CN1931205A - Kindir leaf total flavone extract and its prepn and application - Google Patents
Kindir leaf total flavone extract and its prepn and application Download PDFInfo
- Publication number
- CN1931205A CN1931205A CN 200510123187 CN200510123187A CN1931205A CN 1931205 A CN1931205 A CN 1931205A CN 200510123187 CN200510123187 CN 200510123187 CN 200510123187 A CN200510123187 A CN 200510123187A CN 1931205 A CN1931205 A CN 1931205A
- Authority
- CN
- China
- Prior art keywords
- eluent
- apocyni veneti
- folium apocyni
- general flavone
- extractive
- 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
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention is kinder leaf total flavone extract and its preparation process and application, and features that the kinder leaf total flavone extract contains total flavone in 50-95 %, including rutin 0.2-30.0 %, hyperin 0.5-30.0 %, isoquercitrin 10.0-30.0 %, trifolin 3.0-20.0 %, astragaloside 2.0-5.0 %, 6''-O-acetyl isoquercitrin 1.0-6.0 %, quercitrin 0.5-4.0 %, trifolitin 0.2-3.0 %, etc. The kinder leaf total flavone extract is applied in preparing medicine for treating cardiac and cerebral ischemia.
Description
Technical field:
The present invention relates to Kindir leaf total flavone extract, this preparation method of extract, Chinese medicine preparation, and the application in treatment cardiac-cerebral ischemia medicine.
Background technology:
China's Folium Apocyni Veneti resource has three kinds: Kindir leaf (Apocynum venetum L.) claims ambary, abutilon poacynum hendersonii woodson leaf [Poacynum hendersonni (Hook.f.) Wodson] and abutilon purpura Folium Apocyni Veneti [Poacynum pictum (Schrenk) Baill] again, be referred to as Folium Apocyni Veneti, because of belonging to not congener, its flavone component also has different, there is no comparability each other.That involved in the present invention is Kindir leaf (Apocynumvenetum L.), comprises the Apocynum plant ambary leaf (Apocynum venetum L.) that produce in Xinjiang.
The method of research Herba Apocyni veneti effective ingredient can reduce two kinds at present:
1, first water or alcohol extraction are suspended from the extract mixture behind the recovery solvent in the water, use chloroform, ethyl acetate, n-butanol extraction respectively, are divided into several extraction parts.Reuse silicagel column or polydextran gel column chromatography, be separated into the one pack system material.
The application for a patent for invention " a kind of Herba Apocyni veneti extract and extracting method thereof " of 2, the application for a patent for invention of application number 02110431.X " extraction separation method of effective part from dogbane " and application number 200410064551.0.
Above-mentioned first method is the method for the single flavone component of laboratory study, is not suitable for the preparation of total flavones.In the second method, the patent application of last item for the extraction separation method of effective part from dogbane is: the Herba Apocyni veneti extracting solution passes through macroporous adsorptive resins after treatment, adopt water elution colourless earlier to water elution liquid, and with the ethanol water eluting of 20-39%, the ethanol water eluting of reuse 40-70%.The extractum of collecting the eluent concentrated back formation of 40-70% is effective site, general flavone content is 50-60%, the shortcoming of this technical scheme is: can not the clear and definite effective site that provides which flavone component be made of, though it is 50-60% that the effective site general flavone content is provided, but also do not reach the standard of used for intravenous injection two class crude drug, promptly more than 80%.In second patent application be: get Folium Apocyni Veneti 300g for the high-purity preparation method of extract of Herba Apocyni veneti, measure 40% ethanol water reflux, extract, 3 times with 10 times, each 0.5hr, merge extractive liquid,, standing over night under the room temperature, filter, go precipitation, filtrate decompression is concentrated into cumulative volume 900mL, concentrated solution adds the acetic acid solution 180mL of 1% chitosan, stir 2min, room temperature leaves standstill 2-4hr, sucking filtration, discard residue, supernatant is crossed the polyamide resin column of handling well, subsequently with 600mL water, transfer pH to be 3 with hydrochloric acid after, carry out the eluting remove impurity, then with 70% ethanol water eluting to there not being AlCl
3Reaction is collected 70% ethanol water and is evaporated near doing, and behind the water bath method, 80 ℃ of oven dried get yellowish-brown to yellow powder, are the high-purity extract of Herba Apocyni veneti, and paste-forming rate is 1.8%.The hyperin content of the high-purity extract of Herba Apocyni veneti is 17.8%, total flavones (in hyperin) content is 42.8%, the quercetin content after the hydrolysis is 36.7%.The existing problem of this technical scheme is: though quercetin content after hyperin content, general flavone content, the hydrolysis is provided, can not which flavone component be made of by clear and definite extract, can not intactly reflect this extract quality; This extractive total flavone (in hyperin) content is 42.8%, and this content had not both reached the standard of used for intravenous injection two class crude drug, promptly more than 80%, does not also reach the standard of two class crude drug for oral use, promptly more than 50%.
Folium Apocyni Veneti (Apocynum venetum L.) contains constituents surplus flavone and glucosides, triterpene and sterol, lignanoid, coumarin, organic acid and ester, cyclic alcohol, saccharide and the aminoacid etc. 10 thereof according to the literature.Pharmacological research shows that flavones ingredient is one of main active classification wherein, and chemical research shows the Folium Apocyni Veneti flavones ingredient, and " 8 kinds of component contents such as O-acetyl group isoquercitrin, Quercetin and nimbecetin are higher with rutin, hyperin, isoquercitrin, Trifolin, astragaloside, 6.The extract that different extracting method obtains is owing to comprise different flavone compounds, different content, and there are very big-difference in its pharmacology, the property of medicine, all are a kind of new materials.Therefore under the prerequisite that guarantees drug effect, improve as far as possible that main flavones ingredient is technological difficulties in the purity of extractive total flavone and the clear and definite extract.
