CN107513086B - Method for extracting and separating high-purity scutellarin from scutellaria baicalensis stem and leaf and scutellarin - Google Patents
Method for extracting and separating high-purity scutellarin from scutellaria baicalensis stem and leaf and scutellarin Download PDFInfo
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Abstract
The invention provides a method for extracting and separating high-purity scutellarin from scutellaria baicalensis stem and leaf and scutellarin, and the method comprises the following steps: pulverizing Scutellariae radix stem and leaf; adding ethanol, and heating to boil; filtering the extractive solution, and concentrating under reduced pressure; heating the concentrated solution to boil, adjusting pH to 7-8, and filtering while hot; adjusting the pH value of the filtrate to 1-2, standing to obtain brown precipitate and khaki precipitate, filtering, washing the filter cake with distilled water, then washing with a solvent to neutrality, and drying to obtain crude scutellarin; adding solvent and active carbon, heating, filtering the extractive solution, concentrating the filtrate, standing to precipitate crystal, filtering, and washing with solvent to obtain scutellarin crystal; adding solvent into scutellarin crystal, shaking, adjusting pH to 1-2, standing, filtering, washing precipitate with water to neutral, and drying to obtain high-purity scutellarin. The extraction rate of the scutellarin is more than 90 percent, and the purity is more than 98 percent.
Description
Technical Field
The invention relates to the technical field of extraction and separation of effective components of Chinese herbal medicines, in particular to a method for extracting and separating high-purity scutellarin from stem leaves of scutellaria baicalensis and scutellarin.
Background
Scutellarin, also called scutellarin, has a chemical name of 3', 5, 6-trihydroxy-7-O-glucuronide and a molecular formula of C21H18O12The structural formula is shown in formula I.
Scutellarin is mainly obtained from erigeron breviscapus at present, and due to continuous reduction of erigeron breviscapus wild resources and continuous increase of planting cost, new alternative resources are required to be searched for preparing scutellarin (scutellarin).
Scutellaria baicalensis Georgi (Scutellaria baicalensis Georgi) is a perennial herb of Labiatae, and the root of Scutellaria baicalensis Georgi is a herbal medicine with bitter taste and cold nature, has the effects of clearing heat and drying dampness, purging pathogenic fire and removing toxicity, stopping bleeding, preventing miscarriage and the like, and is used for treating diseases such as damp-warm, summer-heat dampness, chest distress and nausea, damp-heat distention and fullness, diarrhea, jaundice, lung heat cough, hyperpyrexia and polydipsia, blood heat and epistaxis, carbuncle swelling and sore toxicity, threatened abortion and the like. At present, the root of scutellaria baicalensis is mainly used as traditional medicine, and stem and leaf parts with the yield being several times that of the root are regarded as non-medicinal parts and discarded.
At present, the research of extracting scutellarin from the stem and leaf of scutellaria baicalensis is mostly in a laboratory stage, and the scutellarin does not enter an industrial production stage, so that the invention provides a method for industrially producing the scutellarin, and the method has the advantages of simple operation process, low cost, easiness in industrial production and the like.
Disclosure of Invention
The invention mainly aims to provide an industrial production method for extracting scutellarin from scutellaria baicalensis stem and leaf, and the scutellarin extracted by the method has high yield and high purity.
Another object of the present invention is to provide scutellarin with high purity.
