CN102532216A - Method for extracting sophoricoside from sophora fruits - Google Patents
Method for extracting sophoricoside from sophora fruits Download PDFInfo
- Publication number
- CN102532216A CN102532216A CN2010106038682A CN201010603868A CN102532216A CN 102532216 A CN102532216 A CN 102532216A CN 2010106038682 A CN2010106038682 A CN 2010106038682A CN 201010603868 A CN201010603868 A CN 201010603868A CN 102532216 A CN102532216 A CN 102532216A
- Authority
- CN
- China
- Prior art keywords
- fructus sophorae
- extracting
- glycosides
- macroporous resin
- extract
- 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.)
- Pending
Links
- 0 CC(C(C(C1O)O*)N=O)OC1Oc1ccc(C(COc2cc(O)cc(O)c22)C2=O)cc1 Chemical compound CC(C(C(C1O)O*)N=O)OC1Oc1ccc(C(COc2cc(O)cc(O)c22)C2=O)cc1 0.000 description 1
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention provides a method for extracting sophoricoside from sophora fruits, which is characterized by enabling sophora fruit medicinal materials to be smashed, adding 8-12 times amount of alkalinity thin alcohol liquid containing sodium borate to heat and reflux for extracting 2-3 times, adjusting extracting solution to be neutral, passing macroporous resin column, eluting by using ethanol water, enabling eluent to be concentrated to extract, adding defined amount ethyl acetate for dissolving, filtering, dissolving undissolved substance by using acetone, filtering, obtaining filter cakes to conduct backflow dissolving by using 70-90% ethanol, and crystallizing 2-4 times to obtain products. The products manufactured by the method are high in product contents, good in repeatability and large in handling capacity of macroporous resin and have industrialization significances.
Description
Technical field:
The invention belongs to the Separation of Natural Products field, especially relate to a kind of method of from the Fructus Sophorae, extracting Fructus Sophorae glycosides.
Background technology:
The Fructus Sophorae is China's conventional Chinese medicine material, the dry mature fruit of leguminous plants Chinese scholartree (Sophora japonica L.).The medicinal material commodity are claimed the Fructus Sophorae with fruit.It is stated from Eastern Han Dynasty's Shennong's Herbal as medicinal head, and quilt is classified as top grade, and fruit claims that Chinese scholartree is real, the promptly modern Fructus Sophorae, and later successive dynasties book on Chinese herbal medicine is all on the books.Fructus Sophorae bitter, cold in nature.Return liver, large intestine channel.Clearing away heat-fire, blood cooling and hemostatic functions are arranged.Be used for intestines heat and have blood in stool, hemorrhoid are swollen hemorrhage, the headache of liver heat, dizzy hot eyes.The staple of the Fructus Sophorae is compositions such as flavonoid, alkaloids, triterpenes, amino acid and carbohydrate, and wherein NOVASOY 400 and flavonol and glycoside component content thereof are higher.
Fructus Sophorae glycosides has another name called Sophoraflavonoloside, sophorine, and genistein-4 '-glucoside, white tip-like crystallization is insoluble in water, ethanol, is dissolved in hot ethanol slightly, is dissolved in pyridine, diluted alkaline, is insoluble to ETHYLE ACETATE, acetone.Structural formula:
Fructus Sophorae glycosides belongs to isoflavone glycoside, has stronger physiologically active.Modern pharmacological research shows that Fructus Sophorae glycosides is respond well to chronic hepatitis patient's glutamate pyruvate transaminase lowering, can also suppress the pawl oedema that is caused by Oleum Tiglii inductive dropsy of ear and X 5189 simultaneously.The document that Xu Yong etc. deliver " Fructus Sophorae glycosides and genistein are to the influence of the scleroblast biological characteristics " document the is clear and definite estrogen-like effects of Fructus Sophorae glycosides; Document shows that Fructus Sophorae glycosides can effectively stop the bone amount that causes because of estrogen deficiency to run off in vivo; The tissue morphology that keeps bone, Prevention and Treatment of Osteoporosis.Clinical study confirms that also Fructus Sophorae glycosides can be used for preventing and treating the symptom of women's osteosporosis after menopause, and therefore, Fructus Sophorae glycosides has fabulous application prospect and exploitation future.
More in the existing document to researchs such as genistein, Genistosides, and mainly be to rest on the assay aspect to the research of Fructus Sophorae glycosides.The Master's thesis of Liu Xiaohua " research of the Fructus Sophorae and " the Chinese pharmacopoeia version Fructus Sophorae in 2005 assay item standard revision "; The method that this paper openly extracts Fructus Sophorae glycosides is an ethanol ultrasonic extraction, concentrates the first water removal of impurities in back, uses ether defatting again; Obtain product with the N recrystallization at last; Though this method operation is easy, the toxic organic solvent consumption is big, and product content is not high.
