CN103145782A - Novel extracting process of high-purity baicalin - Google Patents
Novel extracting process of high-purity baicalin Download PDFInfo
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- CN103145782A CN103145782A CN2013100127690A CN201310012769A CN103145782A CN 103145782 A CN103145782 A CN 103145782A CN 2013100127690 A CN2013100127690 A CN 2013100127690A CN 201310012769 A CN201310012769 A CN 201310012769A CN 103145782 A CN103145782 A CN 103145782A
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Abstract
The invention discloses a novel extracting process of high-purity baicalin. The novel extracting process of the high-purity baicalin uniquely adopts the technology that baicalin is extracted in weak acid water at low temperature and dissociate in strong acid conditions, and therefore two steps of acid mixing and subsequent complex refining processes in the present process are avoided, the baicalin with the purity more than 93% is obtained in one step.
Description
Technical field
The present invention relates to a kind of novel extraction process of high-purity baicalin.
Background technology
The root of large-flowered skullcap is the dry root of labiate root of large-flowered skullcap Scutellaria baicalensis Georgi.Heat-clearing and damp-drying drug is arranged, and cool blood is antiabortive, detoxicating functions.Cure mainly the diseases such as febrile disease, upper respiratory tract infection, cough due to lung-heat, damp and hot jaundice, pneumonia, dysentery, hemoptysis, hot eyes, threatened abortion, hypertension, the swollen furuncle sore of carbuncle.The clinical application of the root of large-flowered skullcap is antibiotic not worse than the coptis, and does not develop immunity to drugs, and the root of large-flowered skullcap is the optimal Herba indigoferae Pseudotinctoriae of agricultural disease control.Originate in the ground such as Hebei, Liaoning, Shaanxi, Shandong, the Inner Mongol, Heilungkiang.The root of large-flowered skullcap belongs to half kind kind of semi-wild, this in kind year nearly ten thousand tons of sales volumes, be one of 40 kinds of bulk medicinal materials kinds.nineteen nineties begins, family plants the root of large-flowered skullcap and progressively carries out, mainly be distributed in Shandong, Shaanxi, Shanxi, large producing region, Gansu four, wherein concentrate on Nan Fan town, Jiangxian County, Shanxi, Yuncheng Xia County Yao Fengzhen, Wan An town, Xinjiang County, the ground such as Wanrong County, Shanglou, Shaanxi, Linwei District Qiao Nan town, Weinan, Shangzhou City Shangzhou District Xiaoyi town, scape villages and small towns, Luonan County, the Danfeng County kerria spends the town, villages and small towns at night, Shangluo City, the ground such as Feng County Shang Zhen, Yimeng Mountain Area, Shandong Province, mountain area, storehouse, Juxian County, Laiwu City tealeaves mouth town, the ground such as rich government's bank township, the main product west of Gansu Province, Gansu, the Weiyuan, the Zhang County, inferior product Minxian County, the Dangchang, the ground such as the west of a river.The wild root of large-flowered skullcap mainly distribute China Hebei, North of Shanxi, the large section in the central and east, Inner Mongol and three provinces in the northeast of China, the Chengde, several main producing regions on the largest scale such as Chifeng, the Inner Mongol are one of principal item of the wild Chinese medicinal materials of northern China.Have the history of more than 2000 year in root of large-flowered skullcap clinical application, remain now the key medicine of heat-clearing and damp-drying drug, eliminating fire and detoxication.Except traditional Chinese medical science formula, in a large number as the Chinese patent medicine raw material.According to the statistical information of " national Chinese patent medicine products catalogue " First, 66 kinds of honeyed bolus have 45 kinds to use the root of large-flowered skullcap, and 64 kinds of tablets have 46 kinds to use the root of large-flowered skullcap, and 36 kinds of water-bindered pills have 25 kinds to use the root of large-flowered skullcap.Many areas utilize the root of large-flowered skullcap or scutellaria viscidula Bge to extract scutellarin, baicalin as pharmaceutical raw material, and consumption is also very large, and this is a new development approach.Foreign material report, root of large-flowered skullcap tincture can be controlled hypertension and the neuropathic dysfunction of neuro vegetative arteriosclerotic, also can eliminate headache that hypertension causes, insomnia, the disease such as uncomfortable in chest.The application of the root of large-flowered skullcap, more and more paid attention to by domestic and international at present, and the exploitation future is arranged greatly, except normal pharmaceutical factory feeds intake, medicine materical crude slice is filled a prescription, is mainly used in now extracting.Family plants a root of large-flowered skullcap part and is used for medicine materical crude slice processing, more is used for the pharmaceutical factory to the extraction of baicalin.In recent years the exploitation of Chinese patent medicine " SHUANGHUANLIAN " and wideling popularize, a consumption that makes house plant the root of large-flowered skullcap increases.Simultaneously, due to the minimizing year by year of wild resource, the new amount of the product of the wild root of large-flowered skullcap descends just year by year, and it produces the not enough contradiction that needs, the high price of the wild root of large-flowered skullcap can pull house to plant the price of the root of large-flowered skullcap by nature, and the low price of family's kind root of large-flowered skullcap also will suppress rising suddenly and sharply of wild root of large-flowered skullcap price.
