CN101190906A - Method for preparing carthamin yellow carthamus B and application thereof - Google Patents
Method for preparing carthamin yellow carthamus B and application thereof Download PDFInfo
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- CN101190906A CN101190906A CNA2007101177437A CN200710117743A CN101190906A CN 101190906 A CN101190906 A CN 101190906A CN A2007101177437 A CNA2007101177437 A CN A2007101177437A CN 200710117743 A CN200710117743 A CN 200710117743A CN 101190906 A CN101190906 A CN 101190906A
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Abstract
The invention relates to a preparation method of safflower yellow B and the application thereof. The safflower is extracted after immersion and diacolation in polar solvent and is then treated with refinement and separation by a method of combining chromatographic column and alcohol precipitation so as to obtain the safflower yellow B of the invention. The preparation method for the safflower yellow B of the invention can improve the yield of the safflower yellow B and is applicable to commercial production. In addition, the safflower yellow B obtained after separation can be used for preventing and curing cardiovascular and cerebrovascular diseases.
Description
Technical field
The invention belongs to natural drug extracts active ingredients preparation field, be specifically related to from safflower, separate the technology of Hydroxy Carthamus yellow B, the invention still further relates to the application of Hydroxy Carthamus yellow B aspect pharmacy and cardiovascular and cerebrovascular field.
Background technology
Safflower is the dried floral of feverfew safflower Carthamus tinctorius L., and summer flower is plucked when red by xanthochromia, dries in the shade or dries, and has promoting blood circulation to remove blood stasis, inducing meastruation to relieve menalgia effect.Mainly contain three kinds of water-soluble yellow pigment in the safflower, be respectively hydroxyl radical carthamin yellow carthamus A, carthamin yellow carthamus B, carthamin yellow C.It is all at hydroxyl radical carthamin yellow carthamus A, less to the research of all the other two kinds of compositions that present numerous research---comprises extracting method, pharmacology and clinical---.Chinese patent CN1785988A discloses a kind of preparation method and purposes that is rich in the carthamin yellow of carthamin yellow carthamus B, and invention adopts the water logging bubble to extract the polymeric amide separation and purification.Because there are some small molecules solubility amide impurities in polymeric amide, at present also not to its residual unified detection, and polymeric amide to the absorption of polyphenol hydroxyl compounds firmly, and dead adsorptive capacity is big, and difficulty elutes, and the reused number of times of polymeric amide is also less.And carthamin yellow carthamus B contains a plurality of phenolic hydroxyl groups, and faces phenolic hydroxyl group in addition, and by polymeric amide absorption firmly, relative loss is bigger when separating with polymeric amide.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing carthamin yellow carthamus B.The present invention at first adopts the carthamin yellow carthamus B that contains in the aqueous polar solvent diacolation extraction safflower, and with water logging bubble extract phase ratio, extraction yield is higher, and yellow pigment B stripping is more complete.
On the order of alcohol precipitation and mistake macroporous resin, the present invention adopts and crosses macroporous resin column earlier, because of carthamin yellow carthamus B can be preferably by macroporous resin adsorption, when water or the alcohol amount of containing were lower than 15% ethanol elution, yellow pigment B was by under the wash-out, can remove some water-soluble polysaccharides like this and not by the composition of macroporous resin adsorption, as hydroxyl radical carthamin yellow carthamus A, when follow-up alcohol precipitation because the water-soluble impurity interferential reduces, during alcohol precipitation in the yellow mercury oxide yellow pigment B content higher also purer.
The present invention adopts the reverse phase filler post to haematochrome B refining the time, as Sephadex-LH20, GEL-MCI, ODS filler, this class filler can not produce the dead absorption to the polyphenol hydroxyl compounds, but the reuse height, and few pure dissolubility hangs down molecular impurity, and is simpler when handling filler.Adopt this class filler that yellow pigment B is made with extra care, the output of final product carthamin yellow carthamus B is significantly improved.
Used reverse phase filler among the present invention can be dextrane gel, reverse phase silica gel, anti-phase GEL-MCI filler, preferred dextrane gel Sephadex-LH20.
