CN1600817A - Yellow pigment of safflower preparation method and application - Google Patents
Yellow pigment of safflower preparation method and application Download PDFInfo
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- CN1600817A CN1600817A CN 03157479 CN03157479A CN1600817A CN 1600817 A CN1600817 A CN 1600817A CN 03157479 CN03157479 CN 03157479 CN 03157479 A CN03157479 A CN 03157479A CN 1600817 A CN1600817 A CN 1600817A
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Abstract
This invention provides safflower uranidin prepd. from the Chinese herb medicine-safflower which isu sed for promoting blood circulation and removing blood disturbance, and the prepn. method and usage therefor. Said safflower uranidin is tested by high efficiency liquid phase chromatography with its content of 70-99.6%. It can be used for treating and preventing various kinds of diseases, such as cardiovascular disease, cerebrovascular disease and other blood circulation disturbance disease.
Description
Technical field
The present invention relates to the new purposes of a kind of carthamin yellow that from the activating blood herbs safflower, prepares and preparation method thereof and this carthamin yellow.
Background technology
Chinese medicine safflower is the dried floral of feverfew Carthamus tinctorius L., is a kind of common activating blood herbs, can be used for many disturbance of blood circulation treatment of diseases such as coronary heart disease, stenocardia, and safflower is used as medicine with decocting liquid clinically.Carthamin yellow is the main effective constituent in the safflower, be a phenyl styryl ketone glucoside [referring to: pacify the 21st volume the 4th phase " isolation identification of yellow pigment and haematochrome in the safflower " of prosperous strong grade " herbal medicine " nineteen ninety; Takahashi Yet al Lett1982; 23 (49): 5163; Open and face equality " the medicinal academic meeting paper collection of national safflower " P24～27 " research of Flos Carthami powder injection physico-chemical property ", in August, 1996; Wang Chengsong etc. " Chinese patent medicine " 1986 the 4th phases " Flos Carthami injection method for making and Study on Quality Control "].Studies show that it has many-sided cardiovascular pharmacological effect, but anti-freezing, promote fibrinolytic, antithrombotic formations, microcirculation improvement etc. [referring to Wang Huiling " Chinese Chinese materia medica science and technology " 1993 the 5th the 5th phases of volume " modern study of carthamin yellow is summarized "].
At present, on the purity of existing carthamin yellow, be the crude product carthamin yellow, the preparation method of this crude product carthamin yellow is a water extraction and alcohol precipitation method, because of its without method removal of impurity such as chromatographies, its thin layer collection of illustrative plates is that a hangover colour band from the initial point to the forward position is [referring to Tianjin institute of Pharmaceutical Industry etc., the pharmacological research of the research of safflower (two) carthamin yellow and isolate thereof, the Shanxi medical magazine, 1980:9 (1) 2-8], point out its purity lower.Therefore, only there is crude product carthamin yellow to be used as food color at present, still do not have medicine or health-care preparation based on the higher elaboration carthamin yellow preparation of purity by the water extraction and alcohol precipitation method preparation.
Summary of the invention
The object of the present invention is to provide the new purposes of a kind of carthamin yellow that from the activating blood herbs safflower, prepares and preparation method thereof and this carthamin yellow.
The invention provides a kind of carthamin yellow, is 70～99.6% with high effective liquid chromatography for measuring content, and this carthamin yellow can prepare with following method:
(1) with the safflower be raw material, add an amount of temperature and be 50～100 ℃ polar solvent extracting, the filtering dregs of a decoction are cooled to 5～30 ℃ with extracting solution, leave standstill 2～24 hours;
(2) extracting solution that above-mentioned steps is obtained through centrifugal remove insoluble impurities, ultrafiltration and remove macromole impurity after, by macroporous resin adsorption, and be elutriant wash-out carthamin yellow with the polar solvent, collecting elutriant is carthamin yellow crude product elutriant;
(3) the carthamin yellow crude product elutriant that above-mentioned steps is obtained concentrates, and concentrated solution separates with molecular sieve column, is elutriant wash-out carthamin yellow with the polar solvent, collects elutriant, through concentrated, dry, gets the carthamin yellow finished product.
The present invention also provides a kind of preparation method of carthamin yellow, comprises the steps:
(1) with the safflower be raw material, add an amount of temperature and be 50～100 ℃ polar solvent extracting, the filtering dregs of a decoction are cooled to 5～30 ℃ with extracting solution, leave standstill 2～24 hours;
(2) extracting solution that above-mentioned steps is obtained through centrifugal remove insoluble impurities, ultrafiltration and remove macromole impurity after, by macroporous resin adsorption, and be elutriant wash-out carthamin yellow with the polar solvent, collecting elutriant is carthamin yellow crude product elutriant;
(3) the carthamin yellow crude product elutriant that above-mentioned steps is obtained concentrates, and concentrated solution separates with molecular sieve column, is elutriant wash-out carthamin yellow with the polar solvent, collects elutriant, through concentrated, dry, gets the carthamin yellow finished product.
