CN1454899A - Process of extracting baicalin from scutellaria baicalensis - Google Patents
Process of extracting baicalin from scutellaria baicalensis Download PDFInfo
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- CN1454899A CN1454899A CN 03138015 CN03138015A CN1454899A CN 1454899 A CN1454899 A CN 1454899A CN 03138015 CN03138015 CN 03138015 CN 03138015 A CN03138015 A CN 03138015A CN 1454899 A CN1454899 A CN 1454899A
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- siberian cocklebur
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Abstract
The process for extracting baicalin from scutellaia root includes the following steps: breaking scutellaria root into small blocks, according to the weight of scutelliaria root adding 3-10 times boiling water, decocting for 3 times, every time for 1-3 hr. straining, combining colatures, standing still for removing impurities, using hydrochloric acid to regulate pH value of colature to 1-2, heat-insulating for 30-60 min. at 70-80 deg.C, separating out baicalin precipitate, using acidic water or water to wash baicalin precipitate for several times, heat-insulating and standing still for above 12 hr. at 70-80 deg.C, filtering and precipitating, then drying to obtain baicalin crude product. The baicalin crude product content is above 80%, and the extraction rate of baicalin is above 80%.
Description
Technical field
The present invention relates to baicalin novel technology for extracting in a kind of yellow Siberian cocklebur.
Background technology
Huang Ling is that Chinese Pharmacopoeia is gone through the kind that version is recorded, the effect of tool heat-clearing and damp-drying drug, eliminating fire and detoxication, arresting bleeding and miscarriage prevention.Be used for damp-warm syndrome, the heat temperature, the evil of vomitting uncomfortable in chest, damp and hot ruffian is full, rushes down dysentery, jaundice, lung heat, cough, high hot polydipsia, blood-head is told nosebleed, carbuncle sore tumefacting virus, threatened abortion.It is a kind of clinically conventional Chinese medicine.According to the literature, the effective constituent of Huang Ling is flavonoid compounds such as baicalin, Chinese baicalin and aglycon thereof.In preparation, many forms with the baicalin extract feed intake at present.At present, the extracting method of Chang Yong baicalin can reduce following four kinds substantially:
1, gets yellow Siberian cocklebur medicine materical crude slice, boiling three times, collecting decoction, filter, filtrate is concentrated into relative density 1.05-1.10 (80 ℃ of surveys), adds hydrochloric acid soln at 80 ℃, regulate pH value to 1-2, be incubated 1 hour, static 24 hours, filter, throw out adds the water that 6-8 doubly measures, and the sodium hydroxide with 40% transfers to pH value to 7-7.5, adds equivalent ethanol, stirring and dissolving, filter, filtrate is transferred pH value to 2 with hydrochloric acid, and 60 ℃ are incubated 30 minutes, static 12 hours, filter, precipitation washes with water to PH5, continues to be washed till PH7 with 70% ethanol, low temperature volatilizes, promptly.The shortcoming of this extracting method is that energy consumption is big, complex operation, and the rate of loss height of baicalin, extraction yield is low, the cost height.
2, get yellow Siberian cocklebur boiling, collecting decoction filters, and filtrate concentrates, spraying drying.Yellow Siberian cocklebur extraction yield is increased to 22% by 12%, and the content of baicalin rises to 20%-24% by original 4% in the radix scutellariae extract.Though this method is simple, the content of baicalin 20-24% only is lower in the extract.
3, use tributyl phosphate, two (2-ethylhexyl) amine, the trioctyl-phosphine oxide equal solvent directly extracts baicalin from yellow Siberian cocklebur, or with baicalin and the isolating method of Chinese baicalin, extraction yield is up to 90%.This method is the patent in Japanese Jin Cun pharmaceutical factory, though the extraction yield height of baicalin, its used extraction solvent is the organic solvent that is of little use, the cost height, and safety coefficient is little.