The present invention is used solvent in diacolation extracts, and is lower than 60% the aqueous polar solvent that contains for the polar organic solvent massfraction.Water-containing organic solvent wherein can be aqueous methanol, aqueous ethanol or aqueous acetone, all right single water, preferred alcohol.50% ethanol more preferably.
Another object of the present invention is to provide and contain the application of the resulting carthamin yellow carthamus B of the inventive method in pharmacy.
A further object of the present invention has application in prevention and the treatment cardiovascular and cerebrovascular diseases medicament with by the inventive method resulting carthamin yellow carthamus B is provided in preparation.
Realize the present invention, can be achieved through the following technical solutions: safflower polar organic solvent massfraction is lower than 60% the aqueous polar solvent that contains and soaks after 24 hours, water or aqueous ethanol diacolation extract then, to percolate, there is not carthamin yellow carthamus B substantially, merge percolate, 60 ℃ of following concentrating under reduced pressure, to relative density be 1.05～1.15, last macroporous adsorptive resins, the ratio of medicinal material and macroporous adsorbent resin consumption is 1g raw medicinal herbs/0.5～2mL resin, thin out with the ethanol elution that is lower than 15% earlier to the elutriant color, do not flow down to there being carthamin yellow carthamus B with 30%～50% ethanol elution again, merge ethanol eluate, 60 ℃ are evaporated to relative density and are about 1.05～1.30, under constantly stirring, add ethanol and make that to contain the alcohol amount be 75%～85%, placed 24 hours at cold place, separate out yellow mercury oxide, filter, the extracting yellow precipitation, with at least 3 times of sedimentary deionized water dissolvings of amount, leave standstill, filter, get filtrate, filtrate is evaporated to for 60 ℃ does not have the alcohol flavor, relative density is 1.05～1.15, last reverse phase filler post separates, and it is thin out to the elutriant color to be lower than 15% ethanol elution, uses 35%～55% ethanol elution instead, collect carthamin yellow carthamus B content greater than stream part of 90%, merge; Carthamin yellow carthamus B content is gone up reversed-phase column again less than stream part merging of 90%, it is thin out to the elutriant color to be lower than 15% ethanol elution, 35%～55% ethanol elution, collect carthamin yellow carthamus B content greater than stream part of 90%, be incorporated into above-mentioned carthamin yellow carthamus B content greater than in stream part of 90%, refining so repeatedly, be separated to the carthamin yellow carthamus B major part, 60 ℃ of concentrating under reduced pressure carthamin yellow carthamus B content gets concentrated solution greater than 90% amalgamation liquid, the concentrated solution lyophilize, carthamin yellow carthamus B.
Diacolation of the present invention extracts the ethanol of used solvent preferred 50%, the preferred Sephadex-LH20 of filler of refining carthamin yellow carthamus B.
Extract the polymeric amide process for purification by contrast the inventive method and water logging bubble, the extraction yield of carthamin yellow carthamus B and final carthamin yellow carthamus B yield compare during to extraction, and the present invention is improved.
Be described below by the contrast experiment, comparative result sees Table 1.
Extraction scheme one: existing correlation technique scheme
Yunnan safflower 1kg steeps three times with water logging, and solvent load is respectively 10L, 8L, 8L, and soak time was respectively 24 hours, 12 hours, 12 hours.Filter, merging filtrate, 60 ℃ are evaporated to relative density is 1.20, stir adding ethanol to make containing scale is 80%, refining 24 hours, separate out yellow mercury oxide, the extracting yellow precipitation is with the water dissolution of 4 times of amounts, filter, get filtrate, last HP-20 macroporous adsorptive resins is earlier with 10% ethanol elution, use 50% ethanol elution again, collect ethanol eluate, merge, the polyamide column of handling well on behind the concentrating under reduced pressure, earlier with 5 column volumes of ethanol elution of 50%, use 95% ethanol elution again, collect carthamin yellow carthamus B content greater than stream part of 90%, carthamin yellow carthamus B (A2).
