CN101874848A - Digitalis extract, preparation method and application thereof - Google Patents
Digitalis extract, preparation method and application thereof Download PDFInfo
- Publication number
- CN101874848A CN101874848A CN2009102421108A CN200910242110A CN101874848A CN 101874848 A CN101874848 A CN 101874848A CN 2009102421108 A CN2009102421108 A CN 2009102421108A CN 200910242110 A CN200910242110 A CN 200910242110A CN 101874848 A CN101874848 A CN 101874848A
- Authority
- CN
- China
- Prior art keywords
- digitalis
- extract
- mass parts
- water
- ethanol
- 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.)
- Granted
Links
Images
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a digitalis extract, a preparation method and application thereof. The preparation method of the digitalis extract comprises the following steps: (1) carrying out alcohol extraction on digitalis leaves to obtain crude extracting solution; (2) mixing the crude extracting solution with acid ethanol, keeping standing, and then filtering to obtain filtrate; (3) evaporating the filtrate to obtain extracting solution; (4) mixing the extracting solution with n-butyl alcohol, layering and then removing a n-butyl alcohol layer to obtain extract; (5) ultra-filtering the extract through an ultra-filtering column with the molecular weight cut-off of 10K Da and 5K Da to obtain ultrafiltrate; and (6) finally drying the ultrafiltrate by distillation to obtain the digitalis extract. The invention further protects the digitalis extract prepared by the method and ophthalmic gel prepared from the digitalis extract, wherein, the ophthalmic gel can efficiently prevent and treat diabetic retinopathy. The digitalis extract provided by the invention is a first medicine for specially preventing and treating diabetic retinopathy, changes the current condition of treating diabetic retinopathy, and has great economic prospects and social significance.
Description
Technical field
The present invention relates to a kind of Digitalis extract and preparation method thereof and application.
Background technology
Folium Digitalis is the dried leaves of goatweed Digitalis purpurea L. (Digitalis purpurea L.).Kind of cardiotonic glycoside surplus having isolated 20 from the Digitalis purpurea L. leaf at present, by three kinds of different glycoside units: .DELTA.20:22-3,14,21-trihydroxynorcholenic acid lactone (digitoxigenin), gitoxigenin (gitoxigenin) and guitar Lip river glycoside unit (gitaloxigenin) form with different sugared condensation.
To extract the effective ingredient that obtains from Folium Digitalis Purpureae and be applied to the with a long history of clinical disease treatment, for example: Digitoxin is used for the treatment of the history of the existing last 100 years of congestive heart failure.In recent years, studies show that in a large number that some effective ingredient of Folium Digitalis Purpureae can be used for treating the eye asthenopia.Diabetic renal papillary necrosis is the difficult problem of medical field at present, can only take some auxiliary treatment means clinically, does not have the medicine of special for treating so far.
Summary of the invention
The purpose of this invention is to provide a kind of Digitalis extract and preparation method thereof and application.
The invention provides a kind of preparation method of Digitalis extract, comprise the steps:
(1) alcohol extraction is carried out in Folium Digitalis, obtained crude extract;
(2) crude extract and the sour ethanol with step (1) mixes, and leaves standstill after-filtration, obtains filtrate; Described crude extract and the alcoholic acid volume ratio of described acid are 1: 1; Described sour ethanol is the aqueous solution of ethanol and acetic acid, and alcoholic acid content is 94%-95% (quality percentage composition), and the content of acetic acid is 0.6%-0.7% (quality percentage composition);
(3) with filtrate 50-60 ℃, 0.08-0.12MPa evaporation of step (2), obtain extracting solution;
(4) extracting solution with step (3) mixes with n-butyl alcohol, abandons n-butanol layer after the layering, obtains extract;
(5) water of 4-6 times of volume of adding in the extract of step (4), the ultrafiltration post ultrafiltration through molecular cut off 10K Da obtains coarse filtration liquid; With of the ultrafiltration post ultrafiltration of coarse filtration liquid, obtain ultrafiltrate through molecular cut off 5K Da;
(6) with the ultrafiltrate evaporate to dryness of step (5), obtain Digitalis extract.
