CN105001285A - Method for extracting baicalin from radix scutellariae - Google Patents
Method for extracting baicalin from radix scutellariae Download PDFInfo
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- CN105001285A CN105001285A CN201510366682.2A CN201510366682A CN105001285A CN 105001285 A CN105001285 A CN 105001285A CN 201510366682 A CN201510366682 A CN 201510366682A CN 105001285 A CN105001285 A CN 105001285A
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Abstract
The invention discloses a method for extracting baicalin from radix scutellariae. The method comprises crushing radix scutellariae to obtain powder of 40-60 meshes, adding ethanol into the powder according to a weight ratio of powder to ethanol of 1: 4-8, carrying out stirring by an ultrasonic blender for 25-40min to obtain a mixed solution, transferring the mixed solution into a reflux device, carrying out reflux extraction to obtain extract, carrying out reduced pressure concentration on the extract, adjusting pH to 2-3 by citric acid, carrying out drying to obtain a baicalin crude product, carrying out silica gel column chromatography on the crude product, carrying out drying, dissolving the solids in methanol, and carrying out recrystallization, filtration and drying to obtain high purity baicalin. The method has a baicalin extraction rate of 90% and realizes purity of 98.5 or more. The method has the advantages of simple processes, low energy consumption, short extraction time, high extraction rate, high purity, low cost and good industrial production feasibility.
Description
Technical field
The present invention relates to Chinese herbal medicine effective ingredients extractive technique field, especially a kind of method extracting baicalin from the root of large-flowered skullcap.
Background technology
The dry root that the root of large-flowered skullcap (Scutellaria baicalensis Georgi) is the labiate root of large-flowered skullcap, baicalin (Baicalin) is extraction and isolation a kind of flavonoid compound out from scutellariae,radix, is about 10-20% at the content of baicalin in Scutellaria baicalensis Georgi.Baicalin has antibacterial, diuresis, anti-inflammatory, resistance state and spasmolysis, and has the physiological potencies such as stronger antitumor response.Critical role is occupied at clinical medicine.Baicalin can also absorb ultraviolet, scavenging activated oxygen, again can the generation of check melanin, and therefore both can be used for medicine, also can be used for makeup, is a kind of good functional cosmetics raw material.
The traditional extracting method of baicalin is: shredded by fresh Scutellaria baicalensis root, extract with 10 times of water gaging ebuillition of heated, united extraction liquid, place extracting solution to normal temperature, acid adding regulates pH value, namely baicalin is settled down to bottom, removes supernatant liquor, precipitates the stirring that adds water, continue acid adjustment, must crude baicalin be precipitated as, then carry out crystallization and recrystallization with appropriate solvent, both obtain baicalin.But the method exists, and power consumption is large, extraction time long, extraction yield and the problem such as purity is lower.In recent years, the extracting method of baicalin obtains further improvement, reported resin adsorption method, microwave loss mechanisms, enzymolysis process, supercritical carbon dioxide process etc., but also there is the problems such as the extraction yield of baicalin is low, purity is low, production cost is high, extracting cycle is long in these extracting method.
Summary of the invention
The object of the invention is to, for existing baicalin extraction process Problems existing, provide a kind of method extracting high-purity baicalin from the root of large-flowered skullcap.The extraction yield of the method baicalin and purity are obtained for larger raising, and the method also has that operating procedure is simple, cost is low, is easy to realize the advantages such as suitability for industrialized production.
In order to realize above object, the present invention is achieved by the following technical solutions:
From the root of large-flowered skullcap, extract a method for baicalin, comprise the following steps:
(1) root of large-flowered skullcap is crushed to 40-60 order, obtains Baical Skullcap Root;
(2) add in ultrasonic stirrer by Baical Skullcap Root, adding with its weight ratio is 1:4-8 ethanol doubly, then stirs 25-40min, obtains mixed solution;
(3) again mixed solution is transferred to reflux, refluxing extraction 3-4 time, reflux 0.5-1h at every turn, united extraction liquid;
(4) by said extracted liquid temperature be 70-80 DEG C, pressure be the condition of 0.07-0.09Mpa under concentrating under reduced pressure 1.5-2h, concentrated solution can be obtained, regulate the pH value of concentrated solution to 2-3 with citric acid again, by throw out after filtering, be dry 1-2h under the condition of 70-80 DEG C in temperature, can crude baicalin be obtained;
(5) after crude baicalin dissolve with methanol through filtering, the filtrate obtained, through silica gel column chromatography, is made into elutriant with methyl alcohol and the water that volume ratio is 3:1, finally collects sample solution after wash-out, by sample solution drying at 70-80 DEG C, obtains solids;
(6) dissolved by solids with methyl alcohol again, then use ordinary method recrystallization, filter, the crystallisate obtained is dry at 70-80 DEG C, can obtain high-purity baicalin.
