CN102119947A - Preparation method and application of carthamus tinctorius L. active ingredient - Google Patents
Preparation method and application of carthamus tinctorius L. active ingredient Download PDFInfo
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- CN102119947A CN102119947A CN 201110059032 CN201110059032A CN102119947A CN 102119947 A CN102119947 A CN 102119947A CN 201110059032 CN201110059032 CN 201110059032 CN 201110059032 A CN201110059032 A CN 201110059032A CN 102119947 A CN102119947 A CN 102119947A
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Abstract
The invention provides a preparation method and application of a carthamus tinctorius L. active ingredient. The method is characterized by obtaining the active ingredient after heating and extracting the carthamus tinctorius L. medicinal material, concentrating the extract, using a reversed phase column for separation, carrying out elution and concentrating and drying the eluent. The carthamus tinctorius L. active ingredient provided by the invention can be applied to preparing the medicaments for treating and preventing cardiovascular diseases. The preparation method is reasonable in design and has the beneficial effects of quickly and accurately obtaining the active ingredient and more easily controlling the quality of the medicaments in production.
Description
Technical field
The invention belongs to the field of Chinese medicines, relate to the preparation method and the medical usage thereof that from Flos Carthami, extract active component.
Background technology
Cardiovascular disease is first killer of harm humans health, in recent years, along with the variation of China's population senescence and people's work, life, dietary structure and environment etc., the incidence rate of cardiovascular and cerebrovascular diseases such as coronary heart disease also increases year by year, and the people's physical and mental health in serious threat.In the natural product many active substances have resist myocardial ischemia, anoxia functions, some of them have been developed to treatment coronary heart disease and anginal new drug.Thereby from natural product, seek have resist myocardial ischemia, the active substance of anoxia physiologically active, be find, one of effective way of developing new drug.China's medicinal organism resource is very abundant, and its biological active substances is research and finds new drug guide chemicals, the natural treasure-house of developing new drug.At present, China extracts active substance from natural product, be used to be developed to treatment coronary heart disease, safety is good, toxicity is low new drug also seldom, from natural product, extract active substance, be developed to have and resist myocardial ischemia, be used for the treatment of coronary heart disease and anginal new drug, have significant application value and wide development prospect.
Flos Carthami is the tubular flower of feverfew Flos Carthami Carthamus tinctorius L..Nature and flavor are warm in nature, and acrid in the mouth has the effect of the latus rectum of invigorating blood circulation, eliminating stasis to stop pain.Contain Carthamus yellow (Safflor yellow), saffloside (Carthamin), 15 α, 20 beta-dihydroxies-Δ 4-pregnene-3-ketone (15 α, 20 β-Dihydroxy-Δ 4-pregnen-3-one), luteolin-7-glucoside (Luteolin-7-glucoside), carthamone (carthamone), neocarthamin (neo-cqrthamin), ribosidoadenine (adenosine), flavochrome (safflor yellow A), nimbecetin, Quercetin and nimbecetin-3-glucoside, Quercetin-3-glucoside, square rafter skin element-7-glucoside, Shan Nai Fen – 3-rutinoside and rutin (rutin), chemical compounds such as Flos Carthami polysaccharide.
Modern pharmacological research shows: Flos Carthami water extract and Flos Carthami water soluble mixt-Carthamus yellow have the effect of coronary blood flow increasing and myocardial nutrition blood flow, cause on the animal model of expeirmental myocardial ischemia or myocardial infarction rabbit, rat, dog etc., Flos Carthami and preparation thereof all have antagonism in various degree.Flos Carthami can make the rat or the rabbit acute myocardial ischemia that cause because of pituitrin that obvious protective effect is arranged; Can make repeatedly of short duration blocking-up coronary flow cause the degree of anesthetized dog acute myocardial ischemia obviously to alleviate; scope is dwindled; decreased heart rate; and the edge in protection acute myocardial infarction district; dwindle infarction size and reduce the amplitude that the marginal zone ECG ST section is raised, thereby improve the supply-demand relationship of ischemic myocardium oxygen.Flos Carthami has and suppresses the effect of the inductive rabbit platelet aggregation of ADP very significantly, and the accumulative platelet of ADP is also had very significantly depolymerisation.Flos Carthami still can obviously prolong plasma in rabbit recalcification time, prothrombin time and clotting time.Show that it can influence in the body and external blood coagulation system simultaneously.In addition, safflower oil has the blood fat reducing effect.Flos Carthami has above obvious pharmacological action to cardiovascular system, therefore, isolates active component from Flos Carthami, and the modern Chinese medicine of developing the treatment cardiovascular disease has great importance.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of Flos Carthami active component, realize by following steps: flos carthami is added ethyl acetate and ethanol, and heating extraction gets extracting solution, and extracting solution is condensed into extractum, and itself and silica gel mixed sample, with normal phase silicagel column it is separated, at first use petroleum ether and ethyl acetate, get eluent I as mobile phase, abandon it, use chloroform and methanol then instead as mobile phase, get eluent II, will get sample behind the eluent II concentrate drying; Continue to separate the sample that obtains with preparative liquid chromatography; The separation condition of preparative hplc: chromatographic column is a semi-preparative column, and mobile phase is water and acetonitrile, gradient elution.
