CN101181331A - Method for preparing artemisia leaf total chromocor - Google Patents
Method for preparing artemisia leaf total chromocor Download PDFInfo
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- CN101181331A CN101181331A CNA2007101644472A CN200710164447A CN101181331A CN 101181331 A CN101181331 A CN 101181331A CN A2007101644472 A CNA2007101644472 A CN A2007101644472A CN 200710164447 A CN200710164447 A CN 200710164447A CN 101181331 A CN101181331 A CN 101181331A
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Abstract
The invention discloses a preparative method for total flavone in artemisia leaves, comprising the steps that: the artemisia leaves is stirred and extracted twice by C1-c4 low-molecule alcohol solvent in the consistency of 75 to 100 percent under the temperature of 25 to 35 DEG C; the extracted liquid is filtrated in a graded manner by a three-level filtrating film filter, the pressure of the filtrating liquid is reduced and concentrated at 40 to 45 DEG C till the relative consistency thereof reaches 1.01 to 1.04, hexane is extracted and separated in a flux of 40 to 60l/h when the concentrated liquid flows through a high-speed centrifigual extractor in the flux of a speed of 40 to 601/h; the concentrated liquid which is extracted is concentrated to the relative consistency of 1.06 to 1.08 under the temperature of 40 to 45 DEG C, so that the refined total flavone which weights no less than 5 percent of the total artemisia leaves can be extracted in the pure artemisia leaves, wherein, the content of 5,7 dihydroxy 6, 3', 4'-trimethoxy flavone is no less than 1.0 percent, thus, the invention provides a basis for the the application of the total flavone in the artemisia leaves, especially provides the medical prospect of the 5,7 dihydroxy 6, 3', 4'- trimethoxy flavone. The 5, 7 dihydroxy 6, 3', 4'-trimethoxy flavone is applicable for the preparation of the ideal anticoagulant medice in the Chinese traditional medicine.
Description
Technical field
The present invention relates to plant extract technology, be specifically related to a kind of preparation method of artemisia leaf total chromocor.
Background technology
Folium Artemisiae Argyi (Folium Artemisia Argyi) belongs to feverfew, is the conventional Chinese medicine material, has dispersing cold for relieving pain, warming the meridian for stopping bleeding, and regulating menstruation is antiabortive, and effects such as removing damp to relieve itching and dredge the meridian passage are therefore especially suitable to gynaecopathia.
Contain medicinal active ingredients such as volatile oil, flavone, eudesmane, terpenoid and polysaccharide in the Folium Artemisiae Argyi; The main component of artemisia leaf total chromocor has 5,7-dihydroxy-6,3 ', 4 '-trimethoxy flavone, 5-hydroxyl 6,7,3 ', 4 '-tetramethoxy flavone, Quercetin, naringenin etc., wherein 5,7-dihydroxy-6, the weight percentage of 3 ', 4 '-trimethoxy flavone in Folium Artemisiae Argyi is 0.03-0.05%, and pharmacological research confirms, 5,7-dihydroxy-6,3 ', 4 '-trimethoxy flavone has the obvious suppression effect to platelet, has stronger anticoagulation, can be prepared into ideal Chinese medicine anticoagulant.
