CN102793737B - Method for preparing powder of effective part of thunder god vine - Google Patents
Method for preparing powder of effective part of thunder god vine Download PDFInfo
- Publication number
- CN102793737B CN102793737B CN201110139090.9A CN201110139090A CN102793737B CN 102793737 B CN102793737 B CN 102793737B CN 201110139090 A CN201110139090 A CN 201110139090A CN 102793737 B CN102793737 B CN 102793737B
- Authority
- CN
- China
- Prior art keywords
- extraction
- extract
- radix tripterygii
- tripterygii wilfordii
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for preparing powder of an effective part of thunder god vine, and belongs to a traditional Chinese medicine effective component extraction and separation technology. The method comprises the following steps of: extracting rhizome powder of the thunder god vine by alcohol; recycling a solvent; extracting extractum by an ethyl acetate solvent, and concentrating to a certain volume; extracting the ethyl acetate extracted solution by a carbonate aqueous solution with the concentration of 2 to 5 wt percent for 2 to 3 times, and recycling an organic layer; and drying to obtain the powder. The terpene content in the effective part powder is over 50 percent; and the capsanthin content, namely a toxic component, is less than 0.2 percent. The method is easy to operate, low in production cost, high in effective component content and low in toxicity and is mainly used for treating chronic nephritis diseases.
Description
Technical field
The invention belongs to the Effective Component of Chinese Medicine extraction separation method, be specifically related to a kind of preparation method of Radix Tripterygii Wilfordii effective site powder.
Technical background
Relevant survey result demonstration, the chronic nephropathy prevalence of China is in 8% left and right.Various chronic renal diseases, as common chronic nephritis, chronic pyelonephritis, autoimmune disease renal damage etc., bring heavy burden to patient family and society.Chronic nephritis is that the chronic glomerulus pathological changes of one group of multi-pathogenesis is main renal glomerular disease, think that at present it may be due to infection such as various antibacterials, virus or protozoons, cause by the immunologic mechanism inflammatory mediator factor and nonimmune mechanism etc., mainly adopt clinically hormone, immunosuppressant treatment.Radix Tripterygii Wilfordii (Tripterygium Wilfordii Hook.f) is the Celastraceae tripterygium plant, Shennong's Herbal begins to be stated from, main product in Hubei of China, the province such as Hunan, Fujian, there is the multiple pharmacologically actives such as antiinflammatory, immunosuppressant, antitumor, antifertility, so far from Radix Tripterygii Wilfordii, separate and obtained hundreds of chemical compositions, wherein main active component is ter penoids, comprises sesquiterpene alkaloids, diterpene and triterpenoid compound.Since Li Lei stone academicians in 1977 etc. report Chinese herb triperygium wilfordii treatment glomerulonephritis first, Radix Tripterygii Wilfordii has been widely used in the treatment of various constitutionales and Secondary cases nephritis, and has shown unique curative effect.
The Radix Tripterygii Wilfordii chemical composition is numerous, and the pharmacological action complexity had wherein both contained active ingredient, also contain toxic component, this makes Radix Tripterygii Wilfordii extract have good and unique clinical therapeutic efficacy, causes again it to have obvious toxic and side effects, has limited Radix Tripterygii Wilfordii application clinically simultaneously.As far as possible the active ingredient in the enrichment Radix Tripterygii Wilfordii extract and remove invalid and toxic component, can reduce the toxicity of Radix Tripterygii Wilfordii extract greatly, keeps its effectiveness simultaneously, and clinical drug safety is improved.Bibliographical information, tripterine be a kind of toxic component (Zhu Xiaoming etc., Chinese organ transplantation magazine, 1996,1:21), we remove tripterine targetedly thus, reduce its toxic and side effects.