In the step (1), described alcohol extraction can be: Folium Digitalis was extracted 1.5-2.5 hour for ethanol water 75-85 ℃ with 95% (quality percentage composition); The proportioning of described Folium Digitalis and described 95% ethanol water is 1g Folium Digitalis: 9-11mL 95% ethanol water; Described alcohol extraction is preferably: Digitalis Leaf was extracted 2 hours for 80 ℃ with described 95% ethanol water; The proportioning of described Folium Digitalis and described 95% ethanol water is 1g Folium Digitalis: 10mL 95% ethanol water.In the step (1), carry out described alcohol extraction after, can 50 ℃, the 0.092MPa evaporation, evaporation back volume obtains described crude extract for the 1/23-1/24 of evaporation front volume.
In the described step (2), the crude extract and the sour ethanol of step (1) can be mixed, leave standstill 40 minutes after-filtration, obtain filtrate; The alcoholic acid preparation method of described acid is: add 0.5ml glacial acetic acid (glacial acetic acid) in every 100ml 95% (quality percentage composition) ethanol water.
In the described step (3), can be with 55 ℃ of filtrates, the 0.1MPa evaporation of step (2), evaporation back volume obtains extracting solution for the 51%-57% of evaporation front volume.
In the described step (4), the extracting solution of step (3) can be mixed with the n-butyl alcohol equal-volume.
In the described step (5), can in the extract of step (4), add the water of 5 times of volumes.
In the described step (6), 60 ℃ of evaporates to dryness of ultrafiltrate of step (5) can be obtained Digitalis extract.
Described Folium Digitalis Purpureae can be Digitalis purpurea L..
More than the Digitalis extract for preparing of arbitrary described method also belong to protection scope of the present invention.
The present invention also protects a kind of gel for eye use, obtains with following feedstock production: the described Digitalis extract of 2.7-3.2 mass parts, 145-155 mass parts NaOH, 480-520 mass parts carbomer 943,25-29 mass parts dimethyl fumarate and 49300-49350 mass parts water.
Described gel for eye use specifically can be and obtains with following feedstock production: the described Digitalis extract of 3 mass parts, 150 mass parts NaOH, 500 mass parts carbomers, 943,27 mass parts dimethyl fumarates and 49320 mass parts water.
Described gel for eye use specifically can be preparation with the following method: with described Digitalis extract water dissolution, filtering and collecting filter liquid; With described NaOH, described carbomer 943, described dimethyl fumarate water dissolution, obtain aseptic substrate after the sterilization; Described filtrate and described aseptic substrate are mixed, add entry, obtain the lanatoside gel for eye use.
The present invention also protects a kind of medicine that treats and/or prevents diabetic renal papillary necrosis, and its active component is above arbitrary described gel for eye use.
The present invention extracts from Digitalis purpurea L. and obtains a kind of extract, by preparation technique its production is become eye-gel preparation, can efficiently prevent to become with treatment of diabetic retinopathy.First is specifically designed to the medicine of prevention and treatment glycosuria and retinopathy medicine provided by the invention, has changed the treatment present situation of diabetic renal papillary necrosis.
Description of drawings
Fig. 1 is the chromatogram of Digitalis extract.
The chromatogram of Fig. 2 esculin and digitalisglycosides eye drops.
The specific embodiment
Following embodiment is convenient to understand better the present invention, but does not limit the present invention.Experimental technique among the following embodiment if no special instructions, is conventional method.Used test material among the following embodiment if no special instructions, is to buy from routine biochemistry reagent shop and obtains.
Digitalis purpurea L.: purchase in Shanghai Chinese crude drug company; Carbomer 943: purchase in Beijing fellow member of an association or organization's chemical industry company limited; Dimethyl fumarate: purchase in Shanghai Ou Le chemical industry company limited.
The evaluation criterion of diabetic renal papillary necrosis following (change according to the optical fundus, diabetic renal papillary necrosis was divided into for six phases):
I (1): retina have microaneurysm or and little petechia arranged; (+) minute quantity, easily number; (++) is more, is difficult for number.
II (2): retina have HUANGBAI(sic) " rigid oozing out " or and ecchymosis arranged; (+) minute quantity, easily number; (++) is more, is difficult for number.
III (3): retina adularescent " soft oozing out " or and ecchymosis arranged; (+) minute quantity, easily number; (++) is more, is difficult for the number proliferous type.
