CN101475618A - Refining method for scutelloside for injection - Google Patents
Refining method for scutelloside for injection Download PDFInfo
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- CN101475618A CN101475618A CNA2008100559585A CN200810055958A CN101475618A CN 101475618 A CN101475618 A CN 101475618A CN A2008100559585 A CNA2008100559585 A CN A2008100559585A CN 200810055958 A CN200810055958 A CN 200810055958A CN 101475618 A CN101475618 A CN 101475618A
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- Prior art keywords
- baicalin
- ethanol
- temperature
- elutant
- insulation
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000002347 injection Methods 0.000 title claims abstract description 14
- 239000007924 injection Substances 0.000 title claims abstract description 14
- XDQITMCFPPPMBC-TUANDBMESA-N scutelloside Natural products OC[C@H]1O[C@@H](O[C@@H]2O[C@@H]3C[C@H]4[C@H](O)[C@@H](O)[C@@](O)(CO3)[C@@H]24)[C@H](O)[C@@H](O)[C@@H]1O XDQITMCFPPPMBC-TUANDBMESA-N 0.000 title claims description 5
- 238000007670 refining Methods 0.000 title abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 74
- IPQKDIRUZHOIOM-UHFFFAOYSA-N Oroxin A Natural products OC1C(O)C(O)C(CO)OC1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IPQKDIRUZHOIOM-UHFFFAOYSA-N 0.000 claims abstract description 51
- IKIIZLYTISPENI-ZFORQUDYSA-N baicalin Chemical compound O1[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IKIIZLYTISPENI-ZFORQUDYSA-N 0.000 claims abstract description 51
- 229960003321 baicalin Drugs 0.000 claims abstract description 51
- AQHDANHUMGXSJZ-UHFFFAOYSA-N baicalin Natural products OC1C(O)C(C(O)CO)OC1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 AQHDANHUMGXSJZ-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000000243 solution Substances 0.000 claims abstract description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000012043 crude product Substances 0.000 claims abstract description 19
- 239000012153 distilled water Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 238000009413 insulation Methods 0.000 claims description 23
- 230000001105 regulatory effect Effects 0.000 claims description 16
- 238000001556 precipitation Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 7
- 238000000746 purification Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 2
- 229930182470 glycoside Natural products 0.000 abstract description 2
- 150000002338 glycosides Chemical class 0.000 abstract description 2
- 238000004321 preservation Methods 0.000 abstract 2
- 240000004534 Scutellaria baicalensis Species 0.000 abstract 1
- 235000017089 Scutellaria baicalensis Nutrition 0.000 abstract 1
- 241000050051 Chelone glabra Species 0.000 description 6
- 239000007788 liquid Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 235000014676 Phragmites communis Nutrition 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000006023 anti-tumor response Effects 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229940126678 chinese medicines Drugs 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000035619 diuresis Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- -1 flavonoid compound Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000036515 potency Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Landscapes
- Saccharide Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Cosmetics (AREA)
Abstract
本发明公开了一种注射用黄芩苷的精制方法，包括以下步骤：(1)将黄芩苷粗品用蒸馏水溶解，水浴加热，滴加NaOH溶液调节pH为5.0－9.0，使粗品完全溶解；(2)在保温情况下用HCl溶液调节pH为5－9，加乙醇或高浓度乙醇溶液至含乙醇含量为50－90％，过滤；(3)滤液用HCl溶液调节pH为1.0－4.0，保温，使得黄芩苷完全沉淀，静置，过滤，将沉淀水洗至洗出液的pH为2.0－7.0，再用50－90％乙醇溶液洗涤沉淀至洗出液的pH为6.0－8.0，干燥即得黄芩苷精品。使用该方法所得黄芩苷纯度高，可用于生产注射剂。The invention discloses a method for refining baicalin for injection, which comprises the following steps: (1) dissolving crude baicalin in distilled water, heating in a water bath, adding NaOH solution dropwise to adjust the pH to 5.0-9.0, so that the crude product is completely dissolved; (2) ) under the condition of heat preservation, use HCl solution to adjust the pH to 5-9, add ethanol or high-concentration ethanol solution until the ethanol content is 50-90%, and filter; (3) use HCl solution to adjust the pH of the filtrate to 1.0-4.0, heat preservation, Make baicalin completely precipitate, let it stand, filter, wash the precipitate with water until the pH of the eluate is 2.0-7.0, then wash the precipitate with 50-90% ethanol solution until the pH of the eluate is 6.0-8.0, and dry to obtain Scutellaria baicalensis Glycoside boutique. The baicalin obtained by the method has high purity and can be used to produce injections.