In preparation method's of the present invention preferred implementation, the extracting in the step (1) is with polar solvent extracting 2～3 times, and each 0.5～24 hour, the extracting water consumption was 10～30 times of safflower crude drug weight.
In preparation method's of the present invention preferred implementation, the polar solvent in the step (1) is selected from water or ethanol, methyl alcohol, propyl alcohol and isopropanol water solution, is preferably water.As water, be preferably deionized water, distilled water.
In preparation method's of the present invention preferred implementation, the macroporous resin in the step (2) is with centrifugal what remove that insoluble impurities, ultrafiltration remove Flos Carthami extract behind the macromole impurity is 1: 2～5 than by volume.
In the present invention, macroporous resin is existing macroporous resin, is preferably non-polar macroporous resin D
4020, non-polar macroporous resin B201, low-pole macroporous resin AB-8, more preferably non-polar macroporous resin D
4020
In preparation method's of the present invention preferred implementation, the spissated method that is used in the step (3) is a membrane concentration.
In preparation method's of the present invention preferred implementation, the molecular sieve consumption in the step (3) is 1: 0.05～0.15 than by volume with carthamin yellow crude product concentrated solution.
In preparation method's of the present invention preferred implementation, the polarity elutriant in step (2) and the step (3) is respectively water or ethanol, methyl alcohol, propyl alcohol and isopropanol water solution, is preferably water.As water, be preferably deionized water, distilled water.
In the present invention, used molecular sieve is existing molecular sieve, is preferably SephadexLH-20, Sephadex G-25.
The invention provides a kind of medicine and healthcare products for the treatment of cardiovascular and cerebrovascular diseases, it contains the above-mentioned carthamin yellow and the pharmaceutically useful carrier of treatment or prevention cardiovascular and cerebrovascular diseases significant quantity.
Above-mentioned medicine and healthcare products can be made into oral preparations, injection formulations.
The present invention is used to prepare medicine and the Halth-care composition that prevention and treatment relate to damage disease due to myocardial ischemia and cerebral ischemia, the thrombosis, said composition contains as the carthamin yellow of activeconstituents and pharmaceutically-acceptable excipients, carrier or thinner, is made into medicine or health-care preparation with ordinary method.
During the preparation said composition, carthamin yellow can be mixed or use carrier embedding, this carrier with carrier can be capsule or other loading forms.Carrier can be solid, semisolid or liquid substance, and it is as carrier, vehicle or the medium of carthamin yellow.Said composition can be various ways such as tablet, pill, powder, suspension, emulsion, solution, injection.
Variety carrier, vehicle or thinner can be used for this composition.As lactose, glucose, sucrose, sorbyl alcohol, N.F,USP MANNITOL, starch, polyoxyethylene glycol, gelatin etc.Also can add lubricant, wetting agent, correctives, suspension agent, sanitas etc. in the said preparation.Any method preparation that composition of the present invention can use this area to adopt usually, to reach after patient's use, activeconstituents is brought into play the purpose of maximum drug effect.
But this medicine and Halth-care composition oral administration, intravenous injection, intramuscular injection, through skin or various administrations such as subcutaneous injection, per rectum.But single or multiple uses continuously, and the pharmaceutical composition using dosage then should generally should be controlled at 0.001～1.0 gram carthamin yellow/kilogram sky according to patient's particular case decision.
The present invention takes the polar solvent extracting, separates and separates with sieve chromatography through centrifugal ultrafiltration, absorption with macroporous adsorbent resin, makes the higher carthamin yellow of purity after the removal of impurity, and this method is not appeared in the newspapers as yet in the application that the safflower composition extracts in the process for preparing.They can remove amino acid and carbohydrate impurity effectively, obviously improve the purity of carthamin yellow, the carthamin yellow that method of the present invention prepares gained does not all have amino acid and free sugar reaction, method of the present invention prepares the carthamin yellow usable highly effective liquid chromatography for measuring carthamus tinctorius yellow color content of gained, this method circulation ratio, good stability.The carthamus tinctorius yellow color content that method of the present invention prepares gained is 70～99.6% (seeing Figure of description).Because carthamin yellow preparation method of the present invention takes 50～100 ℃ polar solvent to carry out extracting, thus can shorten the production time of a production cycle significantly, thus improved production efficiency.And this method is easy and simple to handle, is easy to grasp, and can be used as the purification process of carthamin yellow preparation and safflower water soluble component.
