CN102391277A - Method for preparing high-purity rhinacanthin C - Google Patents
Method for preparing high-purity rhinacanthin C Download PDFInfo
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- CN102391277A CN102391277A CN2011103046751A CN201110304675A CN102391277A CN 102391277 A CN102391277 A CN 102391277A CN 2011103046751 A CN2011103046751 A CN 2011103046751A CN 201110304675 A CN201110304675 A CN 201110304675A CN 102391277 A CN102391277 A CN 102391277A
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- twig
- leaf
- plain
- bignose rhinacanthus
- purity
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Abstract
The invention discloses a method for preparing high-purity rhinacanthin C. The method comprises the following steps of: crushing a rhinacanthus nasutus material, performing ultrasonic extraction for 2 to 3 times by adding 80 to 90 percent methanol in an amount which is 6 to 10 times weight of the powder, reclaiming the reagent from the extract, adding kieselguhr for drying, filling the extract into a column, flushing the impurity by using ethanol, adding the solution into ethyl acetate for reflux extraction, separating the extract by using high-speed countercurrent chromatography, collecting the component according to a map, performing vacuum drying, and thus obtaining the high-purity rhinacanthin C. The method for preparing the rhinacanthin C is high in efficiency, short in period and high in yield; and the purity of the product is not less than 95 percent.
Description
Technical field
The present invention relates to the preparation method of the plain C of a kind of high purity Twig and leaf of Bignose Rhinacanthus, especially relate to a kind of method that adopts high-speed countercurrent chromatography to prepare the plain C of high purity Twig and leaf of Bignose Rhinacanthus.
Background technology
The plain C of Twig and leaf of Bignose Rhinacanthus (Rhinacanthin C) is a naphthoquinones class material, yellow oil, no sharp melting point, molecular formula C
25H
30O
5, molecular weight 410.51.Modern pharmacological research shows that it has following pharmacological action: (1) cytotoxic activity is respectively KB (6.26), P388 (0.26), A-549 (0.35), HT-29 (0.68), HL-60 (0.68) to the ED50 (mcg/ml) of following cell strain; (2) antiplatelet aggregative activity, 100% suppresses the gathering of arachidonic acid (100 μ M) inductive rabbit platelet during these article 100 mcg/ml; 75.2% suppresses collagen (10 mcg/ml) inductive rabbit platelet assembles; (3) significantly suppress human-like and mouse type cytomegalovirus (CMV), EC
50(mcg/ml) is 0.02 (human-like) and 0.57 (mouse type), and selectivity index is 28 and 4.6.
Twig and leaf of Bignose Rhinacanthus
Rhinacanthus nasutus(L.) how Lindau for Acanthaceae Twig and leaf of Bignose Rhinacanthus platymiscium Twig and leaf of Bignose Rhinacanthus, is used as medicine with dry aerial parts, branches and leaves.Main product in Guangxi, remote mountains, ground such as Guangdong, Yunnan, be the valuable ingredient of traditional Chinese medicine that Miao Jiang secretly hands down, because of its effect just like glossy ganoderma, floral white again, the lip type is given birth on axil or branch top, forms the white crane that crowd's exhibition is circled in the air, so " Twig and leaf of Bignose Rhinacanthus ".Its flavor is sweet, warm in nature, have moistening the lung and relieve the cough, relieving asthma eliminate the phlegm, effects such as heat-clearing is soothing the liver, dampness removing is antipruritic, astringing to arrest bleeding, the diseases such as cough that produced when being used to treat lung-heat type cough, pulmonary tuberculosis and receiving chill.Modern clinical research shows; Twig and leaf of Bignose Rhinacanthus can be treated coronary heart disease, hypertension, mellitus; Also can be to antianginal, improving electrocardiogram(ECG, blood fat, improving nail fold microcirculation and ocular fundus arteriosclerosis and the aspect such as sexually revise certain curative effect is all arranged, and non-evident effect.
