CN102920765A - Method for extracting total flavone of active parts of China ixeris - Google Patents
Method for extracting total flavone of active parts of China ixeris Download PDFInfo
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- CN102920765A CN102920765A CN 201210490726 CN201210490726A CN102920765A CN 102920765 A CN102920765 A CN 102920765A CN 201210490726 CN201210490726 CN 201210490726 CN 201210490726 A CN201210490726 A CN 201210490726A CN 102920765 A CN102920765 A CN 102920765A
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Abstract
The invention discloses a method for extracting the total flavone of active parts of China ixeris and relates to a method for extracting the total flavone, solving the problem that the total flavone in the extract which is obtained through the existing method for extracting the total flavone is low in content. The method for extracting the total flavone comprises the following steps of: 1, decocting the China ixeris twice by adding water, and merging the twice decoction liquids, and concentrating to obtain clear paste; 2, adding water into the clear paste, adding sodium hydroxide solution to regulate the pH value, soaking and collecting supernatant, regulating the pH value of the supernatant through hydrochloric acid solution, standing and connecting a liquid on the upper layer; 3, purifying the supernatant liquid which is collected in the step 2 through a polyamide resin column, eluting with the water and ethanol respectively, and collecting ethanol eluant; and 4, distilling the ethanol eluant at reduced pressure, carrying out reduced pressure concentration and reduced pressure drying on the eluant so as to obtain the total flavone extract. The total flavone content of the extract is not less than 80% based on rutin. The method is mainly applied to the preparation of the high-purity total flavone.
Description
Technical field
The present invention relates to the extracting method of total flavones, be specifically related to extract from the four seasons dish effective site method of total flavones.
Background technology
Four seasons dish (Artemisia laxtiflora Wall) is the herbaceos perennial of Compositae artemisia.Have another name called Radix seu Caulis Embeliae Parviflorae, Herba artemisiae lactiflorae, insidious grass.Four seasons dish aboundresources mainly is distributed in the East China of China, the ground such as Central-South, southwestern.Its property is hot, and sweet in the mouth is flat, has heat-clearing and toxic substances removing, nourishing blood to suppress the hyperactive liver, regulating the flow of QI to dissipate blood stasis, blood circulation promoting and blood stasis dispelling, the effects such as dispelling wind stopping cough.Be used for the treatment of clinically chronic hepatitis, traumatic injury, headache, the diseases such as hematuria, menoxenia of coughing, have loose bowels, have blood in stool.Especially treat qi depression to blood stasis, the chronic active hepatitis of not nourishing the liver of blood, chronic persistent hepatitis significant curative effect is arranged.Liver cirrhosis, acute serious hepatitis also there is preferably effect.Contain flavone, phenols, volatile oil, aminoacid, organic acid and saccharide compound in the four seasons dish herb.
Bibliographical information is arranged, from its stem and leaf, separate the flavonoid obtain and have the effects such as antibiotic, anti-mildew, spasmolytic, diuresis.Clinical research shows that four seasons dish effective ingredient total flavones has significant curative effect for the treatment of chronic hepatitis, acute jaundice sexually transmitted disease (STD) virus hepatitis.Total flavones in the four seasons dish is to CCl
4, the acute liver damage due to the ethanol has significant protective effect.Its total flavones may exhaust to the protective effect of hepatic injury that with its minimizing liver GSH it is relevant to suppress the liver lipid peroxidation effect.Bibliographical information is also arranged, four seasons dish treatment hepatopath, 98% case, liver function recovery is normal in 50 days, and only 2% case reaches recovery in 70 days.
Advanced extractive technique has been applied to the every field that Chinese crude drug extracts processing, still, and for the extraction of the active site total flavones of four seasons dish and have no relevant report.Most still take traditional extracting method, the extracting method of flavones ingredient to have mainly to comprise solvent extraction, microwave extraction, supercritical extraction, the extraction of enzyme dipping, ultrasonic extraction, backflow, Soxhlet extraction, decocting method and diafiltration etc.At present, few to the relevant report of the extraction of the effective site total flavones of four seasons dish, and there are no the relevant report with the total flavones of polyamide purifying four seasons dish, adopt in the extract that existing extracting method obtains general flavone content low, with rutin (C
27H
30O
16) count below 70%.