Summary of the invention:
The technical problem that the present invention will solve provides a kind of method of from the Fructus Sophorae, extracting Fructus Sophorae glycosides, and this technology makes the product content height, quality is good.
The objective of the invention is to realize through following technical scheme:
A kind of method of from the Fructus Sophorae, extracting Fructus Sophorae glycosides is characterized in that comprising following step:
1) extract: with Fructus Sophorae raw material pulverizing, adds after 8～12 times of amount rare pure liquid of alkalescence and borax mix, heating and extracting 2～3 times, extracting solution adds acid and is adjusted to neutrality, must Fructus Sophorae glycosides crude extract;
2) macroporous resin adsorption: above-mentioned crude extract is crossed macroporous resin adsorption, and washing to sugared reaction negative is used 50～70% ethanolic soln wash-out more earlier, collects elutriant and is concentrated into medicinal extract;
3) removal of impurities: above-mentioned medicinal extract is used an amount of acetic acid ethyl dissolution, and insolubles is used acetone solution again, filters, and gets filter cake;
4) recrystallization: with above-mentioned filter cake with 60～80% alcohol reflux crystallization 2～4 times.
The consumption of borax is 1%～2% of the Fructus Sophorae in the said step 1), and the rare pure liquid pH of alkalescence is controlled at 8～9 (15～30% ethanol), and extraction time is 2～4 hours, extracts temperature and is controlled at 60～80 ℃, and being used to regulate neutral acid can be hydrochloric acid or sulfuric acid.
The model of the macroporous resin said step 2) can adopt a kind of among AB-8, HPD450 or the D101, and the ethanolic soln consumption is 3～6BV, and elution flow rate is controlled to be 0.5～2BV/h.
ETHYLE ACETATE in the said step 3) is 2～5 times of medicinal extract amount, and the acetone consumption is 2～4 times of amounts of insolubles.
The present invention adopts the low pure liquid of alkalescence to extract, because under alkaline condition, the leaching effect of flavones ingredient is better, adds borax and extracts, and can protect phenolic hydroxyl group, prevents that neighbour's two phenolic hydroxyl groups in the Fructus Sophorae glycosides from oxidation taking place under alkaline condition; Adopt oil-soluble impuritieses such as other flavones of acetoneand ethyl acetate flush away, flavonoid glycoside; Utilize the dissolubility difference of Fructus Sophorae glycosides in cold and hot ethanol to carry out the recrystallization operation at last, obtain highly purified product, simple to operate, preparation amount is big.
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment:
Embodiment 1:
With Fructus Sophorae pulverizing medicinal materials, take by weighing 1kg, add pH9.0 alkalescence rare pure liquid (20% ethanol) that 10L contains the 20g borax, heating and refluxing extraction 2 times; Each 2.5 hours, united extraction liquid added hydrochloric acid and is adjusted to neutrality, extracting solution is added in the AB-8 type macroporous resin column adsorbs again; Washing to sugared reaction negative is followed 65% ethanol elution with 5BV earlier, and elution flow rate is 0.5BV/h, collects elutriant; Be concentrated into medicinal extract, add the 120ml acetic acid ethyl dissolution, filter, insolubles is used the acetone solution of 100ml again; Filter, filter cake gets Fructus Sophorae glycosides 37.1g, content 98.3% 3 times with 70% dissolve with ethanol crystallization.
Embodiment 2:
With Fructus Sophorae pulverizing medicinal materials, take by weighing 1kg, add pH9.0 alkalescence rare pure liquid (15% ethanol) that 8L contains the 18g borax, heating and refluxing extraction 3 times; Each 2 hours, united extraction liquid added hydrochloric acid and is adjusted to neutrality, extracting solution is added in the HPD450 type macroporous resin column adsorbs again; Washing to sugared reaction negative is followed 70% ethanol elution with 6BV earlier, and elution flow rate is 2BV/h, collects elutriant; Be concentrated into medicinal extract, add the 100ml acetic acid ethyl dissolution, filter, insolubles is used the acetone solution of 80ml again; Filter, filter cake gets Fructus Sophorae glycosides 33.6g, content 98.7% 4 times with 80% dissolve with ethanol crystallization.
Embodiment 3:
With Fructus Sophorae pulverizing medicinal materials, take by weighing 2kg, add pH8.5 alkalescence rare pure liquid (25% ethanol) that 22L contains the 28g borax, heating and refluxing extraction 3 times; Each 3 hours, united extraction liquid added hydrochloric acid and is adjusted to neutrality, extracting solution is added in the HPD450 type macroporous resin column adsorbs again; Washing to sugared reaction negative is followed 50% ethanol elution with 4BV earlier, and elution flow rate is 1.5BV/h, collects elutriant; Be concentrated into medicinal extract, add the 250ml acetic acid ethyl dissolution, filter, insolubles is used the acetone solution of 180ml again; Filter, filter cake gets Fructus Sophorae glycosides 70.3g, content 97.9% 2 times with 70% dissolve with ethanol crystallization.