Extraction scheme two: technical solution of the present invention
Yunnan safflower 1kg, the alcohol immersion of 10L50% is after 24 hours, and diacolation extracts, substantially carry to the greatest extent to carthamin yellow carthamus B, the total solvent consumption is 26L, merges percolate, 60 ℃ are evaporated to relative density is 1.10, and last HP-20 macroporous adsorptive resins is earlier with 10% ethanol elution, abandon this part, use 50% ethanol elution instead, collect 50% ethanol eluate, merge, 60 ℃ are evaporated to relative density is 1.20, stirs to add ethanol down and make that to contain the alcohol amount be 80%, placed 24 hours at cold place, separates out yellow mercury oxide, filters, get precipitation,, filter with the deionized water dissolving of 5 times of precipitation capacities, get filtrate, being evaporated to relative density is 1.10, last Sephadex-LH20 post, 15% ethanol elution, discard, use 50% ethanol elution again, collect carthamin yellow carthamus B content greater than stream part of 90%, merge, concentrating under reduced pressure, drying, both.
Two kinds of methods of table 1 are separated the comparison of carthamin yellow carthamus B
From last table result as can be known, utilize technical solution of the present invention extraction separation carthamin yellow carthamus B, the yield of the extraction yield of carthamin yellow and final carthamin yellow carthamus B all is better than the correlation technique scheme in the extract.
The resulting carthamin yellow carthamus B of technical solution of the present invention has the effect of prevention and treatment cardiovascular and cerebrovascular diseases, as to diseases such as ischemia apoplexy, myocardial ischemias.With the resulting carthamin yellow carthamus B of the technical solution of the present invention that contains significant quantity, can be used for preparing various pharmaceutical dosage forms with prevention and treatment cardiovascular and cerebrovascular diseases, it can be oral solid formulation, as tablet, capsule, pill etc., also can be the injection-type preparation, as injection liquid, freeze-dried powder, infusion solutions etc.
Oral solid formulation of the present invention (capsule) can be achieved by the following scheme:
Carthamin yellow carthamus B 28g
Dry starch 172g
Preparation technology is: take by weighing carthamin yellow carthamus B and dry starch, adopt the equivalent incremental method that carthamin yellow carthamus B and dry starch are mixed, in the Capsules of packing into, both got capsule.
The preparation of pharmaceutical composition tablet of the present invention:
Carthamin yellow carthamus B 28g
85% ethanol is an amount of
Starch is an amount of
Take by weighing carthamin yellow, starch, mixing, the alcohol granulation with 85% adds an amount of disintegrating agent and lubricant, and compressing tablet is made 1000.
The preparation of lyophilized injectable powder of the present invention:
Carthamin yellow carthamus B 14g
N.F,USP MANNITOL is an amount of
Water for injection is an amount of
Take by weighing carthamin yellow carthamus B, with water for injection dissolving, the NaOH of 0.1M transfers about pH to 6.5, adds N.F,USP MANNITOL, and ultrasonic dissolution is crossed the millipore filtration of 0.22um, freeze-drying, both.
Specific embodiment
Below the present invention will be further described from specific embodiment, it is pointed out that cited embodiment is not meant to limit the present invention technical scheme, but for clearer explanation the present invention.The selected raw material of following safflower is all from Yunnan.
Embodiment 1
Take by weighing dry safflower 20kg, after soaking 24 hours with deionized water 200L, change in the diacolation bucket, carrying out diacolation extracts, flow velocity is 0.06BV/min, constantly replenish fresh deionized water on the medicinal material, to percolate, do not have safflower red pigment B substantially, amount to water consumption 520L, merge percolate, 60 ℃ are evaporated to relative density and are about 1.10, on the HP-20 macroporous adsorptive resins handled well, resin demand is 20L, earlier with 5 column volumes of ethanol elution of 10%, abandon this part elutriant, use 50% ethanol elution instead, do not have carthamin yellow carthamus B substantially, merge 50% ethanol eluate to reserving liquid, 60 ℃ are evaporated to relative density is 1.20, stir and to add 95% ethanol down and make that to contain the alcohol amount be 81%, placed 24 hours at cold place, separates out yellow mercury oxide, filter, the extracting yellow precipitation, the deionized water of 5 times of precipitation capacities of adding stirs and makes dissolving, filter, get filtrate, 60 ℃ are evaporated to relative density is 1.10, last Sephadex-LH20 sephadex column, concentrated solution volume ratio is 1: 10 with the packing volume ratio, ethanol elution with 15%, thin out to the effluent liquid color, use 55% ethanol elution instead, collect carthamin yellow carthamus B content greater than stream part of 90%, merge; After carthamin yellow carthamus B content concentrated less than the merging of stream part of 90%, by above-mentioned gel-purified step operation, collect carthamin yellow carthamus B content greater than stream part of 90%, collected carthamin yellow carthamus B content is merged greater than stream part of 90%, 60 ℃ of concentrating under reduced pressure, lyophilize gets carthamin yellow carthamus B 100g, and content is 94.37%.
