CN1800133A - Preparation method of extracting hemostatic substance 1,3-dihydroxyanthraquinone from India madder charcoal - Google Patents
Preparation method of extracting hemostatic substance 1,3-dihydroxyanthraquinone from India madder charcoal Download PDFInfo
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- CN1800133A CN1800133A CN 200610017380 CN200610017380A CN1800133A CN 1800133 A CN1800133 A CN 1800133A CN 200610017380 CN200610017380 CN 200610017380 CN 200610017380 A CN200610017380 A CN 200610017380A CN 1800133 A CN1800133 A CN 1800133A
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- dihydroxyanthraquinone
- radix rubiae
- charred radix
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Abstract
The invention relates to a method for extracting styptic matter 1, 3-alizarin from the gamene wood coal. It heats the gamene medical herb to prepare it into gamene wood coal with the high effect liquid phase testing 1, 3-alizarin content above 0.15%; it then disposes the gamene wood coal powder in the carbinol to do supersonic and filter to obtain the filter liquid which obtains the volatile substance after filter liquid volatilizing; it adds water to dissolve it and dose ether extraction, uses silica gel column to wash, prepares the liquid phase separation and condensation drying to obtain the 1, 3-alizarin.
Description
One, technical field
The present invention relates to a kind of hemostatic substance 1, preparation method of 3-dihydroxyanthraquinone of extracting from charred RADIX RUBIAE.
Two, background technology
Madder is the dry root and rhizome of madder wort madder Rubia cordifolia L-.With Shaanxi, Henan and Shanxi are the main producing region, are consistent with " to the west of many and good ".In addition in Shandong, ground such as northeast, Sichuan, Yunnan, Guizhou, all have root and rhizome that long medicinal history is arranged in the locality with congener, be clinical conventional Chinese medicine.Madder has cooling blood for hemostasis, and the effect that the stasis of blood of dispelling is stimulated the menstrual flow cures mainly haematemesis, bleeding from five sense organs or subcutaneous tissue, metrostaxis, and traumatic hemorrhage is through closing stasis of blood resistance, arthralgia, tumbling and swelling.Clinical Chang Shengyong and stir-fry charcoal are used.Why charred RADIX RUBIAE can stop blooding, hemostatic substance could be prepared from charred RADIX RUBIAE more fully to be used for hemostasis, it is the problem that medical matters circle are concerned about very much always, find after deliberation, why charred RADIX RUBIAE can stop blooding is because charred RADIX RUBIAE contains a kind of 1, the hemostatic substance of 3-dihydroxyanthraquinone, could be with 1, the 3-dihydroxyanthraquinone extracts from madder, to improve medicinal effect? in order to study to the charred RADIX RUBIAE hemostasis is further, improve preparation technology and understand before and after the process of preparing Chinese medicine and pharmacological action, for this reason, the further development and use of charred RADIX RUBIAE being listed in country's 15 tackling of key scientific and technical problems problems studies.
Three, summary of the invention
Tackling key problem requires and the hematostatic actual needs at national science and technology, the present invention's purpose just provides a kind of hemostatic substance 1 that extracts from charred RADIX RUBIAE, the preparation method of 3-dihydroxyanthraquinone, can effectively solve preparation hemostatic substance 1 from charred RADIX RUBIAE, the problem of 3-dihydroxyanthraquinone, the technical scheme of its solution are that the gamene decoction piece heating is concocted and become charred RADIX RUBIAE, high-efficient liquid phase technique detects 1, the content of 3-dihydroxyanthraquinone must not be lower than 0.15%, and it is ultrasonic to place methyl alcohol to carry out the charred RADIX RUBIAE meal then, filters to get filtrate, after doing, the filtrate volatilization gets volatile matter, be dissolved in water, extracted with diethyl ether is used the silicagel column wash-out again, the preparation liquid phase separation, concentrate drying is 1, the 3-dihydroxyanthraquinone, and the inventive method is simple, easy handling, can be effective to deep processing, improve the pharmaceutical use of madder, also open up new prospect for the hemostasis medication to madder, it is succeeded in developing, and is the creative contribution to Chinese materia medica.
Four, embodiment
Below in conjunction with practical situation the specific embodiment of the present invention is elaborated.
