CN105079085A - Extraction process of total flavonoids of oxytropis falcata - Google Patents
Extraction process of total flavonoids of oxytropis falcata Download PDFInfo
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- CN105079085A CN105079085A CN201510573280.XA CN201510573280A CN105079085A CN 105079085 A CN105079085 A CN 105079085A CN 201510573280 A CN201510573280 A CN 201510573280A CN 105079085 A CN105079085 A CN 105079085A
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- Prior art keywords
- herba oxytropis
- extraction process
- ethyl acetate
- oxytropis falcatae
- total flavones
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- 238000000605 extraction Methods 0.000 title claims abstract description 30
- 229930003935 flavonoid Natural products 0.000 title abstract description 4
- 235000017173 flavonoids Nutrition 0.000 title abstract description 4
- 150000002215 flavonoids Chemical class 0.000 title abstract 3
- 241001347883 Oxytropis falcata Species 0.000 title abstract 2
- 241001053158 Oxytropis Species 0.000 claims abstract description 45
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Abstract
The invention discloses an extraction process of total flavonoids of oxytropis falcate, and belongs to the technical field of natural medicinal chemistry. The extraction process comprises the following steps: boiling oxytropis falcata in water, filtering and removing residue, concentrating filtrate and hydrolyzing in an acid condition so as to obtain a hydrolysate, and then regulating the pH value of the hydrolysate to be neutral; extracting the obtained hydrolysate that pH is regulated to be neutral by virtue of ethyl acetate, reserving extract liquor, and extracting the extract liquor with an ethyl acetate-ethanol mixed solvent so as to obtain extract liquor; and drying the solvent in the obtained extract liquor by distillation so as to obtain an extract. The extraction process disclosed by the invention can be used for successfully extracting total flavonoids from the oxytropis falcate, with high extraction yield and high purity.
Description
Technical field
The present invention discloses a kind of extraction process of Herba Oxytropis falcatae total flavones, belongs to Natural Medicine Chemistry technical field.
Background technology
Herba Oxytropis falcatae (OxytropisfalcataBunge) is the one of pulse family Genus Oxytropis Dc, belongs to herbaceos perennial, and Tibetan medicine is called " Russia's Balkh ", is mainly distributed in west area, comprises the ground such as Qinghai, Tibet, Gansu, Sichuan in China.All herbal medicine, primary efficacy has heat-clearing and toxic substances removing, more to create flesh, hemostasis etc., can treat eczema, inflammation, yellow fluid, epidemic disease, scabies, swell and ache
[1], be called as " king of medical herbs ".Previously research shows, Herba Oxytropis falcatae medical material chloroform extract, total-flavonoid aglycone and Main Flavonoids compound have stronger antibacterial, antiinflammatory, antioxidative effect
[2,3].
The Herba Oxytropis falcatae total flavones that this problem is selected is the effective active composition extracted from oxytropis falcate Bunge.Research finds, flavone compounds a large amount of in Herba Oxytropis falcatae and derivant thereof mainly exist with forms such as flavonoid glycoside, flavone and flavanone, flavonol, chalcone derivative, dihydrochalcone, isoflavan and flavanone, have stronger antiinflammatory, antioxidation.Herba Oxytropis falcatae is a kind of important traditional Tibetan medicine material, at Tibet aboundresources and medical value is higher, although carried out some researchs about Herba Oxytropis falcatae chemical composition in recent years, but its pharmacological research is still not enough, a lot of research is still in the junior stage, bioactive substance basis is indefinite, causes the clinical practice of this medicine to be restricted, and this is very unfavorable for exploitation China Resources of Tibetan Medicine in China.Therefore, accelerate the medical value of this medical material of research, illustrate its chemical composition and pharmacologically active, the new drug developing determined curative effect stable is very important.