Preferably, Flos Carthami active component preparation method of the present invention, realize by following steps: flos carthami is added ethyl acetate and the ethanol that volume ratio is 1:1, reflux 1 hour, extract 2 times, merging filtrate gets extracting solution, extracting solution is condensed into extractum, and itself and silica gel are mixed sample, it is separated with normal phase silicagel column, be that the petroleum ether of 50:1 and ethyl acetate are as eluant at first with volume ratio, eluent I, abandon it, use chloroform that volume ratio is 10:1 and methanol then instead as eluant, get eluent II, will get the sample crude product behind the eluent II concentrate drying; Continue separation with preparative liquid chromatography and obtain sample; The separation condition of preparative hplc: chromatographic column is preparative column ZORBAX SB C
18; 9.4mm
250mm, 5
, mobile phase is water A and acetonitrile B, the gradient elution program is as follows: 0min, 30% B, 18 min, 40%B; Flow velocity is 3 ml/min, and flow velocity is 3ml/min, and column temperature is a room temperature; Separate through preparative liquid chromatography, collect solution in 6.7 ~ 10.2min time period, solution obtains active component behind concentrate drying.
A further object of the present invention provides the application of described active component in preparation treatment and angiocardiopathy preventing medicine.Prove that through pharmacological evaluation Flos Carthami active component provided by the invention has the certain protection effect to myocardial cell.
Flos Carthami active component provided by the invention adds the adjuvant of accepting on the pharmaceutics as active component, makes preparation according to the preparation method of the preparation of putting down in writing on the pharmaceutics.
Described preparation comprises injection, drip liquid, injectable powder, granule, tablet, electuary, powder, oral liquid, sugar coated tablet, film coated tablet, enteric coated tablet, capsule, hard capsule, soft capsule, sucks agent, granule, pill, unguentum, sublimed preparation, spray, drop pill, disintegrating agent, oral cavity disintegration tablet, micropill etc.
Beneficial effect of the present invention is: the preparation method that provides is reasonable in design, can obtain effective ingredient rapidly and accurately, is easier to the quality control of medicine aborning.The Flos Carthami active component of acquisition prepared according to the methods of the invention can be in the application in preparation treatment and the angiocardiopathy preventing medicine.
The specific embodiment
Further describe flesh and blood of the present invention and beneficial effect below in conjunction with embodiment, this embodiment only is used to the present invention is described but not limitation of the present invention.
The preparation of embodiment one Flos Carthami active component
Flos carthami is added ethyl acetate and ethanol, heating extraction gets extracting solution, extracting solution is condensed into extractum, and itself and silica gel are mixed sample, it is separated with normal phase silicagel column, at first use petroleum ether and ethyl acetate as mobile phase, get eluent I, abandon it, use chloroform and methanol then instead as mobile phase, get eluent II, will get sample behind the eluent II concentrate drying; Continue to separate the sample that obtains with preparative liquid chromatography; The separation condition of preparative hplc: chromatographic column is a semi-preparative column, and mobile phase is water and acetonitrile, gradient elution.Collect solution in the 6.7-10.2min time period, obtain active component behind the concentrate drying.
The preparation of embodiment two Flos Carthami active components
Get flos carthami 250g, adding volume ratio is 1:1 ethyl acetate and ethanol, and reflux 1 hour is extracted 2 times, filtrate merge extracting solution.Extracting solution is condensed into extractum, and itself and silica gel mixed sample, with normal phase silicagel column it is separated, be that the petroleum ether of 50:1 and ethyl acetate are as eluant at first with volume ratio, eluent I, abandon it, use chloroform that volume ratio is 10:1 and methanol then instead as eluant, get eluent II, will get sample behind the eluent II concentrate drying; Continue to separate the sample that obtains with preparative liquid chromatography: the separation condition of preparative hplc: chromatographic column is preparative column (ZORBAX SB C
18; 9.4mm
250mm, 5
), mobile phase is water A and acetonitrile B, the gradient elution program is as follows: 0min, 30% B, 18 min, 40%B; Flow velocity is 3 ml/min, and column temperature is a room temperature; Separate through preparative liquid chromatography, collect solution in 6.7 ~ 10.2min time period, solution obtains active component behind concentrate drying.
The preparation of embodiment three dropping pill formulations
Get Flos Carthami active component 0.5g and 10.5g Polyethylene Glycol-20000 mix homogeneously, heating and melting moves in the drop pill drip irrigation behind the change material, and in ℃ liquid paraffin of medicine liquid droplet to 6 ~ 8, oil removing makes 400 of drop pill.