IV (4): retina has new vessels and/or vitreous hemorrhage.
V (5): retina has new vessels and fiber propagation.
VI (6): retina has new vessels and fiber to breed concurrent existing network film disengaging.
Wherein, I, II, III phase are referred to as simple retinopathy, and IV, V, VI phase are referred to as proliferative diabetic retinopathy.
The preparation of embodiment 1, Digitalis extract
One, the preparation of Digitalis extract
1, alcohol extraction
Get Digitalis purpurea L. leaf 300g and pulverize, add 95% ethanol water 3000ml,, slightly carried filtrate after the filtration 80 ℃ of temperature reflux, extract, 2 hours.Utilize the rotary evaporation in vacuo instrument will slightly carry filtrate at 50 ℃, decompression removes ethanol to there not being the alcohol flavor under the condition of 0.092MPa, obtains the about 128ml of crude extract.
2, precipitation
In crude extract, add equal-volume acid ethanol, left standstill behind the mixing 40 minutes, filter, get filtrate 252ml; The alcoholic acid prescription of acid: add 0.5ml glacial acetic acid (containing ethanol 94.3%, glacial acetic acid 0.65%) in the ethanol water of every 100ml 95%.Utilize the rotary evaporation in vacuo instrument with filtrate at 55 ℃, decompression removes ethanol to there not being the alcohol flavor under the condition of 0.1MPa, obtains extracting solution 135ml.
3, extraction
In extracting solution, add the equal-volume n-butyl alcohol, keep water layer, abandon n-butanol layer, obtain the about 130ml of extract.
4, ultrafiltration
Add 650ml water in extract, the ultrafiltration post ultrafiltration through molecular cut off 10K Da obtains coarse filtration liquid; Coarse filtration liquid passes through the ultrafiltration post ultrafiltration of molecular cut off 5K Da again, obtains about ultrafiltrate 710ml.
5, drying
60 ℃ of evaporates to dryness of ultrafiltrate obtain the Digitalis extract about 70mg.
Two, the chromatograph of Digitalis extract detects
Adopting octadecylsilane chemically bonded silica is the chromatographic column (200mm * 4.6mm, 5 μ m) of filler; With water-acetonitrile is mobile phase (volume ratio of water and acetonitrile is 18: 1); Flow velocity 1ml/min; Detect wavelength 220nm.
With 1mg Digitalis extract 20ml water dissolution, be made into the solution that concentration is 0.05mg/ml, get 10 μ l sample introductions, under above-mentioned chromatographic condition, to analyze, the gained chromatogram is seen Fig. 1.The esculin and digitalisglycosides eye drops (lot number 081009) of looking the production of pharmaceutical factory, Turin with Germany is a test sample, analyzes under above-mentioned chromatographic condition, and the gained chromatogram is seen Fig. 2.
As shown in Figure 1, Digitalis extract between retention time 10-30 minute, has peak area to account for the gross area and surpasses 6 chromatographic peaks of 15% under this chromatographic condition.The collection of illustrative plates of Digitalis extract and esculin and digitalisglycosides eye drops has tangible difference, shows that both main components are obviously inconsistent.
The production of embodiment 2, lanatoside gel for eye use
1, take by weighing the Digitalis extract 0.3g of embodiment 1 preparation, use the 1000ml water dissolution, solution is collected filtrate through the 0.22um filtering with microporous membrane;
2, take by weighing NaOH 15g, carbomer (943) 50g, dimethyl fumarate 2.7g, get substrate with the 2000ml water dissolution; 121 ℃ of autoclaving 20min obtain aseptic substrate;
3, the filtrate of step 1 and the aseptic substrate of step 2 are mixed, add water to 5000g, mixing obtains the lanatoside gel for eye use.
With the aluminum pipe fill of lanatoside gel for eye use, 5g/ props up.
Above-mentioned steps is all operated under aseptic condition, and employed vessel and aluminum pipe all carry out aseptic process in advance.