The carthamin yellow of the present invention's preparation has following drug effect:
Pharmacodynamics test:
Observe rat heart muscle anoxic and the hemodynamic influence of rat that " carthamin yellow " intravenous injection is brought out dog Acute Myocardial Infarction, dog coronary flow, dog myocardial consumption of oxygen, Pituitrin.The result shows: 1. " carthamin yellow " 10mg/kg intravenous injection can significantly reduce dog Acute Myocardial Infarction precordial lead electrocardiogram ST section and raises degree, " carthamin yellow " 5,10,40mg/kg intravenous injection can be dwindled myocardial infarct size, wherein 10mg/kg group curative effect the best.2. " carthamin yellow " 10mg/kg intravenous injection can significantly increase the dog coronary flow, reduce myocardial consumption of oxygen, and wherein the effect of coronary blood flow increasing is better than compound injection of red sage root.3. " carthamin yellow " 10,20,40mg/kg intravenous injection can significantly reduce the rat ECG ST section that Pituitrin causes and raise degree and premature beat incidence and mortality ratio, and wherein 20mg/kg group curative effect is best and be better than compound injection of red sage root.After " carthamin yellow " 40mg/kg intravenous injection during 5min anesthetized rat systolic pressure and diastolic pressure be one and cross the property reduction, and heart rate, left ventricular systolic pressure, ± dp/dt max do not have obviously in 1 hour after administration and changes.5. shrink during 5min behind intravenous injection " carthamin yellow " 150mg/kg be pressed with one cross property decline and diastolic pressure after administration 5min, 15min, 30min, and 60min obvious decline is all arranged, being pressed in 5min, 15min after the administration, 30min in-dp/dt max and left ventricle shrink has obvious decline, and+dp/dt and heart rate do not have obvious change.
Case one
Huang, man, 44 years old, peasant.Married.
The patient goes to a doctor in outpatient service because of anti-" chest distress a year and a half " repeatedly.
When the patient worked in the other places before a year and a half, do not have obvious inducement and chest distress occurs, can not put down for sleeping in, companion's shortness of breath and fatigue, edema of pair of lower extremities, surplus in the of 20 went to a doctor the court afterwards in the sky, through looking into electrocardiogram(ECG etc., be diagnosed as " anterior myocardial infarction ", after the internal medicine diagnosis and treatment, can put down for sleeping in, do not have obviously breathe hard, weak, two lower limb pneumonedema, but paroxysmal chest distress repeatedly, more than daystart brush teeth, outbreak when washing one's face, or show effect when going up second floor, clivia, continue 10～12 minutes, show effect every day 1～3 time, contain pannonit or have a rest and to alleviate.
Look into Bp100/80mmHg, two lung yin, heart rate 72 times/minute, rule is neat, two lower limb pneumonedema, the ECG prompting: I, aVI are the qR type, and V2-5 is the qs type, V6 is the Qrs type, II, III, aVF are the rs type, and T ripple I, aVL, V3-6 are inverted, and STII, III, aVF, V6 move down 0.05mv, consider outmoded antetheca heart stalk, left front branch block.Blood, urine, just routine, liver, renal function, hemorheology etc. roughly in normal range.Tongue is dark, white and thin fur, thready and hesitant pulse.
Do not use the related drugs of treatment coronary heart disease and angina pectoris before testing.
Diagnosis: tcm diagnosis: the obstruction of qi in the chest, stagnation of heart-blood
Western medicine diagnose: coronary heart disease, stable fatigue stenocardia
Outmoded antetheca heart stalk
Medication: quiet carthamin yellow 100mg every day (2 bottles), continuous 14 days.
The therapeutic condition:
Medication is during 2 weeks, and attack times uncomfortable in chest is 6 times/week, contains 4 of pannonits altogether, and is surplus with the 1st week.
The medication curative effect: curative effect to treat angina pectoris is effectively, original stenocardia III level, and the treatment back is the II level.
ECG curative effect is effective.
Curative effect of disease is judged to be effectively.
Syndrome in TCM marquis's curative effect is effective.
Duration of test is not found untoward reaction.
Case two
Model, the woman, 59 years old, the cadre is married.
The patient goes to a doctor because of " precordialgia of showing effect repeatedly 1 year " outpatient service.
Patient's precordialgia of showing effect repeatedly over 1 year is shown effect during more than fatigue, as carries last the 3rd buildings of weight walking, last abrupt slope etc., continue 3～5 minutes, show effect weekly 2～4 times, continue 5～10 minutes, have a rest or contain pannonit and can alleviate, the time companion uncomfortable in chest, palpitaition, be interrupted Chinese medicine preparations such as taking Tongxinluo.
Look into Bp120/80mmHg, two lung yin, heart rate 60 times/minute, rule is neat, two lower limb pneumonedema, tongue is dark, white and thin fur, thready and hesitant pulse.Blood, urine, just routine, liver, renal function etc. roughly in normal range.Hemorheology whole blood viscosity 10.32, plasma viscosity 1.67 is higher than normally, and ECG:STI, aVL, V2-6 move down 0.05～0.075mv, and ventricular premature contraction takes place frequently.