Existing Tripterygium Preparations, the peeling root extract of the multiplex Radix Tripterygii Wilfordii of its raw material sources.Radix Tripterygii Wilfordii extract has on preparation technology: alcohol extraction ethyl acetate extraction, and column chromatography method after the water extraction chloroform extraction, after the alcohol extraction chloroform extraction, (patent CN 200710043857.1 for the method such as column chromatography method; CN 200910196969.X; US 5580562; Xia Zhilin etc., Chinese Journal of Pharmaceuticals, 1994,3,135), there is following shortcoming in these preparation methoies:
1. the direct extracting process of ethyl acetate, its effective component extracting complexity, active constituent content is low, is unfavorable for next step preparation production.
2. use column chromatography method, although active constituent content is high, consumption of organic solvent is large, in most cases uses chloroform, and toxicity is large.
3. in column chromatography method, use mixed solvent, complicated operation and further recycling difficulty.
4. specific aim is not strong.The contained complex chemical composition of Radix Tripterygii Wilfordii, raw material prepared by existing technique is not accepted or rejected the chemical composition composition targetedly according to various disease, causes side effect high.
Summary of the invention
The preparation method that the purpose of this invention is to provide a kind of Radix Tripterygii Wilfordii effective site powder, solve existing extracting method specific aim not strong, the problems such as production cost is high, complex disposal process.
The preparation method of a kind of Radix Tripterygii Wilfordii effective site powder of the present invention comprises the following steps:
(1) pulverize: select the Radix Tripterygii Wilfordii rhizome, make Common Threewingnut Root after drying and crushing;
(2) alcohol extraction: the alcohol reflux that is 90wt%～100wt% by concentration by Common Threewingnut Root 2～3 times, after each extracting solution merged, reclaim ethanol, obtain thick extracted extract;
(3) extraction for the first time: by ethyl acetate solvent extraction 1～3 time for thick extracted extract, ethyl acetate solvent is 5～8mL: 1g with thick extracted extract amount ratio, merges extract each time, and concentrated extract, to 20%～40% of original volume, obtains concentrated extract;
(4) extraction for the second time: step (3) gained concentrated extract is extracted 2～3 times with carbonate aqueous solution, discard carbonate aqueous solution, obtain extraction fluid, with after isopyknic washing extraction fluid 2～3 times, reclaim the extraction fluid solvent, drying obtains the effective site powder; In described carbonate aqueous solution, the content of carbonate is 2wt%～5wt%, and the volume ratio of carbonate aqueous solution and concentrated extract is 0.5～1.5: 1.
The Radix Tripterygii Wilfordii effective site powder prepared with said method, the ter penoids total content surpasses 50%, and toxic component trypterygine cellulose content is less than 0.2%, is mainly used in the treatment of chronic nephritis.
Described preparation method, preferably, in described pulverising step, the Radix Tripterygii Wilfordii rhizome that described Radix Tripterygii Wilfordii rhizome is belt leather; In described step (4), described carbonate is sodium carbonate or potassium carbonate.
Ethanol used, ethyl acetate solvent in the present invention, continue after can reclaiming to use.
The present invention is simple to operate, poisonous organic solvent is used few, solvent all can reclaim use easily, production cost is low, be easy to suitability for industrialized production, removed the acid ingredient (red pigment) of toxicity in extraction step for the second time, powder prepared by this method is mainly for the chronic nephritis disease, the content of effective ingredient is higher than 50%, and toxic and side effects is few.
The specific embodiment
Total diterpene lactone in ter penoids in the prepared effective site powder of following the present invention, total triterpene contents, sesquiterpene alkaloids, being determined as follows of tripterine.