Embodiment 3, lanatoside gel for eye use are used for the curative effect of prevent diabetes retinopathy
One, makes diabetes rat model
With 0.1mol/L, the dissolving of the citrate buffer solution of pH4.2 is mixed with 2% (the 2g streptozotocin is dissolved in 100 milliliters of buffer) STZ solution with streptozotocin (STZ).60 of SD rats (purchasing the Experimental Animal Center in Liaoning Medical University) are by 65mg/kg body weight tail vein injection streptozotocin (the injection process Chinese medicine places ice bath).Injection back 48h detects glucose in urine and blood glucose, and glucose in urine exists +++more than, it is diabetes rat model that blood glucose is higher than 16.65m mol/L.Diabetes rat model, blood glucose, glucose in urine all remain on higher level, and prolong with the course of disease and to increase, and polydipsia, polyphagia, polyuria all occur simultaneously, become thin, performance such as movable minimizing.
Two, the lanatoside gel for eye use is used for the curative effect of prevent diabetes retinopathy
After 2 weeks, select blood glucose value to be used for experiment 30 of the rats of 350～550mgdl.Laboratory animal is fed the standardization feeding room in animal center, and raises with the standard particle feedstuff.The feeding room condition: room ventilation is good, relative humidity 40%～70%, 18～22 ℃ of room temperatures.
Divide 3 groups at random with 30 diabetes rats, 10 every group.3 groups of rats carry out administration respectively, and are specific as follows:
First group (blank group): drip normal saline, every day three times, each one, splash into (the near ear side tail of the eye) in the conjunctival sac;
Second group (positive controls): drip esculin and digitalisglycosides eye drops (Germany looks pharmaceutical factory, Turin and produces, lot number 081009), every day three times, each one, splash into (the near ear side tail of the eye) in the conjunctival sac;
The 3rd group (treatment group): drip the lanatoside gel for eye use of embodiment 2 preparations, every day three times, each one, splash into (the near ear side tail of the eye) in the conjunctival sac.
20 weeks of successive administration, check retina then, estimate according to the evaluation criterion of diabetic renal papillary necrosis, see Table 1.
Table 1 is the evaluation result of the retinopathy of rat on the same group not
Blank group diabetic renal papillary necrosis is very serious, and 20% was in for 6 phases, and 60% was in for 5 phases, and 20% was in for 4 phases.The positive controls course of disease is alleviated to some extent, and 50% was in for 3 phases, and 50% was in for 2 phases.Treatment group effect is best, and 10% was in for 2 phases, and 60% was in for 1 phase, and 30% does not see diabetic renal papillary necrosis.Experimental result shows that the lanatoside gel for eye use prevent diabetes retinopathy curative effect of gained of the present invention is obvious, and looks the esculin and digitalisglycosides eye drops that pharmaceutical factory, Turin produces significantly better than Germany.
Embodiment 4, lanatoside gel for eye use are used for the treatment of the curative effect of diabetic renal papillary necrosis
One, makes diabetes rat model
Step 1 with embodiment 1.
Two, the lanatoside gel for eye use is used for the treatment of the curative effect of diabetic renal papillary necrosis
Become the retina of 12 week of mould back observation rat, the selection retinopathy was in for 4 phases and 30 close of rats of lesion degree are used for experiment.Laboratory animal is fed the standardization feeding room in animal center, and raises with the standard particle feedstuff.Room ventilation is good, relative humidity 40%～70%, 18～22 ℃ of room temperatures.
Divide 3 groups at random with 30 diabetes rats, 10 every group.3 groups of rats carry out administration respectively, and are specific as follows:
First group (blank group): drip normal saline, every day three times, each one, splash into (the near ear side tail of the eye) in the conjunctival sac;
Second group (positive controls): drip esculin and digitalisglycosides eye drops (Germany looks pharmaceutical factory, Turin and produces, lot number 081009), every day three times, each one, splash into (the near ear side tail of the eye) in the conjunctival sac;
The 3rd group (treatment group): drip the lanatoside gel for eye use of embodiment 2 preparations, every day three times, each one, splash into (the near ear side tail of the eye) in the conjunctival sac.
10 weeks of successive administration, check retina then, estimate according to the evaluation criterion of diabetic renal papillary necrosis, see Table 2.