In order to achieve the above object, the present invention provides a method for extracting and separating high-purity scutellarin from scutellaria baicalensis stem and leaf, comprising the following steps: (1) pulverizing Scutellariae radix stem and leaf to obtain crude powder; (2) according to the weight ratio of 1: 4 to 1:20, adding 30 to 70 percent ethanol into the raw material coarse powder, and heating to boil to obtain a first extracting solution; (3) filtering the first extractive solution to obtain first filtrate, concentrating the first filtrate at 60-70 deg.C under 0.08-0.10 MPa, and removing ethanol to obtain scutellarin concentrated solution; (4) adjusting pH of the scutellarin concentrated solution to 7-8 with weak acid salt solution of alkali metal, and filtering to obtain a second filtrate; (5) adding an acid solution into the second filtrate, adjusting the pH value to 1-2, standing for 24-48 h, separating out a brown precipitate, and pouring out an upper solution; (6) standing the upper layer solution for 18-24 h to separate out an earthy yellow precipitate; (7) mixing the brown precipitate and the khaki precipitate, filtering, washing a filter cake with distilled water, washing with a first solvent to be neutral, and drying at the temperature of 50-60 ℃ to obtain a crude scutellarin product; (8) adding a second solvent and active carbon into the crude scutellarin product, heating to obtain a second extracting solution, filtering the second extracting solution to obtain a third filtrate, concentrating the third filtrate to 60-80% of the original volume, standing to separate out crystals, filtering the crystals, and washing with the second solvent to obtain scutellarin crystals; (9) adding a third solvent into the scutellarin crystals, shaking up, adding an acid solution to adjust the pH value to 1-2, standing, filtering, washing the precipitate with water to be neutral, and drying to obtain the high-purity scutellarin.
In the further scheme, in the step (1), the mesh number of the raw material coarse powder is 10 meshes to 200 meshes.
Preferably, in the step (4), the weak acid salt solution of alkali metal is one or more of potassium bicarbonate, potassium carbonate, sodium bicarbonate, sodium carbonate and the like, and the concentration of the weak acid salt solution of alkali metal is in the range of 10% to 30%.
Preferably, in the step (5), the acid solution is one or more of hydrochloric acid, sulfuric acid, phosphoric acid and the like, and the concentration of the acid solution is in the range of 10% to 30%.
Preferably, in step (7), the first solvent is one or more of water, ethyl acetate, acetone, methanol and ethanol.
Preferably, in step (8), the second solvent is one or more of water, ethyl acetate, acetone, methanol, ethanol, etc., and the amount of activated carbon is 0.1-20% of the weight of the crude scutellarin.
Preferably, in step (9), the third solvent is one or more of water, ethyl acetate, acetone, methanol, ethanol, and the like.
Preferably, in step (9), the acid solution is an aqueous solution of one or more of hydrochloric acid, sulfuric acid and phosphoric acid, and the concentration of the acid solution is in the range of 10% to 30%.
Preferably, the purity of the high-purity scutellarin obtained in the step (9) is more than 98%.
The method has the advantages of simple operation, low cost, easy industrial production and the like, and the extraction rate of the scutellarin reaches more than 90 percent and the purity reaches more than 98 percent.
In order to achieve the above another object, the present invention provides a scutellarin obtained by the following steps: (1) pulverizing Scutellariae radix stem and leaf to obtain crude powder; (2) according to the weight ratio of 1: 4 to 1:20, adding 30 to 70 percent ethanol into the raw material coarse powder, and heating to boil to obtain a first extracting solution; (3) filtering the first extractive solution to obtain first filtrate, concentrating the first filtrate at 60-70 deg.C under 0.08-0.10 MPa, and removing ethanol to obtain scutellarin concentrated solution; (4) adjusting pH of the scutellarin concentrated solution to 7-8 with weak acid salt solution of alkali metal, and filtering to obtain a second filtrate; (5) adding an acid solution into the second filtrate, adjusting the pH value to 1-2, standing for 24-48 h, separating out a brown precipitate, and pouring out an upper solution; (6) standing the upper layer solution for 18-24 h to separate out an earthy yellow precipitate; (7) mixing the brown precipitate and the khaki precipitate, filtering, washing a filter cake with distilled water, washing with a first solvent to be neutral, and drying at the temperature of 50-60 ℃ to obtain a crude scutellarin product; (8) adding a second solvent and active carbon into the crude scutellarin product, heating to obtain a second extracting solution, filtering the second extracting solution to obtain a third filtrate, concentrating the third filtrate to 60-80% of the original volume, standing to separate out crystals, filtering the crystals, and washing with the second solvent to obtain scutellarin crystals; (9) adding a third solvent into the scutellarin crystals, shaking up, adding an acid solution to adjust the pH value to 1-2, standing, filtering, washing the precipitate with water to be neutral, and drying to obtain the high-purity scutellarin.