Diagnosis: tcm diagnosis: the obstruction of qi in the chest, stagnation of heart-blood
Western medicine diagnose: coronary heart disease, stable fatigue stenocardia
Outmoded antetheca heart stalk
Medication: quiet carthamin yellow 100mg every day (2 bottles), continuous 14 days.
The treatment situation:
Activity endurance increases after 1 week of medication, carries weight walking non-evident sympton and occurs, and still has outbreak, this week to show effect 1 time but go up a slope, and precordialgia continues 4 minutes, does not contain the pannonit rest and extenuates, and does not have nervous chest door outbreak.
Medication is during 2 weeks, and situation is basic with the 1st week.
Treatment result is analyzed:
Security: do not have any untoward reaction.
Curative effect:
Curative effect to treat angina pectoris: for effectively, original stenocardia moderate, after treating for slight.
ECG curative effect: for effectively.
Curative effect of disease: for effectively.
Syndrome in TCM marquis's curative effect: for effectively.
The pannonit drug withdrawal.
Case three
Wang certain, the woman, 66 years old, married.
The patient goes to a doctor in outpatient service because of " precordialgia of showing effect repeatedly 40 months ".
Patient's precordialgia of showing effect repeatedly over 40 months, cause more than daily physical exertion, as normal trot 3～4 li of row under the daily condition, Shang Sanlou, on the angina that causes such as abrupt slope, continue 5～10 minutes, send out every day 1～3 time, contain pannonit or have a rest and to alleviate.
Look into Bp140/84mmHg, two lung yin, heart rate 72 times/minute, rule is neat, two lower limb pneumonedema, tongue is dark, white and thin fur, thready and hesitant pulse.Blood, urine, just routine, liver, renal function etc. roughly in normal range.The ECG prompting: STI, aVL, V2-6 move down 0.05～0.07mv.
Do not use the related drugs of treatment coronary heart disease and angina pectoris before testing.
Diagnosis: tcm diagnosis: the obstruction of qi in the chest, stagnation of heart-blood
Western medicine diagnose: coronary heart disease, stable fatigue stenocardia
Outmoded antetheca heart stalk
Medication: quiet carthamin yellow 100mg every day (2 bottles), continuous 14 days.
After 1 week of medication, activity endurance strengthens, and number of times uncomfortable in chest is reduced to 5 times uncomfortable in chest an of week, continues 6 minutes, does not contain pannonit sometimes, and rest can be alleviated.
After 2 weeks of medication, all transference cures recover normal.
Security: do not have any untoward reaction.
The medication curative effect: curative effect to treat angina pectoris is a produce effects, and original stenocardia is moderate, is normal after treating.
ECG curative effect is effective.
Curative effect of disease is judged to be produce effects.
Syndrome in TCM marquis's curative effect is a produce effects.
Case four
Chen, the woman is 61 years old, married.
The patient goes to a doctor because of " showing effect repeatedly 60 months uncomfortable in chest "
Patient's chest distress that shows effect over 60 months, as dailyly carrying weight Shang Sanlou, going up the abrupt slope, walking 3～4 li etc. cause that chest distress, every day show effect 1～3 time, 5～10 minutes time length, have a rest or contain pannonit and can alleviate.
Look into BP120/70mmHg,, two lung yin, heart rate 98 times/minute, rule is neat, and two lower limb pneumonedema tongues are dark, white and thin fur, thready and hesitant pulse.Blood, routine urinalysis, liver, renal function etc. are roughly in normal range, and the ECG prompting: STI, II, aVF, V6 move down 0.05mv.
Do not take treatment coronary heart disease, anginal related drugs before testing.
Diagnosis: tcm diagnosis: the obstruction of qi in the chest, stagnation of heart-blood
Western medicine diagnose: coronary heart disease, stable fatigue stenocardia
Outmoded antetheca heart stalk
Medication: continuous 14 days, quiet carthamin yellow 100mg every day (2 bottles)
After 1 week of medication: minimizing uncomfortable in chest 8 times weekly, does not contain pannonit and has a rest and can alleviate 3 minutes time length.
After 2 weeks of medication: number of times uncomfortable in chest is reduced to 2 times weekly, 1 minute time length, does not contain pannonit and has a rest and can alleviate.
Treatment result is analyzed:
Security: do not have any untoward reaction
Curative effect: curative effect to treat angina pectoris: for effectively.Original stenocardia II level is the I level after treating.
ECG curative effect: be produce effects
Curative effect of disease: for effectively
Tcm syndrome curative effect: for effectively
The pannonit drug withdrawal.
