CN101317869A - Method for extracting flavone from capillary wormwood - Google Patents
Method for extracting flavone from capillary wormwood Download PDFInfo
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- CN101317869A CN101317869A CNA2008100553682A CN200810055368A CN101317869A CN 101317869 A CN101317869 A CN 101317869A CN A2008100553682 A CNA2008100553682 A CN A2008100553682A CN 200810055368 A CN200810055368 A CN 200810055368A CN 101317869 A CN101317869 A CN 101317869A
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- capillary wormwood
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Abstract
The present invention relates to the field of Chinese traditional medicine abstraction, in particular to a method for abstracting flavone from capillary wormwood. The method is used for solving the problems of low extraction yield, high temperature, inactivation of extraction, residue of organic solvent, etc., existing in the prior flavone extracting method. The method comprises edulcoration, screen and dryness of capillary wormwood; extractant is put into a capillary wormwood; then lixiviation and pump filter are performed so that raw extracting solution is obtained. The extractant is obtained by mixing cellulolytic enzyme and pectinase; rarefied flavone extracting solution is obtained after absolute ethyl alcohol is put into the flavone extracting solution subject to vacuum concentration. Then the ethanol is subject to cryoconcentration and reclamation and the concentrated solution is dried at the same time. Powdered flavone extraction is obtained. Low extraction temperature in the present invention decreases solvency of impurity. The extraction is high in purity and the extraction yield is good; the obtained capillary wormwood flavone is pure natural product. Freeze drying prevents effective ingredient of the flavone from being destroyed; the biological activity is high; the end product has no organic solvent residue; the method is simple in technological operation, good in repetitiveness, and high in productive rate. Therefore the method is suitable for industrialized production.
Description
Technical field
The present invention relates to the Chinese medicine extraction field, be specially a kind of method of from capillary wormwood, extracting flavone.
Background technology
Herba Artemisiae Scopariae is the dry aerial parts of Compositae herbaceos perennial BINHAO (Artemisia scoparia Waldst.et kit.) or Herba Artemisiae Scopariae (Artemisia cap illaries Thunb.).All there is distribution in most of area of China, main product in Shaanxi, ground such as Shanxi, Anhui, the habit of gathering spring claims " capillary wormwood ", the title of tapping autumn " Herba Artemisiae Scopariae ".Continuous Artemisia anethoicles Mattf is one of clinical Chinese medicine commonly used, this product bitter in the mouth, suffering, be slightly cold, return spleen, stomach, liver and gall warp, the effect of tool eliminating damp-heat, hepatic cholagogic, can be used for treating diseases such as jaundice oliguria, eczema pruritus, infectious jaundice type hepatitis, contain flavone, chlorogenic acid and volatilization wet goods various active composition.Modern pharmacology discovers that flavone has effects such as blood pressure lowering, blood fat reducing, anticoagulation, antitumor as a kind of important biological composition in the capillary wormwood.In view of capillary wormwood has multiple biological activity, capillary wormwood has wide practical use as natural drug, the functional food factor in the food and medicine field.
At present, there is bibliographical information to adopt ultrasound wave and microwave from capillary wormwood, to extract flavone, as " extraction of Herba Artemisiae Scopariae total flavones and preliminary purification " [Hunan City University's journal, 2005,14 (3): 60-62], " ultrasound wave and microwave assisting method extract the condition research of Herba Artemisiae Scopariae total flavones " [Hunan City University's journal, 2007,16 (3): 56-58], these researchs all adopt organic solvent as extractant, not only extraction ratio is low, and extracts the temperature height, has aggravated the stripping of non-target component (impurity), also easily cause extract inactivation and organic solvent residue, and its equipment cost is higher, complex process.
Summary of the invention
The present invention for solve the existing method of from capillary wormwood, extracting flavone exist extraction ratio low, extract the temperature height, aggravated the stripping of non-target component (impurity), also easily cause extract inactivation and organic solvent residual and production cost than problems such as height, a kind of method of extracting flavone from capillary wormwood is provided.
The present invention adopts following technical scheme to realize: a kind of method of extracting flavone from capillary wormwood may further comprise the steps: (1) with capillary wormwood remove impurity, screening, drying after, pulverizing is that 40～50 orders sieve; (2) adding is equivalent to capillary wormwood weight 20-30 extractant doubly in capillary wormwood, then the sealing, lucifuge, lixiviate 1.0-2.0h under 40-60 ℃ temperature, last sucking filtration obtains flavone and extracts thick liquid, described extractant is to be 0.02% cellulase solution and pectase solution with 1 by concentration: the compound enzyme liquid that the volume ratio of 1.5-2.5 mixes, the pH value of extractant are 4.5-5.5; (3) flavone that obtains in the step (2) is extracted thick liquid and behind vacuum concentration, add dehydrated alcohol, make that concentration of alcohol reaches more than 80% in the flavone extractive, through reacting, precipitate, filter to remove macromolecular substances, obtain the flavone extractive of preliminary purification, concentration of alcohol is big more, more complete with the macromolecular complex qualitative response; In this step, ethanol can extract macromolecular substances such as protein in the thick liquid, polysaccharide with flavone and react and generate precipitation, filters and remove impurity, and flavone extractive is further purified; (4) the flavone extractive cryoconcentration that step (3) is obtained and reclaim alcohol solvent simultaneously with the concentrated solution drying, can obtain pulverous flavone extract, and this step utilizes lower, the volatile characteristic of ethanol fusing point that it is reclaimed, recycling.