Embodiment 4:
With Fructus Sophorae pulverizing medicinal materials, take by weighing 5kg, add pH8 alkalescence rare pure liquid (28% ethanol) that 60L contains the 50g borax, heating and refluxing extraction 3 times; Each 4 hours, united extraction liquid added hydrochloric acid and is adjusted to neutrality, extracting solution is added in the D101 type macroporous resin column adsorbs again; Washing to sugared reaction negative is followed 70% ethanol elution with 3BV earlier, and the collection elution flow rate is 1BV/h, elutriant; Be concentrated into medicinal extract, add the 600ml acetic acid ethyl dissolution, filter, insolubles is used the acetone solution of 500ml again; Filter, filter cake gets Fructus Sophorae glycosides 138.3g, content 98.1% 4 times with 80% dissolve with ethanol crystallization.
Claims (4)
1. method of from the Fructus Sophorae, extracting Fructus Sophorae glycosides is characterized in that comprising following step:
1) extract: with Fructus Sophorae raw material pulverizing, adds after 8～12 times of amount rare pure liquid of alkalescence and borax mix, heating and extracting 2～3 times, extracting solution adds acid and is adjusted to neutrality, must Fructus Sophorae glycosides crude extract;
2) macroporous resin adsorption: above-mentioned crude extract is crossed macroporous resin column absorption, and washing to sugared reaction negative is used 50～70% ethanolic soln wash-out more earlier, collects elutriant and is concentrated into medicinal extract;
3) removal of impurities: above-mentioned medicinal extract is used an amount of acetic acid ethyl dissolution, and insolubles is used acetone solution again, filters, and gets filter cake;
4) recrystallization: with above-mentioned filter cake with 60～80% alcohol reflux crystallization 2～4 times.
2. the method for from the Fructus Sophorae, extracting Fructus Sophorae glycosides as claimed in claim 1; The consumption that it is characterized in that borax in the said step 1) is 1%～2% of the Fructus Sophorae; The rare pure liquid pH of alkalescence is controlled at 8～9 (15～30% ethanol); Extraction time is 2～4 hours, extracts temperature and is controlled at 60～80 ℃, and being used to regulate neutral acid can be hydrochloric acid or sulfuric acid.
3. the method for from the Fructus Sophorae, extracting Fructus Sophorae glycosides as claimed in claim 1; It is characterized in that said step 2) in the model of macroporous resin can adopt a kind of among AB-8, HPD450 or the D101; The ethanolic soln consumption is 3～6BV, and elution flow rate is controlled to be 0.5～2BV/h.
4. the method for from the Fructus Sophorae, extracting Fructus Sophorae glycosides as claimed in claim 1 is characterized in that ETHYLE ACETATE in the said step 3) is 2～5 times of medicinal extract amount, and the acetone consumption is 2～4 times of amounts of insolubles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106038682A CN102532216A (en) | 2010-12-24 | 2010-12-24 | Method for extracting sophoricoside from sophora fruits |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106038682A CN102532216A (en) | 2010-12-24 | 2010-12-24 | Method for extracting sophoricoside from sophora fruits |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102532216A true CN102532216A (en) | 2012-07-04 |
Family
ID=46340373
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010106038682A Pending CN102532216A (en) | 2010-12-24 | 2010-12-24 | Method for extracting sophoricoside from sophora fruits |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102532216A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103724381A (en) * | 2012-10-15 | 2014-04-16 | 天津药物研究院 | Preparation method of robinin-7-O-rhamnose glucoside and application thereof |
| CN108383885A (en) * | 2018-05-02 | 2018-08-10 | 孙波 | From the technique and its purposes in anti-inflammatory for extracting Sophoricoside in the Fructus Sophorae |
| CN113880889A (en) * | 2021-11-15 | 2022-01-04 | 西安久中生物科技有限公司 | Method for extracting sophoricoside, genistein and kaempferol from sophora fruit |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001213775A (en) * | 2000-02-03 | 2001-08-07 | Pola Chem Ind Inc | Stress mitigating preparation and skin care preparation including it |
| CN1417220A (en) * | 2002-11-21 | 2003-05-14 | 吉林天药科技股份有限公司 | Prepn process, medicine prepn and new medicinal use of sophoricosids |
| CN1465570A (en) * | 2002-06-28 | 2004-01-07 | 西安恒泰本草科技有限公司 | Process for preparing genistein, medicinal composition and use thereof |
-
2010
- 2010-12-24 CN CN2010106038682A patent/CN102532216A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001213775A (en) * | 2000-02-03 | 2001-08-07 | Pola Chem Ind Inc | Stress mitigating preparation and skin care preparation including it |
