CN115925769A - Method for extracting baicalin from scutellaria baicalensis - Google Patents
Method for extracting baicalin from scutellaria baicalensis Download PDFInfo
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- CN115925769A CN115925769A CN202310048639.6A CN202310048639A CN115925769A CN 115925769 A CN115925769 A CN 115925769A CN 202310048639 A CN202310048639 A CN 202310048639A CN 115925769 A CN115925769 A CN 115925769A
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- 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 title claims abstract description 38
- 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 title claims abstract description 38
- 229960003321 baicalin Drugs 0.000 title claims abstract description 38
- 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 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 17
- 240000004534 Scutellaria baicalensis Species 0.000 title claims description 17
- 235000017089 Scutellaria baicalensis Nutrition 0.000 title claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000002244 precipitate Substances 0.000 claims abstract description 29
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 238000010992 reflux Methods 0.000 claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical class [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000000047 product Substances 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 12
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 239000003480 eluent Substances 0.000 claims abstract description 6
- 238000010828 elution Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 58
- 238000000605 extraction Methods 0.000 claims description 13
- 238000010898 silica gel chromatography Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 238000004587 chromatography analysis Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000012258 stirred mixture Substances 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 description 4
- 238000003916 acid precipitation Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 208000006454 hepatitis Diseases 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- MOFOLNOWFPVLGZ-BHWDSYMASA-N (2s,3s,4s,5r,6s)-6-(5,8-dihydroxy-4-oxo-2-phenylchromen-7-yl)oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound O1[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1OC1=CC(O)=C2C(=O)C=C(C=3C=CC=CC=3)OC2=C1O MOFOLNOWFPVLGZ-BHWDSYMASA-N 0.000 description 1
- 206010000234 Abortion spontaneous Diseases 0.000 description 1
- 206010008909 Chronic Hepatitis Diseases 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 206010039897 Sedation Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000008845 cholagoga Substances 0.000 description 1
- 229940124571 cholagogue Drugs 0.000 description 1
- 238000001784 detoxification Methods 0.000 description 1
- 230000035619 diuresis Effects 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
- 239000012535 impurity Substances 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 208000015994 miscarriage Diseases 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000036280 sedation Effects 0.000 description 1
- 208000000995 spontaneous abortion Diseases 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
A method for extracting baicalin from Scutellariae radix comprises adding Scutellariae radix powder into a stirrer, adding appropriate amount of ethanol, transferring the stirred mixture to a reflux device, reflux-extracting for 3-4 times, and mixing the extractive solutions to obtain first extractive solution; concentrating the first extractive solution at 62-70 deg.C under 0.1Mpa under reduced pressure for 2.5h, adjusting pH to 4-5 with dilute hydrochloric acid, and filtering to obtain first precipitate and baicalin wet product; adding modified sodium hydroxide solution into the first precipitate, extracting at 18-20 deg.C for 3-4 hr, separating to obtain second precipitate and second extractive solution, dissolving the second extractive solution and baicalin wet product with methanol, filtering, performing chromatography on the filtrate, and purifying with a volume ratio of 3:1, preparing an eluent from methanol and water, collecting the solution after elution, and drying the solution at 80-85 ℃ to obtain a solid; dissolving the solid with methanol, recrystallizing, filtering, and drying the obtained crystal at 55-60 deg.C to obtain high-purity baicalin.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine extraction, and particularly relates to a method for extracting baicalin from scutellaria baicalensis.
Background
Scutellariae radix is a common Chinese medicine, and has effects of clearing heat, eliminating dampness, clearing pathogenic fire, removing toxic substance, stopping bleeding, and preventing miscarriage. Baicalin is one of the main effective components of scutellaria baicalensis, has obvious biological activity, and has the pharmacological proven effects of bacteriostasis, heat clearing, blood pressure reduction, sedation, diuresis, cholagogue, anti-inflammation, allergy resistance, detoxification, cancer resistance and the like. At present, baicalin is successfully developed into baicalin tablets and baicalin capsules for treating acute and chronic hepatitis.
The baicalin has molecular weight of C21H18O11, is a flavonoid compound, has extremely low water solubility, and has certain lipid solubility. At present, a plurality of methods for extracting and purifying baicalin are reported, such as a water extraction acid precipitation method, an alcohol extraction acid precipitation method, an ultrafiltration method, a microwave extraction method and the like, and due to the reasons of cost, scale, equipment and the like, in the methods, the subsequent acid adjustment is difficult and the yield is low because the impurities are more in the extraction process, particularly in the alcohol extraction acid precipitation method.
Disclosure of Invention
The invention aims to provide a method for extracting baicalin from scutellaria baicalensis, which is suitable for industrial production and has high yield.