Table 2 is the evaluation result of the retinopathy of rat on the same group not
Claims (10)
1. the preparation method of a Digitalis extract comprises the steps:
(1) alcohol extraction is carried out in Folium Digitalis, obtained crude extract;
(2) crude extract and the sour ethanol with step (1) mixes, and leaves standstill after-filtration, obtains filtrate; Described crude extract and the alcoholic acid volume ratio of described acid are 1: 1; Described sour ethanol is the aqueous solution of ethanol and acetic acid, and alcoholic acid content is 94%-95% (quality percentage composition), and the content of acetic acid is 0.6%-0.7% (quality percentage composition);
(3) with filtrate 50-60 ℃, 0.08-0.12MPa evaporation of step (2), obtain extracting solution;
(4) extracting solution with step (3) mixes with n-butyl alcohol, abandons n-butanol layer after the layering, obtains extract;
(5) water of 4-6 times of volume of adding in the extract of step (4), the ultrafiltration post ultrafiltration through molecular cut off 10K Da obtains coarse filtration liquid; With of the ultrafiltration post ultrafiltration of coarse filtration liquid, obtain ultrafiltrate through molecular cut off 5K Da;
(6) with the ultrafiltrate evaporate to dryness of step (5), obtain Digitalis extract.
2. the method for claim 1, it is characterized in that: in the step (1), described alcohol extraction is: Folium Digitalis was extracted 1.5-2.5 hour for ethanol water 75-85 ℃ with 95% (quality percentage composition); The proportioning of described Folium Digitalis and described 95% ethanol water is 1g Folium Digitalis: 9-11mL 95% ethanol water; Described alcohol extraction is preferably: Digitalis Leaf was extracted 2 hours for 80 ℃ with described 95% ethanol water; The proportioning of described Folium Digitalis and described 95% ethanol water is 1g Folium Digitalis: 10mL 95% ethanol water.
3. method as claimed in claim 1 or 2 is characterized in that: in the step (1), carry out described alcohol extraction after, 50 ℃, 0.092MPa evaporation, evaporation back volume obtains described crude extract for the 1/23-1/24 of evaporation front volume.
4. as arbitrary described method in the claim 1 to 3, it is characterized in that: in the described step (2),, leave standstill 40 minutes after-filtration, obtain filtrate the crude extract and the mixing of sour ethanol of step (1); The alcoholic acid preparation method of described acid is: add the 0.5ml glacial acetic acid in every 100ml 95% (quality percentage composition) ethanol water.
5. as arbitrary described method in the claim 1 to 4, it is characterized in that: in the described step (3), with 55 ℃ of filtrates, the 0.1MPa evaporation of step (2), evaporation back volume obtains extracting solution for the 51%-57% of evaporation front volume; In the described step (4), the extracting solution of step (3) is mixed with the n-butyl alcohol equal-volume; In the described step (5), in the extract of step (4), add the water of 5 times of volumes; In the described step (6), the 60 ℃ of evaporates to dryness of ultrafiltrate with step (5) obtain Digitalis extract; Described Folium Digitalis Purpureae is a Digitalis purpurea L..
6. the Digitalis extract that arbitrary described method prepares in the claim 1 to 5.
7. a gel for eye use obtains with following feedstock production: the described Digitalis extract of 2.7-3.2 mass parts claim 6,145-155 mass parts NaOH, 480-520 mass parts carbomer 943,25-29 mass parts dimethyl fumarate and 49300-49350 mass parts water.
8. gel for eye use as claimed in claim 7 is characterized in that: obtain with following feedstock production: the described Digitalis extract of 3 mass parts claim 6,150 mass parts NaOH, 500 mass parts carbomers, 943,27 mass parts dimethyl fumarates and 49320 mass parts water.
9. as claim 7 or 8 described gel for eye use, it is characterized in that: prepare with the following method: described Digitalis extract water dissolution, filtering and collecting filter liquid; With described NaOH, described carbomer 943, described dimethyl fumarate water dissolution, obtain aseptic substrate after the sterilization; Described filtrate and described aseptic substrate are mixed, add entry, obtain the lanatoside gel for eye use.