At present the active ingredient technology of preparing of Folium Artemisiae Argyi is generally and extracts volatile oil or polysaccharide, very few to the research of its total flavones, and how with Quercetin as the index composition.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method of extracting total flavones from Folium Artemisiae Argyi.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of preparation method of artemisia leaf total chromocor comprises the steps:
A. pure Folium Artemisiae Argyi is dropped in the extraction pot, under 25-35 ℃ temperature conditions, the concentration that adds 6-14 times of Folium Artemisiae Argyi weight earlier is the C of 75-100%
1-C
4Low molecular alcoholic solvents stirring and leaching 4-8 hour, solid-liquid separation obtain lixiviating solution for the first time, the C that to add 3-8 times of Folium Artemisiae Argyi weight concentration again in extraction pot be 75-100%
1-C
4Low molecular alcoholic solvents stirring and leaching 2-6 hour, solid-liquid separation obtain lixiviating solution for the second time;
B. above-mentioned twice lixiviating solution merged, with 80-120um, 40-60um and three grades of membrane filter classified filterings of 20-30um, filtering velocity is 1000l/h, and the filter internal pressure is not more than 0.8Mpa, obtains filtrate;
C. be in the concentrator of 0.075-0.085Mpa with above-mentioned filtrate suction negative pressure, make the temperature in the concentrator be controlled at 40-45 ℃ with steam, the pressure of steam is not more than 0.01Mpa, concentrating under reduced pressure filtrate, filtrate stops to concentrate when being concentrated into relative density for 1.01-1.04, obtain concentrated solution, reclaim low molecular alcoholic solvents simultaneously;
D. the speed that with above-mentioned concentrated solution with the flow is 40-60l/h is separated for the 40-60l/h hexane extraction with flow by the high speed centrifugation extracter, and centrifugation rate is 12000r/min, the concentrated solution that obtains being extracted;
E. be in the concentrator of 0.075-0.085Mpa with the above-mentioned concentrated solution suction negative pressure that was extracted, make the temperature in the concentrator be controlled at 40-45 ℃ with steam, the concentrated solution that concentrating under reduced pressure was extracted, the pressure of steam is not more than 0.01Mpa, when the concentrated solution that was extracted is concentrated into relative density for 1.06-1.08, stop to concentrate, obtain refining artemisia leaf total chromocor.
Described low molecular alcoholic solvents is an isopropyl alcohol.
The isopropanol solvent stirring and leaching that elder generation's 10 times of Folium Artemisiae Argyi weight concentrations of adding are 99-100% in step a 6 hours, separate and obtain lixiviating solution for the first time, the isopropanol solvent stirring and leaching that to add 6 times of Folium Artemisiae Argyi weight concentrations again be 99-100% 4 hours separates obtaining lixiviating solution for the second time; Concentration is that the isopropyl alcohol extracting effect of 99-100% is better, and lixiviate for the first time is that 6 hours and lixiviate for the second time are that 4 hours efficient is better.
In step b, use 100um, 50um and three grades of membrane filter classified filterings of 25um.
The concentrated solution relative density is 1.02-1.03 in step c.
Concentrated solution discharge is 50l/h in steps d, and the flow of hexane is 50l/h.
Described concentrator is the outer circulation concentrator.
Above-mentioned Folium Artemisiae Argyi weight is with dried Folium Artemisiae Argyi weight metering.
Compared with prior art, the invention has the advantages that the preparation method by the artemisia leaf total chromocor of step a, b, c, d and e: making Folium Artemisiae Argyi under 25-35 ℃ temperature conditions, is the C of 75-100% by concentration
1-C
4Twice stirring and leaching of low molecular alcoholic solvents, to lixiviating solution with three grades of membrane filter classified filterings, filtrate is evaporated to relative density under 40-45 ℃ of condition be 1.01-1.04, concentrated solution is that the speed of 40-60l/h is passed through the high speed centrifugation extracter with the flow, separate for the 40-60l/h hexane extraction with flow, the concentrated solution that was extracted is concentrated into relative density under 40-45 ℃ of condition be 1.06-1.08, can in pure Folium Artemisiae Argyi, extract the refining artemisia leaf total chromocor that weight is not less than 5% Folium Artemisiae Argyi weight, wherein 5,7-dihydroxy-6, the weight of 3 ', 4 '-trimethoxy flavone is not less than 1.0%; With regard to for the application of artemisia leaf total chromocor lays the foundation, especially providing is 5,7-dihydroxy-6, the prospect in medicine of 3 ', 4 '-trimethoxy flavone like this; Can be with 5,7-dihydroxy-6,3 ', 4 '-trimethoxy flavone are prepared into ideal Chinese medicine anticoagulant.