Detailed Description
In the invention, the content determination method of scutellarin comprises the following steps: high Performance Liquid Chromatography (HPLC) with an instrument model of Agilent1260, the conditions of which are as follows:
a chromatographic column: agilent ZORBAX SB-C18(4.6 mm. times.250 mm, 5 um).
Mobile phase: acetonitrile was used as mobile phase a, methanol as mobile phase B, and 0.5% formic acid as mobile phase D, and gradient elution was performed as specified in table 1.
TABLE 1
| Time/min | Mobile phase A/%) | Mobile phase B/%) | Mobile phase D/%) |
| 0 | 3 | 5 | 92 |
| 0～15 | 3→11.5 | 5→15 | 92→73.5 |
| 15～45 | 11.5→11.5 | 15→15 | 73.5→73.5 |
| 45～55 | 11.5→3 | 15→5 | 73.5→92 |
Column temperature: 35 ℃, detection wavelength: 335nm, flow rate: 1 mL/min.
In the following examples, the extraction rate was calculated as follows: the extraction rate is the mass percentage of the scutellarin content in the scutellaria stem to the obtained high-purity scutellarin.
In the following examples, the purity of scutellarin was calculated by the following method: the area normalization method is adopted, namely the percentage of the area of the scutellarin peak to the total peak area.
Example one
The method for extracting and separating high-purity scutellarin from scutellaria baicalensis stem and leaf comprises the following steps:
(1) pulverizing 50kg of stem and leaf of Scutellariae radix (scutellarin content is about 0.5kg) to 10-200 mesh to obtain crude powder of stem and leaf of Scutellariae radix;
(2) adding 50% ethanol into the stem and leaf powder of Scutellariae radix at a weight ratio of 1:8, heating to boil, extracting for 2 times (each for 1.5 hr), and mixing to obtain first extractive solution;
(3) filtering the first extractive solution with filter cloth to obtain first filtrate, concentrating under reduced pressure at 60 deg.C and 0.08MPa, and removing ethanol to obtain scutellarin concentrated solution containing no ethanol;
(4) adjusting pH of the scutellarin concentrated solution to 7 with 10% sodium carbonate solution, filtering to obtain a second filtrate, and discarding the precipitate;
(5) adding 10% hydrochloric acid solution into the second filtrate, adjusting the pH value to 1, standing for 36h, separating out brown precipitate, and pouring out the upper solution;
(6) continuously standing the poured upper-layer solution for 18 hours to separate out a khaki precipitate;
(7) mixing the brown precipitate and the khaki precipitate, filtering, washing the filter cake with distilled water and ethyl acetate to neutrality to obtain a mixed precipitate, and drying at a low temperature of 50 ℃ to obtain a crude product of scutellarin;
(8) adding 95% ethanol with 20 times volume of the crude scutellarin product and 1% activated carbon with weight of the crude scutellarin product into the crude scutellarin product, heating to boil, extracting for 1h to obtain a second extracting solution, filtering the second extracting solution to obtain a third filtrate, concentrating the third filtrate to 80% of the original volume, standing to precipitate crystals, filtering, and washing the obtained crystals with 45% ethanol for 5 times to obtain scutellarin crystals;
(9) adding 10 times volume of 30-50% acetone aqueous solution into the scutellarin crystal, shaking, adding 10% hydrochloric acid to adjust pH to 2, standing, filtering, washing precipitate with water to neutral, and drying to obtain 0.453kg high-purity scutellarin.