The total diterpene lactone content is measured:
(1) preparation of reference substance solution: precision takes the triptolide reference substance, with the ethanol ultrasonic dissolution of concentration 70%, and the reference substance stock solution that preparation concentration is 0.15mg/mL;
(2) preparation of need testing solution: get Radix Tripterygii Wilfordii effective site powder 30mg, after dissolving with the 5mL chloroform, upper prop (SPE pillar, long 6.0cm, diameter 0.8cm, amount of filler 1.5g, for 100-200 order aluminium oxide), with 20mL chloroform-methanol mixed solvent (volume ratio 95: 5) eluting, collect effluent and eluent, evaporated under reduced pressure, ethanol ultrasonic dissolution by concentration 70%, be settled to 25mL;
(3) linear relationship is investigated: accurately pipette respectively reference substance stock solution 0.1mL, 0.2mL, 0.3mL, 0.4mL, 0.5mL, 0.6mL, 0.8mL in the scale test tube with stopper, add the ethanol of concentration 70% to 4.0mL, add again 3 of concentration 2%, 5-dinitrobenzoic acid solution 0.5mL, the KOH solution 0.5mL of concentration 2%, shake up, make it reaction.Be determined under 549nm the absorbance while developing the color 30min, take absorbance as vertical coordinate, reference substance concentration is abscissa, the drawing standard curve, and regression equation is: y=0.0172x+0.0234, R
2=0.9991;
(4) assay: draw the 1.0mL need testing solution, add the ethanol of concentration 70% to 4.0mL, then add 3 of concentration 2%, 5-dinitrobenzoic acid solution 0.5mL, the KOH solution 0.5mL of concentration 2%, shake up, and makes it reaction.Be determined under 549nm the absorbance while developing the color 30min, by following formula, calculate the total diterpene lactone content:
Total diterpene lactone content=(test sample absorbance/reference substance absorbance) * reference substance concentration * 125.
Total triterpene contents is measured:
(1) preparation of reference substance solution: precision takes the wilforlide A reference substance, ethanol ultrasonic dissolution, the reference substance stock solution that preparation concentration is 0.175mg/mL
(2) preparation of need testing solution: get Radix Tripterygii Wilfordii effective site powder 5mg, the 5mL chloroform dissolves upper firmly (SPE pillar, long 6.0cm, diameter 0.8cm, filler 100-200 order aluminium oxide, consumption 1.5g), with 20mL chloroform-methanol mixed solution (95: 5) eluting, collect effluent and eluent, evaporated under reduced pressure, the ethanol ultrasonic dissolution, be settled to 25mL.
(3) linear relationship is investigated: accurately pipette reference substance stock solution 20 μ L, 40 μ L, 60 μ L, 80 μ L, 100 μ L, 120 μ L, in tool plug scale test tube, dry up.Add 5% vanillin-glacial acetic acid 0.2mL, perchloric acid 0.8mL, heating colour developing 15min in 60 ℃ of water-baths, add glacial acetic acid 4mL after cooling.Be determined at absorbance under 540nm, take absorbance as vertical coordinate, reference substance concentration is abscissa drawing standard curve, and regression equation is y=9.9688x+0.5251, R
2=0.9926;
(4) assay: draw the 0.1mL need testing solution, dry up.Add 5% vanillin-glacial acetic acid 0.2mL, perchloric acid 0.8mL, heating colour developing 15min in 60 ℃ of water-baths, add glacial acetic acid 4mL after cooling.Be determined at the absorbance under 540nm, by following formula, calculate total triterpene contents:
Total triterpene contents=(test sample absorbance/reference substance absorbance) * reference substance concentration * 1250.
The total sesquiterpene alkaloid content determination:
(1) preparation of reference substance solution: precision takes the wilforine reference substance, ethanol ultrasonic dissolution, the reference substance stock solution that preparation concentration is 0.4mg/mL.
(2) preparation of need testing solution: get Radix Tripterygii Wilfordii effective site powder 10mg, the 5mL chloroform dissolves upper firmly (SPE pillar, long 6.0cm, diameter 0.8cm, filler 100-200 order aluminium oxide, consumption 1.5g), with 20mL chloroform-methanol mixed solvent (95: 5) eluting, collect effluent and eluent, evaporated under reduced pressure, the ethanol ultrasonic dissolution, be settled to 25mL.