Chinese medicine Herba Apocyni veneti and preparation thereof are at present clinical to be to be used for the treatment of high blood pressure disease, does not see the report that is used for the treatment of cerebral ischemia diseases as yet.
Summary of the invention:
The present invention is for avoiding above-mentioned existing in prior technology problem, a kind of high-load Kindir leaf total flavone extract is provided, and pharmacology and chemical research show that this extract active component is clear and definite, quality controllable.
Another purpose of the present invention provides the preparation method of this Folium Apocyni Veneti extractive of general flavone.
Another object of the present invention is to provide the Chinese medicine preparation of described extract.
The object of the invention also is to provide the application of this Folium Apocyni Veneti extractive of general flavone in the treatment cardiac-cerebral ischemia diseases.
The present invention seeks to be achieved through the following technical solutions:
Kindir leaf total flavone extract of the present invention is characterized in that described extractive total flavone content is 50-95%; Wherein contained flavone component comprises: rutin 0.2-30.0%, hyperin 0.5-30.0%, isoquercitrin 10.0-30.0%, Trifolin 3.0-20.0%, astragaloside 2.0-5.0%, 6 " O-acetyl group isoquercitrin 1.0-6.0%, Quercetin 0.5-4.0%, nimbecetin 0.2-3.0%, other flavones ingredient surpluses.
Folium Apocyni Veneti extractive of general flavone preparation method of the present invention is to operate as follows:
A, exsiccant Folium Apocyni Veneti is ground into coarse powder, the 30-95% alcohol heating reflux of doubly measuring with 8-10 extracted 1-2 hour, extracted 2-3 time altogether;
Wherein, the ethanol that is used for reflux, extract, is preferably 60-80% ethanol.
B, proportion was the extractum of 1.13-1.16 when extracting solution was evaporated to 60 ℃ under being lower than 60 ℃ condition, added primary dose 3-5 and doubly measured boiling water, and filtration in 24 hours is left standstill in the gradation dissolving;
C, filtrate are by polyamide column chromatography, and at first water washes 8-12 column volume, reuse variable concentrations alcohol-water solution stepwise elution, collection, concentrated, and described stepwise elution, collection, spissated operating process are:
With 10%-20% ethanol water or 1-2 column volume of 10%-20% methanol aqueous solution eluting, remove eluent;
With 40-50% ethanol water or 40-50% methanol aqueous solution eluting, according to the sequencing of elution time, Fractional Collections obtains leading portion eluent, stage casing eluent and back segment eluent respectively, removes the leading portion eluent,
With 70-80% ethanol water or 70-80% methanol aqueous solution eluting, collect eluent; After this eluent and the merging of described back segment eluent, be lower than concentrating under reduced pressure under 60 ℃ of conditions, vacuum drying gets the Folium Apocyni Veneti extractive of general flavone that general flavone content reaches 50%-70%;
Described stage casing eluent is being lower than concentrating under reduced pressure under 60 ℃ of conditions, and vacuum drying gets the Folium Apocyni Veneti extractive of general flavone that general flavone content reaches 80%-95%.
The Chinese medicine preparation of Kindir leaf total flavone extract of the present invention, it is characterized in that described Chinese medicine preparation is is the medicine active ingredient with described Folium Apocyni Veneti extractive of general flavone, adds drop pill, tablet, capsule, soft capsule, granule, suspensoid, oral liquid, injectable powder, injection, the transfusion of making behind the pharmaceutic adjuvant.
Kindir leaf total flavone extract of the present invention is used for the treatment of ischemic cardiovascular and cerebral vascular disease.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, Herba Apocyni veneti extract of the present invention is with general flavone content, rutin, hyperin, isoquercitrin, Russian red clover, astragaloside, 6, and " content of O-acetyl group isoquercitrin, Quercetin, nimbecetin carries out definite sign to it; the Flavonoid substances and the Folium Apocyni Veneti extractive of general flavone that characterize with this characteristic manner have significant anti-cerebral ischemia effect, there is no the report of pertinent literature.
2, the present invention adopts high performance liquid chromatography, can be to " flavone component of O-acetyl group isoquercitrin, Quercetin, nimbecetin carries out clear and definite qualitative and quantitative to rutin, hyperin, isoquercitrin, Trifolin, astragaloside, 6 in the extract.
3, dogbane leaf extractive of the present invention is to extract gained with new extracting method from Folium Apocyni Veneti, for ischemic cardiovascular and cerebral vascular disease reliable curative effect is arranged.
4, the present invention forms hydrogen bond according to the amide groups of the phenolic hydroxyl group of phenolic constituents such as flavone in the Folium Apocyni Veneti and polyamide and the principle of being adsorbed by polyamide, designed Folium Apocyni Veneti ethanol extraction water dissolution, adsorb by polyamide column, the impurity that elder generation's water flush away is not adsorbed, and be phenolic acid compositions such as composition such as chlorogenic acid with the low phenol of 10%-20% ethanol water flush away, reuse 40%-80% ethanol water tears degree eluting flavone component, and polyphenol composition tannin is retained on the post, thereby reaches the enrichment flavone component; When 40%-80% ethanol water tears degree eluting flavone component, according to elution curve, Fractional Collections concentrates, and is two crude drug of 50%-95% thereby obtain general flavone content, respectively as oral and raw material intravenous formulations.
5, the present invention can satisfy the requirement of a vast cardiac-cerebral ischemia patient to different dosage form.
Kindir leaf total flavone extract of the present invention, its extraction and separation process is not limited only to above-mentioned technology, also can adopt other extraction separation means to obtain.
Utilize general flavone content and each constituent content assaying method of the Kindir leaf total flavone extract that above-mentioned technology obtains to be:
1, after the Folium Apocyni Veneti extractive of general flavone drying, the mensuration of general flavone content adopts NaNO
2-Al (NO
2)
3-NaOH complexation colorimetry is measured, and it is 50-95% that this product contains total flavones (in rutin).