The extraction rate of scutellarin in this example is 90.6%, the purity of scutellarin obtained in this example is 98.31% by analyzing the purity of HPLC detection map, and example two
The method for extracting and separating high-purity scutellarin from scutellaria baicalensis stem and leaf comprises the following steps:
(1) pulverizing 50kg of stem and leaf of Scutellariae radix (scutellarin content is about 1.2kg) to 10-200 mesh to obtain crude powder of stem and leaf of Scutellariae radix;
(2) adding 70% ethanol into the stem and leaf powder of Scutellariae radix at a weight ratio of 1:15, heating to boil, extracting for 3 times, each for 1.5 hr, and mixing to obtain first extractive solution;
(3) filtering the first extractive solution with filter cloth to obtain first filtrate, concentrating under reduced pressure at 65 deg.C and 0.10MPa, and removing ethanol to obtain scutellarin concentrated solution containing no ethanol;
(4) adjusting pH of the scutellarin concentrated solution to 8 with 15% sodium bicarbonate solution, filtering to obtain a second filtrate, and discarding the precipitate;
(5) adding 10% sulfuric acid solution into the second filtrate, adjusting pH to 2, keeping the temperature at 60 deg.C for 30min, standing for 48h to precipitate brown precipitate, and decanting the upper solution;
(6) continuously standing the poured upper-layer solution for 18 hours to separate out a khaki precipitate;
(7) mixing the brown precipitate and the khaki precipitate, filtering, washing the filter cake with distilled water and ethanol to neutrality, and drying at 60 deg.C to obtain scutellarin crude product;
(8) adding 20 times volume of 85% ethanol and 2% activated carbon of crude scutellarin product weight into crude scutellarin product, heating to boil, extracting for 1h to obtain a second extract, filtering the second extract to obtain a third filtrate, concentrating the third filtrate to 60% of the original volume, standing to precipitate crystals, filtering, and washing the obtained crystals with 45% ethanol for 5 times to obtain scutellarin crystals;
(9) adding 10 times volume of 30-50% acetone aqueous solution into the above crystal, shaking, adding 10% sulfuric acid solution to adjust pH to 2, standing, filtering, washing precipitate with water to neutral, and drying to obtain 1.09kg high purity scutellarin.
In this example, the extraction rate of scutellarin is 90.8%, and the purity of scutellarin obtained in this example is 98.53% by analyzing the purity of HPLC detection spectra.
EXAMPLE III
The method for extracting and separating high-purity scutellarin from scutellaria baicalensis stem and leaf comprises the following steps:
(1) pulverizing 50kg of stem and leaf of Scutellariae radix (scutellarin content is about 1.2kg) to 10-200 mesh to obtain crude powder of stem and leaf of Scutellariae radix;
(2) adding 50% ethanol into the crude powder of stem and leaf of Scutellariae radix at a weight ratio of 1:10, heating to boil, extracting for 3 times, each for 1.5 hr, and mixing to obtain first extractive solution;
(3) filtering the first extractive solution with filter cloth to obtain first filtrate, concentrating under reduced pressure at 70 deg.C and 0.10MPa, and removing ethanol to obtain scutellarin concentrated solution containing no ethanol;
(4) adjusting pH of the scutellarin concentrated solution to 7 with 20% potassium bicarbonate solution, filtering to obtain a second filtrate, and discarding the precipitate;
(5) adding 20% hydrochloric acid solution into the second filtrate, adjusting pH to 1, keeping the temperature at 70 deg.C for 30min, standing for 24h to precipitate brown precipitate, and decanting the upper solution;
(6) continuously standing the poured upper-layer solution for 24 hours to separate out a khaki precipitate;
(7) mixing the brown precipitate and the khaki precipitate, filtering, washing the filter cake with distilled water and ethyl acetate to neutrality to obtain a mixed precipitate, and drying at a low temperature of 60 ℃ to obtain a crude product of scutellarin;
(9) adding 20 times volume of 85% ethanol and 2% activated carbon of crude scutellarin product weight into crude scutellarin product, heating to boil, extracting for 1h to obtain second extractive solution, filtering the second extractive solution to obtain third filtrate, concentrating the third filtrate to 60% of the original volume, standing to precipitate crystals, filtering, and washing the obtained crystals with 45% ethanol for 5 times to obtain scutellarin crystals;
(10) adding 5 times volume of 30-50% acetone aqueous solution into the scutellarin crystal, shaking, adding 20% hydrochloric acid solution to adjust pH to 1, standing, filtering, washing precipitate with water to neutral, and drying to obtain 1.12kg high purity scutellarin.
In this example, the extraction rate of scutellarin is 91.3%, and the purity of scutellarin obtained in this example is 98.76% by analyzing the purity of HPLC detection spectra.
