concentrates
The extracting solution of step 1 gained is concentrated, places, obtain medicinal extract;
Prepared by step 3
By the medicinal extract dissolve with ethanol of step 2 gained, filter; Then in filtrate, add sorbent material carry out desolventing technology, filter, get the filter cake organic solvent dissolution after filtration, concentrated, dry, obtain feverfew lactone products;
Described sorbent material is any one or multiple mixing in gac, aluminum oxide, silica gel, starch; Described organic solvent is the mixing of any one or two kinds in ethyl acetate, methylene dichloride.
Above-mentioned steps 1 is specifically: the wetting 0.5-24h of water adding 0.1-1 times amount in the European feverfew after pulverizing, when 10-60 DEG C, adopts organic solvent extraction 1-3 time, obtain extracting solution; Described organic solvent is any one or multiple mixing in methyl alcohol, ethanol, acetone, ethyl acetate, methylene dichloride, sherwood oil.
Above-mentioned steps 1 is: the wetting 1h of water adding 0.8 times amount in the European feverfew after pulverizing, when 10-60 DEG C, adopts the mixed solvent of ethyl acetate and methylene dichloride to extract 1-3 time, obtains extracting solution; The volume ratio of described ethyl acetate and methylene dichloride is 19:1.
Above-mentioned steps 2 is specifically: under temperature is 20-60 DEG C of condition, and being concentrated by the extracting solution of step 1 gained to proportion is 1.08-1.20, places, obtains medicinal extract.
In above-mentioned steps 2, best thickening temperature is 45 DEG C.
Above-mentioned steps 3 is specifically: is the dissolve with ethanol 1 time of 95% by the mass concentration of the medicinal extract 0.5-6 times of medicinal extract quality of step 2 gained, dissolves 0.5-3h, filter; When 30-70 DEG C, the sorbent material adding medicinal extract quality 1%-10% in filtrate carries out desolventing technology, filters, gets the filter cake organic solvent dissolution after filtration, concentrated, dry, obtains feverfew lactone products; Described sorbent material is any one or multiple mixing in gac, aluminum oxide, silica gel, starch; Described organic solvent is the mixing of any one or two kinds in ethyl acetate, methylene dichloride.
Above-mentioned steps 3 is: being the dissolve with ethanol 1 time of 95% by the mass concentration of 2 times of medicinal extract quality by the medicinal extract of step 2 gained, dissolution time is 1.2h, filters; When 50 DEG C, in filtrate, add gac and the starch mixture decolouring 30min of medicinal extract quality 5%, filter, get the filter cake ethyl acetate after filtration and the dissolving of methylene dichloride mixed solution, concentrated, dry, obtain feverfew lactone products; The mass ratio of described gac and starch is 8:2, and the volume ratio of described ethyl acetate and methylene dichloride is 5:8.
The advantage of the present invention:
Technique of the present invention is simple, and production cost is low, easy suitability for industrialized production, content height, and content can reach 50%.
Embodiment
In order to the present invention is better described, measuring according to the feverfew lactone content in existing disclosed raw material southern magnolia root skin, leaf, flower and Europe of the present invention feverfew, its content is as follows:
| Sample | Feverfew lactone content % |
| Southern magnolia root skin No. 1 sample | 0.15 |
| Southern magnolia root skin No. 2 samples | 0.12 |
| Southern magnolia root skin No. 3 samples | 0.07 |
| Southern magnolia root skin No. 4 samples | 0.16 |
| Yulan leaf | 0.11 |
| Yulan Magnolia | 0.09 |
| Europe feverfew | 1.08 |
| Europe feverfew bar | 0.56 |
| Europe feverfew leaf | 0.90 |
| Domestic feverfew | 0 |
From the above results: Europe each position content of feverfew raw material is higher.
Embodiment 1:
1000kg shatter after European feverfew raw material, add the wetting 0.5h of water of material quantity 0.1 times of raw materials quality, adopt mass concentration to be 98% methanol extraction, Extracting temperature is 10 DEG C, and extraction time is 1 time. It is 1.08 that extracting solution concentrates to proportion, and thickening temperature is 60 DEG C.
Being dissolve above-mentioned medicinal extract 1 time under 95% ethanol room temperature by the mass concentration of 0.5 times of medicinal extract quality, dissolve 0.5h, filter, filtrate adds the gac of the 1% of medicinal extract quality, and when 30 DEG C, decolouring 30min, filters. The gained filter cake acetic acid ethyl dissolution of certain 0.1 times of filter cake quality, filters, and concentrate drying, the receipts rate of products obtained therefrom is 2.1%, and content is 42.1%.
