CN100438884C - Method for increasing yield of prodn. of hypericum japonicum total flavone - Google Patents
Method for increasing yield of prodn. of hypericum japonicum total flavone Download PDFInfo
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- CN100438884C CN100438884C CNB2006100522242A CN200610052224A CN100438884C CN 100438884 C CN100438884 C CN 100438884C CN B2006100522242 A CNB2006100522242 A CN B2006100522242A CN 200610052224 A CN200610052224 A CN 200610052224A CN 100438884 C CN100438884 C CN 100438884C
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- herba hyperici
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Abstract
A process for increasing the output rate of the general flavone of Japanese St. John's-wort herb includes such steps as dissolving in NH3H2O solution, diluting the extracted concentrated liquid, and regulating the pH value of solution to become near neutral or slightly alkaline for increasing the solubility of flavone in water. Its output rate can reach 50-80%.
Description
Technical field
The invention belongs to pharmaceutical field, particularly disclose a kind of employing NH
3H
2O solution upper prop improves the method that macroporous resin is produced the Herba Hyperici Japonici total flavones yield.
Background technology
Herba Hyperici Japonici is the dry herb of Guttiferae hypericum Herba Hyperici Japonici (Hypercum japonicum Thunb).Sweet in the mouth, little hardship, cool in nature.Return liver, gallbladder, large intestine channel.Effect with clearing away heat-damp and promoting diuresis, eliminating stasis to stop pain, subduing swelling and detoxicating.Modern pharmacological research shows multiple pharmacotoxicological effects such as Herba Hyperici Japonici has antibacterial, antiviral, protects the liver, suppresses tumor and cancerous cell, enhance immunity, clinical acute and chronic hepatitis, infectious hepatitis, primary hepatocarcinoma, typhoid fever, the paratyphoid fever etc. of being used for the treatment of.Total flavones is that Herba Hyperici Japonici is antibacterial, antiviral, protect the liver, suppress the material base of effects such as tumor and cancerous cell.
The Herba Hyperici Japonici injection records at Chinese Pharmacopoeia (2002 editions), and generally is used for clinically, adopts traditional decoction and alcohol sedimentation technique in its technology.Most of technologies are all based on traditional Herba Hyperici Japonici injection aqueous extraction-alcohol precipitation technology (Herba Hyperici Japonici total flavones injectable powder and preparation method thereof CN1528288A, a kind of Herba Hyperici Japonici drop pill that adopts the Herba Hyperici Japonici preparation and preparation method thereof CN1698832A, freeze-dried powder injection of Tianjihuang and preparation method thereof CN1679816A) in the relevant patent of existing several Herba Hyperici Japonici.The hypericum japonicum total flavone extraction purity of utilizing aqueous extraction-alcohol precipitation technology to obtain is generally not high.
As everyone knows, utilize macroporous adsorbent resin separation and purification effective ingredient or effective site from Chinese medicine extraction liquid to become isolation technics means the most frequently used in the production.Its advantage is can be highly enriched with effective ingredient, and simple to operate, controlled.This technical method is suitable for the preparation that effective ingredient is flavone compound or saponins compound especially.When adopting Amberlyst process active constituent-enriched, requiring upper prop liquid must be aqueous solution.Flavone compound mostly is the middle polarity chemical compound, be soluble in ethyl acetate, methanol or the ethanol, and the dissolubility in water is very little, therefore, concentrated back of aqueous extract or ethanol extract are after being concentrated into no alcohol, even under the hydrotropy of other impurity, most flavone compounds still can precipitate separates out, residue is few in the supernatant of total flavones after centrifugal, prepare total flavones by supernatant by macroporous resin again, yield lower naturally (being generally less than 40%), the greatest drawback that this has just become to utilize the Amberlyst process refined total flavonoids to exist.How to improve yield, guarantee the purity of extract and the focus that biological activity also just becomes concern simultaneously.Can learn that by top analysis increasing the dissolubility of flavone compound in water is the key point of problem.Flavone compound is faintly acid owing to often having a plurality of phenolic hydroxyl groups, and therefore, dissolubility is good in alkaline aqueous solution, adopts alkaline aqueous solution to dissolve, dilute the problem that extracting solution after concentrated just can solve flavonoid composition poor solubility in water; If but solution alkalescence is excessive, the macroporous resin absorption performance is descended, might destroy the structure of flavone compound simultaneously, cause bioactive forfeiture.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of employing NH is provided
3H
2O solution upper prop improves the method that Amberlyst process is produced the Herba Hyperici Japonici total flavones yield.