The method that described final concentrated solution is produced Powdered flavone extract after drying can adopt a lot of existing methods, in the step of the present invention (4) concentrated solution being carried out exsiccant method is lyophilizing in the dried machine of vacuum freezing, freeze dried condition is: heating-up temperature is 25-35 ℃, condenser temperature is-50-60 ℃, pressure is 30-50Pa, and freeze-drying time is 7.0-9.0h.The dried machine of described vacuum freezing adopts this method to carry out drying for existing known products, and temperature, pressure are lower, can effectively preserve the biological activity of flavone.
Compared with prior art, the method for extracting flavone from capillary wormwood of the present invention has following advantage:
(1) the present invention adopt cellulase and pectase composite enzyme solution as extractant, the capillary wormwood raw cell is carried out broken wall treatment, improved the mass transfer characteristic of material cellular content; Plant cell wall shields, prevent the random discrepancy of the inside and outside material of cell, mainly form by cellulose and pectin substance, therefore adopt cellulase and pectase dissolved cell wall, can promote the stripping of effective ingredient in the plant cell effectively, with comparing as extractant with ethanol or organic solvent, extraction ratio is higher, and it is lower to extract temperature, organic solvent-free is residual, has reduced the solvability to impurity, and the time processing purity of the flavone extract of capillary wormwood is reached more than 82%, therefore, to have extract purity high and extraction ratio is good in the present invention, safe advantage;
(2) the resulting capillary wormwood flavone of the present invention is an all-natural product, adopts lyophilization, keeps the flavone effective ingredient not to be destroyed, and the biological activity height never uses poisonous and hazardous organic solvent in the technical process, and the final products organic solvent-free that obtains is residual;
(3) simple, the good reproducibility of technological operation, the productive rate height is suitable for suitability for industrialized production.
The specific embodiment
Embodiment 1:
A kind of method of extracting flavone from capillary wormwood may further comprise the steps: (1) with capillary wormwood remove impurity, screening, drying after, pulverizing is that 40 orders sieve; (2) in capillary wormwood, add the extractant that is equivalent to 20 times of capillary wormwood weight, then the sealing, lucifuge, lixiviate 1.0h under 40 ℃ temperature, last sucking filtration obtains flavone and extracts thick liquid, described extractant is to be the compound enzyme liquid that 0.02% cellulase solution and pectase solution mix with 1: 1.5 volume ratio by concentration, and the pH value of extractant is 4.5; (3) flavone that obtains in the step (2) is extracted thick liquid and behind vacuum concentration, add dehydrated alcohol, make that concentration of alcohol reaches 98% in the flavone extractive, through reaction, precipitation, filter, obtain the flavone extractive of preliminary purification to remove macromolecular substances; (4) the flavone extractive cryoconcentration that step (3) is obtained and reclaim alcohol solvent, simultaneously with the concentrated solution drying, method is lyophilizing in the dried machine of vacuum freezing, freeze dried condition is: heating-up temperature is 25 ℃, condenser temperature is-50 ℃, pressure is 30Pa, and freeze-drying time is 7.0h, can obtain pulverous flavone extract.
Embodiment 2:
A kind of method of extracting flavone from capillary wormwood may further comprise the steps: (1) with capillary wormwood remove impurity, screening, drying after, pulverizing is that 50 orders sieve; (2) in capillary wormwood, add the extractant that is equivalent to 30 times of capillary wormwood weight, then the sealing, lucifuge, lixiviate 2.0h under 60 ℃ temperature, last sucking filtration obtains flavone and extracts thick liquid, described extractant is to be the compound enzyme liquid that 0.02% cellulase solution and pectase solution mix with 1: 2.5 volume ratio by concentration, and the pH value of extractant is 5.5; (3) flavone that obtains in the step (2) is extracted thick liquid and behind vacuum concentration, add dehydrated alcohol, make that concentration of alcohol reaches 85% in the flavone extractive, through reaction, precipitation, filter, obtain the flavone extractive of preliminary purification to remove macromolecular substances; (4) the flavone extractive cryoconcentration that step (3) is obtained and reclaim alcohol solvent, simultaneously with the concentrated solution drying, method is lyophilizing in the dried machine of vacuum freezing, freeze dried condition is: heating-up temperature is 35 ℃, condenser temperature is-60 ℃, pressure is 50Pa, and freeze-drying time is 9.0h, can obtain pulverous flavone extract.
