CN1299675C - Composition of cupresulflavone and its preparation - Google Patents
Composition of cupresulflavone and its preparation Download PDFInfo
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- CN1299675C CN1299675C CNB2004100149807A CN200410014980A CN1299675C CN 1299675 C CN1299675 C CN 1299675C CN B2004100149807 A CNB2004100149807 A CN B2004100149807A CN 200410014980 A CN200410014980 A CN 200410014980A CN 1299675 C CN1299675 C CN 1299675C
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Abstract
本发明属天然药物制备方法技术领域，本发明所述抗肿瘤干香柏黄酮组合物，由柏科植物干香柏的枝叶部分提取分离，干香柏总黄酮含量为50—65%，儿茶素含量为25—40%；其制备方法为取干香柏水提液，调pH至9—10、过大孔吸附树脂柱，含水醇洗脱、正丁醇萃取、浓缩。干香柏总黄酮抗肿瘤活性提高，吸湿性降低，可制备成治疗肿瘤的药物。The invention belongs to the technical field of natural medicine preparation methods. The anti-tumor dried cedar flavonoid composition of the invention is extracted and separated from the branches and leaves of the dried cedar of the Cupressaceae plant. The total flavonoid content of the dried cedar is 50-65%. The element content is 25-40%; the preparation method is to take the dried cedar cedar water extract, adjust the pH to 9-10, pass through a macroporous adsorption resin column, elute with water-containing alcohol, extract with n-butanol, and concentrate. The anti-tumor activity of the total flavonoids of dried cedar is improved, and the hygroscopicity is reduced, so it can be prepared as a drug for treating tumors.
Description
One, technical field:
The invention belongs to natural drug preparation method technical field, be specifically related to antineoplastic flavone composition in the dry-fragrant cypress branch and leaf and preparation method thereof.
Two, background technology:
Cupressaceae plant dry-fragrant cypress is China's commerical tree species, and material is hard, and structure is fine and closely woven, and fragrance is arranged, and can supply material such as building, papermaking, utensil, furniture.Be distributed in provinces such as Yunnan, Sichuan as the reproducting tree species of checking winds and fixing drifting sand, conserving water and soil.It there is no report as medicinal usage and chemical analysis.
China's Cupressaceae floristics is more, about 20 kinds of hyoscine.In its branch and leaf and the heartwood, generally contain compositions such as volatile oil, flavone, lignanoid, anthraquinone and terpenoid, China is simple water decoction as medicinal Cupressaceae plant among the people, is used for the treatment of flu, has a headache and fever, disease such as haematemesis, dryness of the intestine constipation.
Three, summary of the invention
The problem that the present invention need solve is never as the high compositions of a kind of anti-tumor effective component flavones content of development in the medicinal dry-fragrant cypress branch and leaf, a kind of determined curative effect is provided, steady quality, safe and effective, a kind of new plant origin antitumor natural drug with low cost, the effective site flavones content improves, and helps reducing the dose of clinical use.Impurity reduces not only can improve the hygroscopicity that Chinese patent medicine often has, and effective component content is improved, drug effect is obvious, can not produce the side effect that some impurity causes, the technical problem to be solved in the present invention also relates to the high preparation of compositions technology of a kind of anti-tumor effective component flavones content of development, and this method can improve active component content, remove a large amount of non-flavonoid impurity, simultaneously repeatability, good stability to be arranged, and the yield height of raw material, to be fit to suitability for industrialized production.
For solving the problems of the technologies described above, the present invention has studied and defined following technical scheme.
A kind of antineoplastic dry-fragrant cypress flavone composition, by the isolating dry-fragrant cypress flavonid composition of the branch and leaf extracting section of Cupressaceae plant dry-fragrant cypress, in the said composition, the dry-fragrant cypress general flavone content is 25-40% for the 50-65% catechin content.And it is prepared into tablet, capsule, drop pill, soft capsule, powder pin or the large and small injection of dry-fragrant cypress total flavones.
The flavone composition preparation method of antitumor dry-fragrant cypress:
Dry-fragrant cypress water intaking extracting solution adds caustic lye of soda and transfers PH to 9-10; Get alkaline filtrate and cross macroporous adsorptive resins, wash with water earlier to effluent neutrality, reuse adds the ethanol of 40-95% concentration and washes post; Collect eluent and concentrate concentrate water liquid n-butanol extraction; Concentrate n-butanol extraction solution, get dry-fragrant cypress flavone powder.In the gained dry-fragrant cypress flavone powder, the dry-fragrant cypress general flavone content is 50-70%, and catechin content is 25-40%.Dry-fragrant cypress flavone powder can mix with pharmaceutically acceptable carrier, and dosage form is tablet, capsule, drop pill, soft capsule, powder pin or large and small injection.