Case five
Xu so-and-so, the woman, 70 years old, married.
The patient goes to a doctor because of " show effect repeatedly precordial pain 24 months "
The patient over 24 months every day repeatedly show effect, influence the orthobiosis activity, each duration of seizure is longer, need repeatedly suck pannonit.Under normal operation often trot row 1～2 li, go up second floor and clivia etc. and promptly cause outbreak, show effect weekly 30 times, the time length, the pannonit consumption was 10 weekly more than 13 minutes.
Look into BP150/80mmHg, two lung yin, heart rate 80 times/minute, rule is neat, edema of pair of lower extremities, tongue is dark, white and thin fur, thready and hesitant pulse.Blood, urine, just conventional, liver, renal function etc. are roughly in normal range, and the ECG prompting is unusual.
Do not take treatment coronary heart disease, anginal related drugs before testing.
Diagnosis: tcm diagnosis: the obstruction of qi in the chest, stagnation of heart-blood
Western medicine diagnose: coronary heart disease, stable fatigue stenocardia
Outmoded antetheca heart stalk
Medication: continuous 14 days, quiet carthamin yellow 100mg every day (2 bottles)
Treatment result is analyzed:
Security: do not have any untoward reaction
Curative effect: curative effect to treat angina pectoris: be produce effects.Original stenocardia severe, the treatment back is slight.
ECG curative effect: be produce effects
Curative effect of disease: be produce effects
Tcm syndrome curative effect: be produce effects
The pannonit drug withdrawal.
Case six
Yang, the man is 61 years old, married.
The patient goes to a doctor because of " stenocardia was shown effect 96 months repeatedly "
Patient's stenocardia of showing effect over 96 months simultaneously with slightly uncomfortable in chest, causes more than lighter physical exertion, as 1～2 li of walking under the normal condition, last second floor and clivia etc., show effect weekly 9 times, about 13 minutes time length, need repeatedly suck pannonit could alleviate, the patient since every day angina pectoris attacks repeatedly, thereby influence activities of daily living (as defecating, wear the clothes etc.).
Look into BP150/86mmHg,, two lung yin, heart rate 70 times/minute, rule is neat, edema of pair of lower extremities, tongue is dark, white and thin fur, thready and hesitant pulse.Blood, urine, just conventional, liver, renal function, hemorheology etc. are roughly in normal range, and the ECG prompting is unusual.
Do not take treatment coronary heart disease, anginal related drugs before testing.
Diagnosis: tcm diagnosis: the obstruction of qi in the chest, stagnation of heart-blood
Western medicine diagnose: coronary heart disease, stable fatigue stenocardia
Outmoded antetheca heart stalk
Medication: continuous 14 days, quiet carthamin yellow 100mg every day (2 bottles)
After 2 weeks of medication: attack times is 4 times weekly, and 3 minutes time length, containing pannonit can alleviate.
Treatment result is analyzed:
Security: do not have any untoward reaction
Curative effect: curative effect to treat angina pectoris: for effectively.Original stenocardia severe is moderate after treating.
ECG curative effect: for effectively
Curative effect of disease: for effectively
Tcm syndrome curative effect: for effectively
The pannonit decrement.
Description of drawings
Fig. 1 is the high-efficient liquid phase chromatogram of the carthamin yellow of the embodiment of the invention 1 preparation.
Fig. 2 is the high-efficient liquid phase chromatogram of the carthamin yellow of the embodiment of the invention 2 preparations.
Fig. 3 is the high-efficient liquid phase chromatogram of the carthamin yellow of the embodiment of the invention 3 preparations.
Fig. 4 is the high-efficient liquid phase chromatogram of the carthamin yellow of the embodiment of the invention 4 preparations.
Fig. 5 is the high-efficient liquid phase chromatogram of the carthamin yellow of the embodiment of the invention 5 preparations.
Fig. 6 is a process flow sheet of the present invention.
Embodiment
Below, enumerate embodiment and illustrate in greater detail embodiments of the present invention, but the present invention is not limited to these embodiment.
The said safflower of the present invention is the dried floral of feverfew Carthamus tinctorius L., preferably uses its crude drug medicinal powder.
Carthamin yellow reference substance preparation method:
With carthamin yellow finished product Sephadex LH-20 column chromatography, last sample volume is 5% of a column volume, collects chromatographic solution with the test tube equal-volume, and each test tube high effective liquid chromatography for measuring merges with area normalization method purity greater than 99% part.
The method of high effective liquid chromatography for measuring carthamus tinctorius yellow color content:
Test condition: get the carthamin yellow reference substance, adding water makes every 1ml and contains 0.17mg solution approximately, with methyl alcohol-acetonitrile-water-phosphoric acid (32: 3: 64.5: 0.5) be moving phase, between 200～400nm wavelength, scan that the maximum absorption wavelength of carthamin yellow is 360nm.Determine that detecting wavelength is 360nm.