List of references:
[1] Zhang Xiaojing, Liu Weixia, Wei Peng, etc. oxytropis falcate Bunge toxicity and chemical composition correlation analysis. CHINA JOURNAL OF CHINESE MATERIA MEDICA, 2014,39(7): 1157-1161.
[2]HuaJiang,Wen-qiangZhan,XiaLiu,etal.AntioxidantactivitiesoftheextractsandflavonoidcompoundsfromOxytropisfalcateBunge.NaturalProductResearch，2008，22(18):1650-1656.
[3]HuaJiang,Jun-ruHu,Wen-qiangZhan,etal.ScreeningforfractionsofOxytropisfalcataBungewithantibacterialactivity.NaturalProductResearch,2009，23(10):953-959。
Summary of the invention
The object of the invention is: the extraction process providing a kind of Herba Oxytropis falcatae total flavones.
Technical scheme:
An extraction process for Herba Oxytropis falcatae total flavones, comprises the steps:
1st step, Herba Oxytropis falcatae is added water boil, leach residue, be hydrolyzed in acid condition after filtrate is concentrated, obtain hydrolyzed solution, then by the pH regulator of hydrolyzed solution to neutral;
2nd step, the hydrolyzed solution being adjusted to pH neutrality that the 1st step obtains to be extracted with ethyl acetate, get raffinate, then raffinate ethyl acetate-ethanol mixed solvent to extract, and gets extract;
3rd step, by after the solvent evaporate to dryness in the extract that obtains in the 2nd step, obtain extract.
In the 1st described step, the weight added water in boiling part is 10 ~ 20 times of Herba Oxytropis falcatae weight, and boiling time is 2 hours.
In the 1st described step, acid condition makes the pH of system be 2 by adding 0.3wt% phosphoric acid; Hydrolysis temperature is 80 ~ 100 DEG C, and hydrolysis time is 2 ~ 4 hours.
In the 1st described step, pH regulator to neutrality realizes by adding sodium hydroxide solution in hydrolyzed solution.
In the 2nd described step, the ethyl acetate in ethyl acetate-ethanol mixed solvent and the volume ratio of ethanol are 5:2.
Another object of the present invention, there is provided the Herba Oxytropis falcatae total flavones that said extracted technique prepares.
Another object of the present invention, there is provided the pharmaceutical preparation containing above-mentioned Herba Oxytropis falcatae total flavones.
Above-mentioned pharmaceutical preparation can be that Herba Oxytropis falcatae total flavones is added corresponding adjuvant, is prepared into applicable oral administration.The pharmaceutical preparation being applicable to oral administration refers to that the regular dosage form of pharmaceutically oral administration comprises tablet, powder, granule, capsule, drop pill, oral liquid, pellet etc.Be preferably tablet, capsule, drop pill.Wherein tablet comprises plain sheet, coated tablet, slow releasing tablet, dispersible tablet, enteric coatel tablets, buccal tablet, chewable tablet, effervescent tablet etc.; Capsule comprises hard capsule, soft capsule, slow releasing capsule, enteric coated capsule etc.; Pellet comprises common pellets, slow-release micro-pill, enteric coated micropill, controlled release micro pill etc.Pharmaceutically conventional excipient such as binding agent contained in oral formulations comprises hypromellose, dextrin, Polyethylene Glycol, syrup, arabic gum, sorbitol, gelatin or polyvinylpyrrolidone etc.; Filler comprises lactose, corn starch, calcium phosphate, sorbitol or glycine etc.; Tableting lubricant comprises magnesium stearate, Polyethylene Glycol etc.; Disintegrating agent comprises starch, polyvinylpyrrolidone, Explotab or microcrystalline Cellulose; Or pharmaceutically acceptable wetting agent comprises sodium lauryl sulphate etc.; Correctives and sweeting agent comprise stevioside, aspartame, steviosin, xylitol, menthol, flavoring orange essence etc.Preparation method adopts the preparation method of this area routine.
beneficial effect
Extract in the successful therefrom Herba Oxytropis falcatae of the present invention and obtain total flavones, extract yield is high, and purity is high.