(3) linear relationship is investigated: the above-mentioned reference substance stock solution 0.3mL of accurate absorption, and 0.5mL, 1.0mL, 2.0mL, 4.0mL is placed in the 5mL volumetric flask, and the ethanol standardize solution, shake up.Measure absorbance at the 267nm place, take absorbance as vertical coordinate, reference substance concentration is abscissa drawing standard curve, and regression equation is: y=0.0051x+0.0007, R
2=0.9998.
(4) assay: get need testing solution 1mL, be settled to 5mL, measure absorbance at the 267nm place.Calculate the content of total alkaloids by following formula.
Total sesquiterpene alkaloid=(test sample absorbance/reference substance absorbance) * reference substance concentration * 125.
The tripterine assay:
(1) preparation of reference substance solution: precision takes the tripterine reference substance, methanol ultrasonic dissolution, the reference substance stock solution that preparation concentration is 0.2mg/mL.
(2) preparation of need testing solution: get Radix Tripterygii Wilfordii effective site powder 15mg, with after the 10mL dissolve with ethanol, standardize solution is to 25mL.Solution is got subsequent filtrate as need testing solution after crossing 0.45 μ m microporous filter membrane.
(3) linear relationship is investigated: the above-mentioned reference substance stock solution 0.5mL of accurate absorption, 1.0mL, 2.0mL, 4.0mL, 6.0mL are placed in the 10mL volumetric flask, and methanol constant volume, shake up.Advance HPLC and detect, obtain the red pigment chromatographic peak, and computer chromatography peak-to-peak size.Chromatographic condition: chromatographic column: ZORBAX Eclipse Plus C18 post (250mm * 4.6mm * 5um); Mobile phase: methanol: 1% acetic acid=(90: 10); Flow velocity: 1.0mL/min
-1; Detect wavelength: 425nm, sample size: 10 μ L; Column temperature: 25 ℃.Take peak area as vertical coordinate, and reference substance concentration is abscissa drawing standard curve, and regression equation is: Y=13771X-7.9093 (r=0.9999)
(4) assay: get need testing solution, advance HPLC and detect, sample size: 10 μ L.Record peak area, by following formula, calculate the trypterygine cellulose content.
Red pigment content=(test sample peak area/reference substance peak area) * reference substance concentration * 25.
Further illustrate the present invention below by embodiment.
Embodiment 1
The preparation method of the described Radix Tripterygii Wilfordii effective site of the present embodiment powder comprises the following steps:
(1) pulverising step: select Radix Tripterygii Wilfordii belt leather rhizome 1.0kg, make Common Threewingnut Root after drying and crushing;
(2) alcohol is got step: the alcohol reflux that is 100% by concentration by Common Threewingnut Root 2 times, after 2 extracting solution are merged, reclaim ethanol, and obtain thick extracted extract 70g;
(3) extraction step for the first time: by ethyl acetate solvent extraction for thick extracted extract 1 time, ethyl acetate solvent is 8mL: 1g with thick extracted extract amount ratio, and concentrated extract, to 40% of original volume, obtains concentrated extract;
(4) extraction step for the second time: the aqueous sodium carbonate that the concentration of take is 2wt% is to concentrated extract extraction 3 times, and the volume ratio of aqueous sodium carbonate and concentrated extract is 0.5: 1; Discard aqueous sodium carbonate, obtain extraction fluid, with after isopyknic washing extraction fluid 2 times, reclaim the extraction fluid solvent, drying obtains effective site powder 15g.Ter penoids is 59.3%, and wherein the total diterpene lactone content 1.3%, total triterpene contents 14%, and sesquiterpene alkaloids is 44%, trypterygine cellulose content 0.09%.
