CN101757058A - General flavone extract of hollyhock flower, preparation thereof and application - Google Patents
General flavone extract of hollyhock flower, preparation thereof and application Download PDFInfo
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- CN101757058A CN101757058A CN200910230093A CN200910230093A CN101757058A CN 101757058 A CN101757058 A CN 101757058A CN 200910230093 A CN200910230093 A CN 200910230093A CN 200910230093 A CN200910230093 A CN 200910230093A CN 101757058 A CN101757058 A CN 101757058A
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- 229930003944 flavone Natural products 0.000 title claims abstract description 58
- 235000011949 flavones Nutrition 0.000 title claims abstract description 58
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- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 150000002212 flavone derivatives Chemical class 0.000 title claims abstract description 38
- 235000017334 Alcea rosea Nutrition 0.000 title claims abstract description 27
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- 238000002360 preparation method Methods 0.000 title claims description 18
- 240000000530 Alcea rosea Species 0.000 title description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 58
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- 238000000746 purification Methods 0.000 claims abstract description 16
- 239000003814 drug Substances 0.000 claims abstract description 15
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- IYRMWMYZSQPJKC-UHFFFAOYSA-N kaempferol Chemical compound C1=CC(O)=CC=C1C1=C(O)C(=O)C2=C(O)C=C(O)C=C2O1 IYRMWMYZSQPJKC-UHFFFAOYSA-N 0.000 claims abstract description 14
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- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 3
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- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 2
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Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to the technical field of medicaments and relates to a method for purifying the general flavone resin of hollyhock dried flower which is a Chinese herbal medicament in Uyghur. Extract obtained through the backflow extraction with ethanol and the purification of macroporous resin comprises 50 to 90 weight percent of general flavone, wherein the flavone comprises the following components in percentage by weight: 15.0 to 45.0 percent of quercetin, 5.0 to 20.0 percent of kaempferol, 3.0 to 18 percent of astragaloside and the balance of the other flavonoid components. The general flavone extract of the hollyhock flower of the invention is used for preparing the medicaments for treating cough and asthma, detumescence, poliomyelitis, constipation, hemorrhoids, insomnia and amnesia.
Description
Technical field:
The present invention relates to Uigurs medicine composition purification process, relate in particular to general flavone extract of hollyhock flower, its preparation and application, belong to medical technical field.
Background technology:
Flos althaeae roseae is the dried floral of Malvaceae plant Althaea rosea (L.) Cavan. Althaea rosea (L.) Gavan., is different from Flos abelmoschi manihot.Pluck summer, dries.Be irregular cylindric or long avette, long by 3 to 5cm, minority has the relic of calyx.Pattern is mainly two kinds of aubergine and light white powders, corolla 5 lobes or polyphyll, and to bond agglomerating more, is obovate after the moistening expansion of water, and first end margin has irregular fissure or full edge, and there is the intensive fine hair of cluster the both sides of base portion pawl.The stamen majority, filigree is unified into tubular, the flower pesticide yellow.Petal white, matter is pliable and tough and thin, and is crisp slightly when dried.Feeble QI fragrance, lightly seasoned.Function is nourishing the lung to arrest cough with curing mainly, and diaphoresis is relievingd asthma, detumescence rash, the beneficial heart of calming the nerves.It is more than to be used for cough with asthma, and expectoration is not well, infantile measles, and the constipation hemorrhoid, insomnia forgetfulness, sweating is not smooth.The chemical constitution study report contains compositions such as Quercetin, kaempferol, astragalin.Tie up flower of Althaea officinalis L. as the Uygur medicine medicinal herbs most in use,, the research work of its quality standard relatively lags behind, anxious To be improved.
The purification of traditional flavone compound mainly adopts solvent extraction, polyamide, silica gel chromatography and active carbon adsorption.Wherein the used organic solvent of solvent extraction has toxicity in various degree, and easily emulsifying in the extraction process, can only obtain about 50% of total flavones total amount, therefore needs several different solvents single extractions total flavones could be extracted substantially fully.When polyamide and silica gel purification total flavones, the Irreversible Adsorption rate is respectively about 40% and about 60%, and yield is not high.The adsorption rate height of flavone in the active carbon adsorption, but purity can not get guaranteeing.So said method is all undesirable in Folium Fumicis Dentati total flavones purification.And macroporous resin is as novel polymeric sorbent, is widely used in the purifies and separates of Chinese medicine macromolecular compounds such as active component in pharmacy and the natural plants such as saponin, flavone, lactone, alkaloid.Increasing along with the macroporous resin kind more and more is subject to people's attention for the purification of Chinese herbal medicine effective ingredients.