2. after the Folium Apocyni Veneti extractive of general flavone drying; constituent: the assay of rutin (Rutin), hyperin (Hyperin), isoquercitrin (Isoquercetin), Trifolin (Trifolin), astragaloside (Astragalin), 6 " O-acetyl group isoquercitrin (Isoquercetin-6 "-O-acetate), Quercetin (Quercetin) and nimbecetin (Kaempferol) all adopts high performance liquid chromatography, and each component content is seen embodiment 1-3.
Illustrate its drug action with The pharmacological results below
One, Folium Apocyni Veneti total flavones (AVTF) is to the influence of cerebral ischemia
1, AVTF is to the influence of the time of breathing of dehiscing behind the mice broken end
The result is as shown in table 1, and 40,80,100mg.kg
-1AVTF dehisces the time of breathing after can obviously prolonging the mice broken end, and is certain dose-effect relationship.
Table 1 AVTF is to the influence of the time of breathing of dehiscing behind the mice broken end (x ± s)
| Group | Dosage (mg.kg -1) | N | (sec) dehisces the time of breathing | Prolong percentage rate (%) |
| Contrast EGB AVTF | - 60 40 80 100 | 10 8 8 10 8 | 18.0±2..2 19.5±1.6 21.0±1.6** 22.8±1.8** 24.8±3.0** | - 8.3 16.7 26.7 37.8 |
Compare with matched group,
*P＜0.05.
2, AVTF to cerebral infarction tissue weight influence
The result is as shown in table 2, has tangible cerebral infarction to take place behind the rat MCAO, and AVTF can significantly reduce cerebral infarction tissue weight percentage ratio, at 25～100mg.kg
-1Be certain dose-effect relationship in the scope.
Table 2 AVTF causes the influence (x ± s) of rat cerebral infarction tissue weight to MCAO
| Group | Dosage mg.kg -1 | N | Infraction brain weight percentage ratio (%) | Suppression ratio (%) |
| Sham contrast EGB AVTF | - - 100 25 50 100 | 8 8 8 8 8 8 | 1.5±0.4 ** 18.4±1.7 13.6±2.0 ** 14.6±3.1 * 14.4±3.2 ** 13.6±3.0 ** | - - 26.0 20.5 21.6 26.0 |
Compare with matched group,
*P＜0.05,
*P＜0.01.
Two, Folium Apocyni Veneti total flavones (AVTF) is to thrombotic influence
The result is as shown in table 4, but the formation of rat carotid artery-vein loop hyperamization bolt, 25,50,100mg.kg
-1AVTF can obviously reduce the weight in wet base of thrombosis.
The influence of table 3 pair collagen hyperamization platelet aggregation rate (x ± s, n=8)
| Group | Concentration (mg.ml -1) | 2min(％) | 5min(％) | ||
| Aggregation rate | Suppress percentage rate | Aggregation rate | Suppress percentage rate | ||
| Contrast EGB AVTF | - 0.10 0.025 0.050 0.100 | 23.8±3.0 11.9±2.8 ** 10.2±1.9 ** 6.6±2.3 ** 5.2±2.0 ** | - 50.1 57.0 72.1 78.0 | 26.8±3.4 13.1±3.0 ** 11.8±4.0 ** 6.5±3.4 ** 5.9±1.6 ** | - 51.0 60.1 75.5 78.1 |
Compare with matched group,
*P＜0.01.
Table 4 AVTF causes thrombotic influence (x ± s) to rat carotid artery-vein loop
| Group | Dosage (mg.kg -1) | n | Wet weight of thrombus (mg) |
| Contrast EBG AVTF | - 100 25 50 100 | 9 10 10 8 4 | 8.39±2.51 6.12±1.92 * 5.65±1.11 * 5.10±2.51 ** 3.01±1.24 ** |
Compare with matched group,
*P＜0.05,
*P＜0.01.
Three, conclusion
The model of dehiscing to breathe behind l, the mice broken end is a screening study anti-cerebral ischemia, an anoxic medicine experimental technique preferably, and its characteristics are good reproducibility, fast and convenient.On this model, originally discover 40,80,100mg.kg
-1Folium Apocyni Veneti total flavones (AVTF) is dehisced the time of breathing after can obviously prolonging the mice broken end; Rat MCAO is the animal model of a research cerebral ischemia of using always, and is comparatively approaching with the damage of people's cerebral infarction.This research is found on this model, with 100mg.kg
-1EGB is the same, at 25-100mg.kg
-1In the scope, the Folium Apocyni Veneti total flavones can significantly alleviate cerebral tissue infraction weight, and is certain dose-effect relationship.These results show that the Folium Apocyni Veneti total flavones has protective effect to cerebral ischemia, hypoxic damage.
2, the Folium Apocyni Veneti total flavones is at 0.025-0.100mg.ml
-1In the scope, can significantly suppress the rabbit platelet aggregation reaction that Coll brings out, show that the Folium Apocyni Veneti total flavones has tangible antiplatelet aggregative activity.
3, on rat carotid artery-vein bypass thrombotic model, 25,50,100mg.kg
-1The Folium Apocyni Veneti total flavones can obviously reduce the weight in wet base of thrombosis, and prompting Folium Apocyni Veneti total flavones has inhibitory action to thrombosis.
In sum, the Folium Apocyni Veneti total flavones has protective effect to ischemic brain injury.
Description of drawings:
Fig. 1 is Kindir leaf (Apocynum venetum L.) extractive of general flavone HPLC collection of illustrative plates.
This collection of illustrative plates can be to the constituent of Folium Apocyni Veneti extractive of general flavone: " flavone component of O-acetyl group isoquercitrin, Quercetin, nimbecetin carries out clear and definite qualitative and quantitative for rutin, hyperin, isoquercitrin, Trifolin, astragaloside, 6.