With octadecylsilane chemically bonded silica is weighting agent, and (32: 3: 64.5: 0.5), the detection wavelength was UV360nm to moving phase with methyl alcohol-acetonitrile-water-phosphoric acid.Take by weighing the about 25mg of this product, be dissolved in water, put in the 100ml measuring bottle, and be diluted with water to scale, as test liquid.Other takes by weighing the about 20mg of reference substance, puts in the 100ml measuring bottle and is diluted with water to scale, liquid in contrast.Measure test liquid, each 20 μ l of contrast liquid, inject liquid chromatograph respectively, separate between the record color atlas peak area, the retention time at carthamin yellow peak and other flavonoid compound peak.External standard method is calculated the content of trial-product.
Linear relationship and linearity range are investigated
Through The effects, carthamin yellow has good linear relationship in the concentration range of 1.59～6.36 μ g and between the peak area, and regression equation is y=-183.05+1449.84m, r=0.9996.
Get safflower crude drug medicinal powder, add 10 times of water, be heated to 100 ℃, be incubated 30 minutes, filter and cooling filtrate.Add 10 times of water in the filter residue, be heated to 100 ℃, be incubated 20 minutes, filter, cooling, merging filtrate left standstill 4 hours, and supernatant liquor is removed macromole impurity with ultra-filtration membrane after centrifugal, nonpolar macroporous adsorption resin D on the clear liquid
4020Post absorption, the deionized water wash-out is collected elutriant, and by membrane concentration, concentrated solution is through sieve chromatography, and applied sample amount is 6% of a chromatography column volume.The distilled water wash-out is collected elutriant and is concentrated, and the concentrated solution lyophilize gets carthamin yellow; Use high effective liquid chromatography for measuring, carthamus tinctorius yellow color content is 88.6%.See accompanying drawing 1.
Get safflower crude drug medicinal powder, add 10 times of water, be heated to 100 ℃, be incubated 30 minutes, filter and cooling filtrate.Add 10 times of water in the filter residue, be heated to 100 ℃, be incubated 20 minutes, filter, cooling, merging filtrate left standstill 4 hours, and supernatant liquor is removed macromole impurity with ultra-filtration membrane after centrifugal, nonpolar macroporous adsorption resin D on the clear liquid
4020Post absorption, the deionized water wash-out is collected elutriant, and by membrane concentration, concentrated solution is through sieve chromatography, and applied sample amount is 10% of a chromatography column volume.The distilled water wash-out is collected elutriant and is concentrated, and Sephadex LH-20 column chromatography on the concentrated solution is collected elutriant, and lyophilize gets carthamin yellow; Use high effective liquid chromatography for measuring, carthamus tinctorius yellow color content is 99.6%.See accompanying drawing 2.
Get safflower crude drug medicinal powder, add 10 times of water, be heated to 90 ℃, be incubated 40 minutes, filter and cooling filtrate.Add 8 times of water in the filter residue, be heated to 90 ℃, be incubated 20 minutes, filter, cooling.In filter residue, add 8 times of water again, be heated to 90 ℃, be incubated 20 minutes, filter, cooling, merging filtrate left standstill 2 hours, and supernatant liquor is removed macromole impurity with ultra-filtration membrane after centrifugal, nonpolar macroporous adsorption resin D on the clear liquid
4020Absorption, the deionized water wash-out is collected elutriant, and by membrane concentration, concentrated solution is through sieve chromatography, and applied sample amount is 12% of a chromatography column volume.Use the distilled water wash-out, collect elutriant, lyophilize gets carthamin yellow; Use high effective liquid chromatography for measuring, carthamus tinctorius yellow color content is 86.1%.See accompanying drawing 3.
Get safflower crude drug medicinal powder, add 10 times of water, be heated to 60 ℃, be incubated 2 hours, filter and cooling filtrate.Add 10 times of water in the filter residue, be heated to 60 ℃, be incubated 2 hours, filter, cooling adds 10 times of water again in filter residue, be heated to 60 ℃, be incubated 2 hours, filter, cooling, merging filtrate left standstill 3 hours, and supernatant liquor is removed macromole impurity with ultra-filtration membrane after centrifugal, nonpolar macroporous adsorption resin B201 absorption on the clear liquid, the deionized water wash-out is collected elutriant, by membrane concentration, concentrated solution is through sieve chromatography, and applied sample amount is 10% of a chromatography column volume.Use the distilled water wash-out, collect elutriant, lyophilize gets carthamin yellow; Use high effective liquid chromatography for measuring, carthamus tinctorius yellow color content is 76.7%.See accompanying drawing 4.
