CN1559482A - Preparation method of achillea effective part medicinal preparation - Google Patents
Preparation method of achillea effective part medicinal preparation Download PDFInfo
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- CN1559482A CN1559482A CNA2004100083763A CN200410008376A CN1559482A CN 1559482 A CN1559482 A CN 1559482A CN A2004100083763 A CNA2004100083763 A CN A2004100083763A CN 200410008376 A CN200410008376 A CN 200410008376A CN 1559482 A CN1559482 A CN 1559482A
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- dichloromethane
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- ethyl acetate
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- herba achilleae
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Abstract
An oral Chinese medicine for treating viral hepatitis and liver injuries is prepared from alpine yallow herb through pulverizing, extracting in alcohol and then in ethyl acetate concentrating, dissolving in dichloromethane, extracting by dicarbonate, regulating pH, extracting, concentrating to obtain active component A, extracting the dregs by sodium hydroxide, regulating pH, extracting, concentrating to obtain active component B, proportional mixing A with B, and vacuum drying.
Description
Technical field
The present invention relates to a kind of preparation method of alpine yarrow herb effective parts preparation.
Background technology
Viral hepatitis, hepatic injury are the diseases of infringement human health, and wherein viral hepatitis is the global infectious disease of serious harm human health, patient's poor prognosis, and most patient transfers to chronic, may develop into liver cirrhosis etc.The hepatic injury that viral hepatitis causes is mainly mediated by the immune response reaction, behind the activated viral body immune system, produces primed lymphocyte and specific antibody, particularly virus specificity cell toxicity T cell.They not only can react with the body inner virus and be killed, and cause hepatic injury because of the surface of hepatocytes that is infected by the virus has virus antigen, cause hepatocellular degeneration swelling and necrosis.At present, very not satisfactory for the sick Chinese and western medicine curative effect of this class.For example, the Western medicine interferon is eliminated hepatitis virus certain curative effect, but undesirable through clinical effectiveness, can not kill virus, and also administration time is long, and expenses for medicine is higher.Each is different in the treatment viral hepatitis with aspect protecting the liver for the Chinese patent medicine class, and the Chinese medicine that has biases toward heat-clearing and toxic substances removing, and what have focuses on activating blood circulation to dissipate blood stasis, the nourishing the liver and kidney that has etc., and these medicines all respectively have its deficiency.Clinical clothes bitter cold medicine of a specified duration, but impairment of the spleen kidney reduce appetite, digestion and absorption.In addition, many medicines must carry out oxidation, decomposition, drainage in liver, and what have also can directly cause liver injury, and are unfavorable to the hepatopathy recovery from illness on the contrary.
The present invention is directed to the deficiency that in the Drug therapy hepatopathy, exists at present,, and on the basis of Chinese patent CN021182566, provide the preparation method of alpine yarrow herb effective parts preparation in conjunction with Chinese medicine and both length of national medicine theory.
Summary of the invention
The object of the invention is, the preparation method of the alpine yarrow herb effective parts preparation of development is to be raw material with the Herba Achilleae, the Herba Achilleae herb is pulverized, used ethanol extraction, promptly get the Herba Achilleae ethanol extract, the extractum ethyl acetate extraction, obtain ethyl acetate extract after concentrating, dissolve with dichloromethane; Or the Herba Achilleae ethanol extract directly dissolved with dichloromethane; Then the gained solute is extracted with sodium bicarbonate, transfer pH4-5 with hydrochloric acid, dichloromethane extraction concentrates, and can obtain the effective site I based on keto acid; With its residue sodium hydroxide extraction, transfer pH4-5 with hydrochloric acid, dichloromethane extraction concentrates, and can obtain the effective site II based on flavone; Then with resulting effective site I or II or I and II through vacuum drying, make oral dosage form and liquid dosage form with conventional method.Said preparation is used for the treatment of the oral medicine of viral hepatitis and all kinds of hepatic injury, and it is little to have dosage, and the curative effect height has no side effect through animal experiment and clinical observation, and the treatment total effective rate is 91.0%.