Scutellariae,radix contains flavonoid compound: scutellarin (baicalein); Neobaicalein (neobaicalein); Be skullcapflavone II (skullcapflavone II); Baicalin (baicalin); Wogonin (wogonin); Wogonoside (wogono-side); Oroxylin A A (oroxylin, oroxylin A); 7-methoxyl group scutellarin (7-methoxbaic alein); Skullcapflavone (skullcapflavone) I; Dihydro Oroxylin A A (dihydrooroxylin A); Chrysin (chrysin); 2,5,8-trihydroxy--7-methoxy flavone; 2,5,8-trihydroxy--6, the 7-dimethoxy flavone; 4,5,7-trihydroxy--6-methoxyl group flavanone; 2,3,5,6,7-penta hydroxy group flavanone; Wogonin-5-β-D-Glucose glycosides (wogonin-5-β-D-glucoside); 2-(3-hydroxyl-4-p-methoxy-phenyl)-ethyl-1-O-α-L-rhamanopyranosyl (1 → 3)-β-D (4-asafoetide acyl group)-glucose; 6-C-α-L-arabinose glycosides; Chrysin-6-C-α-L-arabinose glucoside-8-C-β-D-Glucose glycosides; (2S)-2,5,6,7-tetrahydroxy flavanone; 5,7,2,6-kaempferol; 5,8-dihydroxyl-6, the 7-dimethoxy flavone; 5,7,4-trihydroxy--8-methoxy flavone; Oroxylin A A-7-O-glucuronide; 5,7,2-trihydroxy-methoxy flavone; 5,2-dihydroxyl-6,7, the 8-trimethoxy flavone; 5-gate of a lane base-7, the 8-dimethoxy flavone; Norwogonin (norwogonin); Dihydro scutellarin (dihydro-baicalin); 5,7,2-trihydroxyflavone; 5,7,2-trihydroxy--8, the 6-dimethoxy flavone; 5,7,2,5-tetrahydroxy-8,6-dimethoxy flavone are viscidulin III; 5,25-trihydroxy-trimethoxy flavone; Scutellarin-7-O-β-D-glucopyranoside; 5,7,2-trihydroxy--8-methoxy flavone is tenaxin II (tenax-in II); 5,2,6-trihydroxy--7, the 8-dimethoxy flavone; 5,2,6-trihydroxy--6-methoxy-2-phenyl-4H-chromen-4-one; 5,7,2,3-kaempferol; The great basic flavones of 5,7,2,3-four; 3,5,7,2,5,6-pentahydroxyflavone; (2S)-7,2,6-trihydroxy--5-methoxyl group flavanone; 2,6,2,4-tetrahydroxy-6-methoxyl group cinnamophenone; 5,7,2,5-kaempferol; Left-handed eriodictyol (eriodictyol); Herba Scutellariae Barbatae kind element (rivularin) and viscidulin III-2-O-β-D-glucopyranoside etc.Also contain in addition β-sitosterol (β-sitosterol), campesterol (campesterol) and Stigmasterol (stigmasterol).The Yunnan scutellariae,radix contains the river rising in Ningxia and flowing into central Shaanxi scutellarin, scutellarin, baicalin, wogonoside, 5,7,2-trihydroxy--6-methoxy-2-phenyl-4H-chromen-4-one; (2S)-5,7,8-trihydroxy-flavanone; (2S)-2,5,6,7-tetrahydroxy flavane scutellarin, Yunnan baicalin (scuteamoenoside); Scuteamoenin (scuteamoenin); (2R, 3R)-3,5,7-trihydroxy-flavanone, skullcapflavone II; 2,3,5,6,7-pentahydroxyflavone; Chrysin; β-sitosterol; Oroxylin A A.The Sutellaria viscidula root contains baicalin, wogonoside, and scutellarin, wogonin, Oroxylin A A, neobaicalein, 5,2-dihydroxyl dimethoxy flavone (panicolin) is skullcapflavone I, viscidulin I, II, III.The Lijing scutellariae,radix contains scutellarin, wogonin, chrysin, Oroxylin A A, tenaxin II, sticking kilocycle scutellarin I.The scutellaria rehderiana Diels root contains rehderianin (rehderianin) I, viscidulin III, baicalin, wogonin, scutellarin, Oroxylin A A, Gansu a kind of reed mentioned in ancient books aglycon (ganhuangenin).The scutellaria hypericifolia root contains baicalin, wogonoside, scutellarin, viscidulin I, II, Oroxylin A A and wogonin.