It is less that dimension flower of Althaea officinalis L. total flavones preparation is used for the treatment of the report of diseases such as cough with asthma, detumescence, poliomyelitis, constipation hemorrhoid, insomnia forgetfulness.
Summary of the invention:
The weak point that exists on the extraction and purification method at total flavones in the existing Flos althaeae roseae, the invention provides the extraction and purification method and the application thereof of total flavones in a kind of brand-new Flos althaeae roseae, mainly with resin Flos althaeae roseae being carried out post purifies, adopt this method, reduced the application of organic solvent in whole purification process, prevented the influence of organic solvent to end product, the prepared general flavone extract of hollyhock flower of the inventive method can be used for developing the medicine of preparation treatment cough with asthma, detumescence, poliomyelitis, constipation hemorrhoid, insomnia forgetfulness.
General flavone extract of hollyhock flower of the present invention general flavone content by weight percentage is 50%～90%; Wherein contained flavone component comprises: Quercetin (15.0%～45.0%), kaempferol (5.0%～20.0%), astragalin (3.0%～18%), other flavones ingredient surplus.
The preparation method of general flavone extract of hollyhock flower of the present invention, the extraction purification step is:
1) getting and pulverize exsiccant Flos althaeae roseae, is that 40%～90% ethanol is the extractant agent with the volume fraction of 10～20 times of volumes of quality of medicinal material, soaks 12 hours earlier, is heated to reflux, extract, then, collects extracting solution, decompression recycling ethanol, concentrated solution;
2) concentrated solution that step 1 is obtained, select HPD-100 or HPD-400 or HPD-600 or AB-8 or D101 macroporous resin for use, last sample, last sample absorption 0.1～2.0 hour, washing earlier, the washing volume is 1BV～3BV, the washing flow velocity is 1BV/h～3BV/h, uses ethanol elution then, and eluting is 30%～80% with the ethanol volume fraction, elution amount is 2BV～4BV, and elution speed is 1BV/h～4BV/h;
3) ethanol elution of collection step 2 concentrates, and 50 ℃ of vacuum dryings get exsiccant purified product.
Step 2 wherein) preferred processing condition is: HPD-400 or D101 macroporous resin carry out purification, and adsorption time is 0.5～1.0h, and volume fraction 50%～60% ethanol is eluant, and elution amount is 3BV, and elution speed is 2BV/h.Can farthest total flavones be extracted like this, and can not cause the waste of eluant.
Use the Chinese medicine preparation of described general flavone extract of hollyhock flower, it is characterized in that described Chinese medicine preparation is is the medicine active ingredient with described general flavone extract of hollyhock flower, adds drop pill or tablet or capsule or the granule made behind the pharmaceutic adjuvant.
Can be used for developing the medicine of preparation treatment cough with asthma, detumescence, poliomyelitis, constipation hemorrhoid, insomnia forgetfulness.
The present invention has the following advantages:
1. the preparation method of general flavone extract of hollyhock flower provided by the invention is simple to operate, quick;
2. selected macroporous resin has the function that adsorbance is big, desorption efficiency is big;
3. with ethanol be solvent and eluant, inexpensive, nontoxic.
The specific embodiment:
Understand technical scheme of the present invention for better, below describe in further detail by specific embodiment.
Embodiment 1
Getting and pulverize exsiccant Flos althaeae roseae 100g, is that 50% ethanol is the extractant agent with the volume fraction of 15 times of volumes of quality of medicinal material, soaks 12 hours earlier, be heated to reflux, extract, then, collect extracting solution, decompression recycling ethanol, get concentrated solution,, select the D101 purification by macroporous resin for use the concentrated solution that obtains, last sample absorption 1.0 hours, washing earlier, the washing volume is 2BV, the washing flow velocity is 1BV/h, uses ethanol elution then, and eluting is 50% with the ethanol volume fraction, elution amount is 3BV, and elution speed is 2BV/h
Collect ethanol elution, concentrate, 50 ℃ of vacuum dryings get exsiccant purified product.The extractive of general flavone recovery rate is 3.3%, and its total flavones is 67.5% in rutin content by weight percentage, and its component content is: Quercetin 25.6%, kaempferol 16.0%, astragalin 15.4%, other flavones ingredient surplus.