The preparation method of alpine yarrow herb effective parts preparation of the present invention, this method follow these steps to carry out:
A, at first the Herba Achilleae herb is ground into powder, the ethanol extraction with 60%-95% promptly get the Herba Achilleae ethanol extract, with the extractum ethyl acetate extraction, obtains ethyl acetate extract after concentrated, dissolves with dichloromethane, obtains the dichloromethane position; Or with the Herba Achilleae ethanol extract directly with dichloromethane dissolving, obtain the dichloromethane position;
B, again with the dichloromethane position with the extraction of 2%-20% sodium bicarbonate, obtain the sodium bicarbonate position, transfer pH4-5 with hydrochloric acid or sulphuric acid or acetic acid then, dichloromethane extraction or ethyl acetate extraction, concentrate, can obtain the effective site I based on keto acid, its residue is stand-by;
C, with the residue at dichloromethane position 2%-15% sodium hydroxide extraction, obtain the sodium hydroxide position, transfer pH4-5 with hydrochloric acid or sulphuric acid or acetic acid then, dichloromethane extraction or ethyl acetate extraction concentrate, and can obtain the effective site II based on flavone;
D, then with resulting effective site I or II or I and II through vacuum drying, make oral dosage form and liquid dosage form according to a conventional method.
Alpine yarrow herb effective parts of the present invention and preparation thereof, wherein the pharmacological properties of Herba Achilleae is:
The dry herb of Herba Achilleae Artemisia rupestris L..Seven, tap August, dry.10-50 centimetre of this product total length.Root and rhizome are cylindrical, and khaki is to taupe, and length is with minority short hairs root, and section is light yellow.Stem single or several, in the bending of rhizome place, diameter 1.5-3 centimetre, the close tomentellate of sprout and spray top, the bottom of old branch or branch is smooth, inapparent again stria, the surface is an aubergine often, section white, hollow.Function with cure mainly: heat-clearing and toxic substances removing, invigorating the stomach and promoting digestion, expelling wind and activating blood circulation.Be used for flu, allergy, food stagnation, snakebite, furuncle.
Herba Achilleae is the Uygur medicine medicinal herbs most in use, and bibliographical information Herba Achilleae herb contains chemical compounds such as flavonoid, keto acid class, aminoacid, glycoside, polysaccharide, volatile oil, polypeptide, alkaloid.We have analyzed the Herba Achilleae effective ingredient, and experimentatioies such as p53 and Bcl expression of gene when having carried out hepatoprotective effect, treatment autoallergic, antioxidation, the anti-allergic effects research of alpine yarrow herb effective parts preparation on this basis and having induced apoptosis of human hepatoma cell, and adopt electron paramagnetic resonance method detection alpine yarrow herb effective parts preparation to O
2 -°, the inhibitory action of OH °, be intended to illustrate the scientific meaning of this medicine disease preventing and treating.
The preparation method of alpine yarrow herb effective parts preparation of the present invention, the in vitro tests that the alpine yarrow herb effective parts preparation that utilizes this method to develop carries out is as follows:
The effective portion of Herba Achilleae 2.15 cells are to the inhibitory action of HbsAg, HbeAg and HBV DNA:
(1) the effective portion of Herba Achilleae is to the toxicity of 2.2.15 cell culture: the effective portion of Herba Achilleae adds in the 2.2.15 cell cultivated 8 days, was index with the cytopathy, two batches of empirical averages: median toxic concentration TC
50Be 426ug/ml, maximal non-toxic concentration TC
0Be 5ug/ml.
(2) the effective portion of Herba Achilleae in the 2.2.15 cell culture to HBsAg and the excretory inhibitory action of HBeAg: the effective portion of Herba Achilleae cultivated 8 days in the 2.2.15 cell, and maximal non-toxic concentration 5ug/ml does not have obvious inhibitory action to HBsAg, to HBeAg unrestraint effect.