Embodiment 2
Take by weighing dry safflower 20kg, alcohol immersion with 60% is after 24 hours, change in the diacolation bucket, carrying out diacolation extracts, flow velocity is 0.06BV/min, constantly replenish fresh 60% ethanol on the medicinal material, to percolate, there is not safflower red pigment B substantially, the alcohol that amounts to 60% is 520L, merge percolate, 60 ℃ are evaporated to relative density and are about 1.10, on the AB-8 type macroporous adsorptive resins handled well, resin demand is 20L, earlier with 5 column volumes of ethanol elution of 5%, abandons this part elutriant, use 30% ethanol elution instead, substantially do not have carthamin yellow carthamus B to effluent liquid, merge 30% ethanol eluate, 60 ℃ are evaporated to relative density is 1.20, stir and to add 95% ethanol down and make that to contain the alcohol amount be 75%, placed 24 hours at cold place, separates out yellow mercury oxide, filters, the extracting yellow precipitation, the deionized water that adds 4 times of precipitation capacities stirs and makes dissolving, filters, get filtrate, 60 ℃ are evaporated to relative density is 1.10, last GEL-MCI reversed-phase column, and concentrated solution volume ratio is 1: 8 with the packing volume ratio, ethanol elution with 10%, thin out to the effluent liquid color, use 45% ethanol elution instead, collect carthamin yellow carthamus B content greater than stream part of 90%, merge, concentrate, lyophilize, content is 96.82% carthamin yellow carthamus B 110g.
Embodiment 3
Take by weighing dry safflower 20kg, ethanol 200L with 50% soaked after 24 hours, change in the diacolation bucket, carrying out diacolation extracts, flow velocity is 0.06BV/min, constantly replenish fresh 50% ethanol on the medicinal material, substantially do not have safflower red pigment B to percolate, the amount of alcohol that amounts to 50% is 520L, merges percolate, 60 ℃ are evaporated to relative density and are about 1.10, on the D-101 type macroporous adsorptive resins handled well, resin demand is 20L, earlier with 5 column volumes of ethanol elution of 15%, abandon this part elutriant, use 40% ethanol elution instead, do not have carthamin yellow carthamus B substantially, merge 40% ethanol eluate to reserving liquid, 60 ℃ are evaporated to relative density is 1.20, stir and to add 95% ethanol down and make that to contain the alcohol amount be 85%, placed 24 hours at cold place, separates out yellow mercury oxide, filter, the extracting yellow precipitation, the deionized water of 5 times of precipitation capacities of adding stirs and makes dissolving, filter, get filtrate, 60 ℃ are evaporated to relative density is 1.10, goes up anti-phase ODS silicagel column, concentrated solution volume ratio is 1: 12 with the packing volume ratio, ethanol elution with 10%, thin out to the effluent liquid color, use 35% ethanol elution instead, collect carthamin yellow carthamus B content greater than stream part of 90%, merge; After carthamin yellow carthamus B content concentrated less than the merging of stream part of 90%, by above-mentioned gel-purified step operation, collect carthamin yellow carthamus B content greater than stream part of 90%, collected carthamin yellow carthamus B content is merged greater than stream part of 90%, 60 ℃ of concentrating under reduced pressure, lyophilize, content is 92.79% carthamin yellow carthamus B 115g.