Embodiment 2
Getting and pulverize exsiccant Flos althaeae roseae 100g, is that 90% ethanol is the extractant agent with the volume fraction of 10 times of volumes of quality of medicinal material, soaks 12 hours earlier, be heated to reflux, extract, then, collect extracting solution, decompression recycling ethanol, get concentrated solution,, select the HP-400 purification by macroporous resin for use the concentrated solution that obtains, last sample absorption 2.0 hours, washing earlier, the washing volume is 4BV, the washing flow velocity is 3BV/h, uses ethanol elution then, and eluting is 70% with the ethanol volume fraction, elution amount is 4BV, and elution speed is 4BV/h
Collect ethanol elution, concentrate, 50 ℃ of vacuum dryings get exsiccant purified product.The extractive of general flavone recovery rate is 3.1%, and its total flavones is 60.3% in rutin content by weight percentage, and its component content is: Quercetin 23.8%, kaempferol 15.5%, astragalin 15.1%, other flavones ingredient surplus.
Embodiment 3
Getting and pulverize exsiccant Flos althaeae roseae 100g, is that 0% ethanol is the extractant agent with the volume fraction of 20 times of volumes of quality of medicinal material, soaks 12 hours earlier, be heated to reflux, extract, then, collect extracting solution, decompression recycling ethanol, get concentrated solution,, select the AB-8 purification by macroporous resin for use the concentrated solution that obtains, last sample absorption 1.0 hours, washing earlier, the washing volume is 3BV, the washing flow velocity is 2BV/h, uses ethanol elution then, and eluting is 60% with the ethanol volume fraction, elution amount is 2BV, and elution speed is 3BV/h
Collect ethanol elution, concentrate, 50 ℃ of vacuum dryings get exsiccant purified product.The extractive of general flavone recovery rate is 3.4%, and its total flavones is 64.7% in rutin content by weight percentage, and its component content is: Quercetin 22.6%, kaempferol 15.7%, astragalin 16.8%, other flavones ingredient surplus.
Embodiment 4 Flos althaeae roseae total flavones sheets
Group component
General flavone extract of hollyhock flower 1-100g
Starch 20g
Dextrin 80g
Microcrystalline Cellulose 85g
Low-substituted hydroxypropyl methylcellulose 15g
70% alcoholic solution (volume fraction) 15ml
6% starch slurry 5ml
Magnesium stearate 1g
Preparation process: general flavone extract of hollyhock flower, starch, dextrin, microcrystalline Cellulose, magnesium stearate, low-substituted hydroxypropyl methylcellulose pulverize separately are crossed 80 mesh sieves; With Flos althaeae roseae total flavones and dextrin, starch, the low-substituted hydroxypropyl methylcellulose of 2/3 amount and 70% alcoholic solution and 6% starch slurry mixed grinding, be 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 Flos althaeae roseae total flavone capsule agent
Group component
General flavone extract of hollyhock flower 5-100g
Starch 100g
Dextrin 30g
70% alcoholic solution (volume fraction) 20ml
Preparation process: with starch, dextrin and general flavone extract of hollyhock flower mixing, cross 80 mesh sieves, add 70% alcoholic solution of 20ml, the system soft material, reuse 20 mesh sieve system granules, drying, granulate, encapsulated, make 1000 altogether, every contains general flavone extract of hollyhock flower 5-100mg, gets final product.
Embodiment 6 Flos althaeae roseae flavone dripping pills
Group component
General flavone extract of hollyhock flower 1-50g
PEG4000 20g
PEG6000 20g
Preparation process: Macrogol 4000, polyethylene glycol 6000 heating are dissolved, the fusion general flavone extract of hollyhock flower is being added wherein, fully stir, medicine is well-dispersed in the substrate; Above-mentioned medicinal liquid is transferred on the drop pill machine, and 80～90 ℃ of sealings are incubated 10～20 minutes, make coolant with anhydrous methyl-silicone oil, and 10 ℃ of 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 7 Flos althaeae roseae total flavones granules
Group component
General flavone extract of hollyhock flower 1-10g
Dextrin 20g
Starch 10g
Icing Sugar 10g
Tartaric acid 1g
30% alcoholic solution (volume fraction) 10ml
Preparation process: general flavone extract of hollyhock flower, dextrin, starch, Icing Sugar are crossed 100 mesh sieves respectively, mixing, tartaric acid is dissolved in 30% alcoholic solution again, once adds in the said mixture mixing, the system soft material, cross the 20mu nylon mesh, dry below 60 ℃, use plastic bag packaging behind the granulate, every bag of 2g contains general flavone extract of hollyhock flower 50-500mg.