(3) the effective portion of Herba Achilleae in the 2.2.15 cell culture to the inhibitory action of HBV DNA: the effective portion of Herba Achilleae cultivated 8 days in the 2.2.15 cell, and maximal non-toxic concentration 5ug/ml is 43.9 ± 8.7% to the average suppression ratio of HBV DNA; The lamivudine (3TC) of positive drug 1 μ M is 63.9 ± 0.8% to the suppression ratio of HBV DNA.
The effective portion of table 1. Herba Achilleae is to the inhibitory action of 2.2.15 cell to HBsAg, HBeAg and HBV DAN
Cytotoxicity (ug/ml) HBeAg HBsAg HBV DNA
TC
50 TC
0 1C
50(ug/ml) IC
50(ug/ml) IC
50(ug/ml)
426 125 >125 >125 >125
In vivo test is as follows:
Alpine yarrow herb effective parts in the duck body to the therapeutic effect of duck hepatitis B virus infection
Herba Achilleae AR is by the Antihepatitis medicament of institute of materia medica, Xinjiang development, for verifying its effect, carries out therapeutic test in duck hepatitis B virus infection duck body, observes it and whether suppresses DHB.An age in days Beijing duck intravenous injection DHB is adopted in experiment, begin a dosage group after 7 days to the oral Herba Achilleae AR3 of duck, first test 0.25,0.5,1.0g/kg, 1 day 2 times, administration 10 days (Bid * 10), second batch and the 3rd batch test improves dosage, is 1.0,2.0,4.0g/kg, 1 day 2 times, administration 10 days (Bid * 10).Observe medicine to toxicity of duck and the influence of the clear DHB DNA of Sanguis Anas domestica (DHBV-DNA), with the positive contrast medicine of lamivudine.
Experiment shows that 4.0g/kg is oral for the heavy dose of group of Herba Achilleae AR, 1 day 2 times 10 days, and avirulence.By the pairing statistical analysis, T10 shows repeatably statistical significance difference; Suppression ratio statistical analysis in groups, in second batch of experiment, T5, T10 and P3 all have the statistical significance difference, but in the 3rd batch of experiment, and the P value of T10<10% fails to reach<5% remarkable meaning.4.0g/kg group, the pairing statistical analysis in first experiment, after the administration the 5th, 10 day, all shows the statistical significance difference; Press suppression ratio statistical analysis in groups, T10 has the statistical significance difference.But two kinds of statistical analysis techniques in second batch and the 3rd batch of experiment all fail to show the statistical significance difference.2.0g/kg group, in second batch of experiment, the pairing statistical analysis of the 10th day (T10), the significance difference, but fail repetition.1.0g/kg group, the unrestraint effect.The lamivudine matched group has remarkable result, and illustrative experiment is credible.
Prompting: Herba Achilleae AR has therapeutic effect in the 4.0g/kg group to duck hepatitis B virus infection.
Conclusion:
1. alpine yarrow herb effective parts was cultivated 8 days in the 2.2.15 cell, the result, alpine yarrow herb effective parts is 43.9 ± 8.7% at maximal non-toxic concentration 5ug/ml to the average suppression ratio of HBV DNA, and the lamivudine (3TC) of positive drug 1 μ M is 63.8 ± 08%. to the suppression ratio of HBV DNA
2. the effective 4.0g/kg of portion of Herba Achilleae group, the pairing statistical analysis in first experiment, after the administration the 5th, 10 day, all shows the statistical significance difference; 2.0g/kg group, in second batch of experiment, the pairing statistical analysis of the 10th day (T10), the significance difference, but fail repetition.1.0g/kg group, the unrestraint effect.The lamivudine matched group has remarkable result, and illustrative experiment is credible.Prompting: Herba Achilleae AR has therapeutic effect in the 4.0g/kg group to duck hepatitis B virus infection.