The technical scheme adopted by the invention is as follows: a method for extracting baicalin from scutellaria baicalensis comprises the following steps:
(1) Pulverizing Scutellariae radix to 40-60 mesh to obtain Scutellariae radix powder;
(2) Adding the scutellaria baicalensis powder in the step (1) into an ultrasonic stirrer, adding ethanol with the weight ratio of 1;
(3) Transferring the mixed solution in the step (2) to a reflux device, carrying out reflux extraction for 3-4 times, carrying out reflux for 0.5-2h each time, and combining the extracting solutions of each time to form a first extracting solution;
(4) Concentrating the first extractive solution of step (3) at 62-70 deg.C and 0.1Mpa under reduced pressure for 2.5 hr to obtain concentrated solution, adjusting pH to 4-5 with dilute hydrochloric acid, and filtering to obtain first precipitate and baicalin wet product;
(5) Adding a modified sodium hydroxide solution with the concentration of 85-90% into the first precipitate in the step (4), adding 8-15 liters of the modified sodium hydroxide solution into each kilogram of the precipitate, extracting for 3-4h at 18-20 ℃, separating to obtain a second precipitate and a second extracting solution, wherein the second extracting solution and a baicalin wet product are dissolved by methanol and then filtered, and the filtered filtrate is subjected to silica gel column chromatography and is purified by a solvent with the volume ratio of 3:1, preparing an eluent from methanol and water, collecting the solution after elution, and drying the solution at 80-85 ℃ to obtain a solid substance;
(6) Dissolving the solid with methanol, recrystallizing, filtering, and drying the obtained crystal at 55-60 deg.C to obtain high purity baicalin.
The invention has the beneficial effects that the scutellaria baicalensis is crushed into 40-60 meshes to obtain the scutellaria baicalensis powder; then adding the scutellaria baicalensis powder into an ultrasonic stirrer, adding ethanol with the weight ratio of 1-8 times of that of the scutellaria baicalensis powder, and stirring for 30-60 minutes to obtain a mixed solution; then transferring the mixed solution to a reflux device, carrying out reflux extraction for 3-4 times, carrying out reflux for 0.5-2h each time, and combining the extracting solutions of each time to form a first extracting solution; then concentrating the first extractive solution at 62-70 deg.C and 0.1Mpa under reduced pressure for 2.5 hr to obtain concentrated solution, adjusting pH to 4-5 with dilute hydrochloric acid, and filtering to obtain first precipitate and baicalin wet product; adding a modified sodium hydroxide solution with the concentration of 85-90% into the first precipitate, adding 8-15L of the modified sodium hydroxide solution into each kilogram of the precipitate, extracting at 18-20 ℃ for 3-4h, separating to obtain a second precipitate and a second extracting solution, dissolving the second extracting solution and baicalin wet products together with methanol, filtering, and performing silica gel column chromatography on the filtered filtrate by using a solvent in a volume ratio of 3:1, preparing an eluent from methanol and water, collecting the solution after elution, and drying the solution at 80-85 ℃ to obtain a solid; dissolving the solid with methanol, recrystallizing, filtering, and drying the obtained crystal at 55-60 deg.C to obtain high-purity baicalin (more than 96%); the whole extraction process simplifies the extraction process, reduces the production cost, is more suitable for industrial production, improves the quality of baicalin, and can ensure that the content of finished products can reach more than 96 percent.
Detailed description of the preferred embodiments
Examples
The invention relates to a method for extracting baicalin from scutellaria baicalensis, which comprises the following specific steps: (1) pulverizing radix Scutellariae to 45 mesh to obtain radix Scutellariae powder;
(2) Adding the scutellaria baicalensis powder in the step (1) into an ultrasonic stirrer, adding ethanol with the weight ratio of 1;
(3) Transferring the mixed solution in the step (2) to a reflux device, carrying out reflux extraction for 3 times, carrying out reflux for 1h each time, and combining the extracting solutions of each time to form a first extracting solution;
(4) Concentrating the first extractive solution of step (3) at 65 deg.C and 0.1Mpa under reduced pressure for 2.5 hr to obtain concentrated solution, adjusting pH to 4 with dilute hydrochloric acid, and filtering to obtain first precipitate and baicalin wet product;
(5) Adding a modified sodium hydroxide solution with the concentration of 85% into the first precipitate in the step (4), adding 9 liters of the modified sodium hydroxide solution into each kilogram of the precipitate, extracting for 3 hours at 18 ℃, separating to obtain a second precipitate and a second extracting solution, dissolving the second extracting solution and a baicalin wet product together with methanol, filtering, and performing silica gel column chromatography on the filtered filtrate by using a solvent in a volume ratio of 3:1, preparing an eluent from methanol and water, collecting the solution after elution, and drying the solution at 80 ℃ to obtain a solid substance;
(6) Dissolving the solid with methanol, recrystallizing, filtering, and drying the obtained crystal at 55 deg.C to obtain high-purity baicalin.
In the steps, modified sodium hydroxide solution with the concentration of 85% is added into the first precipitate obtained by filtering, 9 liters of modified sodium hydroxide solution is added into each kilogram of precipitate, the mixture is extracted for 3 hours at the temperature of 18 ℃, a second precipitate and a second extracting solution are separated, wherein the second extracting solution and a baicalin wet product are dissolved together by methanol and then filtered, and the filtered filtrate is separated and purified in silica gel column chromatography, so that the extraction process is simplified, the production cost is reduced, and the method is more suitable for industrial production and the quality of baicalin is improved.