Fig. 2 is Apocynum plant Xinjiang ambary leaf (Apocynum venetum L.) extractive of general flavone HPLC collection of illustrative plates.
This collection of illustrative plates can be to the constituent of ambary leaf total flavone extract: " flavone component of O-acetyl group isoquercitrin, Quercetin, nimbecetin carries out clear and definite qualitative and quantitative for rutin, hyperin, isoquercitrin, Trifolin, astragaloside, 6.
The specific embodiment:
Below by embodiment the preparation method of Kindir leaf total flavone extract extracting method and preparation thereof is described in further detail.
For the preparation of Folium Apocyni Veneti extractive of general flavone, specific operation process is as follows:
1, exsiccant Folium Apocyni Veneti is ground into coarse powder, the 30-95% ethanol water heating and refluxing extraction of doubly measuring with 8-10 1-2 hour is extracted 2-3 time altogether;
Proportion is the extractum of 1.13-1.16 when 2, extracting solution being evaporated to 60 ℃ under being lower than 60 ℃ condition, adds primary dose 3-5 and doubly measures boiling water, and filtration in 24 hours is left standstill in the gradation dissolving;
3, filtrate is by polyamide column chromatography, and at first water washes 8-12 column volume, reuse variable concentrations alcohol-water solution stepwise elution, collection, concentrated, and operating process is:
With 40-50% ethanol water or 3 column volumes of 40-50% methanol aqueous solution eluting, with the eluent of per 0.5 column volume is 1 part, sequencing according to elution time, Fractional Collections, obtain first section to the 6th section totally 6 parts of eluents respectively, remove first section eluent, and close wherein that the 2nd to the 4th section eluent gets the stage casing eluent, and close wherein that the 5th, the 6th section eluent gets the back segment eluent;
With 70-80% ethanol water or 1-2 column volume of 70-80% methanol aqueous solution eluting, collect eluent; After this eluent and the merging of back segment eluent, be lower than concentrating under reduced pressure under 60 ℃ of conditions, vacuum drying gets the Folium Apocyni Veneti extractive of general flavone that general flavone content reaches 50%-70%;
The stage casing eluent is being lower than concentrating under reduced pressure under 60 ℃ of conditions, and vacuum drying gets the Folium Apocyni Veneti extractive of general flavone that general flavone content reaches 80%-95%.
Embodiment 1:
Get Kindir leaf crude drug coarse powder 1kg, add 10 times of amount 80% ethanol water heating and refluxing extraction 2 hours, extract altogether 3 times, merge extractive liquid, is put coldly, filters, decompression recycling ethanol is not when having alcohol, and to be concentrated into 60 ℃ of relative densities be 1.13 extractum; Add the boiling water that is equivalent to 5 times of amounts of crude drug, gradation is stirred and is made dissolving, filter, filtrate is added on the polyamide column of handling well according to a conventional method, behind 10 column volumes of water flushing, with 2 column volumes of 10% ethanol water eluting, 3 column volumes of 50% ethanol water eluting, 2 column volumes of 70% ethanol water eluting, Fractional Collections 50% ethanol water, the eluent of per 0.5 column volume is 1 part, collects the 4th part of eluent of 2-; The the 5th, the 6th part of eluent of 70% ethanol water eluting liquid and 50% ethanol water merges, and is being lower than concentrating under reduced pressure under 60 ℃ of conditions respectively, and vacuum drying gets Folium Apocyni Veneti extractive of general flavone A and Folium Apocyni Veneti extractive of general flavone B.
It is 1.2% that 50% ethanol water gets Folium Apocyni Veneti extractive of general flavone A recovery rate; its total flavones (in rutin) content is 90.5%, rutin 1.10%, hyperin 24.41%, isoquercitrin 25.60%, Trifolin 5.50%, astragaloside 4.10%, 6 " O-acetyl group isoquercitrin 2.81%, Quercetin 2.07%, nimbecetin 1.50%, and other several flavones ingredients.
It is 0.6% that 70% ethanol water gets Folium Apocyni Veneti extractive of general flavone B recovery rate; its total flavones (in rutin) content is 61.5%, rutin 0.51%, hyperin 5.21%, isoquercitrin 23.10%, Trifolin 8.75%, astragaloside 4.21%, 6 " O-acetyl group isoquercitrin 5.15%, Quercetin 2.95%, nimbecetin 1.90%, and other several flavones ingredients.
Embodiment 2:
Get ambary leaf crude drug coarse powder 1kg, add 8 times of amount 70% ethanol water heating and refluxing extraction 2 hours, extract altogether 3 times, merge extractive liquid, is put coldly, filters, and decompression recycling ethanol is not when having alcohol, and to be concentrated into 60 ℃ of relative densities be 1.14 extractum; Add the boiling water that is equivalent to 4 times of amounts of crude drug, gradation is stirred and is made dissolving, filter, filtrate is added on the polyamide column of handling well according to a conventional method, behind 10 column volumes of water flushing, with 1 column volume of 10% ethanol water eluting, with 3 column volumes of 50% ethanol water eluting, 2 column volumes of 80% ethanol water eluting, Fractional Collections 50% ethanol water, the eluent of per 0.5 column volume is 1 part, collects the 4th part of eluent of 2-; The the 5th and the 6th part of eluent of 80% ethanol water eluting liquid and 50% ethanol water merges, and is being lower than concentrating under reduced pressure under 60 ℃ of conditions respectively, and vacuum drying gets ambary leaf total flavone extract A and ambary leaf total flavone extract B.
It is 1.7% that 50% ethanol water gets ambary leaf total flavone extract A recovery rate; its total flavones (in rutin) content is 85.0%, rutin 25.81%, hyperin 1.93%, isoquercitrin 28.70%, Trifolin 12.47%, astragaloside 3.61%, 6 " O-acetyl group isoquercitrin 1.38%, Quercetin 0.80%, nimbecetin 0.50%, and other several flavones ingredients.