The specific embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Embodiment 1
A kind of preparation method of artemisia leaf total chromocor comprises the steps:
A. pure 250 kilograms of dried Folium Artemisiae Argyis are dropped in the extraction pot, under 25-35 ℃ temperature conditions, the isopropanol solvent stirring and leaching that it is 99-100% that elder generation adds 2500 kilograms of concentration 6 hours, solid-liquid separation obtains lixiviating solution for the first time, the isopropanol solvent stirring and leaching that to add 1500 kilograms of concentration again in extraction pot be 99-100% 4 hours, solid-liquid separation obtain lixiviating solution for the second time;
B. above-mentioned twice lixiviating solution merged, with 100um, 50um and three grades of membrane filter classified filterings of 25um, filtering velocity is 1000l/h, and the filter internal pressure is not more than 0.8Mpa, obtains filtrate;
C. be in the outer circulation concentrator of 0.075-0.085Mpa with above-mentioned filtrate suction negative pressure, slowly open steam valve, steam is not more than 0.01Mpa to the pressure of outer circulation concentrator sidewall, make the interior temperature of outer circulation concentrator at 40-45 ℃, concentrating under reduced pressure filtrate, filtrate stops to concentrate when being concentrated into relative density for 1.02-1.03, obtains concentrated solution, reclaims isopropyl alcohol simultaneously;
D. the speed that with above-mentioned concentrated solution with the flow is 50l/h enters the high speed centrifugation extracter from inlet, feeding flow from another inlet simultaneously is the hexane of 50l/h, in the high speed centrifugation extracter, use the hexane extraction separation concentrated solution, centrifugation rate is 12000r/min, obtain the concentrated solution and the extract that were extracted respectively from outlet, reclaim extract;
E. be in the concentrator of 0.075-0.085Mpa with the above-mentioned concentrated solution suction negative pressure that was extracted, slowly open steam valve, steam is not more than 0.01Mpa to the pressure of outer circulation concentrator sidewall, make the temperature in the outer circulation concentrator be controlled at 40-45 ℃, the concentrated solution that concentrating under reduced pressure was extracted, the concentrated solution that was extracted stops to concentrate when being concentrated into relative density for 1.06-1.08, obtains refining artemisia leaf total chromocor.
Obtain 12.6 kilograms of refining artemisia leaf total chromocors through weighing, after measured 5,7-dihydroxy-6, the weight of 3 ', 4 '-trimethoxy flavone is 0.15 kilogram.
Lixiviates such as the present invention also can propanol, ethanol, methanol or butanols also can be above-mentioned C
1-C
4The combination in any lixiviate of low mass molecule alcohol.With fresh Folium Artemisiae Argyi, its weight will be scaled the weight of dried Folium Artemisiae Argyi, and dried Folium Artemisiae Argyi is as the criterion can preserve to preserve.
Claims (7)
1. the preparation method of an artemisia leaf total chromocor is characterized in that comprising the steps:
A. pure Folium Artemisiae Argyi is dropped in the extraction pot, under 25-35 ℃ temperature conditions, the low molecular alcoholic solvents stirring and leaching that the first concentration that adds 6-14 times of Folium Artemisiae Argyi weight is 75-100% 4-8 hour, solid-liquid separation obtains lixiviating solution for the first time, the C that to add 3-8 times of Folium Artemisiae Argyi weight concentration again in extraction pot be 75-100%
1-C
4Low molecular alcoholic solvents stirring and leaching 2-6 hour, solid-liquid separation obtain lixiviating solution for the second time;
B. above-mentioned twice lixiviating solution merged, with 80-120um, 40-60um and three grades of membrane filter classified filterings of 20-30um, filtering velocity is 1000l/h, and the filter internal pressure is not more than 0.8Mpa, obtains filtrate;
C. be in the concentrator of 0.075-0.085Mpa with above-mentioned filtrate suction negative pressure, make the temperature in the concentrator be controlled at 40-45 ℃ with steam, the pressure of steam is not more than 0.01Mpa, concentrating under reduced pressure filtrate, filtrate stops to concentrate when being concentrated into relative density for 1.01-1.04, obtain concentrated solution, reclaim low molecular alcoholic solvents simultaneously;
D. the speed that with above-mentioned concentrated solution with the flow is 40-60l/h is separated for the 40-60l/h hexane extraction with flow by the high speed centrifugation extracter, and centrifugation rate is 12000r/min, the concentrated solution that obtains being extracted;
E. be in the concentrator of 0.075-0.085Mpa with the above-mentioned concentrated solution suction negative pressure that was extracted, make the temperature in the concentrator be controlled at 40-45 ℃ with steam, the pressure of steam is not more than 0.01Mpa, the concentrated solution that concentrating under reduced pressure was extracted, the concentrated solution that was extracted stops to concentrate when being concentrated into relative density for 1.06-1.08, obtains refining artemisia leaf total chromocor.