Examples
The invention relates to a method for extracting baicalin from scutellaria baicalensis, which comprises the following steps:
(1) Pulverizing Scutellariae radix to 60 mesh to obtain Scutellariae radix powder;
(2) Adding the scutellaria baicalensis powder in the step (1) into an ultrasonic stirrer, adding ethanol with the weight ratio of 1;
(3) Transferring the mixed solution in the step (2) to a reflux device, carrying out reflux extraction for 4 times, carrying out reflux for 2 hours each time, and combining the extracting solutions of each time to form a first extracting solution;
(4) Concentrating the first extractive solution of step (3) at 70 deg.C and 0.1Mpa under reduced pressure for 2.5 hr to obtain concentrated solution, adjusting pH to 5 with dilute hydrochloric acid, and filtering to obtain first precipitate and baicalin wet product;
(5) Adding a modified sodium hydroxide solution with the concentration of 90% into the first precipitate in the step (4), adding 15 liters of the modified sodium hydroxide solution into each kilogram of the precipitate, extracting for 4 hours at the temperature of 20 ℃, separating to obtain a second precipitate and a second extracting solution, dissolving the second extracting solution and a baicalin wet product together with methanol, filtering, and performing silica gel column chromatography on the filtered filtrate by using a solvent with the volume ratio of 3:1, preparing an eluent from methanol and water, collecting the solution after elution, and drying the solution at 85 ℃ to obtain a solid substance;
(6) Dissolving the solid with methanol, recrystallizing, filtering, and drying the obtained crystal at 60 deg.C to obtain high-purity baicalin.
In the steps, a modified sodium hydroxide solution with the concentration of 90% is added into the first precipitate obtained by filtering, 15 liters of the modified sodium hydroxide solution is added into each kilogram of the precipitate, the mixture is extracted for 3 hours at the temperature of 20 ℃, a second precipitate and a second extracting solution are separated, wherein the second extracting solution and a baicalin wet product are dissolved together by using methanol and then filtered, and the filtered filtrate is separated and purified in silica gel column chromatography, so that the extraction process is simplified, the production cost is reduced, and the method is more suitable for industrial production and further improves the quality of the baicalin.
Claims (1)
1. A method for extracting baicalin from scutellaria baicalensis comprises the following steps:
(1) Pulverizing Scutellariae radix to 40-60 mesh to obtain Scutellariae radix powder;
(2) Adding the scutellaria baicalensis powder in the step (1) into an ultrasonic stirrer, adding ethanol with the weight ratio of 1;
(3) Transferring the mixed solution in the step (2) to a reflux device, carrying out reflux extraction for 3-4 times, carrying out reflux for 0.5-2h each time, and combining the extracting solutions of each time to form a first extracting solution;
(4) Concentrating the first extractive solution of step (3) at 62-70 deg.C under 0.1Mpa under reduced pressure for 2.5 hr to obtain concentrated solution, adjusting pH to 4-5 with dilute hydrochloric acid, and filtering to obtain first precipitate and baicalin wet product;
(5) Adding a modified sodium hydroxide solution with the concentration of 85-90% into the first precipitate in the step (4), adding 8-15 liters of the modified sodium hydroxide solution into each kilogram of the precipitate, extracting for 3-4h at 18-20 ℃, separating to obtain a second precipitate and a second extracting solution, wherein the second extracting solution and a baicalin wet product are dissolved by methanol and then filtered, and the filtered filtrate is subjected to silica gel column chromatography and is purified by a solvent with the volume ratio of 3:1, preparing an eluent from methanol and water, collecting the solution after elution, and drying the solution at 80-85 ℃ to obtain a solid;
(6) Dissolving the solid with methanol, recrystallizing, filtering, and drying the obtained crystal at 55-60 deg.C to obtain high-purity baicalin.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310048639.6A CN115925769A (en) | 2023-01-31 | 2023-01-31 | Method for extracting baicalin from scutellaria baicalensis |
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| CN202310048639.6A CN115925769A (en) | 2023-01-31 | 2023-01-31 | Method for extracting baicalin from scutellaria baicalensis |
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| CN115925769A true CN115925769A (en) | 2023-04-07 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PL444523A1 (en) * | 2023-04-21 | 2024-10-28 | Instytut Włókien Naturalnych I Roślin Zielarskich Państwowy Instytut Badawczy | Dietary supplement, method of preparing a dietary supplement and use of extracts from the roots of Withania somnifera and the roots of Scutellaria baicalensis for producing a dietary supplement |
-
2023
- 2023-01-31 CN CN202310048639.6A patent/CN115925769A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PL444523A1 (en) * | 2023-04-21 | 2024-10-28 | Instytut Włókien Naturalnych I Roślin Zielarskich Państwowy Instytut Badawczy | Dietary supplement, method of preparing a dietary supplement and use of extracts from the roots of Withania somnifera and the roots of Scutellaria baicalensis for producing a dietary supplement |
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