Embodiment 2:
1000kg shatter after European feverfew raw material, add the wetting 24h of water of material quantity 1 times of raw materials quality, adopt mass concentration to be 98% extraction using alcohol, Extracting temperature is 60 DEG C, and extraction time is 3 times. Extracting solution merges, and concentrating to proportion is 1.15, and thickening temperature is 60 DEG C.
Being dissolve above-mentioned medicinal extract 1 time under 95% ethanol room temperature by the mass concentration of 6 times of medicinal extract quality, dissolve 3h, filter, filtrate adds the aluminum oxide of the 10% of medicinal extract quality, and when 70 DEG C, decolouring 30min, filters. The gained filter cake mixed solvent of the ethyl acetate of 0.5 times of filter cake quality and methylene dichloride dissolves, and the volume ratio of ethyl acetate and methylene dichloride is 3:1, filters, and concentrate drying, the receipts rate of products obtained therefrom is 2.3%, and content is 39.8%.
Embodiment 3:
1000kg shatter after European feverfew raw material, add the wetting 4h of water of material quantity 0.5 times of raw materials quality, adopt acetone extraction, Extracting temperature is 30 DEG C, and extraction time is 2 times. Being merged by extracting solution, concentrating to proportion is 1.09, and thickening temperature is 45 DEG C.
Being dissolve above-mentioned medicinal extract 1 time under 95% ethanol room temperature by the mass concentration of 2 times of medicinal extract quality, dissolve 1h, filter, filtrate adds 2% silica gel of medicinal extract quality, and when 45 DEG C, decolouring 30min, filters. The gained filter cake methylene dichloride of 1 times of filter cake quality dissolves, and filters, and concentrate drying, the receipts rate of products obtained therefrom is 2.08%, and content is 49.6%.
Embodiment 4:
2000kg shatter after European feverfew bar raw material, add the wetting 10h of water of material quantity 0.8 times of raw materials quality, adopt ethyl acetate to extract, Extracting temperature is 50 DEG C, and extraction time is 2 times. Being merged by extracting solution, concentrating to proportion is 1.12, and thickening temperature is 40 DEG C.
It is dissolve above-mentioned medicinal extract 1 time under 95% ethanol room temperature by the mass concentration of 2.5 times of medicinal extract quality, dissolve 1.5h, filter, filtrate adds the gac of the 2% of medicinal extract quality and the compound sample of aluminum oxide, the mass ratio of its gac and aluminum oxide is 9:1, when 50 DEG C, decolouring 30min, filters. The gained filter cake acetic acid ethyl dissolution of 0.8 times of filter cake quality, filters, and concentrate drying, the receipts rate of products obtained therefrom is 1.5%, and content is 35.4%.
Embodiment 5:
2000kg shatter after European feverfew bar raw material, add the wetting 6h of water of material quantity 0.6 times of raw materials quality, adopt dichloromethane extraction, Extracting temperature is 20 DEG C, and extraction time is 3 times. Being merged by extracting solution, concentrating to proportion is 1.17, and thickening temperature is 40 DEG C.
It is dissolve above-mentioned medicinal extract 1 time under 95% ethanol room temperature by the mass concentration of 3 times of medicinal extract quality, dissolves 2.5h, filter, filtrate adds the gac of the 4% of medicinal extract quality and the mixture of starch, and the mass ratio of its gac and starch is 8:2, when 65 DEG C, decolouring 30min, filters.The gained filter cake methylene dichloride of 0.3 times of filter cake quality dissolves, and filters, and concentrate drying, the receipts rate of products obtained therefrom is 1.6%, and content is 38.2%.
Embodiment 6:
1000kg shatter after European feverfew leaf raw material, add the wetting 8h of water of material quantity 0.7 times of raw materials quality, adopt Petroleum ether extraction, Extracting temperature is 30 DEG C, and extraction time is 3 times. Being merged by extracting solution, concentrating to proportion is 1.16, and thickening temperature is 35 DEG C.
It is dissolve above-mentioned medicinal extract 1 time under 95% ethanol room temperature by the mass concentration of 4.5 times of medicinal extract quality, dissolves 1.2h, filter, filtrate adds the aluminum oxide of the 6% of medicinal extract quality and the mixture of starch, and the mass ratio of its aluminum oxide and starch is 7:3, when 49 DEG C, decolouring 30min, filters. The gained filter cake mixed solvent of the ethyl acetate of 0.8 times of filter cake quality and methylene dichloride dissolves, and the volume ratio of ethyl acetate and methylene dichloride is 1:10, filters, and concentrate drying, the receipts rate of products obtained therefrom is 2.0%, and content is 45.2%.