10. medicine that treats and/or prevents diabetic renal papillary necrosis, its active component is arbitrary described gel for eye use in the claim 7 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102421108A CN101874848B (en) | 2009-12-08 | 2009-12-08 | Digitalis extract, preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102421108A CN101874848B (en) | 2009-12-08 | 2009-12-08 | Digitalis extract, preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101874848A true CN101874848A (en) | 2010-11-03 |
| CN101874848B CN101874848B (en) | 2012-07-04 |
Family
ID=43017593
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009102421108A Expired - Fee Related CN101874848B (en) | 2009-12-08 | 2009-12-08 | Digitalis extract, preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101874848B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115804752A (en) * | 2023-02-07 | 2023-03-17 | 天津康哲维盛医药科技发展有限公司 | Preparation method of eye drops containing digitoxin |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100428958C (en) * | 2004-09-06 | 2008-10-29 | 段亚东 | Implant agent for treating ophthalmopathy |
| CN101209312B (en) * | 2006-12-26 | 2012-05-23 | 信谊药厂 | Digitalis extract and preparation thereof |
| CN101584769A (en) * | 2008-05-22 | 2009-11-25 | 锦州奥鸿药业有限责任公司 | Novel use of esculin and digitalisglycosides eye drops |
-
2009
- 2009-12-08 CN CN2009102421108A patent/CN101874848B/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115804752A (en) * | 2023-02-07 | 2023-03-17 | 天津康哲维盛医药科技发展有限公司 | Preparation method of eye drops containing digitoxin |
| CN115804752B (en) * | 2023-02-07 | 2023-08-11 | 天津康哲维盛医药科技发展有限公司 | Preparation method of digitalis glycoside-containing eye drops |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101874848B (en) | 2012-07-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102617745B (en) | Preparation method and blood sugar lowering function of Ganoderma lucidum karst polysaccharide F31 | |
| CN103257188A (en) | Construction method for compound thrombus clearing preparation bioactivity chromatography finger print | |
| CN103919967A (en) | Dracaena cochinchinensis resin compound and application thereof in preparation of medicines for treating trauma | |
| CN103623059B (en) | A kind of pharmaceutical composition and application thereof, containing its medicament | |
| CN103432196A (en) | Desmodium styracifolium total flavonoids and preparation method of Desmodium styracifolium total flavonoids and total polysaccharides | |
| CN102068478A (en) | Safflower injection and preparation method thereof | |
| CN101874848B (en) | Digitalis extract, preparation method and application thereof | |
| CN107349244B (en) | Extraction method of malonyl ginsenoside | |
| CN101773553A (en) | Semiaquilegia root extract, preparation method and application thereof | |
| CN101224246B (en) | Preparing method of loquat leaf total triterpenic acid and antidiabetic use thereof | |
| CN107149631A (en) | A kind of method for separating and preparing of Kwangtung purple beautyberry extract and application thereof | |
| CN102327324B (en) | Mulberry leaf total alkali extract and preparation method and application thereof | |
| CN102100737B (en) | Medicinal composition containing general ginsenoside and total salvianolic acid and preparation method thereof | |
| CN102225095B (en) | Effective fraction of plantain seeds as well as preparation method and application thereof | |
| CN101332216B (en) | Xingsiang Tuerfeng total phenolic acid extract and preparation method thereof | |
| WO2022143252A1 (en) | Preparation method for pharmaceutical composition | |
| CN101249129B (en) | Chinese medicine extract combination and medicine use thereof | |
| CN101623377B (en) | Digitalis extract as well as preparation method and application thereof | |
| CN111323513A (en) | Method for detecting content of ginsenoside Re in pig brain extract-containing preparation | |
| CN105079174B (en) | A kind of tonic tablet for kidney-reinforcing and preparation method thereof | |
| CN103239435A (en) | Preparation method of gynura divaricata total caffeoylquinic acid and application in antihyperglycemic agent or health-care product | |
| AU2021101366A4 (en) | A method of preparation of ethanolic extract of IPOMEA reniformis chois in alloxan induced rats for antidiabetic effect | |
| CN108186721A (en) | A kind of preparation method of auxiliary hyperglycemic extract | |
| CN102350230A (en) | Large-aperture composite ultrafilter membrane capable of removing pyrogen and its preparation method and use | |
| CN106692216A (en) | Preparation method and application of selaginella tamariscina flavone and beta-cyclodextrin inclusion compound |
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: 20120704 Termination date: 20171208 |