Detailed description of the invention
Below by detailed description of the invention, the present invention is described in further detail.But it will be understood to those of skill in the art that the following example only for illustration of the present invention, and should not be considered as limiting scope of the present invention.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can by the conventional products of commercial acquisition.
The detection method of the Herba Oxytropis falcatae total flavones in following examples is as follows:
1, instrument and reagent
Ultrasonic cleaner (SB-5200DTN), UV detector (UV-1800), electronic balance (CP225D), rutin (Nat'l Pharmaceutical & Biological Products Control Institute, lot number: 0080-9705) agents useful for same is analytical pure.
2, method and result
1. preparation of reagents:
5%NaNO
2solution: precision takes sodium nitrite 5.0014g, is settled in 100ml volumetric flask with distilled water;
10%Al (NO
3)
3solution: precision takes aluminum nitrate 10.0094g, is settled in 100ml volumetric flask with distilled water;
4%NaOH solution: accurate weighing sodium hydroxide 10.0285g, is settled in 250ml volumetric flask with distilled water.
2. the preparation of reference substance solution:
Get control substance of Rutin appropriate (lot number: 0080-9705), accurately weighed, dissolve with the EtOH Sonicate of 80vol.%, be settled in 50ml volumetric flask, obtaining concentration is 0.0320mg.ml
-1reference substance solution.
3. the preparation of solution and assay
Sample thief powder is appropriate, accurately weighed;
Add 80vol.% ethanol, supersound extraction, filter, filtrate is settled in 100ml volumetric flask, and precision pipettes in 1.0ml to 25ml volumetric flask, adds 5%NaNO
2solution 1ml shakes up, jolting 6min, 10%Al (NO
3)
3solution 1ml shakes up, jolting 6min, 4%NaOH solution 10ml, and the ethanol adding 80vol.% is settled to scale, shakes up, and places 15min, surveys absorbance in 510nm wavelength place, calculates content by one point external standard method.
The extraction of embodiment 1 Herba Oxytropis falcatae total flavones
(1) material
1. raw material: Herba Oxytropis falcatae
2. reagent: water, phosphoric acid, sodium hydroxide, ethyl acetate, ethanol
(2) method
Herba Oxytropis falcatae raw material 4kg, adds 15 times of water gagings (about 60L) and boils 2 hours, and cooling, leaches residue with filter cloth, and aqueous solution reconcentration is to about 20L.Again the Aqueous extracts after concentrated is placed in the glass reactor of 50L, adds 0.3wt% phosphoric acid (making pH be about 2) and stir hydrolysis 3 hours in 90 DEG C.Hydrolysis terminates back end hydrogenation sodium hydroxide solution adjust ph to neutral.Hydrolyzed solution puts extraction bucket isopyknic extraction into ethyl acetate once, then by isopyknic ethyl acetate-ethanol (5:2) extracting twice.Primary acetic acid ethyl acetate extract is not because having more chlorophyll to discard after recycling design containing flavone.Be concentrated into dry with the extract of ethyl acetate-ethanol mixed extractant solvent, obtain extractive of general flavone.20kg Herba Oxytropis falcatae divides 5 extractions by above technique, finally obtains the extractive of general flavone of about 100 grams.In rutin, extracting the Herba Oxytropis falcatae total flavones purity obtained is 26.58%.
Reference examples 1
Be with the difference of embodiment 1: after the adjusted hydrolyzed solution for pH neutrality, only use ethyl acetate-ethanol mixed extractant solvent, and first do not use ethyl acetate to carry out pre-extracted remove impurity.