Embodiment 7:
1000kg shatter after European feverfew leaf raw material, adding the wetting 1h of water of material quantity 0.8 times of raw materials quality, adopt the mixed solvent of ethyl acetate and methylene dichloride to extract, the volume ratio of its ethyl acetate and methylene dichloride is 19:1, Extracting temperature is 25 DEG C, and extraction time is 2 times. Being merged by extracting solution, concentrating to proportion is 1.18, and thickening temperature is 45 DEG C.
It is dissolve above-mentioned medicinal extract 1 time under 95% ethanol room temperature by the mass concentration of 2.8 times of medicinal extract quality, dissolves 1.8h, filter, filtrate adds the gac of the 5% of medicinal extract quality and the mixture of starch, and the mass ratio of its gac and starch is 8:2, when 50 DEG C, decolouring 30min, filters. The gained filter cake mixed solvent of the ethyl acetate of 0.6 times of filter cake quality and methylene dichloride dissolves, and the volume ratio of its ethyl acetate and methylene dichloride is 5:8, filters, and concentrate drying, the receipts rate of products obtained therefrom is 1.8%, and content is 50.0%.
Embodiment 8:
1000kg shatter after European feverfew leaf raw material, add the wetting 15h of water of material quantity 0.3 times of raw materials quality, adopting the mixed solvent of ethyl acetate and sherwood oil to extract, the volume ratio of its ethyl acetate and sherwood oil is 9:5 Extracting temperature is 38 DEG C, and extraction time is 2 times. Being merged by extracting solution, concentrating to proportion is 1.20, and thickening temperature is 38 DEG C.
Being dissolve above-mentioned medicinal extract 1 time under 95% ethanol room temperature by the mass concentration of 2 times of medicinal extract quality, dissolve 1.2h, filter, filtrate adds the gac of the 5.3% of medicinal extract quality, and when 50 DEG C, decolouring 30min, filters. The gained filter cake acetic acid ethyl dissolution of 0.2 times of filter cake quality, filters, and concentrate drying, the receipts rate of products obtained therefrom is 2.41%, and content is 36.2%.
Claims (7)
1. the preparation method of a feverfew lactone, it is characterised in that, comprise the following steps:
Step 1 is extracted
In the European feverfew after pulverizing, add water soak, adopt organic solvent extraction, obtain extracting solution;
Described organic solvent is any one or multiple mixing in methyl alcohol, ethanol, acetone, ethyl acetate, methylene dichloride, sherwood oil;
Step 2 concentrates
The extracting solution of step 1 gained is concentrated, places, obtain medicinal extract;
Prepared by step 3
By the medicinal extract dissolve with ethanol of step 2 gained, filter; Then in filtrate, add sorbent material carry out desolventing technology, filter, get the filter cake organic solvent dissolution after filtration, concentrated, dry, obtain feverfew lactone products;
Described sorbent material is any one or multiple mixing in gac, aluminum oxide, silica gel, starch;Described organic solvent is the mixing of any one or two kinds in ethyl acetate, methylene dichloride.
2. the preparation method of feverfew lactone according to claim 1, it is characterized in that, described step 1 specifically: the wetting 0.5-24h of water adding 0.1-1 times amount in the European feverfew after pulverizing, when 10-60 DEG C, adopt organic solvent extraction 1-3 time, obtain extracting solution; Described organic solvent is any one or multiple mixing in methyl alcohol, ethanol, acetone, ethyl acetate, methylene dichloride, sherwood oil.
3. the preparation method of feverfew lactone according to claim 2, it is characterized in that, described step 1 is: the wetting 1h of water adding 0.8 times amount in the European feverfew after pulverizing, when 10-60 DEG C, adopt the mixed solvent of ethyl acetate and methylene dichloride to extract 1-3 time, obtain extracting solution; The volume ratio of described ethyl acetate and methylene dichloride is 19:1.
4. the preparation method of feverfew lactone according to claim 1, it is characterised in that, described step 2 specifically: under temperature is 20-60 DEG C of condition, the extracting solution of step 1 gained is concentrated to proportion be 1.08-1.20, place, obtain medicinal extract.
5. the preparation method of feverfew lactone according to claim 4, it is characterised in that: in described step 2, best thickening temperature is 45 DEG C.