The present invention is achieved in that Herba Hyperici Japonici medicinal material coarse powder or decoction pieces, add 6～12 times of (V/W) water or 30～95% aquiferous ethanol, heating and refluxing extraction 1～3 time, each extraction time is 0.5～3 hour, merge extractive liquid, is isolated the supernatant of aqueous extract or ethanol extract; It is 1.2～1.35 that the supernatant of aqueous extract or ethanol extract is evaporated to relative density; NH with 0.25%～1.0% (V/V)
3H
2In aqueous extract after O is added to and concentrates or the ethanol extract it is diluted, making aqueous extract or ethanol extract ultimate density is 0.25～1.0g crude drug/mL, and filter PH to 4～8, isolates supernatant; By the chromatographic column of macroporous adsorbent resin is housed, supernatant is 1: 1～1: 5 (W/W) by the ratio of the amount of Herba Hyperici Japonici crude drug and dried resin with this supernatant, and last column flow rate is 1～4BV/h, and the resin path height ratio is 1: 3～1: 9; With the water washing resin of 3～12BV, elution flow rate is 1～6BV/h, discards water elution liquid; With 30～95% aquiferous ethanol eluting of 2～6BV, flow velocity is 1～6BV/h, collects ethanol elution; It is 1.1～1.25 that ethanol elution is evaporated to relative density, and drying promptly gets hypericum japonicum total flavone extraction.
The isolating method of the supernatant of described aqueous extract or ethanol extract adopts centrifugal or filtering method.Centrifugal rotation speed is 2000-10000 rev/min, and the time is 5～90 minutes.
Described macroporous resin is nonpolar or the low pole macroporous adsorbent resin.
The present invention adopts NH
3H
2Concentrated solution is extracted in the dissolving of O solution, dilution, adjust the nearly neutrality of pH value of solution or slightly be alkalescence, most of flavone compound of separating out after concentrating is redissolved, improve the dissolubility of flavone compound in water, thereby guaranteed to utilize supernatant to pass through the yield of Amberlyst process enrichment total flavones effective ingredient; By screening, guarantee in the process of the abundant stripping of total flavones active ingredient, not change the character of total flavones simultaneously to concentration of lye and consumption, thus the biological activity that it can be brought into normal play.Adopt the inventive method, the purity of Herba Hyperici Japonici extract is 50%～90%, and wherein the content of Quercitroside is 4%～30%, and the yield of Herba Hyperici Japonici total flavones reaches 50%～80%.
Description of drawings
Fig. 1 extracts the HPLC collection of illustrative plates of the centrifugal back of concentrated solution supernatant for the pure water dilution;
Fig. 2 extracts the HPLC collection of illustrative plates of the centrifugal back of concentrated solution supernatant for the alkaline aqueous solution dilution.
The specific embodiment
Get Herba Hyperici Japonici medicinal material coarse powder 2kg, add 6 times of water, heating and refluxing extraction 1 time, each extraction time is 0.5 hour, merge extractive liquid,, centrifugal (rotating speed 2000,5 minutes time); Aqueous extract is concentrated into relative density 1.2, adds 0.25% NH
3H
2O dissolving, dilution make its concentration to 0.25g crude drug/mL, PH to 4, recentrifuge, supernatant be by being equipped with the chromatographic column of D101 type macroporous adsorbent resin (nonpolar), and extracting solution is 1: 1 by the ratio of the amount of Herba Hyperici Japonici crude drug and dried resin, last column flow rate 1BV/h, resin path height ratio are 1: 3; Wash resin 3BV with water, elution flow rate is 1BV/h, and water elution liquid discards; With 30% aquiferous ethanol eluting 2BV, flow velocity is 1BV/h, collects ethanol elution; It is 1.1 that ethanol elution is evaporated to relative density, drying, promptly.The purity of the hypericum japonicum total flavone extraction that makes is 50%, and the response rate of total flavones is 50%, and wherein the amount of Quercitroside is 4%.