the root of large-flowered skullcap has following pharmacological action: 1) antifungic action root of large-flowered skullcap decocting liquid can suppress dog denticle born of the same parents bacterium, trichophyton, oidium schoenleinii, the mutation of oidium schoenleinii Mongolia, the homocentricity trichophyton, the rust trichophyton, Trichophyton concentricum, Microsporon audouini, wool sample microspore tinea bacterium, dysentery bacterium, Corynebacterium diphtheriae, paratyphosum Bacterium, vibrio cholerae, intestinal bacteria, Bacillus proteus, Pseudomonas aeruginosa, staphylococcus, hemolytic vessel used to hold grain at the imperial sacrifice coccus, pneumococcus, diphtheria corynebacterium, shigella flexneri, the bacillus tuberculosis typus humanus, vibrio cholerae, dysentery bacterium, tangerine grass bacillus, streptococcus aureus, meningococcus, epidermophyton rubrum and star nocardia etc. have bacteriostatic action in various degree.2) antivirus action root of large-flowered skullcap decoction has copied restraining effect to hepatitis B virus DNA.3) anti-inflammatory anti-allergic balcalin extract can suppress mouse peritoneal and oozes out increase, to the rat foot is swollen, restraining effect is arranged also, and rat assist agent arthritis is had restraining effect.Reaction has restraining effect to root of large-flowered skullcap aqueous extract to models of passive skin irritability of rats.Antihistamine is arranged, cholinolytic and the effect of Papaverine sample.Allergic asthma there is restraining effect, suppresses the Forssman cutaneous vasculitis.Antibody-mediated anaphylaxis has high degree of specificity to reaginic antibody (Reagin), also suppresses the reaction of non-reaginic antibody mediation.Rat epoxidase and lipoxygenase all there is restraining effect.White corpuscle 5-HETE is formed also suppress, scavenger cell generation PGE2 and TXA2 are all had obvious restraining effect.4) to the mouse defensive conditionedreflex, positive reflex time is extended the effect root of large-flowered skullcap decoction of central nervous system, can strengthen the cortex process of inhibition, refrigeration function is arranged.5) to cardiovascular effect root of large-flowered skullcap alcohol extract, anaesthetized dog blood pressure is descended, obvious hypotensive effect is arranged.6) platelet aggregation-against and anti-freezing root of large-flowered skullcap alcohol extract can suppress rat platelet aggregation, platelet aggregation to arachidonic acid-induction also has restraining effect, Fibrinogen is converted into scleroproein also suppresses, can prevent the reduction of thrombocyte and fibrinogen content.7) reducing blood lipid root of large-flowered skullcap infusion can make serum cholesterol content descend.Can reduce the content of serum free fatty acid, triglyceride level and liver triglyceride level, can reduce serum and liver total cholesterol, free cholesterol and content of triglyceride, 8) protect the liver, infringement has restraining effect to rats'liver for cholagogic, anti-oxidant balcalin extract, can suppress the increase of serum bilirubin, choleretic effect is arranged, mda (MDA) content is descended, the rat liver homogenate lipid peroxidation there is restraining effect, the formation of liver MDA is significantly descended.9) antitumous effect root of large-flowered skullcap ether extract has cytotoxicity to mouse leukemia L1210 cell.10) other effect root of large-flowered skullcap has diuretic properties to anesthetized dog, and rat galactose-cataract is had preventive and therapeutic effect, and the effect that suppresses the aldose enzyme is also arranged in animal body, might be used for the control of diabetic complication, and the Mouse Liver sialidase is had restraining effect.
The root of large-flowered skullcap is treated children with acute respiratory infection clinically, treatment chronic tracheitis, treatment acute bacillary dysentery, treatment leptospirosis, treatment infectious hepatitis, treatment ephritis, pyelonephritis, Hypertension.
At present, a lot of about the extracting method of baicalin, water extraction alkali extraction and acid precipitation method, water extraction stone sulphur alcohol deposition method, alkali alcohol glue peptone method, the alcohol extracting-water precipitating acidization, degreasing alcohol extracting method, resin adsorption method, grading extraction method, the microwave extraction method, water extraction alcohol deposition method, ultrafiltration process, ultrasonic method etc.The present invention adopts weak acid to extract, and a step can obtain highly purified baicalin, has avoided two step acid systems in present technique, and the treating process of postorder.
Summary of the invention
First gets the raw materials ready: the root of large-flowered skullcap is rinsed well, be crushed to 10～20 orders, and standby.