Embodiment 2
The preparation method of the described Radix Tripterygii Wilfordii effective site of the present embodiment powder comprises the following steps:
(1) pulverising step: select Radix Tripterygii Wilfordii belt leather rhizome 1.0kg, make Common Threewingnut Root after drying and crushing;
(2) alcohol is got step: the alcohol reflux that is 90wt% by concentration by Common Threewingnut Root 3 times, after each extracting solution merged, reclaim ethanol, and obtain thick extracted extract 76g;
(3) extraction step for the first time: by ethyl acetate solvent extraction for thick extracted extract 2 times, ethyl acetate solvent is 5mL: 1g with thick extracted extract amount ratio, merges extract each time, and concentrated extract, to 20% of original volume, obtains concentrated extract;
(4) extraction step for the second time: with the aqueous sodium carbonate of 5wt%, to concentrated extract extraction 2 times, the volume ratio of aqueous sodium carbonate and concentrated extract is 1: 1; Discard aqueous sodium carbonate, obtain extraction fluid, with after isopyknic washing extraction fluid 2 times, reclaim the extraction fluid solvent, drying obtains effective site powder 19g; Ter penoids is 56%, and wherein the total diterpene lactone content 1.2%, total triterpene contents 15%, and the total sesquiterpene alkaloid is 40%, trypterygine cellulose content 0.11%.
Embodiment 3
The preparation method of the described Radix Tripterygii Wilfordii effective site of the present embodiment powder comprises the following steps:
(1) pulverising step: select Radix Tripterygii Wilfordii belt leather rhizome 1.0kg, make Common Threewingnut Root after drying and crushing;
(2) alcohol is got step: the alcohol reflux that is 90wt% by concentration by Common Threewingnut Root 3 times, after each extracting solution merged, reclaim ethanol, and obtain thick extracted extract 76g;
(3) extraction step for the first time: by ethyl acetate solvent extraction for thick extracted extract 3 times, ethyl acetate solvent is 5mL: 1g with thick extracted extract amount ratio, merges extract each time, and concentrated extract, to 20% of original volume, obtains concentrated extract;
(4) extraction step for the second time: with the aqueous sodium carbonate of 5wt% to concentrated extract extraction 3 times, the volume ratio of carbonate aqueous solution and concentrated extract is 1: 1, discard carbonate aqueous solution, obtain extraction fluid, with after isopyknic washing extraction fluid 3 times, reclaim the extraction fluid solvent, drying obtains effective site powder 18g; Ter penoids is 57.5%, and wherein the total diterpene lactone content 1.5%, total triterpene contents 14%, and the total sesquiterpene alkaloid is 42%, trypterygine cellulose content 0.08%.
Embodiment 4
The preparation method of the described Radix Tripterygii Wilfordii effective site of the present embodiment powder comprises the following steps:
(1) pulverising step: select Radix Tripterygii Wilfordii peeling rhizome 1.0kg, make Common Threewingnut Root after drying and crushing;
(2) alcohol is got step: the alcohol reflux that is 100% by concentration by Common Threewingnut Root 3 times, after each extracting solution merged, reclaim ethanol, and obtain thick extracted extract 45g;
(3) extraction step for the first time: by ethyl acetate solvent extraction for thick extracted extract 2 times, ethyl acetate solvent is 8mL: 1g with thick extracted extract amount ratio, merges extract each time, and concentrated extract, to 20% of original volume, obtains concentrated extract;
(4) extraction step for the second time: the wet chemical that the concentration of take is 2wt% is to concentrated extract extraction 3 times, and the volume ratio of wet chemical and concentrated extract is 1.5: 1; Discard wet chemical, obtain extraction fluid, with after isopyknic washing extraction fluid 3 times, reclaim the extraction fluid solvent, drying obtains effective site powder 11g; Ter penoids is 52.5%, and wherein the total diterpene lactone content 1.5%, total triterpene contents 14%, and the total sesquiterpene alkaloid is 37%, trypterygine cellulose content 0.02%.
By said determination, can find out, in Radix Tripterygii Wilfordii effective site powder prepared by the present invention, active component ter penoids content is high, and toxic component red pigment content is limited in low scope.