Of course, the above examples are only preferred embodiments of the present invention, and many more variations are possible in practice, for example, the acidic solution for adjusting the pH can be phosphoric acid, or a mixture of acids; the alkaline solution for adjusting the pH value can also be potassium carbonate or a mixture of weak acid salts of various alkali metals; the solvent for washing the filter cake to be neutral in the step (7) can also be acetone or methanol, or one or more of water, ethyl acetate, acetone, methanol or ethanol. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (8)
1. A method for extracting and separating high-purity scutellarin from scutellaria baicalensis stem and leaf is characterized by comprising the following steps:
(1) pulverizing Scutellariae radix stem and leaf to obtain crude powder;
(2) according to the weight ratio of 1: 4 to 1:20, adding 30 to 70 percent ethanol into the raw material powder, and heating to boil to obtain a first extracting solution;
(3) filtering the first extracting solution to obtain a first filtrate, concentrating the first filtrate under reduced pressure at the temperature of 60-70 ℃ and the pressure of 0.08-0.10 MPa, and removing ethanol in the first filtrate to obtain a scutellarin concentrated solution;
(4) adjusting the pH value of the scutellarin concentrated solution to 7-8 by using weak acid salt solution of alkali metal, stirring to completely dissolve the scutellarin concentrated solution, and filtering to obtain a second filtrate;
(5) adding an acid solution into the second filtrate, adjusting the pH value to 1-2, standing for 24-48 h, separating out a brown precipitate, and pouring out an upper solution;
(6) standing the upper layer solution for 18-24 h to separate out an earthy yellow precipitate;
(7) combining the brown precipitate and the khaki precipitate, filtering, washing a filter cake with distilled water, washing with a first solvent to be neutral, and drying at the temperature of 50-60 ℃ to obtain a crude scutellarin product;
(8) adding a second solvent and activated carbon into the crude scutellarin product, heating to boil to obtain a second extracting solution, filtering the second extracting solution to obtain a third filtrate, concentrating the third filtrate to 60-80% of the original volume, standing to precipitate crystals, filtering the crystals, and washing with the second solvent to obtain scutellarin crystals;
(9) adding a third solvent into the scutellarin crystals, shaking up, adding an acid solution to adjust the pH value to 1-2, standing, filtering, washing precipitates to be neutral, and drying to obtain high-purity scutellarin; the third solvent is one or more of water, ethyl acetate, acetone, methanol and ethanol.
2. The method of claim 1, wherein:
in the step (1), the mesh number of the raw material coarse powder is 10-200 meshes.
3. The method of claim 1, wherein:
in the step (4), the weak acid salt solution of alkali metal is one or more of potassium bicarbonate, potassium carbonate, sodium bicarbonate and sodium carbonate, and the concentration of the weak acid salt solution of alkali metal is 10% to 30%.
4. The method of claim 1, wherein:
in the step (5), the acid solution is one or more of hydrochloric acid, sulfuric acid and phosphoric acid, and the concentration of the acid solution is in the range of 10% to 30%.
5. The method of claim 1, wherein:
in the step (7), the first solvent is one or a mixture of water, ethyl acetate, acetone, methanol and ethanol.
6. The method of claim 1, wherein:
in the step (8), the second solvent is one or more of water, ethyl acetate, acetone, methanol and ethanol, and the amount of the activated carbon is 0.1-20% of the weight of the scutellarin crude product.
7. The method of claim 1, wherein:
in the step (9), the acid solution is one or more of hydrochloric acid, sulfuric acid and phosphoric acid, and the concentration of the acid solution is in the range of 10% to 30%.
8. The method of claim 1, wherein:
the purity of the high-purity scutellarin obtained in the step (9) is more than 98%.
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| CN112028953A (en) * | 2020-09-21 | 2020-12-04 | 云南省药物研究所 | Preparation process of high-purity breviscapine raw material medicine |
| CN114849276A (en) * | 2022-06-06 | 2022-08-05 | 河北金元康药业有限公司 | Scutellaria baicalensis stem element separation and purification device and purification method |
| CN116370367B (en) * | 2023-01-31 | 2024-05-17 | 西安绿天生物技术有限公司 | Plant extract for cosmetics and preparation method and application thereof |
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