The dry-fragrant cypress flavone composition that the present invention makes, owing to adopted the macroporous adsorption resin technology in the modernization of Chinese medicine technology, the content of active component is wherein improved, thereby improved drug effect, and a large amount of non-flavonoid impurity have been removed, both solve the big problem of moisture absorption that Chinese patent medicine often has, reduced side effect again.
In the dry-fragrant cypress flavone composition that employing the present invention makes, content of total flavone is 50-65%, the raw material standard that meets Chinese medicine two classes of People's Republic of China's " law of medicine management " regulation, clear and definite its main component is the anti-tumor active ingredient catechin, measure by high-efficient liquid phase technique, the content of catechin accounts for the 25-40% of dry-fragrant cypress flavone composition.
The dry-fragrant cypress flavone composition that the present invention makes has carried out antitumor activity screening MODEL C CLT and CDC25 test respectively.In CCLT test, 2500-4000/people from hole nonsmall-cell lung cancer A549 cell strain is inoculated on the ELISA Plate, grow into 24 hours after, add the 0.1mg/ml sample and cultivate again and measure living cells quantity after 48 hours.Antitumor CCLT experimental result shows that the dry-fragrant cypress flavone composition is 72.8% to the suppression ratio of growth of tumour cell, median effective dose (IC
50) being: 0.069mg/ml selection index (SI) is 8.62 ± 0.93; In the CDC25 test, cdc25 gene expression molecular weight is the phosphoprotein phosphatase p80cdc25 of 80KDa, it is the activity factor of main cell division cycle gene cdc2, therefore suppress the cdc25 expression of gene, can suppress tumour cell division, thereby by the anti-tumor activity of test sample to enzyme CDC25 activity influence test sample, the active suppression ratio of dry-fragrant cypress flavone composition antitumor CDC25 is 63.6%, median effective dose (IC
50) be 0.096mg/ml.People's nonsmall-cell lung cancer A549 cell strain is provided by the institute of materia medica, Shanghai, and recombination human source phosphoprotein phosphatase (CDC25) is provided by Bayer company.The dry-fragrant cypress flavone composition that the present invention makes can be prepared into the medicine of treatment tumor.
The dry-fragrant cypress flavone composition extracts with branch and leaf, and abundant raw material and cost are low.In addition, the present invention has overcome the defective of Chinese medicine traditional handicraft, macroporous adsorption resin technology in the utilization modernization of Chinese medicine technology, a kind of content height, definite ingredients, quality controllable, drug effect is definite, side effect is little dry-fragrant cypress flavone composition and preparation method thereof are provided, have been a kind of two class Chinese medicine antitumor of high-efficiency low-toxicity.Preparation technology of the present invention by multiple authentication, proves that its repeatability, stability are all good, and the yield height of raw material is fit to suitability for industrialized production.
Four, the specific embodiment
Among the embodiment, used extraction water is a tap water, and used ethanol is pharmaceutical grade, and sodium hydroxide and n-butyl alcohol are technical grade.The dry-fragrant cypress branch and leaf part medical material place of production is Kunming, Yunnan; Macroporous resin is available from Chemical Plant of Nankai Univ.; The reference substance rutin of measuring general flavone content is provided by the national drug biological products assay institute; The reference substance catechin of measuring catechin content is available from SIGMA company.
Measure the method for general flavone content in the raw material, according to the colorimetry among 2000 editions appendix VB of Chinese Pharmacopoeia.
Measure the method for catechin content in the raw material, according to the high performance liquid chromatography among 2000 editions appendix VID of Chinese Pharmacopoeia.Chromatographic condition is: with octadecylsilane chemically bonded silica is filler; Acetonitrile-water (20: 80) is a mobile phase; The detection wavelength is 254nm; Number of theoretical plate calculates by catechin should be not less than 2500.