Embodiment 4
Take by weighing dry safflower 20kg, ethanol 200L with 30% soaked after 24 hours, change in the diacolation bucket, carrying out diacolation extracts, flow velocity is 0.06BV/min, constantly replenish fresh 30% ethanol on the medicinal material, to percolate, there is not safflower red pigment B substantially, the amount of alcohol that amounts to 30% is 520L, merge percolate, 60 ℃ are evaporated to relative density and are about 1.10, on the HP-20 macroporous adsorptive resins handled well, resin demand is 20L, earlier with 5 column volumes of ethanol elution of 10%, abandon this part elutriant, use 50% ethanol elution instead, do not have carthamin yellow carthamus B substantially, merge 50% ethanol eluate to reserving liquid, 60 ℃ are evaporated to relative density is 1.20, stir and to add 95% ethanol down and make that to contain the alcohol amount be 80%, placed 24 hours at cold place, separates out yellow mercury oxide, filter, the extracting yellow precipitation, the deionized water of 5 times of precipitation capacities of adding stirs and makes dissolving, filter, get filtrate, 60 ℃ are evaporated to relative density is 1.10, last Sephadex-LH20 sephadex column, concentrated solution volume ratio is 1: 10 with the packing volume ratio, ethanol elution with 15%, thin out to the effluent liquid color, use 55% ethanol elution instead, collect carthamin yellow carthamus B content greater than stream part of 96%, merge; After carthamin yellow carthamus B content concentrated less than the merging of stream part of 96%, above-mentioned repeatedly gel purification operations, about 3 times, merge the carthamin yellow carthamus B of each time gained, 60 ℃ of concentrating under reduced pressure, lyophilize must content be 98.97% carthamin yellow carthamus B 95g.
Embodiment 5
Take by weighing dry safflower 20kg, ethanol 200L with 10% soaked after 24 hours, change in the diacolation bucket, carrying out diacolation extracts, flow velocity is 0.06BV/min, constantly replenish fresh 10% ethanol on the medicinal material, to percolate, there is not safflower red pigment B substantially, the amount of alcohol that amounts to 10% is 520L, merge percolate, 60 ℃ are evaporated to relative density and are about 1.10, on the HP-20 macroporous adsorptive resins handled well, resin demand is 20L, earlier with 5 column volumes of ethanol elution of 10%, abandon this part elutriant, use 50% ethanol elution instead, do not have carthamin yellow carthamus B substantially, merge 50% ethanol eluate to reserving liquid, 60 ℃ are evaporated to relative density is 1.20, stir and to add 95% ethanol down and make that to contain the alcohol amount be 80%, placed 24 hours at cold place, separates out yellow mercury oxide, filter, the extracting yellow precipitation, the deionized water of 5 times of precipitation capacities of adding stirs and makes dissolving, filter, get filtrate, 60 ℃ are evaporated to relative density is 1.10, last Sephadex-LH20 sephadex column, concentrated solution volume ratio is 1: 10 with the packing volume ratio, ethanol elution with 15%, thin out to the effluent liquid color, use 55% ethanol elution instead, collect carthamin yellow carthamus B content greater than stream part of 96%, merge; After carthamin yellow carthamus B content concentrated less than the merging of stream part of 96%, above-mentioned repeatedly gel purification operations, about 3 times, merge the carthamin yellow carthamus B of each time gained, 60 ℃ of concentrating under reduced pressure, lyophilize must content be 98.97% carthamin yellow carthamus B 90g.
Embodiment 5
Carthamin yellow carthamus B is to the provide protection experiment of cerebral ischemia.
Animal: the Wistar rat, male, body weight 250～300g.
Medicine: carthamin yellow carthamus B (preparation of the medical limited-liability company of star sky)
Superoxide-dismutase (SOD) measure test kit, mda (MDA) measure test kit,
Serum lactic dehydrogenase (LDH) test kit, TCC (TTC)
Rat acute imperfection cerebral ischemia re-pouring model: get 40 of Wistar rats, be divided into 5 groups at random, the administration group gives carthamin yellow carthamus B 3,6,9mg/kg respectively, iv, and 1 time/day, for three days on end.Capacity physiological saline such as control group iv, sham operated rats is removed the total artery of not ligation, and all the other handle same control group.10min after the last administration; rat is anaesthetized with urethane 1.0g/kgip; reference literature (Pan Xinxin; Liu Tianpei. Radix Ginseng total saponins is to the provide protection [J] of acute cerebral ischemia. Nanjing Medical College's journal; 1992; 12 (3): 237～239.) method ligation bilateral common carotid arteries, recover cerebral blood supply behind the 30min again, it is standby to get brain behind the 24h.