Get Herba Hyperici Japonici pharmaceutical decocting piece 2kg, add 12 times of 95% ethanol, heating and refluxing extraction 3 times, each extraction time is 3.0 hours, merge extractive liquid,, centrifugal (10000 rev/mins of rotating speeds, 90 minutes time); Ethanol extract is concentrated into relative density 1.35, adds 1.0% NH
3H
2O dissolving, dilution make its concentration to 1.0g crude drug/mL, PH to 8, recentrifuge, supernatant be by being equipped with the chromatographic column of AB-8 type macroporous adsorbent resin (low pole), and extracting solution is 1: 5 by the ratio of the amount of Herba Hyperici Japonici crude drug and dried resin, last column flow rate 4BV/h, resin path height ratio are 1: 9; Wash resin 12BV with water, elution flow rate is 6BV/h, discards water elution liquid; With the 95% aquiferous ethanol eluting of 6BV, flow velocity is 6BV/h, collects ethanol elution; It is 1.25 that ethanol elution is evaporated to relative density, drying, promptly.The purity of the hypericum japonicum total flavone extraction that makes is 70%, and the response rate of total flavones is 80%, and wherein the content of Quercitroside is 30%
Get Herba Hyperici Japonici pharmaceutical decocting piece 1kg, add 8 times of 50% ethanol, heating and refluxing extraction 2 times, each extraction time is 2.0 hours, merge extractive liquid, filters; Ethanol extract is concentrated into relative density 1.2, adds 0.5% NH
3H
2O dissolving, dilution make its concentration to 0.5g crude drug/mL, PH to 6, recentrifuge, supernatant be by being equipped with the chromatographic column of AB-8 type macroporous adsorbent resin (low pole), and extracting solution is 1: 3 by the ratio of the amount of Herba Hyperici Japonici crude drug and dried resin, last column flow rate 2BV/h, resin path height ratio are 1: 5; With the water washing resin of 6BV, elution flow rate is 3BV/h, discards water elution liquid; With the 70% aquiferous ethanol eluting of 4～6BV, flow velocity is 2BV/h, collects ethanol elution; It is 1.1 that ethanol elution is evaporated to relative density, drying, promptly.The purity of the hypericum japonicum total flavone extraction that makes is 60%, and the response rate of total flavones is 70%, and wherein the content of Quercitroside is 15%
Get Herba Hyperici Japonici decoction pieces 1kg, add 7 times of amount 30% ethanol, heating and refluxing extraction 3 times, each extraction time is 2.0 hours, merge extractive liquid,, centrifugal or filtration; Ethanol extract is concentrated into relative density 1.2, adds 0.8% NH
3H
2O dissolving, dilution make its concentration to 0.75 crude drug/mL, PH to 6, recentrifuge, supernatant be by being equipped with the chromatographic column of D101 type macroporous adsorbent resin (nonpolar), and extracting solution is 1: 4 by the ratio of the amount of Herba Hyperici Japonici crude drug and dried resin, last column flow rate is 2BV/h, and the resin path height ratio is 1: 7; With the water washing resin of 8BV, elution flow rate is 4BV/h, discards water elution liquid; With the 75% aquiferous ethanol eluting of 5BV, flow velocity is 3BV/h, collects ethanol elution; It is 1.2 that ethanol elution is evaporated to relative density, drying, promptly.The purity of the hypericum japonicum total flavone extraction that makes is 55%, and the response rate of total flavones is 65%, and wherein the content of Quercitroside is 12%.