Herba Oxytropis falcatae raw material 4kg, adds 15 times of water gagings (about 60L) and boils 2 hours, and cooling, leaches residue with filter cloth, and aqueous solution reconcentration is to about 20L.Again the Aqueous extracts after concentrated is placed in the glass reactor of 50L, adds 0.3wt% phosphoric acid (making pH be about 2) and stir hydrolysis 3 hours in 90 DEG C.Hydrolysis terminates back end hydrogenation sodium hydroxide solution adjust ph to neutral.Hydrolyzed solution puts the extraction isopyknic ethyl acetate-ethanol of bucket (5:2) extraction, is concentrated into dry, obtains extractive of general flavone with the extract of ethyl acetate-ethanol mixed extractant solvent.20kg Herba Oxytropis falcatae divides 5 extractions by above technique, finally obtains the extractive of general flavone of about 112 grams.In rutin, extracting the Herba Oxytropis falcatae total flavones purity obtained is 16.22%.Compare by embodiment 1 can find out with reference examples 1, by using ethyl acetate, pre-extracted remove impurity is carried out to hydrolysate, effectively can to remain valid material total flavones, the magazins' layout such as the chlorophyll wherein contained can also be fallen simultaneously, effectively can improve the purity of end product.
Reference examples 2
Be with the difference of embodiment 1: after obtaining hydrolyzed solution, do not use sodium hydroxide to be adjusted to neutrality, but directly extract.
Herba Oxytropis falcatae raw material 4kg, adds 15 times of water gagings (about 60L) and boils 2 hours, and cooling, leaches residue with filter cloth, and aqueous solution reconcentration is to about 20L.Again the Aqueous extracts after concentrated is placed in the glass reactor of 50L, adds 0.3wt% phosphoric acid (making pH be about 2) and stir hydrolysis 3 hours in 90 DEG C.Hydrolyzed solution puts extraction bucket isopyknic extraction into ethyl acetate once, then by isopyknic ethyl acetate-ethanol (5:2) extracting twice.Primary acetic acid ethyl acetate extract is not because having more chlorophyll to discard after recycling design containing flavone.Be concentrated into dry with the extract of ethyl acetate-ethanol mixed extractant solvent, obtain extractive of general flavone.20kg Herba Oxytropis falcatae divides 5 extractions by above technique, finally obtains the extractive of general flavone of about 88 grams.In rutin, extracting the Herba Oxytropis falcatae total flavones purity obtained is 22.46%.Compare with embodiment 1 as can be seen from reference examples 2, after the pH regulator of hydrolysate is neutrality, can effectively in extraction process, impurity be separated with effective flavone, improve total flavones DNA purity.
Embodiment 2
Be with the difference of embodiment 1: in the process of boiling, also add kieselguhr.
Herba Oxytropis falcatae raw material 4kg, adds 15 times of water gagings (about 60L) and 100g kieselguhr boils 2 hours altogether, and cooling, leaches residue with filter cloth, and aqueous solution reconcentration is to about 20L.Again the Aqueous extracts after concentrated is placed in the glass reactor of 50L, adds 0.3wt% phosphoric acid (making pH be about 2) and stir hydrolysis 3 hours in 90 DEG C.Hydrolysis terminates back end hydrogenation sodium hydroxide solution adjust ph to neutral.Hydrolyzed solution puts extraction bucket isopyknic extraction into ethyl acetate once, then by isopyknic ethyl acetate-ethanol (5:2) extracting twice.Primary acetic acid ethyl acetate extract is not because having more chlorophyll to discard after recycling design containing flavone.Be concentrated into dry with the extract of ethyl acetate-ethanol mixed extractant solvent, obtain extractive of general flavone.20kg Herba Oxytropis falcatae divides 5 extractions by above technique, finally obtains the extractive of general flavone of about 100 grams.In rutin, extracting the Herba Oxytropis falcatae total flavones purity obtained is 28.41%.Can be found out by embodiment 1 and embodiment 2, in the process of boiling, a part of impurity can be got rid of by diatomaceous adsorption, the purity extracting product can be improved.