Embodiment 3:
A kind of method of extracting flavone from capillary wormwood may further comprise the steps: (1) with capillary wormwood remove impurity, screening, drying after, pulverizing is that 45 orders sieve; (2) adding is equivalent to capillary wormwood weight 20-30 extractant doubly in capillary wormwood, then the sealing, lucifuge, lixiviate 1.5h under 50 ℃ temperature, last sucking filtration obtains flavone and extracts thick liquid, described extractant is to be the compound enzyme liquid that 0.02% cellulase solution and pectase solution mix with 1: 2.0 volume ratio by concentration, and the pH value of extractant is 5.0; (3) flavone that obtains in the step (2) is extracted thick liquid and behind vacuum concentration, add dehydrated alcohol, make that concentration of alcohol reaches 90% in the flavone extractive, through reaction, precipitation, filter, obtain the flavone extractive of preliminary purification to remove macromolecular substances; (4) the flavone extractive cryoconcentration that step (3) is obtained and reclaim alcohol solvent, simultaneously with the concentrated solution drying, method is lyophilizing in the dried machine of vacuum freezing, freeze dried condition is: heating-up temperature is 30 ℃, condenser temperature is-55 ℃, pressure is 40Pa, and freeze-drying time is 8.0h, can obtain pulverous flavone extract.
Embodiment 4:
A kind of method of extracting flavone from capillary wormwood may further comprise the steps: (1) with capillary wormwood remove impurity, screening, drying after, pulverizing is that 40 orders sieve; (2) adding is equivalent to capillary wormwood weight 20-30 extractant doubly in capillary wormwood, then the sealing, lucifuge, lixiviate 1.0h under 60 ℃ temperature, last sucking filtration obtains flavone and extracts thick liquid, described extractant is to be the compound enzyme liquid that 0.02% cellulase solution and pectase solution mix with 1: 1.8 volume ratio by concentration, and the pH value of extractant is 4.5; (3) flavone that obtains in the step (2) is extracted thick liquid and behind vacuum concentration, add dehydrated alcohol, make that concentration of alcohol reaches 95% in the flavone extractive, through reaction, precipitation, filter, obtain the flavone extractive of preliminary purification to remove macromolecular substances; (4) the flavone extractive cryoconcentration that step (3) is obtained and reclaim alcohol solvent, simultaneously with the concentrated solution drying, method is lyophilizing in the dried machine of vacuum freezing, freeze dried condition is: heating-up temperature is 32 ℃, condenser temperature is-60 ℃, pressure is 35Pa, and freeze-drying time is 7.5h, can obtain pulverous flavone extract.
Claims (2)
1, a kind of method of extracting flavone from capillary wormwood is characterized in that may further comprise the steps:
(1) with after capillary wormwood remove impurity, screening, the drying, pulverizing is that 40～50 orders sieve;
(2) adding is equivalent to capillary wormwood weight 20-30 extractant doubly in capillary wormwood, then the sealing, lucifuge, lixiviate 1.0-2.0h under 40-60 ℃ temperature, last sucking filtration obtains flavone and extracts thick liquid, described extractant is to be 0.02% cellulase solution and pectase solution with 1 by concentration: the compound enzyme liquid that the volume ratio of 1.5-2.5 mixes, the pH value of extractant are 4.5-5.5;
(3) flavone that obtains in the step (2) is extracted thick liquid and behind vacuum concentration, add dehydrated alcohol, make that concentration of alcohol reaches more than 80% in the flavone extractive, through reaction, precipitation, filter, obtain the flavone extractive of preliminary purification to remove macromolecular substances;
(4) the flavone extractive cryoconcentration that step (3) is obtained and reclaim alcohol solvent simultaneously with the concentrated solution drying, can obtain pulverous flavone extract.
2, a kind of method of from capillary wormwood, extracting flavone according to claim 1, it is characterized in that in the above-mentioned steps (4) concentrated solution being carried out exsiccant method is lyophilizing in the dried machine of vacuum freezing, freeze dried condition is: heating-up temperature is 25-35 ℃, condenser temperature is-50-60 ℃, pressure is 30-50Pa, and freeze-drying time is 7.0-9.0h.
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| CN2008100553682A CN101317869B (en) | 2008-07-05 | 2008-07-05 | Method for extracting flavone from capillary wormwood |
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| CN2008100553682A CN101317869B (en) | 2008-07-05 | 2008-07-05 | Method for extracting flavone from capillary wormwood |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114272195A (en) * | 2021-12-29 | 2022-04-05 | 科丝美诗(中国)化妆品有限公司 | Composition for resisting ultraviolet and blue light damage and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101053589B (en) * | 2007-04-30 | 2010-11-10 | 王智森 | Method for extracting active constituent from Tibetan capillary |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114272195A (en) * | 2021-12-29 | 2022-04-05 | 科丝美诗(中国)化妆品有限公司 | Composition for resisting ultraviolet and blue light damage and preparation method and application thereof |
| CN114272195B (en) * | 2021-12-29 | 2023-10-27 | 科丝美诗(中国)化妆品有限公司 | Composition for resisting ultraviolet and blue light damage, and preparation method and application thereof |
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