Description
Technical field
The present invention relates to the field of Chinese medicines, particularly the process for purification of scutelloside for injection.
Background technology
Baicalin (Baicalin) is the effective constituent of the root of large-flowered skullcap, can be from scutellariae,radix extraction separation and getting, it is flavonoid compound, has significant biological activity, have antibacterial, diuresis, anti-inflammatory, resistance attitude and spasmolysis, and have stronger physiological potencies such as antitumor response, occupied critical role at clinical medicine.Baicalin can also absorb ultraviolet ray, removes oxyradical, can suppress melanic generation again, therefore both can be used for medicine, also can be used for makeup, is a kind of good functional cosmetics raw material.
At present, report to some extent about the method for existence baicalin.The method that is commonly used to produce baicalin has water to carry heavy method of acid and alkali extraction and acid precipitation, but the purity of these method gained baicalins is generally lower.Now relevant for the report of producing the baicalin novel method.For example, application number is that 200610046117.9 Chinese patent application discloses the method for extracting crude baicalin in a kind of root of large-flowered skullcap, utilizes the flocculate and clarify method to handle root of large-flowered skullcap water extract; Before acid is heavy, purify; Use has the finings of the wilkinite of selective adsorption effect as root of large-flowered skullcap water extract, uses the flocculence removal of impurities before the heavy method of root of large-flowered skullcap water extract acid is extracted crude baicalin, root of large-flowered skullcap water extract is used the method purification and impurity removal of selective flocculation.But the quality of its gained baicalin crude product still can not be used for injection, and processing requirement is higher.
Summary of the invention
The object of the present invention is to provide a kind of process for purification of baicalin, gained baicalin purity height can be used for producing injection.
The process for purification of scutelloside for injection provided by the invention may further comprise the steps:
(1) with baicalin crude product dissolved in distilled water, heating in water bath, dripping NaOH solution adjusting pH is 5.0-9.0, and crude product is dissolved fully;
(2) regulating pH with HCl solution under the insulation situation is 5-9, and adding ethanol or high concentration ethanol solution is 50-90 volume % to containing ethanol content, filters;
(3) filtrate is 1.0-4.0 with HCl solution adjusting pH, and insulation makes baicalin precipitate fully, leave standstill, filter, the pH that precipitation is washed to elutant is 2.0-7.0, again with the washing precipitation of 50-90% ethanolic soln to the pH of elutant be 6.0-8.0, be drying to obtain the baicalin elaboration.
Wherein, in the step (1), the amount of dissolving used distilled water be baicalin crude product quality 2-30 doubly, be preferably 3-20 doubly, more preferably 5-15 doubly, also more preferably 5-10 is doubly.The preferred 30-120 of the temperature of heating in water bath ℃, more preferably 50-100 ℃, also more preferably 80-100 ℃.The concentration of regulating the used sodium hydroxide solution of pH is preferably 1-20%, 1-10% more preferably, 1-5% more preferably, also 1-3% more preferably.
In the step (2), the temperature of described insulation is preferably 30-120 ℃, and more preferably 50-100 ℃, also more preferably 70-90 ℃.Adding ethanol or high concentration ethanol solution is 50-90% to containing ethanol content, preferred 60-85%, and more preferably 70-80% filters again.
In the step (3), the purpose of described insulation is that baicalin is precipitated fully.The temperature of described insulation is preferably 50-100 ℃, and more preferably 60-90 ℃, also more preferably 70-80 ℃.The time of described insulation preferably was not less than 2 minutes, was preferably 2-50 minute, was preferably 3-20 minute, more preferably 5-20 minute.The described time of leaving standstill preferably was not less than 1 hour, more preferably was not less than 2 hours, for example 2-24 hour, was preferably 2-12 hour.When described precipitation washed with water, preferably the pH to elutant was 2.0-6.0,2.0-5.0 more preferably, also 2.0-4.0 more preferably.When described precipitation was washed with the 50-90% ethanolic soln, preferably the pH to elutant was about 7.0.
The present invention gropes to draw the process for purification of baicalin of the present invention through big quantity research and experiment, use the baicalin product purity of the inventive method gained can reach more than 92%, can be used for producing injection liquid, make process for preparing injection liquid simplify, easy to operate, improve the stability of injection liquid, improve the controllability of injection quality, and help avoiding, reducing the generation of injection liquid untoward reaction.
Embodiment
Below further describe the present invention by specific embodiment, it is more clear that characteristics of the present invention and advantage can become along with the description of these embodiment.But these embodiment only are exemplary, scope of the present invention are not constituted any restriction.