Claims (7)
1. an extraction process for Herba Oxytropis falcatae total flavones, is characterized in that, comprises the steps:
1st step, Herba Oxytropis falcatae is added water boil, leach residue, be hydrolyzed in acid condition after filtrate is concentrated, obtain hydrolyzed solution, then by the pH regulator of hydrolyzed solution to neutral;
2nd step, the hydrolyzed solution being adjusted to pH neutrality that the 1st step obtains to be extracted with ethyl acetate, get raffinate, then raffinate ethyl acetate-ethanol mixed solvent to extract, and gets extract;
3rd step, by after the solvent evaporate to dryness in the extract that obtains in the 2nd step, obtain extract.
2. the extraction process of Herba Oxytropis falcatae total flavones according to claim 1, is characterized in that: in the 1st described step, and the weight added water in boiling part is 10 ~ 20 times of Herba Oxytropis falcatae weight, and boiling time is 2 hours.
3. the extraction process of Herba Oxytropis falcatae total flavones according to claim 1, is characterized in that: in the 1st described step, and acid condition makes the pH of system be 2 by adding 0.3wt% phosphoric acid; Hydrolysis temperature is 80 ~ 100 DEG C, and hydrolysis time is 2 ~ 4 hours.
4. the extraction process of Herba Oxytropis falcatae total flavones according to claim 1, is characterized in that: in the 1st described step, and pH regulator to neutrality realizes by adding sodium hydroxide solution in hydrolyzed solution.
5. the extraction process of Herba Oxytropis falcatae total flavones according to claim 1, is characterized in that: in the 2nd described step, the ethyl acetate in ethyl acetate-ethanol mixed solvent and the volume ratio of ethanol are 5:2.
6. the Herba Oxytropis falcatae total flavones that the extraction process described in any one of Claims 1 to 5 prepares.
7. the pharmaceutical preparation containing Herba Oxytropis falcatae total flavones according to claim 6.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105106289A (en) * | 2015-09-10 | 2015-12-02 | 甘肃省中医药研究院 | Application of total flavone of oxyptropis falcate bunge in preparation of diabetes treating drug |
| CN105884736A (en) * | 2016-04-19 | 2016-08-24 | 中国科学院西北高原生物研究所 | Method for separating and preparing 5 flavonoid compounds from Oxytropis falcate Bunge |
| CN106727881A (en) * | 2017-03-15 | 2017-05-31 | 中国科学院西北高原生物研究所 | A kind of extracting method with anti-inflammatory activity general flavone from falcate crazyweed herb |
| CN110917236A (en) * | 2020-01-07 | 2020-03-27 | 四川农业大学 | Oxytropis falcate anti-fungal infection extract and preparation method and application thereof |
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| CN103058978A (en) * | 2012-12-27 | 2013-04-24 | 甘肃奇正藏药有限公司 | Method for synchronized preparation of pinocembrin and 2', 4'-dihydroxy chalcone from oxytropis falcate bunge |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105106289A (en) * | 2015-09-10 | 2015-12-02 | 甘肃省中医药研究院 | Application of total flavone of oxyptropis falcate bunge in preparation of diabetes treating drug |
| CN105884736A (en) * | 2016-04-19 | 2016-08-24 | 中国科学院西北高原生物研究所 | Method for separating and preparing 5 flavonoid compounds from Oxytropis falcate Bunge |
| CN106727881A (en) * | 2017-03-15 | 2017-05-31 | 中国科学院西北高原生物研究所 | A kind of extracting method with anti-inflammatory activity general flavone from falcate crazyweed herb |
| CN110917236A (en) * | 2020-01-07 | 2020-03-27 | 四川农业大学 | Oxytropis falcate anti-fungal infection extract and preparation method and application thereof |
| CN110917236B (en) * | 2020-01-07 | 2022-10-14 | 四川农业大学 | Antifungal infection extract of Thorn bean falciparum and its preparation method and use |
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