Alcohol concn described in above step (2) is 80-90%.
The concentration of above-described citric acid is 6-8%.
The stirring velocity of above step (2) is 300-500r/min.
The concentration of the above methyl alcohol is 90-95%.
The purity of above-described high-purity baicalin reaches more than 98.5%.
Compared with prior art, beneficial effect of the present invention is:
(1) in the present invention before refluxing extraction baicalin first through ultrasonic stirring, utilizing hyperacoustic cavatition to make, baicalin is easier extracts from the root of large-flowered skullcap, after ultrasonic wave makes extracting solution constantly be shaken simultaneously, more be conducive to solutes accumulation, thus further improve the extraction yield of baicalin.
(2) before the refluxing extraction root of large-flowered skullcap of the present invention first through ultrasonic stirring, shorten reflux extracting time greatly.
(3) in the present invention, the extraction rate reached of the root of large-flowered skullcap is to more than 90%, and the purity of Artemisinin reaches more than 98.5%.
(4) extracting method of the present invention also have simple to operate, consume energy low, extraction time is short, low cost and other advantages, easily in realizing suitability for industrialized production.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described, but be not limited to protection scope of the present invention.
embodiment 1
From the root of large-flowered skullcap, extract a method for high-purity baicalin, comprise the following steps:
(1) the 50kg root of large-flowered skullcap (content of baicalin is 6kg) is crushed to 40 orders, obtains Baical Skullcap Root;
(2) Baical Skullcap Root is added in ultrasonic stirrer, add the ethanol 300L that concentration is 80%, under rotating speed is 300r/min, stirs 25min, obtains mixed solution;
(3) again mixed solution is transferred to reflux, refluxing extraction 3 times, reflux 0.5h at every turn, united extraction liquid;
(4) by said extracted liquid temperature be 70 DEG C, pressure be the condition of 0.08Mpa under concentrating under reduced pressure 2h, concentrated solution can be obtained, the pH to 2 of concentrated solution is regulated again with the citric acid that concentration is 6%, by throw out after filtering, be dry 2h under the condition of 70 DEG C in temperature, can crude baicalin be obtained;
(5) crude baicalin concentration is through filtering after the dissolve with methanol of 90%, the filtrate obtained, through silica gel column chromatography, is that the methyl alcohol of 3:1 and water are made into elutriant by volume ratio, finally collects sample solution after wash-out, sample solution is dry at 70-80 DEG C, obtain solids;
(6) be that solids dissolves by 90% methyl alcohol by concentration again, then use ordinary method recrystallization, filter, the crystallisate obtained is dry at 70 DEG C, can obtain 5.464kg high-purity baicalin.
In the present embodiment, the extraction yield (content that extraction yield is baicalin in Scutellaria baicalensis Georgi and the mass percent of high-purity tea baicalin obtained) of baicalin is 91.08%, and purity is 98.66%.
embodiment 2
From the root of large-flowered skullcap, extract a method for high-purity baicalin, comprise the following steps:
(1) the 50kg root of large-flowered skullcap (content of baicalin is 6kg) is crushed to 60 orders, obtains Baical Skullcap Root;
(2) Baical Skullcap Root is added in ultrasonic stirrer, add the ethanol 400L that concentration is 85%, under rotating speed is 500r/min, stirs 30min, obtains mixed solution;
(3) again mixed solution is transferred to reflux, refluxing extraction 3 times, reflux 1h at every turn, united extraction liquid;
(4) by said extracted liquid temperature be 80 DEG C, pressure be the condition of 0.08Mpa under concentrating under reduced pressure 1.5h, concentrated solution can be obtained, the pH to 3 of concentrated solution is regulated again with the citric acid that concentration is 6%, by throw out after filtering, be dry 1h under the condition of 80 DEG C in temperature, can crude baicalin be obtained;
(5) crude baicalin concentration is through filtering after the dissolve with methanol of 95%, the filtrate obtained, through silica gel column chromatography, is that the methyl alcohol of 3:1 and water are made into elutriant by volume ratio, finally collects sample solution after wash-out, sample solution is dry at 80 DEG C, obtain solids;
(6) be that solids dissolves by 95% methyl alcohol by concentration again, then use ordinary method recrystallization, filter, the crystallisate obtained is dry at 80 DEG C, can obtain 5.608kg high-purity baicalin.