Research to Twig and leaf of Bignose Rhinacanthus at present mainly concentrates on GAP (GAP) and Quality Control Technology aspect, but the effective constituent of Twig and leaf of Bignose Rhinacanthus and the research of index property composition aspect relatively are short of.Do not see the method that adopts the plain C of high-speed countercurrent chromatography purifying Twig and leaf of Bignose Rhinacanthus as yet through retrieval.
Summary of the invention
The objective of the invention is to overcome the defective of prior art, efficient, the fast preparation method of the plain C of a kind of high purity Twig and leaf of Bignose Rhinacanthus is provided.
The objective of the invention is to realize through following technical scheme:
Get the Twig and leaf of Bignose Rhinacanthus pulverizing medicinal materials, add 6-10 times of 80-90% methyl alcohol supersound extraction 2-3 time, extracting solution reclaims reagent and adds the zeyssatite drying; The dress post; Earlier use alcohol flushing impurity, be added to refluxing extraction in the ETHYLE ACETATE again, extracting solution separates with high speed adverse current chromatogram after concentrating again; Collect composition according to collection of illustrative plates, concentrate drying promptly gets the plain C of high purity Twig and leaf of Bignose Rhinacanthus.
The preparation method of the plain C of said high purity Twig and leaf of Bignose Rhinacanthus; It is characterized in that the isolating solvent systems of described high speed adverse current chromatogram is sherwood oil, ETHYLE ACETATE, methyl alcohol, water; Blending ratio is 2-5:3-7:4-6:3, gets to go up mutually and does moving phase mutually, and phase mutually fixes down.
Positively effect of the present invention is: adopting high-speed countercurrent chromatography to separate, is a kind of liquid liquid distribution chromatography, and isolating sample is not produced dead absorption, and reagent dosage is few, and can reclaim and re-use, and the single preparation amount is big, and the cycle is short, can prepare continuously.
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to the following example.
Embodiment
Embodiment 1:
With the Twig and leaf of Bignose Rhinacanthus pulverizing medicinal materials, get 2kg, add 10 times of 90% methyl alcohol supersound extraction 2 times; Each 1 hour, extracting solution recovery reagent added 200g zeyssatite and mixes oven dry thoroughly; The dress post, earlier with alcohol flushing impurity to there not being flavone component, pour in the 500ml ETHYLE ACETATE zeyssatite into refluxing extraction 2 times again; Collect the extracting solution concentrating under reduced pressure, get medicinal extract.Get sherwood oil, ETHYLE ACETATE, methyl alcohol, water, in separating funnel, mix, fully after the layering, take off and fill with the high speed adverse current chromatogram spiral tube mutually, rotate main frame by 2:3:4:3; Speed adjustment is 700rpm, pumps into to do moving phase mutually, treat running balance after, flow rate regulation is 2ml/min; Dissolve medicinal extract with moving phase,, collect composition, reclaim reagent according to collection of illustrative plates by the sampling valve sample introduction; Concentrate drying gets the plain C of 1.4g Twig and leaf of Bignose Rhinacanthus, detects content 95.4% through HPLC.
Embodiment 2:
With the Twig and leaf of Bignose Rhinacanthus pulverizing medicinal materials, get 2kg, add 6 times of 80% methyl alcohol supersound extraction 3 times; Each 1 hour, extracting solution recovery reagent added 250g zeyssatite and mixes oven dry thoroughly; The dress post, earlier with alcohol flushing impurity to there not being flavone component, pour in the 500ml ETHYLE ACETATE zeyssatite into refluxing extraction 2 times again; Collect the extracting solution concentrating under reduced pressure, get medicinal extract.Get ETHYLE ACETATE, propyl carbinol, water, in separating funnel, mix, fully after the layering, take off and fill with the high speed adverse current chromatogram spiral tube mutually, rotate main frame by 5:7:6:3; Speed adjustment is 900rpm, pumps into to do moving phase mutually, treat running balance after, flow rate regulation is 2ml/min; Dissolve medicinal extract with moving phase simultaneously,, collect composition, reclaim reagent according to collection of illustrative plates by the sampling valve sample introduction; Concentrate drying gets the plain C of 1.6g Twig and leaf of Bignose Rhinacanthus, detects content 98.1% through HPLC.