Summary of the invention
The low problem of general flavone content in the extract that the objective of the invention is to obtain for the extracting method that solves existing total flavones, and the extracting method of four seasons dish effective site total flavones is provided.
The extracting method of four seasons dish effective site total flavones of the present invention is to realize through the following steps:
One, get 40～60kg four seasons dish Chinese crude drug and put into water and decoct 1～3 hour after, collect for the first time fried decoction liquor, after decocting with water 1～3 hour in the four seasons dish medical material again, collect for the second time fried decoction liquor, merge decoction liquor twice, be condensed into take the clear paste of 75～80 ℃ of relative densities as 1.12～1.14;
Two, adding water to volume in the clear paste that obtains to step 1 is 130～160L, then add the sodium hydroxide solution adjust pH to 6 of 1.5～2.5mol/L～7, soak and collected supernatant in 12～24 hours, transfer supernatant pH value to 2.0～3.0 with 3～5mol/L hydrochloric acid solution, then left standstill 12～24 hours, and collected supernatant liquid;
Three, the supernatant liquid of step 2 being collected uses the water elution of 6～10 column volumes with pretreated polyamide column purification, and then is the alcoholic solution eluting of 50%～75%, 9～11 column volumes with volumetric concentration, the collection ethanol elution;
Four, the ethanol in use distilling under reduced pressure recycling step three ethanol elution again to the eluent concentrating under reduced pressure, then carries out drying under reduced pressure, obtains the extractive of general flavone of four seasons dish effective site;
The quality of water was 10～16 times of four seasons dish Chinese crude drug during wherein step 1 described for the first time decocted, and the quality of water is 6～12 times of four seasons dish Chinese crude drug in decocting for the second time;
The mass ratio of polyamide quality and four seasons dish Chinese crude drug is 1:(2～4 in the step 3);
Pretreated polyamide resin column is that polyamide is packed in the chromatographic column in the step 3, wash to eluate with the flow velocity of 0.2～0.4BV/h with acetone and to be colourless, be 90～96% with volumetric concentration again, consumption is that the ethanol of 4～6 times of column volumes is with the flow velocity flushing of 0.2～0.4BV/h, then pour out ethanol, put into baking oven with 80～100 ℃ of oven dry, obtain pretreated polyamide resin column.
General flavone content is with rutin (C in the extract that extracting method by four seasons dish effective site total flavones of the present invention obtains
27H
30O
16) meter, content is no less than 80%, also has coumarin, herniarin etc. in the extract monomer component, has improved the content of total flavones in the extract.Press practice of pharmacy, four seasons dish effective site total flavones among the present invention can be made the dosage form that is applicable to clinical oral formulations and parenterai administration.Said oral formulations can be made into a kind of in the middle of the granule, tablet, capsule, pill, drop pill, suspensoid, oral liquid.Said parenterai administration dosage form can be made into a kind of in the middle of injection, aerosol, suppository or the subcutaneous administration dosage form.Four seasons dish total flavones of the present invention is made in the various dosage forms, also can add conventional drug excipient, such as solvent, disintegrating agent, correctives, antiseptic, coloring agent etc.The present invention is mainly used in the preparation of high-purity total flavones, and the gained total flavones can be used for oral formulations and non-intestinal drug delivery agent.