4, get Huang Ling and pulverize after, use ethanol percolate extraction, after percolate reclaims ethanol, dilute with water, last resin column chromatography for separation, water and organic solvent wash-out, collection organic solvent elutriant, the recovery solvent promptly gets radix scutellariae extract.This method is that Chinese patent CN1268512AS is disclosed, and its shortcoming is that technology is more loaded down with trivial details, the cost height, and yield is low.
Summary of the invention
It is easy that technical problem to be solved by this invention provides a kind of technology, extraction yield height, baicalin novel technology for extracting in the low yellow Siberian cocklebur of cost
The technical solution adopted for the present invention to solve the technical problems:
Get the Huang Ling pulverizing and be fritter, add the 3-10 boiling water doubly of yellow Siberian cocklebur weight, boil and carry 3 times, each 1-3 hour, coarse filtration merged coarse filtration liquid, static removal of impurities, filtrate is regulated pH value to 1-2 with hydrochloric acid, 70-80 ℃ of insulation 30-60 minute, separates out the baicalin precipitation, with sour water or water washing baicalin precipitation several, 70-80 ℃ of insulation is static more than 12 hours, filtering-depositing, and drying gets the baicalin crude product then.
Described dry the employing dry below 70 ℃.Also can adopt direct spraying drying.
Principle of the present invention is as follows:
According to baicalin is phenolic hydroxyl group, and the glycosides compound of band a part glucose, water-soluble big, easily oxidation, enzymolysis, rotten character.Adopted to add proper amount of boiling water and boil and carry, without concentrating, alkalinisation treatment only needs coarse filtration, and static removal of impurities is with sour water or the sedimentary method of water washing.Kill enzyme through boiling water, shorten technology, removal of impurities and washing precipitation have stoped enzymolysis, the oxidation, rotten of baicalin, have increased substantially its extraction yield and content purity.
Beneficial effect of the present invention is as follows:
1, the present invention only adopts water and sour water in the process of obtaining through refining, and need not any organic solvent, and safety in production coefficient height in addition, has saved concentrated and alkalinisation treatment program, has reduced facility investment, shortened technology and reduced energy consumption, and cost is lower.
2, the baicalin crude product that the present invention obtained through refining, through using the high-efficient liquid phase technique assay determination, the purity of its baicalin is more than 80%, and the extraction yield of baicalin from yellow Siberian cocklebur medicinal material be more than 80%, (seeing accompanying drawing 1,2).Because the baicalin that the present invention obtained through refining, purity height, extraction yield height have not only been saved cost, but also have improved the utilization ratio of effective constituent and yellow Siberian cocklebur medicinal material.
Description of drawings
The baicalin reference substance HPLC color atlas that Fig. 1 Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides.
The baicalin rough piece HPLC color atlas that Fig. 2 the present invention obtains through refining.
In Fig. 1,1 is reference substance baicalin chromatographic peak.
In Fig. 2, the 2 baicalin chromatographic peaks of obtaining through refining for the present invention.
Embodiment
Embodiment 1:
Get different yellow Siberian cocklebur medicinal material 400g, 150g, 50g and 300g respectively, coarse crushing becomes fritter, respectively press medicinal material weight, add the boiling water that 3-1O doubly measures, boil and carry 3 times, each 1-3 hour, coarse filtration, merging filtrate, static removal of impurities, filtrate was regulated pH value to 1-2 with hydrochloric acid, 70-80 ℃ of insulation 30-60 minute, separate out the baicalin precipitation, with sour water (or water) washing precipitation for several times, 70-80 ℃ of insulation is static more than 12 hours, filtering-depositing, dry (also can adopt direct spraying drying) below 70 ℃ gets baicalin crude product 46.5g, 25g, 8.6g and 35.6g respectively.Press the high-efficient liquid phase technique under yellow Siberian cocklebur item of Chinese Pharmacopoeia version in 2000, measure each yellow Siberian cocklebur medicinal material and the content of the corresponding baicalin crude product obtained through refining, calculate the extraction yield of baicalin, result such as subordinate list 1.