Embodiment 5:
Toxicity test
In clinical practice, the Radix Tripterygii Wilfordii extract liver toxicity is common side reaction
.we
select the people normalhepatic cell line HL-7702, by the thick extracted extract of Radix Tripterygii Wilfordii, Radix Tripterygii Wilfordii effective site powder solution and hepatocyte co-cultivation 24 hours, with blank solvent (100% survival) in contrast, adopt IC
50(median lethal dose(LD 50)) value reflects the toxicity size of tester, and experimental result is in Table 1.
Evaluating drug effect
In chronic nephritis, the inflammatory of mesangial cell propagation is the initial stage reflection of chronic nephritis, is also the follow-up promoter that sb.'s illness took a turn for the worse.Suppress the effectively relieve chronic nephritis development of propagation of mesangial cell.Get the thick extracted extract of Radix Tripterygii Wilfordii, Radix Tripterygii Wilfordii effective site powder is suppressed proliferation of glomerular mesangial cells and is tested to estimate the activity size of each position for chronic nephritis, adopts EC
50(median effective dose) reflects the active size in each position, and experimental result is in Table 1.
Table 1 embodiment 1 each position toxicity and active size
IC
50show that more greatly toxicity is less, toleration is higher; EC
50littlely show that activity is stronger, effective, IC
50/ EC
50the value concentrated expression safety of medicine, value shows that more greatly safety range is wider, medicine is safer.By table 1, can find out, Radix Tripterygii Wilfordii effective site powder prepared by the present invention shows good inhibition proliferation of glomerular mesangial cells effect, EC
50be 2.42 μ g/mL, and toxic effect is than (IC
50/ EC
50) larger than the thick extracted extract of Radix Tripterygii Wilfordii, this shows for the chronic nephritis disease, the safety of Radix Tripterygii Wilfordii effective site powder is higher.
Be more than for the illustrating of possible embodiments of the present invention, but this embodiment is not in order to limit the scope of the claims of the present invention, allly do not break away from the equivalence that skill spirit of the present invention does and implement or change, all should be contained in the scope of the claims of the present invention.
Claims (3)
1. the preparation method of a Radix Tripterygii Wilfordii effective site powder, is characterized in that, comprises the following steps:
(1) pulverize: select the Radix Tripterygii Wilfordii rhizome, make Common Threewingnut Root after drying and crushing;
(2) alcohol extraction: the alcohol reflux that is 90wt%～100wt% by concentration by Common Threewingnut Root 2～3 times, after each extracting solution merged, reclaim ethanol, obtain thick extracted extract;
(3) extraction for the first time: by ethyl acetate solvent extraction 1～3 time for thick extracted extract, ethyl acetate solvent is 5～8mL: 1g with the amount ratio of thick extracted extract, merges extract each time, and concentrated extract, to 20%～40% of original volume, obtains concentrated extract;
(4) extraction for the second time: step (3) gained concentrated extract is extracted 2～3 times with carbonate aqueous solution, discard carbonate aqueous solution, obtain extraction fluid, with after isopyknic washing extraction fluid 2～3 times, reclaim the extraction fluid solvent, drying obtains the effective site powder; In described carbonate aqueous solution, the content of carbonate is 2wt%～5wt%, and the volume ratio of carbonate aqueous solution and concentrated extract is 0.5～1.5: 1.
2. preparation method according to claim 1, is characterized in that, in described step (1), and the Radix Tripterygii Wilfordii rhizome that described Radix Tripterygii Wilfordii rhizome is belt leather.