| CN1465570A (en) * | 2002-06-28 | 2004-01-07 | 西安恒泰本草科技有限公司 | Process for preparing genistein, medicinal composition and use thereof |
| CN1417220A (en) * | 2002-11-21 | 2003-05-14 | 吉林天药科技股份有限公司 | Prepn process, medicine prepn and new medicinal use of sophoricosids |
Non-Patent Citations (2)
| Title |
|---|
| 丛艳波，等: "亚临界水提取槐角中总异黄酮的研究", 《中草药》 * |
| 袁崇均，等: "大孔树脂对槐角总黄酮分离纯化工艺研究", 《四川中医》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103724381A (en) * | 2012-10-15 | 2014-04-16 | 天津药物研究院 | Preparation method of robinin-7-O-rhamnose glucoside and application thereof |
| CN108383885A (en) * | 2018-05-02 | 2018-08-10 | 孙波 | From the technique and its purposes in anti-inflammatory for extracting Sophoricoside in the Fructus Sophorae |
| CN108383885B (en) * | 2018-05-02 | 2021-07-23 | 孙波 | Process for extracting sophoricoside from fructus Sophorae and its application in anti-inflammation |
| CN113880889A (en) * | 2021-11-15 | 2022-01-04 | 西安久中生物科技有限公司 | Method for extracting sophoricoside, genistein and kaempferol from sophora fruit |
| CN113880889B (en) * | 2021-11-15 | 2023-12-29 | 西安久中生物科技有限公司 | Method for extracting sophoricoside, genistein and kaempferol from sophora fruit |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Ye et al. | Anoectochilus roxburghii: A review of its phytochemistry, pharmacology, and clinical applications | |
| CN102816066B (en) | Method for extracting chlorogenic acid and hyperoside from lonicera japonica leaves | |
| CN102349959B (en) | Preparation method of effective part of lilac daphne flower bud general flavone aglycon and application of effective part in medicament for resisting immuno-inflammation | |
| CN104013659A (en) | Purified plains coreopsis flavone tablet and preparation method thereof | |
| CN106810622A (en) | It is a kind of that neohesperidin and the method to dried immature fruit of citron orange comprehensive utilization are extracted from the dried immature fruit of citron orange | |
| CN105541776A (en) | Method for extracting rutin from Japanese pagodatree flower buds and preparing quercetin | |
| CN102040593A (en) | Method for simultaneously extracting vitexin and quercetin from Chinese hawthorn leaf | |
| CN102532216A (en) | Method for extracting sophoricoside from sophora fruits | |
| CN102365089B (en) | Medicine for preventing and treating alzheimer's disease and preparative method thereof | |
| CN102764294B (en) | Cough relieving and sputum eliminating combination and preparation method thereof | |
| CN101933967A (en) | Honeysuckle extract preparation method | |
| CN101880303A (en) | Method for extracting bitter gourd saponin from bitter gourd | |
| CN101665479B (en) | Technology for synchronously extracting isofraxidin and flavonoids compounds from sarcandra glabra and applications thereof | |
| CN100477996C (en) | Extract of star of bethlehem and its prepn process, medicinal composition and use | |
| CN103724381A (en) | Preparation method of robinin-7-O-rhamnose glucoside and application thereof | |
| CN103408522B (en) | A kind of method extracting high-purity aesculetin from Euphorbia lathyris fruit | |
| CN101507760B (en) | Medicine composite for treating kidney disease | |
| CN102827128A (en) | Method for extracting and purifying hinokiflavone | |
| CN102603826A (en) | Method for extracting 8-acetylharpagide from decumbent bugle herb plant | |
| CN106117279A (en) | Polyphenol and the continuous extraction method of amygdaloside in a kind of loquat nut | |
| CN103626811B (en) | A kind of method of extraction and isolation phlorizin from cynomorium songaricum | |
| CN104306463A (en) | Method for preparing buckwheat total flavone from buckwheat leftovers and application thereof | |
| CN103815507A (en) | Artemisia leaf beverage and production process thereof | |
| CN103585366A (en) | Medicine for treating ischemic hyperlipidemia and preparation method thereof | |
| CN101862371A (en) | Method for preparing flavone and alkaloid from mulberry leaves |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| DD01 | Delivery of document by public notice |
Addressee: Suzhou Bao Tong Tang Pharmaceutical Technology Co., Ltd. Han Shuyu Document name: Notification of Publication and of Entering the Substantive Examination Stage of the Application for Invention |
|
| DD01 | Delivery of document by public notice |
Addressee: Han Shuyu Document name: the First Notification of an Office Action |
|
| DD01 | Delivery of document by public notice |
Addressee: Han Shuyu Document name: Notification that Application Deemed to be Withdrawn |
|
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120704 |