Baicalin content and extraction yield in subordinate list 1 yellow Siberian cocklebur medicinal material and the baicalin crude product
| Yellow Siberian cocklebur medicinal material amount (g) | Medicinal material content (%) | Total content in the medicinal material (g) | Baicalin crude product amount (g) | Baicalin content (%) in the crude product | The total content of baicalin (g) | Extraction yield (%) |
| ??400 | ??10.99 | ????43.96 | ????46.5 | ????80.52 | ??37.44 | ??85.17 |
| ??150 | ??16.38 | ????24.57 | ????25 | ????81.10 | ??20.275 | ??82.52 |
| ??50 | ??16.91 | ????8.455 | ????8.6 | ????80.03 | ??6.88 | ??81.37 |
| ??300 | ??10.99 | ????28.31 | ????35 | ????81.00 | ??22.96 | ??80.99 |
Claims (3)
1, baicalin novel technology for extracting in the yellow Siberian cocklebur is characterized in that: get the Huang Ling pulverizing and be fritter, add the 3-10 boiling water doubly of yellow Siberian cocklebur weight, boil and carry 3 times, each 1-3 hour, coarse filtration, merge coarse filtration liquid, static removal of impurities, filtrate is regulated pH value to 1-2 with hydrochloric acid, 70-80 ℃ of insulation 30-60 minute, separate out the baicalin precipitation, with sour water or water washing baicalin precipitation several, 70-80 ℃ of insulation is static more than 12 hours, filtering-depositing, drying gets the baicalin crude product then.
2, baicalin novel technology for extracting in the yellow Siberian cocklebur according to claim 1 is characterized in that described dry the employing dry below 70 ℃.
3, baicalin novel technology for extracting in the yellow Siberian cocklebur according to claim 1 is characterized in that the described dry direct spraying drying that adopts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03138015 CN1207301C (en) | 2003-05-25 | 2003-05-25 | Process of extracting baicalin from scutellaria baicalensis |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03138015 CN1207301C (en) | 2003-05-25 | 2003-05-25 | Process of extracting baicalin from scutellaria baicalensis |
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| CN1454899A true CN1454899A (en) | 2003-11-12 |
| CN1207301C CN1207301C (en) | 2005-06-22 |
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| CN 03138015 Expired - Fee Related CN1207301C (en) | 2003-05-25 | 2003-05-25 | Process of extracting baicalin from scutellaria baicalensis |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100361662C (en) * | 2004-09-28 | 2008-01-16 | 北京中医药大学 | Preparation method of traditional Chinese medicine compositions formulation |
| CN100384431C (en) * | 2004-09-28 | 2008-04-30 | 北京中医药大学 | Traditional Chinese medicine compositions |
| CN102091085A (en) * | 2011-01-11 | 2011-06-15 | 中山大学 | Compound pharmaceutical composition for improving oral bioavailability of taxol and application thereof |
| CN101642487B (en) * | 2009-09-15 | 2011-09-07 | 韩桂茹 | Simultaneous extraction and separation process of baicalin and baicalein in baikal skullcap root |
| CN102335232A (en) * | 2011-10-17 | 2012-02-01 | 宁波立华植物提取技术有限公司 | Device and method for preparing scutellaria baicalensis extract |
| CN103145782A (en) * | 2013-01-14 | 2013-06-12 | 李玉山 | Novel extracting process of high-purity baicalin |
| CN103694294A (en) * | 2014-01-10 | 2014-04-02 | 河南智晶生物科技有限公司 | Method for extracting baicalin by use of flash extraction technology |
| CN104004037A (en) * | 2014-06-12 | 2014-08-27 | 宜春学院 | Baicalin, 8-position methylamine derivative of baicalin ester, and preparation method of 8-position methylamine derivative of baicalin ester |
| CN104130230A (en) * | 2014-06-30 | 2014-11-05 | 施佩蓓 | Baicalein production method |
| CN101993461B (en) * | 2009-08-27 | 2015-02-25 | 河北以岭医药研究院有限公司 | Method for refining crude baicalin |