Get safflower crude drug medicinal powder, add 15 times of water, be heated to 80 ℃, be incubated 2 hours, filter and cooling filtrate.Add 10 times of water in the filter residue, be heated to 80 ℃, be incubated 2 hours, filter, cooling, merging filtrate left standstill 2 hours, and supernatant liquor is removed macromole impurity with ultra-filtration membrane after centrifugal, nonpolar macroporous adsorption resin AB-8 absorption on the clear liquid, the deionized water wash-out is collected elutriant, passes through membrane concentration, concentrated solution is through sieve chromatography, and applied sample amount is 15% of a chromatography column volume.Use the distilled water wash-out, collect elutriant, lyophilize gets carthamin yellow; Use high effective liquid chromatography for measuring, carthamus tinctorius yellow color content is 70%.See accompanying drawing 5.
Example of formulations 1 safflower uranidin injection liquid
Carthamin yellow 50 grams
Water for injection is an amount of
1000 milliliters of total amounts
Get 50 gram carthamin yellows and add to 1000 milliliters after with the dissolving of an amount of water for injection, according to a conventional method through can, seal, step such as sterilization makes carthamus tinctorius yellow colour injection.
Example of formulations 2 injection carthamin yellow freeze-dried powders
Carthamin yellow 50 grams
Water for injection is an amount of
1000 milliliters of total amounts
Get 50 gram carthamin yellows and add to 1000 milliliters after with the dissolving of an amount of water for injection, according to a conventional method through can, freeze-drying, step such as seal and make the carthamin yellow powder injection.
Example of formulations 3 carthamin yellow oral hard capsule agent
Carthamin yellow 100 grams
Dry starch 100 grams
Lactose 50 grams
Cross 80 eye mesh screens after said components is mixed respectively, mix, 70% ethanolic soln of the polyvinylpyrrolidone with an amount of 1.5% is made 20～30 order particles, 50 ℃ of dryings, and the whole grain of 20 orders, filled capsules is promptly.
Example of formulations 4 anthoxanthin tablets
Carthamin yellow 100 grams
Microcrystalline Cellulose 200 grams
Lactose 150 grams
Magnesium Stearate 1.5 grams
Make 1000
Carthamin yellow, Microcrystalline Cellulose, lactose, 1/2 sodium starch glycolate are crossed 80 mesh sieves respectively, mix, 70% ethanolic soln of the polyvinylpyrrolidone with an amount of 3% is made 20 order particles, 50 ℃ of dryings, the whole grain of 18 orders, the Magnesium Stearate, other 1/2 sodium starch glycolate of mistake 80 purposes that added 120 mesh sieves mix, and compressing tablet, dressing are promptly.
In addition, in not running counter to spirit of the present invention, can carry out various changes and modifications to given embodiment.Selectable embodiment by in the art technician recognizes is also included within the claim scope of the present invention.
Claims (11)
1. carthamin yellow is 70～99.6% with the content of high effective liquid chromatography for measuring, and this carthamin yellow can prepare with following method:
(1) with the safflower be raw material, add an amount of temperature and be 50～100 ℃ polar solvent extracting, the filtering dregs of a decoction are cooled to 5～30 ℃ with extracting solution, leave standstill 2～24 hours;
(2) extracting solution that above-mentioned steps is obtained through centrifugal remove insoluble impurities, ultrafiltration and remove macromole impurity after, by macroporous resin adsorption, and be elutriant wash-out carthamin yellow with the polar solvent, collecting elutriant is carthamin yellow crude product elutriant;
(3) the carthamin yellow crude product elutriant that above-mentioned steps is obtained concentrates, and concentrated solution separates with molecular sieve column, is elutriant wash-out carthamin yellow with the polar solvent, collects elutriant, through concentrated, dry, gets the carthamin yellow finished product.
2. the preparation method of a carthamin yellow is characterized in that comprising the steps:
(1) with the safflower be raw material, add an amount of temperature and be 50～100 ℃ polar solvent extracting, the filtering dregs of a decoction are cooled to 5～30 ℃ with extracting solution, leave standstill 2～24 hours;
(2) extracting solution that above-mentioned steps is obtained through centrifugal remove insoluble impurities, ultrafiltration and remove macromole impurity after, by macroporous resin adsorption, and be elutriant wash-out carthamin yellow with the polar solvent, collecting elutriant is carthamin yellow crude product elutriant;
(3) the carthamin yellow crude product elutriant that above-mentioned steps is obtained concentrates, and concentrated solution separates with molecular sieve column, is elutriant wash-out carthamin yellow with the polar solvent, collects elutriant, through concentrated, dry, gets the carthamin yellow finished product.
3. the preparation method of carthamin yellow as claimed in claim 2, it is characterized in that: the described extracting in the step (1) is with polar solvent extracting 2～3 times, each 0.5～24 hour, extracting was 10～30 times of safflower crude drug weight with the polar solvent amount.