In the present embodiment, the extraction yield of baicalin is 93.46%, and purity is 98.93%.
embodiment 3
From the root of large-flowered skullcap, extract a method for high-purity baicalin, comprise the following steps:
(1) the 50kg root of large-flowered skullcap (content of baicalin is 6kg) is crushed to 60 orders, obtains Baical Skullcap Root;
(2) Baical Skullcap Root is added in ultrasonic stirrer, add the ethanol 350L that concentration is 90%, under rotating speed is 300r/min, stirs 40min, obtains mixed solution;
(3) again mixed solution is transferred to reflux, refluxing extraction 3 times, reflux 0.5h at every turn, united extraction liquid;
(4) by said extracted liquid temperature be 70 DEG C, pressure be the condition of 0.09Mpa under concentrating under reduced pressure 2h, concentrated solution can be obtained, the pH to 2 of concentrated solution is regulated again with the citric acid that concentration is 8%, by throw out after filtering, be dry 1.5h under the condition of 70 DEG C in temperature, can crude baicalin be obtained;
(5) crude baicalin concentration is through filtering after the dissolve with methanol of 95%, the filtrate obtained, through silica gel column chromatography, is that the methyl alcohol of 3:1 and water are made into elutriant by volume ratio, finally collects sample solution after wash-out, sample solution is dry at 70 DEG C, obtain solids;
(6) be that solids dissolves by 95% methyl alcohol by concentration again, then use ordinary method recrystallization, filter, the crystallisate obtained is dry at 70 DEG C, can obtain 5.582kg high-purity baicalin.
In the present embodiment, the extraction yield of baicalin is 93.04%, and purity is 98.52%.
embodiment 4
From the root of large-flowered skullcap, extract a method for high-purity baicalin, comprise the following steps:
(1) the 50kg root of large-flowered skullcap (content of baicalin is 6kg) is crushed to 40 orders, obtains Baical Skullcap Root;
(2) Baical Skullcap Root is added in ultrasonic stirrer, add the ethanol 450L that concentration is 90%, under rotating speed is 500r/min, stirs 30min, obtains mixed solution;
(3) again mixed solution is transferred to reflux, refluxing extraction 4 times, reflux 0.5h at every turn, united extraction liquid;
(4) by said extracted liquid temperature be 80 DEG C, pressure be the condition of 0.08Mpa under concentrating under reduced pressure 1.5h, concentrated solution can be obtained, the pH to 3 of concentrated solution is regulated again with the citric acid that concentration is 8%, by throw out after filtering, be dry 1h under the condition of 80 DEG C in temperature, can crude baicalin be obtained;
(5) crude baicalin concentration is through filtering after the dissolve with methanol of 90%, the filtrate obtained, through silica gel column chromatography, is that the methyl alcohol of 3:1 and water are made into elutriant by volume ratio, finally collects sample solution after wash-out, sample solution is dry at 80 DEG C, obtain solids;
(6) be that solids dissolves by 90% methyl alcohol by concentration again, then use ordinary method recrystallization, filter, the crystallisate obtained is dry at 80 DEG C, can obtain 5.573kg high-purity baicalin.
In the present embodiment, the extraction yield of baicalin is 92.88%, and purity is 99.14%.