The specific embodiment
The specific embodiment one: the extracting method of present embodiment four seasons dish effective site total flavones follows these steps to implement:
One, get 40～60kg four seasons dish Chinese crude drug and put into water and decoct 1～3 hour after, collect for the first time fried decoction liquor, after decocting with water 1～3 hour in the four seasons dish medical material again, collect for the second time fried decoction liquor, merge decoction liquor twice, be condensed into take the clear paste of 75～80 ℃ of relative densities as 1.12～1.14;
Two, adding water to volume in the clear paste that obtains to step 1 is 130～160L, then add the sodium hydroxide solution adjust pH to 6 of 1.5～2.5mol/L～7, soak and collected supernatant in 12～24 hours, transfer supernatant pH value to 2.0～3.0 with 3～5mol/L hydrochloric acid solution, then left standstill 12～24 hours, and collected supernatant liquid;
Three, the supernatant liquid of step 2 being collected uses the water elution of 6～10 column volumes with pretreated polyamide column purification, and then is the alcoholic solution eluting of 50%～75%, 9～11 column volumes with volumetric concentration, the collection ethanol elution;
Four, the ethanol in use distilling under reduced pressure recycling step three ethanol elution again to the eluent concentrating under reduced pressure, then carries out drying under reduced pressure, obtains the extractive of general flavone of four seasons dish effective site;
The quality of water was 10～16 times of four seasons dish Chinese crude drug during wherein step 1 described for the first time decocted, and the quality of water is 6～12 times of four seasons dish Chinese crude drug in decocting for the second time;
The mass ratio of polyamide quality and four seasons dish Chinese crude drug is 1:(2～4 in the step 3);
Pretreated polyamide resin column is that polyamide is packed in the chromatographic column in the step 3, wash to eluate with the flow velocity of 0.2～0.4BV/h with acetone and to be colourless, be 90～96% with volumetric concentration again, consumption is that the ethanol of 4～6 times of column volumes is with the flow velocity flushing of 0.2～0.4BV/h, then pour out ethanol, put into baking oven with 80～100 ℃ of oven dry, obtain pretreated polyamide resin column.
Main component is flavone, ayapanin and herniarin in the extractive of general flavone of present embodiment four seasons dish effective site.
The specific embodiment two: present embodiment and the specific embodiment one are different is the step 2 sodium hydroxide solution adjust pH to 6 that adds 1.7～2.3mol/L～7.Other step and parameter are identical with the specific embodiment one.
The specific embodiment three: present embodiment and the specific embodiment one are different is the step 2 sodium hydroxide solution adjust pH to 6 that adds 2mol/L～7.Other step and parameter are identical with the specific embodiment one.
The specific embodiment four: what present embodiment was different from one of specific embodiment one to three is that step 2 is transferred supernatant pH value to 2.0～3.0 with 3.5～4.5mol/L hydrochloric acid solution.Other step and parameter are identical with one of specific embodiment one to three.
The specific embodiment five: what present embodiment was different from one of specific embodiment one to three is that step 2 is transferred supernatant pH value to 2.0～3.0 with the 4.2mol/L hydrochloric acid solution.Other step and parameter are identical with one of specific embodiment one to three.
The specific embodiment six: what present embodiment was different from one of specific embodiment one to five is that the described drying under reduced pressure of step 4 is spray drying.Other step is identical with one of specific embodiment one to five with parameter.
The specific embodiment seven: the extracting method of present embodiment four seasons dish effective site total flavones follows these steps to implement:
One, gets 50kg four seasons dish Chinese crude drug and put into the water decoction after 1.5 hours, collect for the first time fried decoction liquor, decoct with water 1.5 hours in the four seasons dish medical material again after, collect for the second time fried decoction liquor, merge decoction liquor twice, being concentrated into into 80 ℃ of meter relative densities is 1.14 clear paste;
Two, adding water to volume in the clear paste that obtains to step 1 is 150L, then the sodium hydroxide solution adjust pH to 6 that adds 2mol/L soaks and collected supernatant in 24 hours, transfers supernatant pH value to 3.0 with the 4mol/L hydrochloric acid solution, then left standstill 24 hours, and collected supernatant liquid;
Three, the supernatant liquid of step 2 being collected uses the water elution of 8 column volumes with pretreated polyamide column purification, and then is the alcoholic solution eluting of 75%, 10 column volume with volumetric concentration, the collection ethanol elution;
Four, the ethanol in use distilling under reduced pressure recycling step three ethanol elution again to the eluent concentrating under reduced pressure, then carries out drying under reduced pressure, obtains the extractive of general flavone of four seasons dish effective site;
The quality of water was 10 times of four seasons dish Chinese crude drug during wherein step 1 described for the first time decocted, and the quality of water is 12 times of four seasons dish Chinese crude drug in decocting for the second time;
The mass ratio of polyamide quality and four seasons dish Chinese crude drug is 1:2 in the step 3;
Pretreated polyamide resin column is that polyamide is packed in the chromatographic column in the step 3, wash to eluate with the flow velocity of 0.3BV/h with acetone and to be colourless, be 95% with volumetric concentration again, consumption is that the ethanol of 5 times of column volumes is with the flow velocity flushing of 0.3BV/h, then pour out ethanol, put into baking oven with 90 ℃ of oven dry, obtain pretreated polyamide resin column.