4. as the preparation method of claim 2 or 3 described carthamin yellows, it is characterized in that: the described polar solvent in the step (1) is selected from water or ethanol, methyl alcohol, propyl alcohol and isopropanol water solution.
5. the preparation method of carthamin yellow as claimed in claim 2 is characterized in that: the described macroporous resin in the step (2) is with centrifugal what remove that insoluble impurities, ultrafiltration remove Flos Carthami extract behind the macromole impurity is 1: 2～5 than by volume.
6. the preparation method of carthamin yellow as claimed in claim 2, it is characterized in that: the spissated method that is used in the step (3) is a membrane concentration.
7. the preparation method of carthamin yellow as claimed in claim 2, it is characterized in that: the described molecular sieve consumption in the step (3) is 1: 0.05～0.15 than by volume with carthamin yellow crude product concentrated solution.
8. the preparation method of carthamin yellow as claimed in claim 2, it is characterized in that: the described polarity elutriant in step (2) and the step (3) is selected from water or ethanol, methyl alcohol, propyl alcohol and isopropanol water solution respectively.
9. medicine and healthcare products for the treatment of cardiovascular and cerebrovascular diseases is characterized in that: the described carthamin yellow of claim 1 and the pharmaceutically useful carrier that contain treatment or prevention cardiovascular and cerebrovascular diseases significant quantity.
10. medicine as claimed in claim 9 and healthcare products is characterized in that: can be made into oral preparations, injection formulations.
11. the medicine of the described carthamin yellow of claim 1 damage disease due to preparation prevention and treatment relate to myocardial ischemia and cerebral ischemia, thrombosis and the application in the healthcare products.
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| CNB031574793A CN1300161C (en) | 2003-09-22 | 2003-09-22 | Yellow pigment of safflower preparation method and application |
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| CN1300161C CN1300161C (en) | 2007-02-14 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774989B (en) * | 2009-02-04 | 2011-07-27 | 王来忠 | Method for extracting refined yellow pigment from red flowers |
| CN102382151A (en) * | 2011-09-08 | 2012-03-21 | 成都中医药大学 | Separation and purification method for safflower yellow |
| CN102702150A (en) * | 2012-06-19 | 2012-10-03 | 浙江永宁药业股份有限公司 | Preparation method and application of hydroxysafflor yellow A |
| CN104559302A (en) * | 2014-12-03 | 2015-04-29 | 雅安三九药业有限公司 | Method for extracting and refining carthamin yellow |
| CN108593794A (en) * | 2018-04-25 | 2018-09-28 | 陕西步长制药有限公司 | Active constituent content method in a kind of multi-target ingredient UPLC detection safflower |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5750379A (en) * | 1989-03-18 | 1998-05-12 | Toyo Ink Manufacturing Co., Ltd. | Process for the production of carthamin |
| CN1085674C (en) * | 1998-11-24 | 2002-05-29 | 北京市心肺血管疾病研究所 | Safflower total uranidin, its preparation and application |
| CN1205216C (en) * | 2000-10-30 | 2005-06-08 | 长春三真实业有限公司 | Safflower lyochrome rich in carthamin A, its preparing process, its preparation and its medical usage |
-
2003
- 2003-09-22 CN CNB031574793A patent/CN1300161C/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774989B (en) * | 2009-02-04 | 2011-07-27 | 王来忠 | Method for extracting refined yellow pigment from red flowers |
| CN102382151A (en) * | 2011-09-08 | 2012-03-21 | 成都中医药大学 | Separation and purification method for safflower yellow |
| CN102702150A (en) * | 2012-06-19 | 2012-10-03 | 浙江永宁药业股份有限公司 | Preparation method and application of hydroxysafflor yellow A |
| CN102702150B (en) * | 2012-06-19 | 2014-09-17 | 浙江永宁药业股份有限公司 | Preparation method and application of hydroxysafflor yellow A |
| CN104559302A (en) * | 2014-12-03 | 2015-04-29 | 雅安三九药业有限公司 | Method for extracting and refining carthamin yellow |
| CN108593794A (en) * | 2018-04-25 | 2018-09-28 | 陕西步长制药有限公司 | Active constituent content method in a kind of multi-target ingredient UPLC detection safflower |
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| Publication number | Publication date |
|---|---|
| CN1300161C (en) | 2007-02-14 |
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Denomination of invention: Safflower yellow pigment and its preparation method and Application Effective date of registration: 20210914 Granted publication date: 20070214 Pledgee: Industrial Commercial Bank of China Ltd. Taizhou Huangyan branch Pledgor: ZHEJIANG YONGNING PHARMACEUTICAL Co.,Ltd. Registration number: Y2021330001585 |
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