It is 0.4% that 80% ethanol water gets ambary leaf total flavone extract B recovery rate; its total flavones (in rutin) content is 60.5%, rutin 1.05%, hyperin 2.59%, isoquercitrin 25.06%, Trifolin 15.08%, astragaloside 3.99%, 6 " O-acetyl group isoquercitrin 4.05%, Quercetin 1.50%, nimbecetin 0.78%, and other several flavones ingredients.
Embodiment 3:
Get Folium Apocyni Veneti crude drug coarse powder 1kg, add 8 times of amount 60% ethanol water heating and refluxing extraction 2 hours, extract altogether 3 times, merge extractive liquid, is put coldly, filters, and decompression recycling ethanol is not when having alcohol, and to be concentrated into 60 ℃ of relative densities be 1.16 extractum; Add the boiling water that is equivalent to 4 times of amounts of crude drug, gradation is stirred and is made dissolving, filter, filtrate is added on the polyamide column of handling well according to a conventional method, 10 column volumes of water flushing, with 1 column volume of 10% ethanol water eluting, with 3 column volumes of 40% methanol aqueous solution eluting, 2 column volumes of 70% methanol aqueous solution eluting, Fractional Collections 40% methanol aqueous solution, the eluent of per 0.5 column volume is 1 part, collects the 4th part of eluent of 2-; The the 5th and the 6th part of eluent of 70% methanol aqueous solution eluent and 40% methanol aqueous solution merges, and is being lower than concentrating under reduced pressure under 60 ℃ of conditions respectively, and vacuum drying gets Folium Apocyni Veneti extractive of general flavone A and Folium Apocyni Veneti extractive of general flavone B.
It is 1.4% that 40% methanol aqueous solution gets Folium Apocyni Veneti extractive of general flavone A recovery rate; its total flavones (in rutin) content is 81.5%, rutin 1.20%, hyperin 23.05%, isoquercitrin 25.57%, Trifolin 5.21%, astragaloside 4.07%, 6 " O-acetyl group isoquercitrin 1.80%, Quercetin 2.60%, nimbecetin 0.75%, and other several flavones ingredients.
It is 0.65% that 70% methanol aqueous solution gets Folium Apocyni Veneti extractive of general flavone B recovery rate; its total flavones (in rutin) content is 60.0%, rutin 0.50%, hyperin 5.20%, isoquercitrin 23.05%, Trifolin 8.20%, astragaloside 3.75%, 6 " O-acetyl group isoquercitrin 4.50%, Quercetin 2.10%, nimbecetin 1.80%, and other several flavones ingredients.
Embodiment 4: Folium Apocyni Veneti total flavones sheet
Group component
Folium Apocyni Veneti extractive of general flavone 1-100g
Dextrin 90g
Microcrystalline Cellulose 105g
Low-substituted hydroxypropyl methylcellulose 15g
70% alcoholic solution 15ml
Magnesium stearate 1g
Preparation process: Folium Apocyni Veneti extractive of general flavone, dextrin, magnesium stearate, low-substituted hydroxypropyl methylcellulose pulverize separately are crossed 80 mesh sieves; With Herba Apocyni veneti total flavones and dextrin, the low-substituted hydroxypropyl methylcellulose of 2/3 amount and 70% alcoholic solution mixed grinding, make evenly the system soft material; 20 mesh sieve system granules again, drying adds remaining low-substituted hydroxypropyl methylcellulose behind the granulate, and mixing adds the magnesium stearate mixing again, presses 1000; Pack after the assay was approved.
Embodiment 5: the Folium Apocyni Veneti flavone dripping pill
Group component
Folium Apocyni Veneti extractive of general flavone 1-50g
PEG4000 15g
PEG6000 22g
Preparation process: with Macrogol 4000, polyethylene glycol 6000 heating, again fusion Folium Apocyni Veneti extractive of general flavone is added wherein, fully stir, medicine is well-dispersed in the substrate; Above-mentioned medicinal liquid is transferred on the drop pill machine, and 70 ℃～80 ℃ airtight insulations 10～20 minutes are made coolant with anhydrous methyl-silicone oil, and 10 ℃～20 ℃ gradients coolings with 30～60/component velocity system of dripping, promptly get the molding pill.Regather drop pill, with 30～60/component velocity system of dripping, promptly get the molding pill with the washing of dry oil ether.Regather drop pill, with dry oil ether washing 2 times, airing, packing gets final product.
Embodiment 6: the transfusion of Folium Apocyni Veneti total flavones
With preparation content is that the Folium Apocyni Veneti total flavones infusion preparation 250ml bottle of 0.04% (g/ml) is an example.
After 2g Folium Apocyni Veneti extractive of general flavone joined 1000ml fresh water for injection heating for dissolving, add 5 gram needle-use activated carbons, 20 minutes after-filtration of heated and boiled, filtrate is cooled to below 40 ℃, be diluted to 5000ml with fresh water for injection, it is about 7.0 that the sodium bicarbonate of reuse 1mol/L is transferred PH, adds 45 gram medicinal sodium chloride and the medicinal sodium sulfite stirring and dissolving of 6g, makes it to become to contain 0.4 gram Herba Apocyni veneti total flavones in the 1L solution.Survey pH, content qualified after, aseptic canning in 115 ℃ of following pressure sterilizings 30 minutes, promptly gets every bottle of 250ml solution and contains 0.1g Folium Apocyni Veneti total flavones infusion preparation in the 250ml infusion bottle.