Claims (6)
1. from the root of large-flowered skullcap, extract a method for baicalin, it is characterized in that, comprise the following steps:
(1) root of large-flowered skullcap is crushed to 40-60 order, obtains Baical Skullcap Root;
(2) add in ultrasonic stirrer by Baical Skullcap Root, adding with its weight ratio is 1:4-8 ethanol doubly, then stirs 25-40min, obtains mixed solution;
(3) again mixed solution is transferred to reflux, refluxing extraction 3-4 time, reflux 0.5-1h at every turn, united extraction liquid;
(4) by said extracted liquid temperature be 70-80 DEG C, pressure be the condition of 0.07-0.09Mpa under concentrating under reduced pressure 1.5-2h, concentrated solution can be obtained, regulate the pH value of concentrated solution to 2-3 with citric acid again, by throw out after filtering, be dry 1-2h under the condition of 70-80 DEG C in temperature, can crude baicalin be obtained;
(5) after crude baicalin dissolve with methanol through filtering, the filtrate obtained, through silica gel column chromatography, is made into elutriant with methyl alcohol and the water that volume ratio is 3:1, finally collects sample solution after wash-out, by sample solution drying at 70-80 DEG C, obtains solids;
(6) dissolved by solids with methyl alcohol again, then use ordinary method recrystallization, filter, the crystallisate obtained is dry at 70-80 DEG C, can obtain high-purity baicalin.
2. a kind of method extracting baicalin from the root of large-flowered skullcap according to claim 1, is characterized in that: the alcohol concn described in step (2) is 80-90%.
3. a kind of method extracting baicalin from the root of large-flowered skullcap according to claim 1, is characterized in that: the concentration of described citric acid is 6-8%.
4. a kind of method extracting baicalin from the root of large-flowered skullcap according to claim 3, is characterized in that: the stirring velocity of step (2) is 300-500r/min.
5. a kind of method extracting baicalin from the root of large-flowered skullcap according to claim 4, is characterized in that: the concentration of described methyl alcohol is 90-95%.
6. a kind of method extracting baicalin from the root of large-flowered skullcap according to claim 4, is characterized in that: the purity of described baicalin reaches more than 98.5%.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107091889A (en) * | 2017-04-20 | 2017-08-25 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE methods extract baicalin in Scutellaria baicalensis Georgi |
| CN108329368A (en) * | 2017-01-20 | 2018-07-27 | 武汉回盛生物科技股份有限公司 | A method of preparing scutelloside from radix scutellariae |
| CN108744584A (en) * | 2018-07-10 | 2018-11-06 | 山东端信堂大禹药业有限公司 | A kind of device and its extracting method extracting scutelloside from radix scutellariae |
| CN109705179A (en) * | 2019-03-15 | 2019-05-03 | 李小冬 | A method of the extraction purification high-purity scutellarin from radix scutellariae seed shell |
| CN111840149A (en) * | 2019-04-26 | 2020-10-30 | 东莞自然衡健康科技有限公司 | Preparation process and application of radix scutellariae whitening and anti-allergy extracting solution |
| CN112552357A (en) * | 2021-01-08 | 2021-03-26 | 南京邦康生物技术有限公司 | Method for preparing hypolipidemic compound by fermentation |
| CN114028452A (en) * | 2021-12-24 | 2022-02-11 | 宁波杰顺生物科技有限公司 | Baicalin extract and preparation method thereof |
| RU2783445C1 (en) * | 2022-05-05 | 2022-11-14 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Кемеровский государственный университет" | Method for isolation and purification of baicalin from root cultures of scutellaria baicalensis georgi |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108329368A (en) * | 2017-01-20 | 2018-07-27 | 武汉回盛生物科技股份有限公司 | A method of preparing scutelloside from radix scutellariae |
| CN107091889A (en) * | 2017-04-20 | 2017-08-25 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE methods extract baicalin in Scutellaria baicalensis Georgi |
| CN108744584A (en) * | 2018-07-10 | 2018-11-06 | 山东端信堂大禹药业有限公司 | A kind of device and its extracting method extracting scutelloside from radix scutellariae |
| CN109705179A (en) * | 2019-03-15 | 2019-05-03 | 李小冬 | A method of the extraction purification high-purity scutellarin from radix scutellariae seed shell |
| CN111840149A (en) * | 2019-04-26 | 2020-10-30 | 东莞自然衡健康科技有限公司 | Preparation process and application of radix scutellariae whitening and anti-allergy extracting solution |
| CN112552357A (en) * | 2021-01-08 | 2021-03-26 | 南京邦康生物技术有限公司 | Method for preparing hypolipidemic compound by fermentation |
| CN114028452A (en) * | 2021-12-24 | 2022-02-11 | 宁波杰顺生物科技有限公司 | Baicalin extract and preparation method thereof |
| RU2783445C1 (en) * | 2022-05-05 | 2022-11-14 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Кемеровский государственный университет" | Method for isolation and purification of baicalin from root cultures of scutellaria baicalensis georgi |
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