Claims (2)
1. the preparation method of the plain C of high purity Twig and leaf of Bignose Rhinacanthus is characterized in that: get the Twig and leaf of Bignose Rhinacanthus pulverizing medicinal materials, add 6-10 times of 80-90% methyl alcohol supersound extraction 2-3 time; Extracting solution reclaims reagent and adds the zeyssatite drying, and the dress post is used earlier alcohol flushing impurity; Be added to refluxing extraction in the ETHYLE ACETATE again; Separate with high speed adverse current chromatogram after extracting solution concentrates again, collect composition according to collection of illustrative plates, concentrate drying promptly gets the plain C of high purity Twig and leaf of Bignose Rhinacanthus.
2. the preparation method of the plain C of high purity Twig and leaf of Bignose Rhinacanthus according to claim 1; It is characterized in that the isolating solvent systems of described high speed adverse current chromatogram is sherwood oil, ETHYLE ACETATE, methyl alcohol, water; Blending ratio is 2-5:3-7:4-6:3, gets to go up mutually and does moving phase mutually, and phase mutually fixes down.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103046751A CN102391277A (en) | 2011-10-10 | 2011-10-10 | Method for preparing high-purity rhinacanthin C |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103046751A CN102391277A (en) | 2011-10-10 | 2011-10-10 | Method for preparing high-purity rhinacanthin C |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102391277A true CN102391277A (en) | 2012-03-28 |
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|---|---|---|---|
| CN2011103046751A Pending CN102391277A (en) | 2011-10-10 | 2011-10-10 | Method for preparing high-purity rhinacanthin C |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017006407A1 (en) * | 2015-07-04 | 2017-01-12 | 株式会社Ａｏｂ慧央グループ | Nerve cell death inhibitor, anti-alzheimer's disease agent, brain hypofunction inhibitor, drug or food having anti-alzheimer's disease effect or brain hypofunction-inhibiting effect, and method for producing nerve cell death inhibitor |
| CN115385795A (en) * | 2022-10-11 | 2022-11-25 | 广西中医药大学赛恩斯新医药学院 | Preparation method and application of rhinacanthus nasutus and ganoderma naphthoquinone monomer rhinacanthin-C |
-
2011
- 2011-10-10 CN CN2011103046751A patent/CN102391277A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017006407A1 (en) * | 2015-07-04 | 2017-01-12 | 株式会社Ａｏｂ慧央グループ | Nerve cell death inhibitor, anti-alzheimer's disease agent, brain hypofunction inhibitor, drug or food having anti-alzheimer's disease effect or brain hypofunction-inhibiting effect, and method for producing nerve cell death inhibitor |
| JPWO2017006407A1 (en) * | 2015-07-04 | 2017-09-21 | 株式会社Ａｏｂ慧央グループ | Neuronal cell death inhibitor, anti-Alzheimer's disease agent, anti-brain function-lowering agent, drug or food having anti-Alzheimer's disease action or anti-brain function-lowering action, and method for producing neuronal cell death inhibitor |
| CN107708717A (en) * | 2015-07-04 | 2018-02-16 | 株式会社奥碧慧央集团 | Nerve cell apoptosis inhibitor, the agent of anti-Alzheimer disease, anti-Aging agent, the pharmaceuticals or the manufacture method of food and nerve cell apoptosis inhibitor with the effect of anti-Alzheimer disease or the effect of anti-Aging |
| CN115385795A (en) * | 2022-10-11 | 2022-11-25 | 广西中医药大学赛恩斯新医药学院 | Preparation method and application of rhinacanthus nasutus and ganoderma naphthoquinone monomer rhinacanthin-C |
| CN115385795B (en) * | 2022-10-11 | 2023-11-17 | 广西中医药大学赛恩斯新医药学院 | Preparation method and application of Rhinacanthus nasuta (L.) kurz naphthoquinone monomer Rhinacanthin-C |
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Application publication date: 20120328 |