Embodiment 7: Folium Apocyni Veneti total flavones freeze-dried powder
Group component
Folium Apocyni Veneti extractive of general flavone 5-100g
Tween 80 120g
Active carbon 4g
Mannitol 400g
The husky nurse 8g of pool network
Preparation process: take by weighing the husky nurse of Folium Apocyni Veneti extractive of general flavone dry powder, tween, pool network and mortar is put in its fusion ground it is fully disperseed, the fresh water for injection that adds the saturated mistake of carbon dioxide is to 3500ml, add mannitol, add needle-use activated carbon in water-bath (50-70 ℃), stir while adding, after boiling 5-10 minute, be cooled to 40 ℃ and filter with the incipient fusion filter.Be diluted to 4000ml with fresh water for injection, survey pH, content qualified after,, cross the 0.45um film, after the 0.22um film, in 1000 cillin bottles of fill, pre-freeze freezingly promptly gets every bottle and contains 5-100mg Herba Apocyni veneti extractive of general flavone lyophilized powder.
Embodiment 8: the Folium Apocyni Veneti total flavone injection
Group component
Folium Apocyni Veneti extractive of general flavone 5-50g
Sodium bicarbonate 12g
Sodium pyrosulfite 2g
Water for injection 1000m
Preparation process: get water for injection 1000ml, boil, be cooled to room temperature, standby.Get the injection of configuration amount 20% by prescription and get water for injection 1000ml, boil, be cooled to room temperature, standby.Get the water for injection of configuration amount 20% by prescription, add the Folium Apocyni Veneti extractive of general flavone and make dissolving, gradation slowly adds sodium bicarbonate and constantly stirs, and when treating that liquid level does not have the bubble generation, adds the sodium pyrosulfite dissolving, adds remaining water for injection to full dose.With the PH acidometer measure liquid PH value should be 5.5-8.0, if not in this scope, available sodium bisulfate is regulated.Medicinal liquid filters to clear and bright with No. 3 incipient fusion glass pans, 500 ampoules of embedding, and 100 ℃, sterilization in 30 minutes, promptly.
Embodiment 9: Folium Apocyni Veneti total flavones soft capsule
Group component
Folium Apocyni Veneti extractive of general flavone 5-100g
Cera Flava 10g
Edible vegetable oil 150g
Gelatin 10g
Glycerol 3g
Water 13g
Preparation process: take by weighing the Folium Apocyni Veneti extractive of general flavone and mix, fully stir evenly and promptly get capsule core material through heat sterilization, clarifying edible vegetable oil and Cera Flava fused mass.Get gelatin adding suitable quantity of water and make its expansion; In addition the water of glycerol and remainder is put and be heated to 70 ℃～80 ℃ in the glue pot, mix homogeneously adds expansible gelatin and stirs, and fusing is incubated 1-2 hour, leaves standstill, and makes the foam come-up, removes the foam of come-up, filters heat preservation for standby use with clean calico.With the gelatin solution that has made, put and control temperature in the gelatin solution storage tank about 60 ℃, the Folium Apocyni Veneti extractive of general flavone is put into liquor tank; The liquid Paraffin temperature is advisable with 10-25 ℃, and room temperature 10-20 ℃, 30-60 ℃ of water dropper temperature, beginning drop pill.Evenly the stall with goods spread out on the ground for sale was on gauze earlier for the soft gelatin capsule that oozes, and more than 4 hours, the reuse pill wiping machine is wiped the paraffin on surface in the blowing of low temperature below 10 ℃, and then low temperature (below 10 ℃) blowing is more than 20 hours, in about 24 hours of 40-50 ℃ of drying.Take out exsiccant soft gelatin capsule, lamp inspection, remove useless ball after, use 95% washing with alcohol, again drying up below 40-50 ℃, after quality examination is qualified, can pack.
Embodiment 10: the agent of Folium Apocyni Veneti total flavone capsule
Group component
Folium Apocyni Veneti extractive of general flavone 5-100g
Starch 125g
70% ethanol is an amount of
Preparation process: with starch, Folium Apocyni Veneti extractive of general flavone mixing, cross 80 mesh sieves, add 70% an amount of ethanol, the system soft material, reuse 20 mesh sieve system granules, drying, granulate, encapsulated, make 1000 altogether, every contains Folium Apocyni Veneti extractive of general flavone 5-100mg, gets final product.
Embodiment 11: Folium Apocyni Veneti total flavones granule
Group component
Folium Apocyni Veneti extractive of general flavone 1-10g
Dextrin 28g
Icing Sugar 10g
Tartaric acid 1g
50% ethanol (volume fraction) is an amount of
Folium Apocyni Veneti extractive of general flavone, dextrin, Icing Sugar are crossed 100 mesh sieves respectively, increase progressively the facing-up method with Folium Apocyni Veneti flavonid composition and auxiliary materials and mixing by equal-volume, tartaric acid is dissolved in 50% ethanol (volume fraction) again, once adds in the said mixture mixing, the system soft material, cross 16 order nylon mesh, dry below 60 ℃, use plastic bag packaging behind the granulate, every bag of 2g contains Folium Apocyni Veneti extractive of general flavone 50-500mg.
Embodiment 12: Folium Apocyni Veneti total flavones suspensoid
Group component
Folium Apocyni Veneti extractive of general flavone 5-50g
Carboxymethyl cellulose sodium 5g
Glycerol 100ml
Distilled water is an amount of
Preparation process: get the Folium Apocyni Veneti extractive of general flavone in mortar, glycerol adding grinds to form fine and smooth pasty state, in addition Carboxymethyl cellulose sodium is made rubber cement with 200ml water, under agitation slowly add in the mortar and grind well, move in the measuring device, adding distil water is to full dose, stir evenly, promptly.
Embodiment 13: Folium Apocyni Veneti total flavones oral liquid
Group component
Folium Apocyni Veneti extractive of general flavone 2-50g
Refined honey 30g
Sorbic acid 5g
Sodium citrate 5g
Essence 1ml
Water is an amount of
Preparation process: the Folium Apocyni Veneti extractive of general flavone is soluble in water, add refined honey, sorbic acid, sodium citrate, essence mixing, make 200ml, encapsulation, promptly.