By Fig. 1 and Fig. 2 relatively, from the HPLC collection of illustrative plates retention time of effective ingredient as can be seen, when adopting NH
3H
2O solution dissolves, concentrated solution is extracted in dilution, when adjusting the nearly neutrality of pH value of solution or slightly being alkalescence, can't change the character of effective ingredient in the solution, but dissolubility increases greatly.
Claims (3)
1, a kind of method of producing the Herba Hyperici Japonici total flavones yield that improves, it is characterized in that this method is: Herba Hyperici Japonici medicinal material coarse powder or decoction pieces, the adding envelope-bulk to weight ratio is 6～12 times water or 30～95% aquiferous ethanol, heating and refluxing extraction 1～3 time, each extraction time is 0.5～3 hour, merge extractive liquid, is isolated the supernatant of aqueous extract or ethanol extract; It is 1.2～1.35 that the supernatant of aqueous extract or ethanol extract is evaporated to relative density; With volume ratio 0.25%～1.0% NH
3H
2In aqueous extract after O is added to and concentrates or the ethanol extract it is diluted, making aqueous extract or ethanol extract ultimate density is 0.25～1.0g crude drug/mL, and filter PH to 4～8, isolates supernatant; By the chromatographic column of macroporous adsorbent resin is housed, supernatant is 1: 1～1: 5 by the weight ratio of the amount of Herba Hyperici Japonici crude drug and dried resin with this supernatant, and last column flow rate is 1～4BV/h, and the resin path height ratio is 1: 3～1: 9; With the water washing resin of 3～12BV, elution flow rate is 1～6BV/h, discards water elution liquid; With 30～95% aquiferous ethanol eluting of 2～6BV, flow velocity is 1～6BV/h, collects ethanol elution; It is 1.1～1.25 that ethanol elution is evaporated to relative density, and drying promptly gets hypericum japonicum total flavone extraction.
2, a kind of method of producing the Herba Hyperici Japonici total flavones yield that improves as claimed in claim 1 is characterized in that the isolating method of supernatant of described aqueous extract or ethanol extract adopts centrifugal or filtering method.
3, a kind of method of producing the Herba Hyperici Japonici total flavones yield that improves as claimed in claim 1 is characterized in that described macroporous resin is nonpolar or the low pole macroporous adsorbent resin.
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| CNB2006100522242A CN100438884C (en) | 2006-06-30 | 2006-06-30 | Method for increasing yield of prodn. of hypericum japonicum total flavone |
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| CN100438884C true CN100438884C (en) | 2008-12-03 |
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| CN104817601B (en) * | 2015-03-31 | 2018-04-10 | 浙江大学 | Three flavones ingredient mixtures, preparation and its method are extracted from Herba lysimachiae capillipedis |
| CN106723010A (en) * | 2016-11-19 | 2017-05-31 | 青海泰柏特生物科技有限公司 | The method of Extraction and enrichment polyphenol from quinoa seed |
| CN106728137A (en) * | 2016-11-24 | 2017-05-31 | 广州和匠科技有限公司 | It is a kind of that the preparation method for preventing and treating hyperuricemia and gout medicine-food two-purpose monomer is extracted from coffee |
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Non-Patent Citations (4)
| Title |
|---|
| 田基黄的研究进展. 傅芃，田红丽，张卫东.药学实践杂志，第22卷第2 期. 2004 |
| 田基黄的研究进展. 傅芃，田红丽，张卫东.药学实践杂志，第22卷第2 期. 2004 * |
| 田基黄黄酮类化学成分的研究. 傅芃，李廷钊，张薇，枊润辉，张川，张卫东，陈海生.中国天然药物，第2卷第5期. 2004 |
| 田基黄黄酮类化学成分的研究. 傅芃，李廷钊，张薇，枊润辉，张川，张卫东，陈海生.中国天然药物，第2卷第5期. 2004 * |
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