6. the preparation method of feverfew lactone according to claim 1, it is characterised in that, described step 3 specifically: be the dissolve with ethanol 1 time of 95% by the medicinal extract 0.5-6 times amount mass concentration of step 2 gained, dissolve 0.5-3h every time, filter; When 30-70 DEG C, the sorbent material adding medicinal extract quality 1%-10% in filtrate carries out desolventing technology, filters, gets the filter cake organic solvent dissolution after filtration, concentrated, dry, obtains feverfew lactone products; Described sorbent material is any one or multiple mixing in gac, aluminum oxide, silica gel, starch; Described organic solvent is the mixing of any one or two kinds in ethyl acetate, methylene dichloride.
7. the preparation method of feverfew lactone according to claim 6, it is characterised in that, described step 3 is: being the dissolve with ethanol 1 time of 95% by the mass concentration of 2 times of medicinal extract quality by the medicinal extract of step 2 gained, dissolution time is 1.2h, filters; When 50 DEG C, in filtrate, add gac and the starch mixture decolouring 30min of medicinal extract quality 5%, filter, get the filter cake ethyl acetate after filtration and the dissolving of methylene dichloride mixed solution, concentrated, dry, obtain feverfew lactone products; The mass ratio of described gac and starch is 8:2, and the volume ratio of described ethyl acetate and methylene dichloride is 5:8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510998196.2A CN105646515A (en) | 2015-12-28 | 2015-12-28 | Preparation method of parthenolide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510998196.2A CN105646515A (en) | 2015-12-28 | 2015-12-28 | Preparation method of parthenolide |
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| CN105646515A true CN105646515A (en) | 2016-06-08 |
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| CN201510998196.2A Pending CN105646515A (en) | 2015-12-28 | 2015-12-28 | Preparation method of parthenolide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109516994A (en) * | 2017-09-18 | 2019-03-26 | 天津尚德药缘科技股份有限公司 | Preparation method, detection method of content and the adsorbent composition of parithenolide |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19800330C2 (en) * | 1998-01-07 | 2002-09-26 | Delta 9 Pharma Gmbh | Pharmaceutical CO¶2¶ extract from Tanacetum parthenium |
| WO2008010335A1 (en) * | 2006-07-21 | 2008-01-24 | Mmt Co., Ltd. | Plant extract having arthritis-preventive effect |
| CN101190258A (en) * | 2007-05-30 | 2008-06-04 | 北京星昊医药股份有限公司 | Total sesquiterpene lactone extract containing rich parthenolide and preparation method and application thereof |
| CN102241684A (en) * | 2010-05-11 | 2011-11-16 | 天津尚德药缘科技有限公司 | Preparation method of parthenolide |
| CN102863452A (en) * | 2011-07-06 | 2013-01-09 | 天津尚德药缘科技有限公司 | Method for preparing parthenolide originated from magnolia delavayi, magnolia liliiflora and magnolia denudate |
-
2015
- 2015-12-28 CN CN201510998196.2A patent/CN105646515A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19800330C2 (en) * | 1998-01-07 | 2002-09-26 | Delta 9 Pharma Gmbh | Pharmaceutical CO¶2¶ extract from Tanacetum parthenium |
| WO2008010335A1 (en) * | 2006-07-21 | 2008-01-24 | Mmt Co., Ltd. | Plant extract having arthritis-preventive effect |
| CN101190258A (en) * | 2007-05-30 | 2008-06-04 | 北京星昊医药股份有限公司 | Total sesquiterpene lactone extract containing rich parthenolide and preparation method and application thereof |
| CN102241684A (en) * | 2010-05-11 | 2011-11-16 | 天津尚德药缘科技有限公司 | Preparation method of parthenolide |
| CN102863452A (en) * | 2011-07-06 | 2013-01-09 | 天津尚德药缘科技有限公司 | Method for preparing parthenolide originated from magnolia delavayi, magnolia liliiflora and magnolia denudate |
Non-Patent Citations (3)
| Title |
|---|
| ANNA STOJAKOWSKA 等: "Production of parthenolide in organ cultures of feverfew", 《PLANT CELL, TISSUE AND ORGAN CULTURE》 * |
| KRISZTINA VÉGH 等: "Supercritical fluid extraction and convergence chromatographic chromatographicdetermination of parthenolide in Tanacetum parthenium L.: Experimental design, modeling and optimization", 《THE JOURNAL OF SUPERCRITICAL FLUIDS》 * |
| TATIANA SHIOJI TIUMAN 等: "Antileishmanial Activity of Parthenolide, a Sesquiterpene Lactone Isolated from Tanacetum parthenium", 《ANTIMICROBIAL AGENTS AND CHEMOTHERAPY》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109516994A (en) * | 2017-09-18 | 2019-03-26 | 天津尚德药缘科技股份有限公司 | Preparation method, detection method of content and the adsorbent composition of parithenolide |
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Application publication date: 20160608 |