The specific embodiment
Embodiment 1
A, at first the Herba Achilleae herb is ground into powder, the ethanol extraction with 60% promptly gets the Herba Achilleae ethanol extract, with the extractum ethyl acetate extraction, obtains ethyl acetate extract after concentrating, and the dissolving of reuse dichloromethane obtains the dichloromethane position;
B, the dichloromethane position is extracted with 2% sodium bicarbonate again, obtain the sodium bicarbonate position, transfer pH4-5 with hydrochloric acid then, use dichloromethane extraction, concentrate, can obtain the effective site I based on keto acid, its residue is stand-by;
C, with the residue at dichloromethane position 2% sodium hydroxide extraction, obtain the sodium hydroxide position, transfer pH4-5 with hydrochloric acid then, use dichloromethane extraction, concentrate, can obtain effective site II based on flavone;
D, then with resulting effective site I or II or I and II behind vacuum drying, promptly can be made into oral dosage form and liquid dosage form according to a conventional method.
Embodiment 2
A, at first the Herba Achilleae herb is ground into powder, the ethanol extraction with 95% promptly gets the Herba Achilleae ethanol extract, and the Herba Achilleae ethanol extract directly with the dichloromethane dissolving, is obtained the dichloromethane position;
B, the dichloromethane position is extracted with 20% sodium bicarbonate again, obtain the sodium bicarbonate position, transfer pH4-5 with sulphuric acid then, use ethyl acetate extraction, concentrate, can obtain the effective site I based on keto acid, its residue is stand-by;
C, with the residue at dichloromethane position 15% sodium hydroxide extraction, obtain the sodium hydroxide position, transfer pH4-5 with sulphuric acid then, use ethyl acetate extraction, concentrate, can obtain effective site II based on flavone;
D, then with resulting effective site I or II or I and II behind vacuum drying, promptly can be made into oral dosage form and liquid dosage form according to a conventional method.
Embodiment 3
A, at first the Herba Achilleae herb is ground into powder, the ethanol extraction with 80% promptly gets the Herba Achilleae ethanol extract, with the extractum ethyl acetate extraction, obtains ethyl acetate extract after concentrating, and the dissolving of reuse dichloromethane obtains the dichloromethane position;
B, the dichloromethane position is extracted with 12% sodium bicarbonate again, obtain the sodium bicarbonate position, transfer pH4-5 with acetic acid then, use dichloromethane extraction, concentrate, can obtain the effective site I based on keto acid, its residue is stand-by;
C, with the residue at dichloromethane position 10% sodium hydroxide extraction, obtain the sodium hydroxide position, transfer pH4-5 with acetic acid then, use dichloromethane extraction, concentrate, can obtain effective site II based on flavone;
D, then with resulting effective site I or II or I and II behind vacuum drying, promptly can be made into oral dosage form and liquid dosage form according to a conventional method.
Claims (1)
1, a kind of preparation method of alpine yarrow herb effective parts preparation is characterized in that pressing routine step and carries out:
A, at first the Herba Achilleae herb is ground into powder, the ethanol extraction with 60%-95% promptly get the Herba Achilleae ethanol extract, with the extractum ethyl acetate extraction, obtains ethyl acetate extract after concentrated, and the reuse dichloromethane dissolves, and obtains the dichloromethane position; Or with the Herba Achilleae ethanol extract directly with dichloromethane dissolving, obtain the dichloromethane position;
B, again with the dichloromethane position with the extraction of 2%-20% sodium bicarbonate, obtain the sodium bicarbonate position, transfer pH4-5 with hydrochloric acid or sulphuric acid or acetic acid then, dichloromethane extraction or ethyl acetate extraction, concentrate, can obtain the effective site I based on keto acid, its residue is stand-by;
C, with the residue at dichloromethane position 2%-15% sodium hydroxide extraction, obtain the sodium hydroxide position, transfer pH4-5 with hydrochloric acid or sulphuric acid or acetic acid then, dichloromethane extraction or ethyl acetate extraction concentrate, and can obtain the effective site II based on flavone;
D, then with resulting effective site I or II or I and II behind vacuum drying, promptly can be made into oral dosage form and liquid dosage form according to a conventional method.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2009138860A1 (en) * | 2008-05-16 | 2009-11-19 | Veritron Limited | Plant extract and its therapeutic use |
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2004
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2009138860A1 (en) * | 2008-05-16 | 2009-11-19 | Veritron Limited | Plant extract and its therapeutic use |
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