Claims (4)
1. general flavone extract of hollyhock flower, general flavone content by weight percentage is 50%～90%; Wherein contained flavone component comprises: Quercetin 15.0%～45.0%, kaempferol 5.0%～20.0%, astragalin 3.0%～18%, other flavones ingredient surplus.
2. the preparation method of general flavone extract of hollyhock flower as claimed in claim 1 is characterized in that: extracting purification step is:
1) getting and pulverize exsiccant Flos althaeae roseae, is that 40%～90% ethanol is the extractant agent with the volume fraction of 10～20 times of volumes of quality of medicinal material, soaks 12 hours earlier, is heated to reflux, extract, then, collects extracting solution, decompression recycling ethanol, concentrated solution;
2) concentrated solution that step 1 is obtained, select HPD-100 or HPD-400 or HPD-600 or AB-8 or D101 macroporous resin for use, last sample, last sample absorption 0.1～2.0 hour, washing earlier, the washing volume is 1BV～3BV, the washing flow velocity is 1BV/h～3BV/h, uses ethanol elution then, and eluting is 30%～80% with the ethanol volume fraction, elution amount is 2BV～4BV, and elution speed is 1BV/h～4BV/h;
3) ethanol elution of collection step 2 concentrates, and 50 ℃ of vacuum dryings get exsiccant purified product.
3. preparation method according to claim 2, it is characterized in that: preferred processing condition is described step 2): HPD-400 or D101 macroporous resin carry out purification, adsorption time is 0.5～1.0h, volume fraction 50%～60% ethanol is eluant, elution amount is 3BV, and elution speed is 2BV/h.
4. use the Chinese medicine preparation of general flavone extract of hollyhock flower as claimed in claim 1, it is characterized in that described Chinese medicine preparation is is the medicine active ingredient with described general flavone extract of hollyhock flower, adds drop pill or tablet or capsule or the granule made behind the pharmaceutic adjuvant.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102008081A (en) * | 2010-11-11 | 2011-04-13 | 浙江农林大学 | Abelmoschus manihot leaf extract and production method of health-care instant tea thereof |
| CN104082846A (en) * | 2014-07-24 | 2014-10-08 | 中国烟草总公司郑州烟草研究院 | Application of althaea rosa seed extractive to cigarettes |
| CN104087421A (en) * | 2014-07-24 | 2014-10-08 | 中国烟草总公司郑州烟草研究院 | Althaea rosea flower extract coproduction preparation method and applications thereof |
| CN112569266A (en) * | 2019-09-27 | 2021-03-30 | 疆维吾尔医学专科学校 | Uighur medicine extract, preparation method thereof and application thereof in preparing anti-inflammatory analgesic medicines |
| CN115304571A (en) * | 2022-09-02 | 2022-11-08 | 陕西医药控股医药研究院有限公司 | Method for preparing high-purity quercetin from marshmallow |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102008081A (en) * | 2010-11-11 | 2011-04-13 | 浙江农林大学 | Abelmoschus manihot leaf extract and production method of health-care instant tea thereof |
| CN102008081B (en) * | 2010-11-11 | 2012-09-26 | 浙江农林大学 | Abelmoschus manihot leaf extract and production method of health-care instant tea thereof |
| CN104082846A (en) * | 2014-07-24 | 2014-10-08 | 中国烟草总公司郑州烟草研究院 | Application of althaea rosa seed extractive to cigarettes |
| CN104087421A (en) * | 2014-07-24 | 2014-10-08 | 中国烟草总公司郑州烟草研究院 | Althaea rosea flower extract coproduction preparation method and applications thereof |
| CN104082846B (en) * | 2014-07-24 | 2016-02-24 | 中国烟草总公司郑州烟草研究院 | The application of a kind of hollyhock seed extract in cigarette |
| CN112569266A (en) * | 2019-09-27 | 2021-03-30 | 疆维吾尔医学专科学校 | Uighur medicine extract, preparation method thereof and application thereof in preparing anti-inflammatory analgesic medicines |
| CN115304571A (en) * | 2022-09-02 | 2022-11-08 | 陕西医药控股医药研究院有限公司 | Method for preparing high-purity quercetin from marshmallow |
| CN115304571B (en) * | 2022-09-02 | 2024-03-12 | 陕西医药控股医药研究院有限公司 | Method for preparing high-purity quercetin by using marshmallow |
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