Above embodiment is only for the invention will be further described, and the scope of the invention is not subjected to the limitation of illustrated embodiment.
Claims (6)
1, a kind of Kindir leaf total flavone extract is characterized in that described extractive total flavone content is 50-95%; Wherein contained flavone component comprises: rutin 0.2-30.0%, hyperin 0.5-30.0%, isoquercitrin 10.0-30.0%, Trifolin 3.0-20.0%, astragaloside 2.0-5.0%, 6 " O-acetyl group isoquercitrin 1.0-6.0%, Quercetin 0.5-4.0%, nimbecetin 0.2-3.0%, other flavones ingredient surpluses.
2, the preparation method of the described Folium Apocyni Veneti extractive of general flavone of claim 1 is characterized in that operating as follows:
A, exsiccant Folium Apocyni Veneti is ground into coarse powder, the 30-95% ethanol water heating and refluxing extraction of doubly measuring with 8-10 1-2 hour is extracted 2-3 time altogether;
B, proportion was the extractum of 1.13-1.16 when extracting solution was evaporated to 60 ℃ under being lower than 60 ℃ condition, added primary dose 3-5 and doubly measured boiling water, and filtration in 24 hours is left standstill in the gradation dissolving;
C, filtrate are by polyamide column chromatography, and at first water washes 8-12 column volume, reuse variable concentrations alcohol-water solution stepwise elution, collection, concentrated, and described stepwise elution, collection, spissated operating process are:
With 10-20% ethanol water or 1-2 column volume of 10-20% methanol aqueous solution eluting, remove eluent;
With 40-50% ethanol water or 40-50% methanol aqueous solution eluting, according to the sequencing of elution time, Fractional Collections obtains leading portion eluent, stage casing eluent and back segment eluent respectively, removes the leading portion eluent;
With 70-80% ethanol water or 70-80% methanol aqueous solution eluting, collect eluent; After this eluent and the merging of described back segment eluent, be lower than concentrating under reduced pressure under 60 ℃ of conditions, vacuum drying gets the Folium Apocyni Veneti extractive of general flavone that general flavone content reaches 50%-70%;
Described stage casing eluent is being lower than concentrating under reduced pressure under 60 ℃ of conditions, and vacuum drying gets the Folium Apocyni Veneti extractive of general flavone that general flavone content reaches 80%-95%.
3, method according to claim 2 is characterized in that stepwise elution, collection, the spissated operating process in described step c is:
With 40-50% ethanol water or 3 column volumes of 40-50% methanol aqueous solution eluting, with the eluent of per 0.5 column volume is 1 part, sequencing according to elution time, Fractional Collections, obtain first section to the 6th section totally 6 parts of eluents respectively, remove first section eluent, and close wherein that the 2nd to the 4th section eluent gets the stage casing eluent, and close wherein that the 5th, the 6th section eluent gets the back segment eluent;
With 70-80% ethanol water or 1-2 column volume of 70-80% methanol aqueous solution eluting, collect eluent; After this eluent and the merging of back segment eluent, be lower than concentrating under reduced pressure under 60 ℃ of conditions, vacuum drying gets the Folium Apocyni Veneti extractive of general flavone that general flavone content reaches 50%-70%;
The stage casing eluent is being lower than concentrating under reduced pressure under 60 ℃ of conditions, and vacuum drying gets general flavone content and reaches 80%-95% Folium Apocyni Veneti extractive of general flavone.
4, method according to claim 2, the ethanol that it is characterized in that being used among the described step a reflux, extract, is 60-80% ethanol.
5, the Chinese medicine preparation of claim 1 or 2 described Kindir leaf total flavone extracts, it is characterized in that described Chinese medicine preparation is is the medicine active ingredient with described Folium Apocyni Veneti extractive of general flavone, adds drop pill, tablet, capsule, soft capsule, granule, suspensoid, oral liquid, injectable powder, injection, the transfusion of making behind the pharmaceutic adjuvant.
6, the described Kindir leaf total flavone extract of claim 1 is used for the treatment of ischemic cardiovascular and cerebral vascular disease.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2005101231875A CN1931205B (en) | 2005-12-16 | 2005-12-16 | Kindir leaf total flavone extract and its preparation and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2005101231875A CN1931205B (en) | 2005-12-16 | 2005-12-16 | Kindir leaf total flavone extract and its preparation and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1931205A true CN1931205A (en) | 2007-03-21 |
| CN1931205B CN1931205B (en) | 2011-04-13 |
Family
ID=37877327
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2005101231875A Expired - Fee Related CN1931205B (en) | 2005-12-16 | 2005-12-16 | Kindir leaf total flavone extract and its preparation and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1931205B (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101690739B (en) * | 2009-06-30 | 2011-07-13 | 长春师范学院 | Preparation method of dogbane leaf extractive |
| CN102286575A (en) * | 2011-09-14 | 2011-12-21 | 江苏科技大学 | Method for synthesizing isoquercitrin by metal ion-reinforced enzyme method |
| CN102603831A (en) * | 2011-01-25 | 2012-07-25 | 苏州宝泽堂医药科技有限公司 | Preparation method of high-content trifolin |
| CN103830292A (en) * | 2014-03-05 | 2014-06-04 | 吉林化工学院 | Apocynum flavonoid extract and preparation method thereof |
| CN103989175A (en) * | 2014-05-06 | 2014-08-20 | 宁波市成大机械研究所 | Deep sea fish oil soft capsule containing apocynum venetum extract |
| CN104490961A (en) * | 2014-12-25 | 2015-04-08 | 长春师范大学 | Preparation method and application of folium apocyni veneti extract |