The extractive of general flavone main component of present embodiment four seasons dish effective site is flavone, ayapanin and herniarin, and general flavone content is with anhydrous rutin (C in the extract
27H
30O
16) count 83%.
Claims (4)
1. the extracting method of four seasons dish effective site total flavones is characterized in that the four seasons extracting method of dish effective site total flavones is to realize through the following steps:
One, get 40～60kg four seasons dish Chinese crude drug and put into water and decoct 1～3 hour after, collect for the first time fried decoction liquor, after decocting with water 1～3 hour in the four seasons dish medical material again, collect for the second time fried decoction liquor, merge decoction liquor twice, be condensed into take the clear paste of 75～80 ℃ of relative densities as 1.12～1.14;
Two, adding water to volume in the clear paste that obtains to step 1 is 130～160L, then add the sodium hydroxide solution adjust pH to 6 of 1.5～2.5mol/L～7, soak and collected supernatant in 12～24 hours, transfer supernatant pH value to 2.0～3.0 with 3～5mol/L hydrochloric acid solution, then left standstill 12～24 hours, and collected supernatant liquid;
Three, the supernatant liquid of step 2 being collected uses the water elution of 6～10 column volumes with pretreated polyamide column purification, and then is the alcoholic solution eluting of 50%～75%, 9～11 column volumes with volumetric concentration, the collection ethanol elution;
Four, the ethanol in use distilling under reduced pressure recycling step three ethanol elution again to the eluent concentrating under reduced pressure, then carries out drying under reduced pressure, obtains the extractive of general flavone of four seasons dish effective site;
The quality of water was 10～16 times of four seasons dish Chinese crude drug during wherein step 1 described for the first time decocted, and the quality of water is 6～12 times of four seasons dish Chinese crude drug in decocting for the second time;
The mass ratio of polyamide quality and four seasons dish Chinese crude drug is 1:(2～4 in the step 3);
Pretreated polyamide resin column is that polyamide is packed in the chromatographic column in the step 3, wash to eluate with the flow velocity of 0.2～0.4BV/h with acetone and to be colourless, be 90～96% with volumetric concentration again, consumption is that the ethanol of 4～6 times of column volumes is with the flow velocity flushing of 0.2～0.4BV/h, then pour out ethanol, put into baking oven with 80～100 ℃ of oven dry, obtain pretreated polyamide resin column.
2. the extracting method of four seasons dish effective site total flavones according to claim 1 is characterized in that step 2 adds the sodium hydroxide solution adjust pH to 6 of 1.7～2.3mol/L～7.
3. the extracting method of four seasons dish effective site total flavones according to claim 1 is characterized in that step 2 transfers supernatant pH value to 2.0～3.0 with 3.5～4.5mol/L hydrochloric acid solution.
4. according to claim 1, the extracting method of 2 or 3 described four seasons dish effective site total flavones, it is characterized in that the described drying under reduced pressure of step 4 is spray drying.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210490726 CN102920765A (en) | 2012-11-27 | 2012-11-27 | Method for extracting total flavone of active parts of China ixeris |
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| CN 201210490726 CN102920765A (en) | 2012-11-27 | 2012-11-27 | Method for extracting total flavone of active parts of China ixeris |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104523797A (en) * | 2014-11-28 | 2015-04-22 | 刘新江 | Artemisia lactiflora human physiological balance regulator |
| CN104667892A (en) * | 2015-02-11 | 2015-06-03 | 北海和思科技有限公司 | Macroporous resin pretreatment method |
-
2012
- 2012-11-27 CN CN 201210490726 patent/CN102920765A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104523797A (en) * | 2014-11-28 | 2015-04-22 | 刘新江 | Artemisia lactiflora human physiological balance regulator |
| CN104667892A (en) * | 2015-02-11 | 2015-06-03 | 北海和思科技有限公司 | Macroporous resin pretreatment method |
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Application publication date: 20130213 |