2. the preparation method of a kind of artemisia leaf total chromocor as claimed in claim 1 is characterized in that described low molecular alcoholic solvents is an isopropyl alcohol.
3. the preparation method of a kind of artemisia leaf total chromocor as claimed in claim 2, it is characterized in that in step a, adding 10 times of Folium Artemisiae Argyi weight concentrations earlier the isopropanol solvent stirring and leaching that is 99-100% 6 hours, separate and obtain lixiviating solution for the first time, the isopropanol solvent stirring and leaching that to add 6 times of Folium Artemisiae Argyi weight concentrations again be 99-100% 4 hours separates obtaining lixiviating solution for the second time.
4. the preparation method of a kind of artemisia leaf total chromocor as claimed in claim 1 is characterized in that in step b with 100um, 50um and three grades of membrane filter classified filterings of 25um.
5. the preparation method of a kind of artemisia leaf total chromocor as claimed in claim 1 is characterized in that the concentrated solution relative density is 1.02-1.03 in step c.
6. the preparation method of a kind of artemisia leaf total chromocor as claimed in claim 1 is characterized in that concentrated solution discharge is 50l/h in steps d, and the flow of hexane is 50l/h.
7. the preparation method of a kind of artemisia leaf total chromocor as claimed in claim 1 is characterized in that described concentrator is the outer circulation concentrator.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101644472A CN101181331B (en) | 2007-12-11 | 2007-12-11 | Method for preparing artemisia leaf total chromocor |
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| CN2007101644472A CN101181331B (en) | 2007-12-11 | 2007-12-11 | Method for preparing artemisia leaf total chromocor |
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| CN101181331A true CN101181331A (en) | 2008-05-21 |
| CN101181331B CN101181331B (en) | 2010-09-22 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105232603A (en) * | 2015-10-10 | 2016-01-13 | 宁波绿之健药业有限公司 | Folium artemisiae argyi extract preparation method |
| CN109316416A (en) * | 2018-09-06 | 2019-02-12 | 广州华玺生物科技有限公司 | A kind of Folium Artemisiae Argyi extract and its application in cosmetics |
| CN111358821A (en) * | 2020-04-17 | 2020-07-03 | 铜仁职业技术学院 | Method for optimizing enzymolysis-assisted ultrasonic extraction of folium artemisiae argyi total flavonoids by response surface method |
-
2007
- 2007-12-11 CN CN2007101644472A patent/CN101181331B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105232603A (en) * | 2015-10-10 | 2016-01-13 | 宁波绿之健药业有限公司 | Folium artemisiae argyi extract preparation method |
| CN109316416A (en) * | 2018-09-06 | 2019-02-12 | 广州华玺生物科技有限公司 | A kind of Folium Artemisiae Argyi extract and its application in cosmetics |
| CN111358821A (en) * | 2020-04-17 | 2020-07-03 | 铜仁职业技术学院 | Method for optimizing enzymolysis-assisted ultrasonic extraction of folium artemisiae argyi total flavonoids by response surface method |
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| Publication number | Publication date |
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| CN101181331B (en) | 2010-09-22 |
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Owner name: KAIFENG SHANGGONG PHARMACEUTICAL CO., LTD. Free format text: FORMER OWNER: NINGBO SINO-TAIPIO HERBAL SCIENCE CO., LTD. Effective date: 20131211 |
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Effective date of registration: 20131211 Address after: 475399, Kaifeng County, Kaifeng City, Henan province high field village north Patentee after: Kaifeng Shang Shang Pharmaceutical Co., Ltd. Address before: The State Economic and Technological Development Zone, Zhejiang province Ningbo City Road 315800 No. 493 dragon A2 Patentee before: Ningbo Sino-Taipio Herbal Science Co., Ltd. |
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