| CN104530161A (en) * | 2014-12-03 | 2015-04-22 | 安徽海神寿春药业有限公司 | Production process of baikal skullcap root extract |
| CN113533598A (en) * | 2021-07-30 | 2021-10-22 | 海南葫芦娃药业集团股份有限公司 | High performance liquid chromatography analysis method for content of scutellaria baicalensis in infantile lung heat cough and asthma granules |
-
2003
- 2003-05-25 CN CN 03138015 patent/CN1207301C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100361662C (en) * | 2004-09-28 | 2008-01-16 | 北京中医药大学 | Preparation method of traditional Chinese medicine compositions formulation |
| CN100384431C (en) * | 2004-09-28 | 2008-04-30 | 北京中医药大学 | Traditional Chinese medicine compositions |
| CN101993461B (en) * | 2009-08-27 | 2015-02-25 | 河北以岭医药研究院有限公司 | Method for refining crude baicalin |
| CN101642487B (en) * | 2009-09-15 | 2011-09-07 | 韩桂茹 | Simultaneous extraction and separation process of baicalin and baicalein in baikal skullcap root |
| CN102091085A (en) * | 2011-01-11 | 2011-06-15 | 中山大学 | Compound pharmaceutical composition for improving oral bioavailability of taxol and application thereof |
| CN102335232A (en) * | 2011-10-17 | 2012-02-01 | 宁波立华植物提取技术有限公司 | Device and method for preparing scutellaria baicalensis extract |
| CN103145782A (en) * | 2013-01-14 | 2013-06-12 | 李玉山 | Novel extracting process of high-purity baicalin |
| CN103694294A (en) * | 2014-01-10 | 2014-04-02 | 河南智晶生物科技有限公司 | Method for extracting baicalin by use of flash extraction technology |
| CN104004037A (en) * | 2014-06-12 | 2014-08-27 | 宜春学院 | Baicalin, 8-position methylamine derivative of baicalin ester, and preparation method of 8-position methylamine derivative of baicalin ester |
| CN104004037B (en) * | 2014-06-12 | 2016-10-19 | 宜春学院 | 8-position methylamine like derivative of baicalin and ester thereof and preparation method thereof |
| CN104130230A (en) * | 2014-06-30 | 2014-11-05 | 施佩蓓 | Baicalein production method |
| CN104530161A (en) * | 2014-12-03 | 2015-04-22 | 安徽海神寿春药业有限公司 | Production process of baikal skullcap root extract |
| CN113533598A (en) * | 2021-07-30 | 2021-10-22 | 海南葫芦娃药业集团股份有限公司 | High performance liquid chromatography analysis method for content of scutellaria baicalensis in infantile lung heat cough and asthma granules |
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| Publication number | Publication date |
|---|---|
| CN1207301C (en) | 2005-06-22 |
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| TR01 | Transfer of patent right |
Effective date of registration: 20090220 Address after: Hebei province Shijiazhuang City Xinshi Road No. 88 Yan peak, zip code: 050091 Patentee after: Zhang Wenchen Address before: No. 44 Fu Qiang street, Shijiazhuang, Hebei, Hebei Provincial Institute for drug control, zip code: 050011 Co-patentee before: Li Xiaoyan Patentee before: Han Gu Lu Co-patentee before: Zhao Shaohua |
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Owner name: ZHANG WENCHEN Free format text: FORMER OWNER: HAN GUIRU Effective date: 20090220 |
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Assignee: Chengde Yanfeng Pharmaceutical Industry Co., Ltd. Assignor: Zhang Wenchen Contract fulfillment period: 2009.2.24 to 2019.2.23 contract change Contract record no.: 2009130000020 Denomination of invention: Process of extracting baicalin from scutellaria baicalensis Granted publication date: 20050622 License type: Exclusive license Record date: 2009.3.2 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.2.24 TO 2019.2.23; CHANGE OF CONTRACT Name of requester: CHENGDE YANFENG DRUG INDUSTRY CO.,LTD. Effective date: 20090302 |
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Granted publication date: 20050622 Termination date: 20150525 |
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