3. preparation method according to claim 1 and 2, is characterized in that, in described step (4), described carbonate is sodium carbonate or potassium carbonate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110139090.9A CN102793737B (en) | 2011-05-26 | 2011-05-26 | Method for preparing powder of effective part of thunder god vine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110139090.9A CN102793737B (en) | 2011-05-26 | 2011-05-26 | Method for preparing powder of effective part of thunder god vine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102793737A CN102793737A (en) | 2012-11-28 |
| CN102793737B true CN102793737B (en) | 2014-01-08 |
Family
ID=47193206
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110139090.9A Expired - Fee Related CN102793737B (en) | 2011-05-26 | 2011-05-26 | Method for preparing powder of effective part of thunder god vine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102793737B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104407081B (en) * | 2014-08-15 | 2016-08-24 | 衢州出入境检验检疫局综合技术服务中心 | The detection method of wilforine in a kind of honey |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1240292C (en) * | 2003-11-25 | 2006-02-08 | 浙江省农业科学院 | Method for extracting and separating insecticidal active substance from Tripterygium wilfordii |
| CN100422188C (en) * | 2006-08-25 | 2008-10-01 | 浙江大学 | Method for separating preparing tripterygium wilfordii monomer from tripterygium wilfordii by countercurrent flow chromatography |
| CN101088519B (en) * | 2007-07-17 | 2010-08-18 | 上海美通生物科技有限公司 | Tripterygium glycosides extract and its extraction process |
| CN101991633B (en) * | 2009-10-10 | 2012-11-07 | 上海复旦复华药业有限公司 | Method for extracting tripterygium glycosides, and product and inclusion compound and medicinal composition thereof |
-
2011
- 2011-05-26 CN CN201110139090.9A patent/CN102793737B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN102793737A (en) | 2012-11-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100577677C (en) | Caulis trachelospermi total lignans extractive, extraction method and medicine use of the active constituent thereof | |
| CN103848875A (en) | Preparation method of gentiopicroside raw material | |
| CN102327309B (en) | Barberry bark extractive and use of barberry bark extractive and barberry bark | |
| WO2012061984A1 (en) | Method for preparing albiflorin and paeoniflorin | |
| CN101791366A (en) | Method for testing quality of Discorea nipponica Makino in different places and medicinal materials of same genera | |
| CN102793737B (en) | Method for preparing powder of effective part of thunder god vine | |
| CN104257768A (en) | Application of total anthraquinone with various ingredients in stable and uniform proportion and composition of total anthraquinone to treatment of pancreatitis | |
| CN102397260B (en) | Method for preparing sinomenine hydrochloride tablet | |
| CN102293811B (en) | Extraction method of total coumarin and application of extracted total coumarin | |
| CN101766664B (en) | Detection method of total saponin of Radix Ilicis Asprellae | |
| CN103494850B (en) | Process for extracting and purifying total organic acid of aralia cordata | |
| CN105669621A (en) | Pharmaceutical composition of chlortetracycline hydrochloride and medical application of pharmaceutical composition | |
| CN102786472B (en) | Method for extraction separation of huperzine A in all-grass of snake foot clubmoss and its hairy root by supercritical extraction-crystallization technology | |
| CN101862353B (en) | Method for extracting total triterpenes in fungus larch | |
| CN102058829A (en) | Medicine composition and detection method of preparations of medicine composition | |
| CN101596273A (en) | The method of quality control of Radix Ophiopogonis in the YIXINSHU Chinese medicine preparation | |
| CN103239435A (en) | Preparation method of gynura divaricata total caffeoylquinic acid and application in antihyperglycemic agent or health-care product | |
| CN107501282B (en) | The preparation method of isoquinolone Alkaloid compound in a kind of short-tube lycoris | |
| CN102370691A (en) | Ibufenac traditional Chinese preparation detection method | |
| CN102643281A (en) | High-content euonine and wilforidine preparing method | |
| CN102188468B (en) | Preparation method of Xinnaoshutong tablet | |
| CN105311118B (en) | Industrial purification method of total alkaloids of corydalis amabilis, product and application | |
| CN102241682A (en) | Preparation method for fissistigine A | |
| CN105311117B (en) | Method for removing bicolor from rhizoma corydalis decumbentis total alkaloids, product and application | |
| CN101451957A (en) | Method for detecting anthraquinone content in medicaments |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140108 Termination date: 20180526 |