The preparation of embodiment four lyophilized injectable powders
Get Flos Carthami active component 0.5g, glucose 4.5g, sodium thiosulfate 0.9g and distilled water 1000ml, behind the said components mix homogeneously, 400 of packing, lyophilization, promptly.
The active appraisal experiment of embodiment five Flos Carthami components
1. the Flos Carthami component is to H
2O
2The protective effect of injury of myocardium cell
In vitro culture H
9C
2Myocardial cell, culture fluid are that DMEM (high sugar)+10%FBS (G)+1% non essential amino acid+0.1% pair is anti-.The trophophase cell of taking the logarithm places on the 96 porocyte culture plates, behind constant temperature culture 24 h, adds 200 μ mol/mL H
2O
2Injury of myocardium cell 30 min, the Flos Carthami component that adds final concentration again and be 50 μ g/mL is hatched 24 h, adopts mtt assay to measure cell viability.The result shows that this component is to H
2O
2The protective rate of injury of myocardium cell is 13.8%.
2. the Flos Carthami component is to the protective effect of hypoxia-reoxygenation induced injured myocardium cell
In vitro culture H
9C
2Myocardial cell, culture fluid are that DMEM (high sugar)+10%FBS (G)+1% non essential amino acid+0.1% pair is anti-.The trophophase cell of taking the logarithm places on the 96 porocyte culture plates, behind constant temperature culture 24 h, cultivates 6 h in the anoxia cell.After anoxia finished, taking out the Tissue Culture Plate adding was the Flos Carthami component of 50 μ g/mL through the final concentration of sugar-free Hank ' s dilution, is hatching 6 h under normal condition of culture, gets cell culture supernatant and measures lactic acid dehydrogenase (LDH) content.The result shows that this component is 9.4% to the myocardial cell protection rate of anoxia reoxygenation injury.
Claims (5)
1. the preparation method of a Flos Carthami active component, it is characterized in that, obtain by following steps: flos carthami is added ethyl acetate and the ethanol that volume ratio is 1:0.8-1.2, reflux 0.8-1.2 hour, extract 1-3 time, merging filtrate gets extracting solution, and extracting solution is condensed into extractum, uses dissolve with ethanol extractum, and itself and silica gel mixed sample, with normal phase silicagel column it is separated, at first with volume ratio be the petroleum ether of 47-53:1 and ethyl acetate as eluant, eluent I, abandon it, use volume ratio then instead and be 8-13:1 chloroform and methanol as eluant, eluent II, will be behind the eluent II concentrate drying sample; Continue to separate the sample that obtains with preparative liquid chromatography; The separation condition of preparative hplc: chromatographic column is a semi-preparative column, and mobile phase is water and acetonitrile, and gradient elution, flow velocity are 2.8-3.2ml/min, and column temperature is a room temperature.
2. the preparation method of a kind of Flos Carthami active component according to claim 1 is characterized in that, wherein the semi-preparative column condition is ZORBAX SB C
18; 9.4mm
250mm, 5
, mobile phase is water A and acetonitrile B, the gradient elution program is as follows: 0min, 30% B, 18 min, 40%B; Flow velocity is 3 ml/min, and column temperature is a room temperature; Separate through preparative liquid chromatography, collect solution in the 6.7-10.2 min time period, solution obtains active component behind concentrate drying.
3. the application of a kind of Flos Carthami active component according to claim 1 in preparation treatment and angiocardiopathy preventing medicine.
4. application according to claim 3 is characterized in that, described medicine adds acceptable auxiliary on the pharmaceutics by the Flos Carthami active component, makes according to the formulation preparation method of putting down in writing on the pharmaceutics.
5. application according to claim 3 is characterized in that described preparation comprises liquid preparation or solid preparation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100590325A CN102119947B (en) | 2011-03-13 | 2011-03-13 | Preparation method and application of carthamus tinctorius L. active ingredient |
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|---|---|---|---|
| CN2011100590325A CN102119947B (en) | 2011-03-13 | 2011-03-13 | Preparation method and application of carthamus tinctorius L. active ingredient |
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| CN102119947A true CN102119947A (en) | 2011-07-13 |
| CN102119947B CN102119947B (en) | 2012-11-21 |
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| CN2011100590325A Expired - Fee Related CN102119947B (en) | 2011-03-13 | 2011-03-13 | Preparation method and application of carthamus tinctorius L. active ingredient |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1428170A (en) * | 2002-11-10 | 2003-07-09 | 边冬梅 | Effective component of safflower, its powder injection, preparation method and medicinal application |
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2011
- 2011-03-13 CN CN2011100590325A patent/CN102119947B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1428170A (en) * | 2002-11-10 | 2003-07-09 | 边冬梅 | Effective component of safflower, its powder injection, preparation method and medicinal application |
Non-Patent Citations (1)
| Title |
|---|
| 《中国野生植物资源》 20040229 吴冬青,等 红花黄色素提取工艺研究 50-52 1-5 第23卷, 第1期 2 * |
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| CN102119947B (en) | 2012-11-21 |
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Granted publication date: 20121121 |