Embodiment 1
Baicalin crude product 3g (wherein content of baicalin 70%) is used the 60mL dissolved in distilled water, 100 ℃ of heating in water bath, it is 5.0 that the NaOH solution of dropping 2% is regulated pH, and crude product is dissolved fully;
Regulating pH with HCl solution under 100 ℃ of insulation situations is 5, and adding ethanol is 50v% to containing ethanol content, filters;
It is 1.0 that gained filtrate is regulated pH with HCl solution, 90 ℃ are incubated 20 minutes, make baicalin precipitate fully, left standstill 12 hours, filter, the pH that precipitation is washed to elutant is about 2.0-3.0, washes with 50% ethanol to be precipitated to elutant pH and to be about 6.0-7.0 again, drying obtains baicalin elaboration 1.89 grams, and wherein content of baicalin is 92%.
Embodiment 2
Baicalin crude product 3g (wherein content of baicalin 70%) is used the 30mL dissolved in distilled water, 80 ℃ of heating in water bath, it is 9.0 that the NaOH solution of dropping 1% is regulated pH, and crude product is dissolved fully;
Regulating pH with HCl solution under 70 ℃ of insulation situations is 9, and adding ethanol is 90v% to containing ethanol content, filters;
It is 4.0 that gained filtrate is regulated pH with HCl solution, 60 ℃ are incubated 10 minutes, make baicalin precipitate fully, left standstill 12 hours, filter, the pH that precipitation is washed to elutant is about 4.0-5.0, washes with 90% ethanol to be precipitated to elutant pH and to be about 7.0 again, drying obtains baicalin elaboration 1.89 grams, and wherein content of baicalin 92.5%.
Embodiment 3
Baicalin crude product 3g (wherein content of baicalin is 70%) is used the 15mL dissolved in distilled water, and 50 ℃ of heating in water bath, the NaOH solution of dropping 1% are regulated pH and are about 8.0, and crude product is dissolved fully;
Regulate pH with HCl solution and be about 6 under 50 ℃ of insulation situations, adding ethanol is 70v% to containing ethanol content, filters;
It is 3.0 that gained filtrate is regulated pH with HCl solution, 70 ℃ are incubated 20 minutes, make baicalin precipitate fully, left standstill 12 hours, filter, the pH that precipitation is washed to elutant is about 4.0, washes with 70% ethanol to be precipitated to elutant pH and to be about 8.0 again, drying obtains baicalin elaboration 1.88g, and wherein content of baicalin 92.3%.
Embodiment 4
Baicalin crude product 3g (wherein a kind of reed mentioned in ancient books glycosides content is 70%) is used the 10mL dissolved in distilled water, and 30 ℃ of heating in water bath, the NaOH solution of dropping 1% are regulated pH and are about 6.0, and crude product is dissolved fully;
Regulate pH with HCl solution and be about 5 under 80 ℃ of insulation situations, adding ethanol is 60v% to containing ethanol content, filters;
It is 2.0 that gained filtrate is regulated pH with HCl solution, 80 ℃ are incubated 20 minutes, make baicalin precipitate fully, left standstill 10 hours, filter, the pH that precipitation is washed to elutant is about 2.0, washes with 60% ethanol to be precipitated to elutant pH and to be about 6.0 again, drying obtains baicalin elaboration 1.88g, and wherein content of baicalin 92.2%.
Embodiment 5
Baicalin crude product 3g (wherein content of baicalin is 70%) is used the 6mL dissolved in distilled water, and 120 ℃ of heating in water bath, the NaOH solution of dropping 1% are regulated pH and are about 9.0, and crude product is dissolved fully;
Regulate pH with HCl solution and be about 7 under 90 ℃ of insulation situations, adding ethanol is 70v% to containing ethanol content, filters;
(3) filtrate is 1.0 with HCl solution adjusting pH, 70 ℃ are incubated 5 minutes, make baicalin precipitate fully, left standstill 6 hours, filter, the pH that precipitation is washed to elutant is about 2.0, washes with 70% ethanol to be precipitated to elutant pH and to be about 6.0 again, drying obtains baicalin elaboration 1.89g, and wherein content of baicalin is 92.6%.
Claims (10)
1, a kind of process for purification of scutelloside for injection may further comprise the steps:
(1) with baicalin crude product dissolved in distilled water, heating in water bath, dripping NaOH solution adjusting pH is 5.0-9.0, and crude product is dissolved fully;
(2) regulating pH with HCl solution under the insulation situation is 5-9, and adding ethanol or high concentration ethanol solution is 50-90% to containing ethanol content, filters;
(3) filtrate is 1.0-4.0 with HCl solution adjusting pH, and insulation makes baicalin precipitate fully, leave standstill, filter, the pH that precipitation is washed to elutant is 2.0-7.0, again with the washing precipitation of 50-90% ethanolic soln to the pH of elutant be 6.0-8.0, be drying to obtain the baicalin elaboration.