Cerebral tissue LDH, SOD activity and MDA Determination on content: the rat broken end is got brain, remove cerebellum and brain stem, make 10% homogenate, classifiedly get supernatant liquor after centrifugal, press the thiobarbituricacid method and measure MDA content, press test kit specification sheets method and measure LDH activity and SOD vigor, quantification of protein Folin phenol method.The results are shown in Table 2
Table 2 carthamin yellow carthamus B is to the influence of rat acute imperfection ischemical reperfusion injury (x ± s)
Compare with sham operated rats,
#P＜0.01; Compare with control group,
*P＜0.05,
*P＜0.01
The result shows, rat whole brain ischemic 30min poured into 24 hours again, cerebral tissue LDH, SOD are active obviously to be reduced, MDA content obviously raises, and carthamin yellow 6.0,9.0mg/kg iv can significantly improve LDH, the SOD vigor of ischemic tissue of brain, reduce MDA content, but can not reach the sham operated rats level.
Embodiment 6
Carthamin yellow carthamus B is to the influence of rat heart muscle oxygen-consumption
Laboratory animal is used vetanarcol (30mg/kg) intravenous anesthesia, trachea cannula, and the link breathing apparatus opens chest, separates arteria carotis communis and extracts arterial blood, gets coronary vein blood through external jugular vein intubate to coronary sinus vein, surveys the oxygen content of blood in blood oxygen.
Experiment is divided into two groups, and dosage is respectively 8,4mg/kg iv, and 10 every group, mensuration is respectively organized the oxygen content of blood before the administration.
The result shows that carthamin yellow carthamus B 8mg/kg dosage can obviously reduce myocardial consumption of oxygen and oxygen consumption index.1min after the administration, myocardial consumption of oxygen 53.2 ± 1.28 reduces to 34.3 ± 1.20 before by administration, has reduced by 35.5 ± 1.3%; Oxygen consumption index reduces to 116.36 ± 75.50 by 184.28 ± 53.23, and 36.85 ± 22.27% (P＜0.05, P＜0.01) have descended.
Claims (8)
1. the preparation method of a carthamin yellow carthamus B, with the safflower is raw material, after it is characterized in that safflower is lower than 60% contain aqueous polar solvent and soak with the polar organic solvent massfraction, diacolation extracts, merge percolate, being evaporated to relative density is 1.05～1.15, last macroporous adsorptive resins, earlier to be lower than 15% ethanol elution thin out to the elutriant color to contain the alcohol amount, abandon this part elutriant, be that 30%～50% ethanol elution does not flow down to there being carthamin yellow carthamus B with the alcohol amount of containing again, merge this part alcohol washing lotion, being evaporated to relative density is 1.05～1.30, adds ethanol and make that to contain the alcohol amount be 75%～85% under constantly stirring, and place at cold place, separate out yellow mercury oxide, filtration extracting yellow precipitation, the water dissolution with being at least 3 times of precipitation capacities leaves standstill, filter, get filtrate, it is 1.05～1.15 that filtrate decompression is concentrated into relative density, last reverse phase filler post, the ratio of concentrated solution and filler is 1: 8-12, earlier thin out to the effluent liquid color with the ethanol elution that is lower than 15%, use 35%～55% ethanol elution again, collect carthamin yellow carthamus B content more than or equal to stream part of 90%, merge, concentrating under reduced pressure, drying gets carthamin yellow carthamus B.