Embodiment one:
Get the aerial parts 60kg of dry-fragrant cypress, be ground into coarse powder, put into extraction pot; Add entry 360L reflux, extract, 3 times respectively, each 2 hours; Extracting solution leaves standstill after adding caustic lye of soda accent PH to 9.0, the filtering precipitation; Filtrate is crossed the HP-20 macroporous adsorptive resins, adds deionized water and is eluted to the effluent clarification and is neutrality; The ethanol of adding 50% is washed post, collects eluent and concentrated, adds water 60L dissolving again, filtration; Filtrate adds the 30L n-butanol extraction respectively 3 times, merges alcoholic solution; Vacuum decompression concentrates alcoholic solution to doing routinely, and drying obtains yellow dry-fragrant cypress flavone raw material 1.0kg.
Through high effective liquid chromatography for measuring: general flavone content is 59% in the above-mentioned experiment gained dry-fragrant cypress flavone raw material, and antitumor main component catechin content is 36% in its raw material.
Embodiment two:
Get the branch and leaf part 150kg of dry-fragrant cypress, be ground into the section of 2-3cm, put into extraction pot; Add entry 900L reflux, extract, 3 times respectively, each 2 hours; Extracting solution leaves standstill after adding caustic lye of soda accent PH to 9.0; The filtering precipitation; Filtrate is crossed the HD-2025 macroporous adsorptive resins, adds deionized water and is eluted to the effluent clarification and is neutrality; The ethanol of adding 75% is washed post, collects eluent and concentrated, is adding water 75L dissolving, filtration.Filtrate adds the 75L n-butanol extraction respectively 3 times, merges alcoholic solution.The concentrating under reduced pressure alcoholic solution is to doing, and drying obtains yellow dry-fragrant cypress flavone powder 1.8kg.
Through high effective liquid chromatography for measuring: general flavone content is 55% in this dry-fragrant cypress flavone powder stock, and antitumor main component catechin content is 33% in its raw material.
Claims (4)
1, a kind of dry-fragrant cypress extractive of general flavone, it is characterized in that: the branch and leaf extracting section by Cupressaceae plant dry-fragrant cypress is separated, wherein, dry-fragrant cypress total flavones amount is 50-65%, catechin content is 25-40%, and it is to be prepared by following method: the dry-fragrant cypress aqueous extract, transfer pH to 9-10, get alkaline filtrate and cross macroporous adsorbent resin, wash with water earlier to effluent and be neutral; The ethanol elution of reuse 40-95% concentration is collected eluent and concentrated; Concentrate concentrates butanol extraction liquid with the water dissolution n-butanol extraction, gets the dry-fragrant cypress extractive of general flavone.
2, the method for preparation dry-fragrant cypress extractive of general flavone according to claim 1 is characterized in that carrying out according to the following steps: the dry-fragrant cypress aqueous extract, and accent pH to 9-10 gets alkaline filtrate and crosses macroporous adsorbent resin, washes with water earlier to effluent to be neutral; The ethanol elution of reuse 40-95% concentration is collected eluent and concentrated; Concentrate water liquid n-butanol extraction concentrates butanol extraction liquid, gets the dry-fragrant cypress extractive of general flavone.
3, dry-fragrant cypress extractive of general flavone according to claim 1 is characterized in that being prepared into tablet, capsule, drop pill, soft capsule, powder pin or big small-volume injection dosage form.
4, the purposes of dry-fragrant cypress extractive of general flavone according to claim 1 in the medicine of preparation treatment tumor.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100149807A CN1299675C (en) | 2004-05-24 | 2004-05-24 | Composition of cupresulflavone and its preparation |
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| CNB2004100149807A CN1299675C (en) | 2004-05-24 | 2004-05-24 | Composition of cupresulflavone and its preparation |
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| CN1583004A CN1583004A (en) | 2005-02-23 |
| CN1299675C true CN1299675C (en) | 2007-02-14 |
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| CNB2004100149807A Expired - Fee Related CN1299675C (en) | 2004-05-24 | 2004-05-24 | Composition of cupresulflavone and its preparation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962665B (en) * | 2006-12-01 | 2011-05-18 | 大连医科大学 | Extraction method of antineoplastic composition bhang flavone A from bhang |
| CN101502536B (en) * | 2008-02-10 | 2012-05-02 | 薛永新 | Cedar total flavone and preparation method and medical application thereof |
| CN110051682B (en) * | 2018-01-18 | 2022-01-18 | 复旦大学 | Application of polysaccharide of thuja in preparation of medicine for preventing and treating viral acute lung injury |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401380A (en) * | 2002-09-05 | 2003-03-12 | 南京大学 | Anti-gout composition and preparing process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1401380A (en) * | 2002-09-05 | 2003-03-12 | 南京大学 | Anti-gout composition and preparing process thereof |
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