Provide by technique scheme, the present invention is, at first madder is cut into the sheet of 0.2-0.5cm, 200-228 ℃ fry down 8-12min (minute) make it the surface and be burnt brown, inner coke yellow becomes the charred RADIX RUBIAE medicine materical crude slice, the charred RADIX RUBIAE medicine materical crude slice is detected by high-efficient liquid phase technique, in its medicine materical crude slice 1, and the content of 3-dihydroxyanthraquinone 〉=0.15% (promptly must not be lower than 0.15%), then the charred RADIX RUBIAE medicine materical crude slice is pulverized, with every 100g place carry out in the methyl alcohol 500ml ultrasonic 30min (minute), filter, after volatilizing, add water 100ml dissolving, the ether position is collected in ether 500ml extraction 3 times, concentrates, silicagel column is used sherwood oil successively: ethyl acetate was with 100: 1,50: 1,30: 1,10: 1 mixed solution carries out wash-out, collect 10: 1 elutriants, concentrate, the preparation liquid phase is done moving phase with methanol-water, the ratio of first alcohol and water is 7.6: 2.4, flow velocity 10ml/min collects corresponding flow, concentrates, dry, promptly get 1,3-dihydroxyanthraquinone yellow crystal, its molecular structural formula is:
Optimum implementation of the present invention is, at first madder is cut into the sheet of 0.4cm, gets charred RADIX RUBIAE medicine materical crude slice 2kg, put in the electric heating machine for stir-frying Chinese medicine 220 ℃ of controlled temperature, heating 10min takes out and pulverizes, it is 0.21% that the high-efficient phase chromatogram method is measured content, places with every 100g and carries out ultrasonic 30 minutes in the methyl alcohol 500ml, filters, after volatilizing, add water 100ml dissolving, the ether position is collected in ether 500ml extraction 3 times, concentrate, silicagel column is used sherwood oil successively: ethyl acetate was with 100: 1,50: 1,30: 1,10: 1 mixed solution carries out wash-out, observes chromatographic column and thin layer and detects spot, collects 10: 1 elutriants, concentrate, through the preparation liquid phase, do moving phase with methanol-water, the ratio of first alcohol and water is 7.6: 2.4, flow velocity 10ml/min, flow when collecting 7 minutes concentrates drying, promptly get 1,3-dihydroxyanthraquinone yellow crystal.
Gained material of the present invention is 1 after measured, the 3-dihydroxyanthraquinone, be by a kind of medicinal novel substance that extracts in the charred RADIX RUBIAE, through animal and clinical trial, haemostatic effect is very good, is far superior to madder itself, and purposes is very extensive, and compare with other haemostatic medicaments outstanding superiority is also arranged, now relevant situation is described as follows:
One, gets 30 of mouse, male and female half and half, be divided into 3 groups at random, be respectively blank group, 1,3-dihydroxyanthraquinone, Yunnan white powder group, its empty group is given and physiological saline, all the other each group was given separately medicine 3 days,, disposable 20 μ l heparin tubes are inserted mouse endocanthion ball posterior vein get blood after one hour in the last administration, get full 20 μ l blood.Every 15 seconds the capillary vessel that fractures a bit of, check to have or not the blood clotting silk to occur that the meter record to the time that the trace of blood occurs, is the clotting time from blood sampling.Experimental result sees the following form.
1, the 3-dihydroxyanthraquinone is to the influence of clotting time of mice (x ± s)
| Group | Number of animals (only) | Dosage (g/kg) | Clotting time (min) |
| Blank group | 10 | - | 5.98±0.99 |
| The Yunnan white powder group | 10 | 0.5 | 2.13±1.00 ** |
| 1,3-dihydroxyanthraquinone group | 10 | - | 2.08±1.04 ** |
Annotate: compare with the blank group,
*P＜0.01.
During the experimental result table: 1, the 3-dihydroxyanthraquinone has the effect of tangible shortening clotting time of mice, and utmost point significance meaning (p＜0.01) is arranged, results suggest 1, the 3-dihydroxyanthraquinone has tangible anastalsis.
Two, to the wound bleeding straightway testing
1, gets 10 of mouse, draw little stomatorrhagia with scalpel, with spreading on medicine of the present invention at shank, hemorrhage 1-2 promptly ended in second, and spread on the edge of a knife with the powder that former madder is made, and did not have obvious haemostatic effect, that is to say that the madder powder should not be directly used in wound, prepared product of the present invention is remarkably productive.
2, clinical in outpatient service and inpatient's 11 people's wound application, behind the application material of the present invention, 1-2 minute hemorrhage stops or obviously alleviates, and pain relief, has obtained gratifying effect.