2. the preparation method of carthamin yellow carthamus B as claimed in claim 1, after it is characterized in that safflower is lower than 60% contain aqueous polar solvent and soak 24 hours with the polar organic solvent massfraction, diacolation extracts, to percolate, there is not carthamin yellow carthamus B substantially, merge percolate, 60 ℃ of following concentrating under reduced pressure, to relative density be 1.10, last HP20 macroporous adsorptive resins, the ratio of medicinal material and macroporous adsorbent resin consumption is 1g raw medicinal herbs/0.8-1.2mL resin, earlier thin out to the elutriant color with 10% ethanol elution, do not flow down to there being carthamin yellow carthamus B with 45% ethanol elution again, merge 45% ethanol eluate, 60 ℃ are evaporated to relative density and are about 1.20, add ethanol and make that to contain the alcohol amount be 81% under constantly stirring, placed 24 hours at cold place, separate out yellow mercury oxide, filter, the extracting yellow precipitation, with 5 times of sedimentary deionized water dissolvings of amount, leave standstill, filter, get filtrate, filtrate is evaporated to for 60 ℃ does not have the alcohol flavor, relative density is 1.10, last sephadex column, and the ratio of concentrated solution and gel is 1: 8-12,10% ethanol elution is thin out to the elutriant color, use 50% ethanol elution instead, collect carthamin yellow carthamus B content, merge greater than stream part of 90%; Carthamin yellow carthamus B content is gone up sephadex column again less than stream part merging of 90%, 15% ethanol elution is thin out to the elutriant color, 45% ethanol elution, collect carthamin yellow carthamus B content greater than stream part of 90%, be incorporated into above-mentioned carthamin yellow carthamus B content greater than in stream part of 90%, refining so repeatedly, be separated to the carthamin yellow carthamus B major part, 60 ℃ of concentrating under reduced pressure carthamin yellow carthamus B content gets concentrated solution greater than 90% amalgamation liquid, the concentrated solution lyophilize, carthamin yellow carthamus B.
3. the preparation method of carthamin yellow carthamus B as claimed in claim 1, wherein said reverse phase filler can also be GEL-MCI, ODS filler.
4. as the preparation method of claim 1 or two described carthamin yellow carthamus Bs, it is characterized in that the described aqueous polar solvent that contains is meant aqueous ethanol, aqueous methanol or aqueous acetone.
5. the preparation method of carthamin yellow carthamus B as claimed in claim 1 or 2, the content that it is characterized in that described carthamin yellow carthamus B greater than 90% less than 100%.
6. preparation that contains the carthamin yellow carthamus B that preparation method as claimed in claim 1 or 2 obtains.
7. preparation as claimed in claim 5 is characterized in that being mainly oral preparations.
8. the carthamin yellow carthamus B that is obtained by claim 1 or 2 described preparation methods has purposes in prevention and the treatment cardiovascular and cerebrovascular diseases medicament in preparation.
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| CN104288169A (en) * | 2014-08-31 | 2015-01-21 | 江苏康缘药业股份有限公司 | Flavone glycoside compound and preparation method and application thereof |
| CN105777724A (en) * | 2016-03-23 | 2016-07-20 | 浙江中医药大学 | Method for extracting and purifying dehydrated safflower yellow B in safflower |
| CN108392486A (en) * | 2018-01-23 | 2018-08-14 | 滨州医学院 | Applications of the Sydroxy carthamin B in terms of preventing myocardial ischemia-reperfusion injury |
| CN109602737A (en) * | 2019-01-25 | 2019-04-12 | 滨州医学院 | Application and drug of the Sydroxy carthamin B in preparation treatment gastric cancer medicament |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1785988A (en) * | 2004-12-06 | 2006-06-14 | 山东绿叶天然药物研究开发有限公司 | Saflor yellow pigment rich in saflor yellow pigment B, its preparation method and use |
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| CN104288169A (en) * | 2014-08-31 | 2015-01-21 | 江苏康缘药业股份有限公司 | Flavone glycoside compound and preparation method and application thereof |
| CN105777724A (en) * | 2016-03-23 | 2016-07-20 | 浙江中医药大学 | Method for extracting and purifying dehydrated safflower yellow B in safflower |
| CN105777724B (en) * | 2016-03-23 | 2018-07-24 | 浙江中医药大学 | The extraction of dehydration carthamin yellow carthamus B and purification process in a kind of safflower |
| CN108392486A (en) * | 2018-01-23 | 2018-08-14 | 滨州医学院 | Applications of the Sydroxy carthamin B in terms of preventing myocardial ischemia-reperfusion injury |
| CN109602737A (en) * | 2019-01-25 | 2019-04-12 | 滨州医学院 | Application and drug of the Sydroxy carthamin B in preparation treatment gastric cancer medicament |
| CN109602737B (en) * | 2019-01-25 | 2021-02-19 | 滨州医学院 | Application of hydroxysafflor yellow B in preparation of medicine for treating gastric cancer and medicine |
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