2, method as claimed in claim 1 is characterized in that, in the step (1):
The amount of dissolving used distilled water is 2-30 a times of baicalin crude product quality;
And/or
The temperature of heating in water bath is 30-120 ℃;
And/or
The concentration of regulating the used sodium hydroxide solution of pH is 1-20%.
3, method as claimed in claim 2 is characterized in that, in the step (1), the amount of dissolving used distilled water is 3-20 a times of baicalin crude product quality, is preferably 5-15 doubly, is preferably 5-10 doubly;
And/or
The temperature of heating in water bath is 50-100 ℃, also more preferably 80-100 ℃;
And/or
The concentration of regulating the used sodium hydroxide solution of pH is 1-10%, 1-5% more preferably, also 1-3% more preferably.
4, as each described method of claim 1-3, it is characterized in that, in the step (2):
The temperature of described insulation is 30-120 ℃;
And/or
Adding ethanol or high concentration ethanol solution is 50-90% to containing ethanol content, filters again.
5, method as claimed in claim 4 is characterized in that, in the step (2):
The temperature of described insulation is 50-100 ℃;
And/or
Adding ethanol or high concentration ethanol solution is 60-85% to containing ethanol content, filters again.
6, method as claimed in claim 5 is characterized in that, in the step (2):
The temperature of described insulation is 70-90 ℃;
And/or
Adding ethanol or high concentration ethanol solution is 70-80% to containing ethanol content, filters again.
7, as each method of claim 1-6, it is characterized in that, in the step (3):
The temperature of described insulation is 50-100 ℃, more preferably 60-90 ℃, and also more preferably 70-80 ℃;
And/or
The time of described insulation was not less than 2 minutes;
And/or
The described time of leaving standstill was not less than 1 hour;
And/or
When described precipitation washes with water, to the pH of elutant be 2.0-6.0.
8, method as claimed in claim 7 is characterized in that, in the step (3):
The temperature of described insulation is 60-90 ℃;
And/or
The time of described insulation is 2-50 minute;
And/or
The described time of leaving standstill was not less than 2 hours;
And/or
When described precipitation washes with water, to the pH of elutant be 2.0-5.0.
9, method as claimed in claim 8 is characterized in that, in the step (3):
The temperature of described insulation is 70-80 ℃;
And/or
The time of described insulation is 3-20 minute, more preferably 5-20 minute;
And/or
The described time of leaving standstill is 2-24 hour, is preferably 2-12 hour;
And/or
When described precipitation washes with water, to the pH of elutant be 2.0-4.0.
10, method as claimed in claim 9 is characterized in that, in the step (3):
The time of described insulation is 5-20 minute;
And/or
The described time of leaving standstill is 2-12 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100559585A CN101475618A (en) | 2008-01-03 | 2008-01-03 | Refining method for scutelloside for injection |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100559585A CN101475618A (en) | 2008-01-03 | 2008-01-03 | Refining method for scutelloside for injection |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101475618A true CN101475618A (en) | 2009-07-08 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008100559585A Pending CN101475618A (en) | 2008-01-03 | 2008-01-03 | Refining method for scutelloside for injection |
Country Status (1)
| Country | Link |
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| CN (1) | CN101475618A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103316113A (en) * | 2013-07-05 | 2013-09-25 | 石强 | Natural pharmaceutical composition |
| CN104189492A (en) * | 2014-09-12 | 2014-12-10 | 广西中医药大学 | Traditional Chinese medicine preparation with hypoglycemic effect |
| 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 |
| CN105497131A (en) * | 2014-09-26 | 2016-04-20 | 天津中敖生物科技有限公司 | Preparation method for large-flowered skullcap root extract |
-
2008
- 2008-01-03 CN CNA2008100559585A patent/CN101475618A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103316113A (en) * | 2013-07-05 | 2013-09-25 | 石强 | Natural pharmaceutical composition |
| CN104189492A (en) * | 2014-09-12 | 2014-12-10 | 广西中医药大学 | Traditional Chinese medicine preparation with hypoglycemic effect |
| CN105497131A (en) * | 2014-09-26 | 2016-04-20 | 天津中敖生物科技有限公司 | Preparation method for large-flowered skullcap root extract |
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Application publication date: 20090708 |