| CN106074641A (en) * | 2016-06-22 | 2016-11-09 | 任立群 | One treats atherosclerotic medicine |
| CN106474139A (en) * | 2016-08-28 | 2017-03-08 | 张金凤 | One kind is for paracmastic tablet of pulmonary heart disease and preparation method thereof |
| CN109200072A (en) * | 2018-11-02 | 2019-01-15 | 河北医科大学第二医院 | A kind of Folium Apocyni Veneti extraction process |
| CN112957380A (en) * | 2020-02-11 | 2021-06-15 | 厦门大学 | Apocynum venetum leaf extract, preparation method and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100352457C (en) * | 2004-11-18 | 2007-12-05 | 李青山 | Apocynum extract and extracting method thereof |
-
2005
- 2005-12-16 CN CN2005101231875A patent/CN1931205B/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101690739B (en) * | 2009-06-30 | 2011-07-13 | 长春师范学院 | Preparation method of dogbane leaf extractive |
| CN102603831A (en) * | 2011-01-25 | 2012-07-25 | 苏州宝泽堂医药科技有限公司 | Preparation method of high-content trifolin |
| CN102286575A (en) * | 2011-09-14 | 2011-12-21 | 江苏科技大学 | Method for synthesizing isoquercitrin by metal ion-reinforced enzyme method |
| CN102286575B (en) * | 2011-09-14 | 2013-11-06 | 江苏科技大学 | Method for synthesizing isoquercitrin by metal ion-reinforced enzyme method |
| CN103830292A (en) * | 2014-03-05 | 2014-06-04 | 吉林化工学院 | Apocynum flavonoid extract and preparation method thereof |
| CN103989175A (en) * | 2014-05-06 | 2014-08-20 | 宁波市成大机械研究所 | Deep sea fish oil soft capsule containing apocynum venetum extract |
| CN104490961A (en) * | 2014-12-25 | 2015-04-08 | 长春师范大学 | Preparation method and application of folium apocyni veneti extract |
| CN106074641A (en) * | 2016-06-22 | 2016-11-09 | 任立群 | One treats atherosclerotic medicine |
| CN106474139A (en) * | 2016-08-28 | 2017-03-08 | 张金凤 | One kind is for paracmastic tablet of pulmonary heart disease and preparation method thereof |
| CN109200072A (en) * | 2018-11-02 | 2019-01-15 | 河北医科大学第二医院 | A kind of Folium Apocyni Veneti extraction process |
| CN112957380A (en) * | 2020-02-11 | 2021-06-15 | 厦门大学 | Apocynum venetum leaf extract, preparation method and application thereof |
| CN112957380B (en) * | 2020-02-11 | 2022-05-03 | 厦门大学 | Apocynum venetum leaf extract, preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1931205B (en) | 2011-04-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1931205A (en) | Kindir leaf total flavone extract and its prepn and application | |
| CN1754541A (en) | Steroid saponin pharmaceutical composition and its preparation method and uses | |
| CN101385748A (en) | Maniod ebish flower extract, extraction and analysis method and extract preparation and use thereof | |
| CN1803787A (en) | Hypericum perforatum L. total flavone extracts, its preparation and application | |
| CN1895264A (en) | Medicinal use of quercetin-3-0-beta-D-glucancoside | |
| CN1144803C (en) | Chinese chestnut flower flavone compound and its extraction process | |
| CN101062113A (en) | Milkwort extract, its preparation method and application | |
| CN1821255A (en) | Total giamt St.John' swort Herb flavone extract, its preparing method and use | |
| CN1872199A (en) | Composition of Chinese traditional medicine, and preparation method | |
| CN1199682C (en) | Medicine composition for treating depression and its prepn | |
| CN1947736A (en) | Prepn. method and application of injection contg. Erigeron breviscapus | |
| CN100346820C (en) | Jindilan detoxin medicinal composition, preparation and its preparation method | |
| CN1579518A (en) | Trditional Chinese medicinal composition for treating colonitis, its preparation method and quality control method | |
| CN1903265A (en) | Traditional Chinese medicine composition for treating nycturia and its preparing method | |
| CN1853688A (en) | Chinese medicinal preparation for treating heart cerebrovascular disease and ischemic apoplexia and making method thereof | |
| CN1857385A (en) | Medicine composition for treating cervical spondylosis and its preparing method | |
| CN1582952A (en) | Use of asiaticoside in preparation of medicines for diseases of cardio-cerebral blood vessels | |
| CN1218701C (en) | Use of spirosterol type steroid saponin in preparing medicine for treating cardio-cerebral vascular disease | |
| CN1220510C (en) | Chinese patent medicine with the functions of replenishing qi and blood and nourishing the heart to calm the mind, its preparation method and quality control method | |
| CN1511553A (en) | Infantile antipyretic | |
| CN1712034A (en) | Chinese medicinal composition, preparation and quality control thereof | |
| CN1628830A (en) | Chinese medicinal formulation for treating dizziness and its quality control method | |
| CN1626145A (en) | Medication for treating cough | |
| CN1559525A (en) | Red tangerine peel medicine for treating sputum cough and its preparation method | |
| CN1923191A (en) | Use of flavanone kind composition in preparation of medicine for curing cardio vascular diseases |
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 | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20070321 Assignee: Anhui Wanbang Medical Technology Co., Ltd. Assignor: Zhou Yaqiu|Wang Xianrong Contract record no.: 2013340000001 Denomination of invention: Kindir leaf total flavone extract and its prepn and application Granted publication date: 20110413 License type: Exclusive License Record date: 20130110 |
|
| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model | ||
| EC01 | Cancellation of recordation of patent licensing contract |
Assignee: Anhui Wanbang Medical Technology Co., Ltd. Assignor: Zhou Yaqiu|Wang Xianrong Contract record no.: 2013340000001 Date of cancellation: 20150615 |
|
| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model | ||
| 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: 20110413 Termination date: 20161216 |