Second extracts: the root of large-flowered skullcap material that crushes is dropped in multi-function extractor, transfer purified water pH3～4 to extract the root of large-flowered skullcap with hydrochloric acid.Filter residue press dry, and collects the extracting solution Plate Filtration, obtains extracting solution.
The 3rd acid out: extract in filtered liquid and add hydrochloric acid, under high temperature, the salt of baicalin is free under acidity is monomeric compound.
The 4th press filtration: the free baicalin of gained is with the plate-and-frame filter press press filtration.
The 5th washing: filter cake washs with purified water.
The 6th drying: low-temperature vacuum drying.
Embodiment
Get clean dried scutellariae,radix 500g, be crushed to 10～20 orders, extract 2h with 10 times of amounts of purified water (w/w) of pH value 3～4 at 40～60 ℃, filter, obtain filtrate; Filter residue extracts 1.5h with 8 times of amounts of purified water (w/w) of pH value 4～5 at 40～60 ℃ again, filters, and obtains filtrate; Filter residue extracts 1.0h with 6 times of amounts of purified water (w/w) of pH value 4～5 at 40～60 ℃ again, filters, and obtains filtrate, and filter residue press dry.Merge 3 times filtered liquid, add 1: 1 hydrochloric acid adjust pH 1～2, at 70～80 ℃ of insulation 0.5～1.0h, filter, be washed to neutrality, 40～45 ℃ of vacuum-dryings, obtain faint yellow baicalin finished product 61.5g, content 93.6% (HPLC).
Claims (6)
1. the novel extraction process of a high-purity baicalin, is characterized in that, take the root of large-flowered skullcap as raw material, this technique is successively through following steps:
(1) get the raw materials ready: the root of large-flowered skullcap is rinsed well, pulverized, standby.
(2) extract: the root of large-flowered skullcap material that crushes is dropped in multi-function extractor, add acid purified water extraction.Filter residue press dry, and collects the extracting solution Plate Filtration, obtains extracting solution.
(3) acid out: add hydrochloric acid in extracting solution, react under high temperature, obtain the reaction solution of free baicalin.
(4) press filtration: the reaction solution of gained is cooling, and precipitation is rear with the plate-and-frame filter press press filtration.
(5) washing: filter cake washs with purified water.
(6) drying: low-temperature vacuum drying.
2. the novel extraction process of a kind of high-purity baicalin as claimed in claim 1, is characterized in that, the root of large-flowered skullcap before step (1) is pulverized must be dry, and is clean, is crushed to 10～20 orders.
3. the novel extraction process of a kind of high-purity baicalin as claimed in claim 1, is characterized in that, transferring purified water pH value with hydrochloric acid in step (2) is 3～4 extraction solvents as the root of large-flowered skullcap.10 times of amounts (w/w) are extracted 2h at 40～60 ℃, and 8 times of amounts (w/w) are extracted 1.5h at 40～60 ℃, and 6 times of amounts (w/w) are extracted 1.0h at 40～60 ℃.
4. the novel extraction process of a kind of high-purity baicalin as claimed in claim 1, is characterized in that, transferring extracting liquid pH value with hydrochloric acid in step (3) is 1～2,70～80 ℃ of reaction 0.5～1.0h of temperature.
5. the novel extraction process of a kind of high-purity baicalin as claimed in claim 1, is characterized in that, in step (5), is washed till pressing filtering liquid pH value with purified water and is neutral.
6. the novel extraction process of a kind of high-purity baicalin as claimed in claim 1, is characterized in that, in step (6), drying temperature is 40～45 ℃.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| CN105131062A (en) * | 2015-08-12 | 2015-12-09 | 山西大学 | Scutellaria baicalensis extract preparation method |
| CN106977565A (en) * | 2017-03-30 | 2017-07-25 | 广东利泰制药股份有限公司 | A kind of extracting method of scutelloside |
| CN107626220A (en) * | 2016-07-19 | 2018-01-26 | 丁观军 | A kind of method and its application for promoting flavones or glycosides compound dissolving |
| CN113896754A (en) * | 2021-11-29 | 2022-01-07 | 郑州大学 | Industrial production method for extracting and purifying baicalin from scutellaria baicalensis |
| CN114853834A (en) * | 2022-06-01 | 2022-08-05 | 诸城市浩天药业有限公司 | Environment-friendly process method for producing baicalin |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
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| CN106977565A (en) * | 2017-03-30 | 2017-07-25 | 广东利泰制药股份有限公司 | A kind of extracting method of scutelloside |
| CN113896754A (en) * | 2021-11-29 | 2022-01-07 | 郑州大学 | Industrial production method for extracting and purifying baicalin from scutellaria baicalensis |
| CN114853834A (en) * | 2022-06-01 | 2022-08-05 | 诸城市浩天药业有限公司 | Environment-friendly process method for producing baicalin |
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Application publication date: 20130612 |