In a word, of the present invention succeeding in developing, solved a difficult problem of madder tackling key problem, can be widely used in haematemesis, bleeding from five sense organs or subcutaneous tissue, metrostaxis, traumatic hemorrhage, hemorrhage through closing stasis of blood resistance, arthralgia and tumbling and swelling and causing by a variety of causes, combination with other components, can prepare various hemostasis good medicine, for development and use and the Chinese materia medica treasure-house of madder are made creative contribution.
Claims (2)
1, a kind of hemostatic substance 1 that from charred RADIX RUBIAE, extracts, the preparation method of 3-dihydroxyanthraquinone, it is characterized in that being, at first madder is cut into the sheet of 0.2-0.5cm, make it the surface at 200-228 ℃ of following stir-fry 8-12min and be burnt brown, inner coke yellow becomes the charred RADIX RUBIAE medicine materical crude slice, its medicine materical crude slice interior 1, the content of 3-dihydroxyanthraquinone 〉=0.15%, then the charred RADIX RUBIAE medicine materical crude slice is pulverized, placed with every 100g and carry out ultrasonic 30min in the methyl alcohol 500ml, filter, after volatilizing, add water 100ml dissolving, the ether position is collected in ether 500ml extraction 3 times, concentrate, silicagel column is used sherwood oil successively: ethyl acetate was with 100: 1,50: 1,30: 1,10: 1 mixed solution carries out wash-out, collects 10: 1 elutriants, concentrates, the preparation liquid phase is done moving phase with methanol-water, the ratio of first alcohol and water is 7.6: 2.4, and flow velocity 10ml/min collects corresponding flow, concentrate drying.
2, the hemostatic substance 1 that from charred RADIX RUBIAE, extracts according to claim 1, the preparation method of 3-dihydroxyanthraquinone is characterized in that, the said sheet that at first madder is cut into 0.4cm, get charred RADIX RUBIAE medicine materical crude slice 2kg, put in the electric heating machine for stir-frying Chinese medicine 220 ℃ of controlled temperature, heating 10min, take out and pulverize, it is 0.21% that the high-efficient phase chromatogram method is measured content, places with every 100g and carries out ultrasonic 30 minutes in the methyl alcohol 500ml, filters, after volatilizing, add water 100ml dissolving, the ether position is collected in ether 500ml extraction 3 times, concentrate, silicagel column is used sherwood oil successively: ethyl acetate was with 100: 1,50: 1,30: 1,10: 1 mixed solution carries out wash-out, observes chromatographic column and thin layer and detects spot, collects 10: 1 elutriants, concentrate, through the preparation liquid phase, do moving phase with methanol-water, the ratio of first alcohol and water is 7.6: 2.4, flow velocity 10ml/min, flow when collecting 7 minutes concentrates drying, promptly get 1,3-dihydroxyanthraquinone yellow crystal.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100173805A CN100408535C (en) | 2006-01-25 | 2006-01-25 | Preparation method of extracting hemostatic substance 1,3-dihydroxyanthraquinone from India madder charcoal |
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| CNB2006100173805A CN100408535C (en) | 2006-01-25 | 2006-01-25 | Preparation method of extracting hemostatic substance 1,3-dihydroxyanthraquinone from India madder charcoal |
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| CN1800133A true CN1800133A (en) | 2006-07-12 |
| CN100408535C CN100408535C (en) | 2008-08-06 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101664462B (en) * | 2008-09-04 | 2012-02-01 | 河南大学 | Hypoglycemic active part and hypoglycemic effective component of madder, preparation method and application thereof |
| CN107807100A (en) * | 2017-09-14 | 2018-03-16 | 广州中医药大学 | A kind of method for building up and purification process of madder medicinal material Radix Rubiae total anthraquinones assay |
-
2006
- 2006-01-25 CN CNB2006100173805A patent/CN100408535C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101664462B (en) * | 2008-09-04 | 2012-02-01 | 河南大学 | Hypoglycemic active part and hypoglycemic effective component of madder, preparation method and application thereof |
| CN107807100A (en) * | 2017-09-14 | 2018-03-16 | 广州中医药大学 | A kind of method for building up and purification process of madder medicinal material Radix Rubiae total anthraquinones assay |
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| Publication number | Publication date |
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| CN100408535C (en) | 2008-08-06 |
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